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Hochschule Karlsruhe Technik und Wirtschaft
Fakultt fr Maschinenbau

Study of different surface substrates for an ice slurry generator
development.

{Master Thesis Nr.: 11/14}

von
Daniel De La Cuesta De Cal
geb. am 01.09.1987
in A Corua (Spanien)
Matr. Nr. 35297

Betreuer an der Hochschule Karlsruhe:

Prof. Dr.-Ing. Michael Kauffeld
Dipl.-Ing. (FH) Susanne Frank

Karlsruhe, Oktober 2010 - Mrz 2011.
I
E r k l r u n g

Ich versichere hiermit wahrheitsgem, die Diplomarbeit bis auf die dem
Betreuungsdozenten bereits bekannte Hilfe selbstndig angefertigt, alle benutzten Hilfsmittel
vollstndig und genau angegeben und alles kenntlich gemacht zu haben, was aus Arbeiten
anderer unverndert oder mit Abnderungen entnommen wurde.

Karlsruhe, den 28.03.2011,

Unterschrift

S p e r r v e r m e r k

Diese Arbeit enthlt vertrauliche, geheime Informationen. Die darin enthaltenen
Unterlagen und Ausarbeitungen sind streng vertraulich zu behandeln und drfen Dritten nicht
zugnglich gemacht werden und weder direkt noch indirekt verwendet werden. Es drfen
weder Abschriften noch Kopien auch nicht digital angefertigt werden. Verffentlichungen
bedrfen der schriftlichen Genehmigung der Institut fr Klte-, Klima- und Umwelttechnik
(Hochschule Karlsruhe Technik und Wirtschaft).

II
D a n k s a g u n g.
I would like to thank my two advisors, Prof.Dr.-Ing. Michael Kauffeld and
Dipl.-Ing. (FH) Susanne Frank for the opportunity offered and the help given at any moment
during the stat. Especially I want to thank not only my advisors but all IKKU co-workers for
the patience shown in everyday language problems.
As well, assitance offered by Agnes Marciniak in experiments made and the possibility
of going to FZK is also thankworthy. In FZK, Immanuel Schufele offered his help and
advices always in an obliging way. Workers in the IMP workshop collaborated in the develop
of the work too.
Finally, I want to thank my family and girlfriend for having helped me whenever the
distance was not an obstacle.

III
Content:

Formula symbols and abbreviations. ......................................................................................... V
Figure index. .......................................................................................................................... VIII
Tables and graphs index. .......................................................................................................... IX
Abstract. .................................................................................................................................... XI
1 Tasks ..................................................................................................................................... 1
2 Introduction. ......................................................................................................................... 2
2.1 Ice slurry: background information. ............................................................................... 2
2.2 Ice slurry technology. ..................................................................................................... 3
2.3 Modern ice slurry technologies. ..................................................................................... 4
2.4 Focus on IKKU. .............................................................................................................. 4
2.5 Daily problems in the test rig. ........................................................................................ 6
3 Ice adhesion. ......................................................................................................................... 8
3.1 Crystallisation. ................................................................................................................ 8
3.2 Ice adhesion: background information. .......................................................................... 9
3.3 Parameters affecting ice adhesion. ............................................................................... 10
3.3.1 Surface energy. ...................................................................................................... 10
3.3.2 Contact angle and wettability. ............................................................................... 11
3.3.3 Hydrophobicity. ..................................................................................................... 12
3.3.4 Surface roughness. ................................................................................................. 13
3.3.5 Polarity. .................................................................................................................. 14
3.3.6 Other parameters. ................................................................................................... 15
4 Surfaces: materials and coatings......................................................................................... 18
4.1 Non-coated copper plates. ............................................................................................ 18
4.1.1 Procedure. .............................................................................................................. 19
4.1.2 Oxide layer............................................................................................................. 20
4.1.3 Roughness. ............................................................................................................. 20
4.1.4 Conclusions ........................................................................................................... 21
4.2 Coated plates. ............................................................................................................... 22
4.2.1 Plastic coatings. ..................................................................................................... 22
4.2.2 Metallic coatings. ................................................................................................... 24
4.2.3 Organometallic coatings. ....................................................................................... 25
4.2.4 Tin/zinc coating. .................................................................................................... 30

IV
4.2.5 Other coatings. ....................................................................................................... 31
4.3 Summary. ...................................................................................................................... 32
5 Experimental procedures. ................................................................................................... 34
5.1 Contact angle measurements. ....................................................................................... 34
5.2 Surface free energy. ...................................................................................................... 37
6 Results and discussion. ....................................................................................................... 42
6.1 Discussion on ethanol concentration. ........................................................................... 43
6.2 Discussion on the effect of oxide layer. ....................................................................... 46
6.3 Discussion on the effect of surface roughness. ............................................................ 47
6.4 Surface energy results. .................................................................................................. 51
6.5 Polarity results. ............................................................................................................. 54
6.6 Supercooling degree. .................................................................................................... 55
7 Conclusions. ....................................................................................................................... 56
8 Bibliography ....................................................................................................................... 59
9 Appendixes ......................................................................................................................... 62
9.1 Appendix A: Refractometer.......................................................................................... 62
9.2 Appendix B: Redesigning of the heat exchanger. ........................................................ 71
9.3 Appendix C and D: Datasheets and catalogs.............76

V
Formula symbols and abbreviations.
Lateinische Formelzeichen
Symbol

Unit (S.I.) Description
A m
2
Area.
b - y-intercept.
f - Area fraction.
l m Length.
L J/kg Latent heat.
m - Slope.
M g/mol Molar mass.
m/m - Mass concentration.
n - Refractive index.
P - Grit size parameter
r - Wenzels roughness ratio of areas.
R m Surface roughness parameter.
T K Temperature.
v/v - Volume concentration.
W J/kg Work.
x - Independent variable.
y - Dependent variable.
Z m Vertical deviation from the center line.
G J/kg Gibbs free energy.
T K Supercooling degree

Griechische Formelzeichen
mN/m Surface tension.

- Variation.

- Number of moles.
Contact angle.

- Hydrophilicity number.
Pa s Viscosity.
mN/m Surface energy.
- Fraction.

VI
Subscripts
0 - Nominal.
1 - Media 1.
2 - Media 2.
3 - Media 3.
a - Average value.
ad - Adhesion.
aq - Aqueous.
bin - Binary.
c - Cohesion.
c - Calculated.
f - Fusion.
i - Counter 1.
ifp - Initial freezing point.
j - Counter 2.
l - Liquid phase.
m - Evaluation.
m - Measured.
mix - Mixture.
n - Nucleation.
r - Sampling.
s - Solid phase.
t - Total.
ter - Ternary.
z - Maximum.

Superscripts
* - Critical.
- Includes roughness.
D - Dispersive component.
E - Excess.
I - Ideal.
P - Polar component.
R - Real.

VII
Abbreviations
DSC Differential Scanning Calorimetry.
FZK Forschungzentrum Karlsruhe.
HR Hand refractometer
HsKA Hochschule Karlsruhe.
HTF Heat transfer fluid.
HX Heat exchanger.
IKKU Institut fr Kalte-, Klima- und Umwelttechnik.
IMP Institute of Materials and Processes (HsKA).
IS Ice slurry.
i.e. id est, latin form for that is.
MEK Methyl ethyl ketone.
MT Measuring template.
SD Standard angle.

VIII
Figure index.
Figure 1. Experimental ice slurry test rig [ 2 ]............................................................................ 4
Figure 2 Experimental setup of Project 3E at IKKU (HsKA). ................................................... 5
Figure 3 Cross section of the heat exchanger [ 2 ]. .................................................................... 5
Figure 4 Heat exchanger redesigned .......................................................................................... 6
Figure 5 Insulation over pipes. ................................................................................................... 7
Figure 6 Cassie-Baxter model [ 42 ]. ........................................................................................ 13
Figure 7 Wenzel model [ 42 ]. .................................................................................................. 13
Figure 8 Different orientation of water molecules [ 19 ]. ......................................................... 15
Figure 9 R
a
graphical description from Hommel-etamic catalog ............................................. 20
Figure 10 ProbeA shows great adhesion and homogeneity. ..................................................... 23
Figure 11 Copper plates after the silver mirror experiment ..................................................... 24
Figure 12 Probe1. ..................................................................................................................... 27
Figure 13 Probe3. ..................................................................................................................... 27
Figure 14 Probe2. ..................................................................................................................... 27
Figure 15 Metal film, glass powder and substrate [ 12 ]. ......................................................... 27
Figure 16 Probe1A, 2A and 3A. ............................................................................................... 29
Figure 17 Contact angle measurement equipment. .................................................................. 35
Figure 18 Disposition for a contact angle measurement. ......................................................... 36
Figure 21 Plate R08 after oxidising. ......................................................................................... 47
Figure 23 Current sealing between copper test plate and polycarbonate cover
(aluminium strenghtened) ............................................................................. 71
Figure 24 Heat exchanger CATIA 3D model ........................................................................... 72
Figure 25 Fluid inlet view (detail). ........................................................................................... 72
Figure 26 First scheme of the heat exchanger. ......................................................................... 74
Figure 27 Main dimensions in O-ring installations [Trelleborg catalog]. ................................ 74
Figure 28 Fitting by Swagelok. ................................................................................................ 75

IX
Tables index.
Table 1 Different thermal conductivity coefficientes [ 5 ]. ...................................................... 18
Table 2 Roughness measurements of copper non-coated plates. ............................................. 21
Table 3 Roughness measurements of plastic coatings.............................................................. 23
Table 4 Properties of both references considered as suitable for the experiment. ................... 28
Table 5 Roughness measurements comparing REF, Probe2A and Probe 2B. ......................... 30
Table 6 Codenames of all plates involved in further experiments. .......................................... 33
Table 7 Compilation of contact angle measurements. .............................................................. 43
Table 8 Compilation of surface energy values. ........................................................................ 52
Table 9 Surface energy values from lowest to highest. ............................................................ 53
Table 10 Supercooling degree calculated according to Faucheux. .......................................... 55
Table 11 Volume to mass concentration change of ethanol 70 % by Carl Roth. ..................... 65
Table 12 Volume to mass concentration change of ethanol 99 % by Scharr. .......................... 65
Table 13 Samples prepared with ethanol 70 % solution by Carl Roth. .................................... 66
Table 14 Samples prepared with ethanol 99 % by Scharr. ....................................................... 66
Table 15 Densities at several ethanol mass concentrations at 20 C [ 41 ]. ............................. 67
Table 16 Experimental results with ethanol 70 % solution by Carl Roth. ............................... 67
Table 17 Experimental results with ethanol 99 % solution by Scharr...................................... 68
Table 18 Analysis of the results with ethanol 70 % by Carl Roth ........................................... 69
Table 19 Analysis of the results with ethanol 99 % by Scharr. ................................................ 70

X
Graphs index.
Graph 1 Heat treating 1: temperature (C) vs. time (minutes). ................................................. 26
Graph 2 Ideal and real heat treating for the glass powder 8465. .............................................. 28
Graph 3 Ideal and real treating for the glass powder G017-393. ............................................. 29
Graph 4 Linear regression to calculate dispersive surface energy component [ 30 ]. .............. 38
Graph 5 Linear regression to calculate polar surface energy component [ 30 ]. ...................... 39
Graph 6 Linear regression for the OWRK SE determination method [ 30 ]. ........................... 40
Graph 7 Contact angle measurements of ProbeA plate with ethanol 12 %. ............................. 42
Graph 8 Contact angle versus ethanol concentration for silicone coatings. ............................. 44
Graph 9 Contact angle versus ethanol concentration for resinates coating
(plate 2A). ..................................................................................................... 44
Graph 10 Series of graphs where contact angle is represented against ethanol
concentration. ............................................................................................... 45
Graph 11 Series of graphs where contact angle is represented against surface
roughness for both oriented and non oriented copper plates. ....................... 49
Graph 12 Contact angle vs surface roughness for every oriented plates measuring
conditions...................................................................................................... 50
Graph 13 Contact angle vs surface roughness for every non-oriented plates
measuring conditions. ................................................................................... 51
Graph 14 Study of the influence of surface roughness of oriented and non-oriented
copper plates on surface energy determined by measurements of
the contact angle. .......................................................................................... 53
Graph 15 Polarity vs surface roughness for oriented and non-oriented copper
plates. ............................................................................................................ 54
Graph 16 Contact angle measurements compared with polarity for every surface
studied. .......................................................................................................... 54
Graph 17 Relationship between real ethanol concentration and measured ethanol
concentration done with ethanol 70 % by Carl Roth. ................................... 68
Graph 18 Relationship between real ethanol concentration and measured ethanol
concentration done with ethanol 99 % by Scharr. ........................................ 69
Abstract.
XI
Abstract.
The main objective of 3E doctoral thesis by Dipl.-Ing. (FH) Susanne Frank is finding a
combination of parameters which can lead to the development of an ice slurry (IS) generator
based on non moving parts, improving current technology and helping in its expansion in a
wider range of industrial applications. Part of this thesis is the study of the surfaces which act
as an interface between the refrigerant and the IS circuit. This study is necessary because of
its relevance in IS formation, as the heat exchanger where both circuits get in touch also
works as an IS generator.
In order to achieve the experimental requirements for these surfaces to be tested in
prototype-like conditions, additional help in the IS setup development was needed. Leakage
problems, as well as difficult mounting of the test rig, made necessary the redesign of the heat
exchanger. As well, insulating tasks and analysis of a refractometer were dealt with and some
additional improvements for the test rig were proposed.
Nevertheless, main task for this project is analysing different coatings and surface
finishings to achieve certain conditions that would lead to a situation in which ice adhesion is
as low as possible. Therefore, first task of the project was the experimental development
needed to modify each surface of different copper samples. Surface roughness and plastic,
metallic and organometallic coatings were the surface modifications selected and both
experimental development and results obtained are described during this project.
So as to predict which of the surfaces shows better conditions to present low ice
adhesion, a literature survey was done and both crystallisation and parameters involved in
adhesion between two materials are here presented under the point of view of several authors.
Finally, a study of some of these parameters involved in ice adhesion was developed,
trying to find experimental conclusions which lead to a conclusion of which plates of the
considered ones show better conditions for the IS generator. Some of the results obtained
were not conclusive, that leads to further experiments in this prediction or a different
approach to it.

Tasks
Page 1
1 Tasks

The tasks offered to write this master thesis about are the following ones:

- Helping in the development of an ice slurry generator without moving parts which can
avoid usual problems with blocking and excess in investment and operational costs.
- Designing and mounting of a research ice slurry test rig in where the ice slurry
generator operation can be checked.
- Study of the different parameters that can take effect over the operation of the ice
slurry generator, especially related to the heat exchange surface.
- Modification of standard surfaces in order to achieve better properties for the
requirements considered.
- Determination of the aptitude of each surface for the heat exchanger by the
measurement of contact angle and the evaluation of the surface free energy.

The main task of this Master Thesis is finding a range of surfaces which fulfill
theoretical requirements and could be tested in real working conditions.
Introduction.
Page 2
2 Introduction.

In the latest years, concern in enviromental matters grows continuously affecting us all
and, of course, making its impact at industry. Different conventions and agreements among
specialists have changed the methodologies and materials involved in traditional laboratory
and industrial procedures.
Research on new ways and materials suitable for the current requirements becomes
necessary since most of the components employed are now prohibited due to the possibility of
causing enviromental damage. Nowadays, fluids employed as substitutes of the forbidden
ones are not much better at this point. Thus, research on enviromental friendly and energy
saving fluids for using in refrigeration is one of the fields in which more effort is being made
in universities and research centres, but there is still a long way to go.
Concerning this aspect, further work in new and different heat transfer fluids (HTFs
from now on) is nowadays more and more important. Water, the more abundant and harmless
liquid on Earth, is often used as a second fluid in refrigeration cycles, but its limitations avoid
a wide range of applications.
Many possibilities have been proposed in these years in order to solve this problem,
but the usage of phase changing refrigerants is the one this project is studying, ice slurry in
particular.
2.1 Ice slurry: background information.
As defined by most of the references considered, ice slurry is a phase changing fluid,
mixture of small ice particles, 0,1 to 1 mm in diameter, and a carrier fluid, consisting of water
and a freezing point depressant (usually alcohols, salt or sugar) [ 1 ].
The main advantage in using ice slurry is its heat transfer capacity eight times higher
than a traditional single-phase secondary refrigerant for similar flow rates due to latent heat
stored [ 1 ]. Consequently, investment costs in equipment are reduced instantly because the
piping system needed decrease its size. Operational costs are reduced as well, due to the lower
mass flow of HTF necessary to transport the same heat, resulting in lower pumping work and
energy saving. On the other hand, current ice slurry platforms are expensive, inefficient and
non completely reliable, since they include moving parts and require a redundant ice slurry
generator for solving forced stops in IS production caused by blockings or mechanical failures
in the main generator.
In consequence, the ice slurry generator remains as one of the critical components in
an ice slurry system, regarding mainly to its reliability and the cost of redundant equipment.
Thus, developing an ice slurry generator that enhance both parameters is one of the tasks that
can improve its competitiveness in industrial markets.
Usually, an ice slurry generator is a heat exchanger that close the loop of the ice slurry
circuit and acts as a joint between primary and secondary refrigerant circuit. Aim of the IS
Introduction.
Page 3
generator is regenerating the ice particles that have melted during the operational zone of the
circuit or produce new ones when the generator is starting.

2.2 Ice slurry technology.
As it has been said, IS allows refrigeration systems to reduce operative section of tubes
and pipes by about 50 % as well as flow velocity inside these tubes and pipes. Energy saving
and heat transfer capacity are raised considerably with the IS technology introduction, but a
complete study in its possibilities is required.
IS technology present a wide range of operational methods, therefore its industrial
application also can find a way into many fields. Despite the description already made may
create the sensation of being a new choice, IS has been applied in some areas but great
importance was given by current environmental friendly requisites.
Controlling the way in which ice particles are produced requires the knowledge of
crystallisation mechanism, which involves nucleation and crystal growth. Both processes have
its importance in ice slurry systems. Ice nucleation occurs via metastable states, in particular
from supercooled metastable water to completely stable ice nuclei, where supercooling (SC)
means to remain below the corresponding freezing point in liquid state. Depending on the
starting source (internal or external) of the process, the nucleation would be homogeneus or
heterogeneus, respectively. When some of the nuclei formed reach the critical radius, crystal
growth occurs, being the phenomenon that controls the final ice particle size in the mixture.
In particular, ice nucleation is the key issue in IS generation and a phenomenon worthy
of further study in order to a better comprehension on the matter. Nowadays, IS generators
classifying depends on the nucleation method.
Those based on heterogeneus nucleation include scraped-surface IS generators ice is
formed over a surface and it is removed by mechanical scrapers, wipers or turbulators, first
prototypes date from 1976 , hydroscraped-surface IS generators scraping is caused by
volume flow, high concentration of freezing point depressant is needed which leads lower
temperatures and more operational limitations or fluidized bed heat exchangers which
avoid ice adhesion by the presence of solid components carried by the main flow.
On the other hand, those based on homogeneus nucleation include vacuum ice method
the biggest and most efficient generator, detracts heat from the sublimation of refrigerant
water obtained by pressure reduction , direct contact generators based in inmiscibility of
the liquids involved, introduces directly the refrigerant among the ice slurry, causing the
cooling and little contamination of the HTF, direct contact generators can also work with
heterogeneus nucleation and generators based on supercooling which is released by
methods like ultrasonic vibrations or mechanical shock, avoiding possible disturbances that
can lead to the crystallisation being out of control [ 1 ] [ 2 ].

Introduction.
Page 4
As well, these methods of IS generation allow the IS technology to be nowadays present
in industry, but not as widespread as desired. Some examples quoted by [ 1 ] are mentioned
below to show the variety of possible real applications: air and yeast cooling in a brewery,
cooled food storage in great kitchens or as a coolant in trucks and other means of transport.
2.3 Modern ice slurry technologies.
Research lines in IS technology are boosted by present concern about environment and
energy saving. The main interest lies on the adaptation of current knowledge in the field to
industrial applications.
Besides, further research on basic physical properties of the phase-changing materials is
also needed to continue the improvement of designs and technology. Additives which can
allow current systems to work in lower temperatures without contamination of the products
involved, efficiency optimisation, improvement of hydraulic systems, study of ice storage and
stratification are some of the main issues in which there is still a lot of work to do [ 1 ].
2.4 Focus on IKKU.
This project about STUDY OF DIFFERENT SURFACE SUBSTRATES FOR AN ICE SLURRY
GENERATOR DEVELOPMENT has been carried out in the Hochschule Karlsruhe, at the Institut
fr Kalte-, Klima- und Umwelttechnik (IKKU) in the Mechanical Engineering Faculty. In
particular, under the Ph.D. thesis on the topic of ice slurry generation processes by
Dipl.-Ing. (FH) Susanne Frank, who is one of the supervisors together with
Prof. Dr.-Ing. habil. Michael Kauffeld.
Aim of this thesis is to develop completely an IS generator in which moving parts are
not included, avoiding the
abovementioned problems and extra
costs. An experimental assembly of
such IS generator was built to show
that there is a combination of
flowing conditions, additive
concentration, ice content of the
HTF, heat exchanger surface and
surface temperature of the heat
exchanger that the crystal growth
occurs directly in the HTF [ 2 ].

Figure 1. Experimental ice slurry
test rig [ 2 ].
Introduction.
Page 5
This experimental assembly consists of two refrigerant circuits. The primary circuit is
filled with R134a and cooled down by two thermostatic baths through an isobaric process and
secondary is filled with an ethanol-water mixture of varying concentrations. Both circuits are
connected with a heat exchanger where ice slurry is produced, the so called test section. Initial
IS can be provided by an additional slush ice machine. In Figure 2 a view of the complete test
rig is shown, where main components can be seen: both Julabo thermostatic baths, Agilent
data acquisition unit, slush machine, test section, heaters, mass flow meters, pumps and
transport pipes.

Figure 2 Experimental setup of Project 3E at IKKU (HsKA).

Aim of the project lies on the heat exchanger and its working conditions at any time, so
ten equispaced PT1000 resistive temperature sensors were placed in between the primary
circuit and the second circuit area as
shown in Figure 3 in order to
calculate the heat flow between both
circuits from the temperature
gradient measured. Besides, mass
flow meters are placed in the
secondary circuit in order to measure
mass flow and density of the mixture
and to evaluate ice content basing in
Figure 3 Cross section of the heat exchanger [ 2 ].
Data acquisition system
Heaters
Slush machine
Thermostatic baths
Pumps
Test section (HX)
Introduction.
Page 6
the data measured. The plate between the HTF and the PT1000 is called measuring plate and
is the one whose surface is the main goal of study along this project. Dimension of the
measuring plate is 1000 mm x 40 mm.
2.5 Daily problems in the test rig.
As in every laboratory experimental rig, problems arise continuously and some of them
affect hugely to equipment running and the experimental results achieved. One of the
objectives of this project is helping in the development of the previously described test rig,
main aspects where this help was done will be mentioned from now on.
First of all, a redesign of the heat exchanger was required. The current HX has leaks in
some points and its design does not allow an easy change of the test plate (measuring plate).
The new design should fulfill these requirements and is presented in Figure 4.

Figure 4 Heat exchanger redesigned
Main aspects of this redesign are:
Guidance and easier fixing of the test plate.
Removal of the silicone and glue which avoided fast test plate changes.
Merging of polycarbonate cover and polycarbonate inlet/outlet.
Inclusion of a Swagelock fitting between inlet and piping system.
New O-ring sealing between test plate and polycarbonate cover.
New flat sealing between test plate and polycarbonate inlet.

Further explanations of the development of this redesign are available in the report
attached in page 71, Appendix B: Redesigning of the heat exchanger.
Relating with this redesign, some addtional changes in the platform were proposed.
Including a stirrer in the slush machine where IS is generated would suppose this ice
slurry not to block so easile when ice concentration is too high. Several brands and
Introduction.
Page 7
possibilities were found and contact was made with different companies but no result at this
point was achieved, because of high costs, no suitability or no answer received. A topic of a
future work could be finding this stirrer, determining the suitable power and rotatory speed
acording to available prices and models and placing it in the machine, either horizontal or
vertical.
Besides, in order to place the stirrer, a cover for the slush machine was thought. The
main reason is the protection of the ice generated, since this ice will be inside of the piping
system and dirt could cause blockings. As
no stirrer was acquired, the cover was
dismissed.
Another point where help was
needed was insulating of the platform. A
complete insulation task were developed
(Figure 5) and no condensation was
achieved, at least in most of the piping
and refrigeration devices. This will result
in energy saving and efficiency. A
comparison of the starting of the platform
before and after the insulation was made,
showing that before the insulating this starting lasted longer than after the insulating was
done. Avoiding condensation and future icing of this condensed water is an important matter
not only because of energy saving but cleanliness and dryness of the installation, especially
when electrical devices are involved.
Last point in which emphasis are going to be made is the work developed to study the
possible usage of the handheld refractometer available at the laboratory. A complete report
was made and can be found on Appendix A: Refractometer (page 62), but just conclusions are
going to be presented here. Results obtained with HR in different experiments show that this
HR can be reliability used when ethanol 99 % is part of the mixture. Some additives present
in 70 % ethanol by Carl-Roth also used modify the measurement and make the error
committed be too big. Theoretical approach was also studied but it was too complicated to
develop it for such a simple task.
Figure 5 Insulation over pipes.
Ice adhesion.
Page 8
3 Ice adhesion.
In this chapter, theoretical approach to ice adhesion and its relationship with different
parameters is described in detail, including a literature survey of several topics involved in ice
adhesion.
3.1 Crystallisation.
The crystallisation is defined as the formation of solid crystals precipitating from a
liquid or gaseous solution. It requires two steps: nucleation and crystal growth. The nucleation
occurs when supersaturation is achieved in any of the following ways: decrease of the
temperature, the pressure or the concentration of the freezing point depressant additive. The
nucleation can be heterogeneous or homogeneous if an external element takes part in the
phenomenon or not, respectively. It can be primary or secondary, when ice crystals are
formed for the first time or are formed from another previously formed ice crystals,
respectively. Depending on the supersaturation, the critical radius of nuclei is reached or not
and therefore, the crystallization occurs or not. If not, the solution remains in a metastable
state until supersaturation (for the case of most IS generators, supercooling) is high enough to
form nuclei of the required size and the conversion from this metastable state to stable ice
crystals starts.
For the particular case of heterogeneous nucleation and ice nucleus sphere shaped, the
variation of Gibbs free energy barrier that supercooling should exceed to release metastable
state is given by [ 38 ]:
A0
n
-
=
16 .n
3
.
y
3
.1
i]p
2
(L
]
.A1)
2
. (0) ( 1 )
Where:
G*
n
: Critical variation of the free energy for nucleation start.
: Surface tension between substrate and ice crystal.
T
ifp
: Initial freezing point temperature.
L
f
: Latent heat of fusion.
T: Supercooling degree.
f(): Factor depending on the wetting angle.

A higher degree of supercooling results in a lower energy barrier to achieve nucleation.
Besides, nuclei formation speed at higher degrees of supercooling is higher than with lower
supercooling degrees.
When the nucleus reachs the critical size and the supercooling degree does not decrease,
crystal growth of this nucleus occurs adding more water molecules to the initial structure. The
crystallisation releases energy in form of latent heat of solidification, which should be
evacuated in order to continue the crystallisation process. The way in which this latent heat is
Ice adhesion.
Page 9
removed is important in ice crystal shape, resulting in dendritic growth when the liquid is at
lower temperature than the ice-water interface and smooth when the opposite.
Understanding the crystallisation is a very important topic in order to achieve the main
objective of the 3E project: find a combination of parameters which results in ice slurry
formation without sticking to the heat exchange surface. Controlling the crystallisation in a
continuous operating crystalliser would lead to avoid blockings and current limitations of IS
technology [ 1 ] [ 19 ] [ 34 ]. Nucleation of supercooled water on solid surfaces is also subject
of deep study by Okawa [ 36 ] at molecular structure level.
3.2 Ice adhesion: background information.
Ice adhesion is a topic worth of study not only in IS generation, but in many fields as
aviation or space engineering. In particular, for IS generators, ice adhesion means the
necessity of ice scrapers and redundant equipments to avoid possible blockings or even
mechanical failures.
Adhesion is defined as the phenomenon in which intermolecular interactions in solid-
liquid limit phase take place, resulting in an opposition against any external stress made
[ 35 ].
At least five different theories exist for explaining ice adhesion phenomenon, but
adsorption theory is commonly referred as the most significant one, despite each theory
should be mentioned as primary or secondary effect. By the way, every interatomic force has
its influence in bond formation between ice molecules and the substrate, but adsorption theory
gives more importance to secondary forces hydrogen bonding, London dipole force,
Keeson dipole force and Debye dipole force than to primary ionic force, covalent force,
metallic force. For further details on adsorption theory, reference [ 19 ] should be consulted,
regardless of the main points of this theory are going to be defined here following the same
reference.
Cohesive energy is defined as the amount of energy per area which is necessary to
divide a material into two parts, creating two new surfaces [ 19 ] and it can be expressed:
w
c
= 2 . y ( 2 )
Where represents the surface tension, commonly expressed in mN/m.
Similarly, the work of adhesion is the energy per area which is necessary to break a
boundary surface between two media, 1 and 2 [ 19 ], and it can be expressed:
w
ud
= y
1
+y
2
-y
12
( 3 )
Where represents the surface energy of each media and
12
the boundary energy
between both media. The surface tension can be divided into a polar component and a
dispersive as can be seen later on this chapter. Polar component involves any dipole
interaction forces and dispersive component is related to the formation of universal van der
Waals bindings.
Ice adhesion.
Page 10
As well, in the latest years, dielectric theory is gaining ground to adsorption theory.
Sarkar (2009) [ 21 ] states that ice adhesion in mainly governed by electrostatic interactions
between ice and metallic substrates because of charges existing in both phases. This results in
materials with lower dielectric constant to reduce ice adhesion reducing electrostatic
interaction between the ice and the substrate. Nevertheless, Matsumoto has proved
experimentally that surface energy is the main factor governing ice adhesion [ 31 ], both in
micro and nano scale [ 37 ] and even existing or not an oxide layer over the metallic surface
[ 6 ]. Besides, Andersson in his work about ice adhesion over rubber surfaces [ 25 ] mention
seven points to reduce ice adhesion that are going to be summarised here:
Introduce low-energy surfaces or coatings.
Remove high-energy contaminations on the surface and surface tension reducing
surfactants in water.
Introduce contamination with lower energy materials.
Occlude air at the interface between ice and the substrate.
Introduce air, insoluble in ice.
Achieve an optimum degree of roughness.
Induce failure through vibrations, stresses, etc

3.3 Parameters affecting ice adhesion.
Many different parameters take their part in ice adhesion, turning the phenomenon in
something whose study involves high complexity. Most of these parameters are mentioned in
the literature consulted and they are going to be detailed from now on during this subchapter.
3.3.1 Surface energy.
Adsorption theory-model for ice adhesion was described above and its relationship with
surface energy was there detailed. In adhesion technology often surface tension and surface
energy to be an equivalent concept due to the difficulty to carry out precise measurements of
both magnitudes.
Ice adhesion is closely related to wettability of a surface as the same parameters (surface
energies) are involved. Surface energy of a surface is both related to formation and failure of
and adhesion bond and fracture energy can be expressed as and addition of G
0
(surface energy
term: W
ad
or W
c
) and (other energetic processes) resulting the second term much larger than
the first.
3.3.1.1 Relationship with contact angle.
Contact angle is the main parameter in relationship between surface energy and
wettability of a surface. Dependence of the surface energy on the contact angle can be
expressed by Youngs equation:
Ice adhesion.
Page 11
y
s
= y
sI
+y
I
. cos 0 ( 4 )
Where:
s
: Surface tension of the solid phase.
l
: Surface tension of the solid phase.
sl
: Surface tension of the solid-liquid interface.
: Macroscopic contact angle of the liquid over the solid substrate.

Combining ( 3 ) and ( 4 ), the work of adhesion can be expressed by means of
Young-Dupr equation:
w
ud
= y
I
. (1 + cos 0) ( 5 )
References [ 9 ], [ 19 ] and [ 31 ] develop this relationship in more detail.
Usually, on the determination of surface energy of a solid surface, contact angle is
included as a parameter. Detailed development of these point can be found in Page 37,
including the correlations commonly used in the calculation and description of typical
methods employed.
3.3.1.2 Relationship with polarity.
Surface tension can be separated in a polar and a dispersive component:
y = y
P
+y
( 6 )
That means that influence of each dipole or van der Waals forces in ice adhesion can be
quantified in terms of polar and dispersive components of the surface tension. This influence
is quite important in determination of surface tension in the liquid-solid interface
sl
for its
application in Youngs equation ( 4 ). Some authors collect different correlations previoulsy
proposed for estimation of this value ([ 9 ] or [ 19 ]), including the harmonic mean expression,
the geometric mean expression and the arithmetic mean expression.
This relationship between polarity and surface energy is deeply detailed in search for
the optimum wettability conditions by Wu, reference [ 32 ].
3.3.1.3 Conclusions.
In order to achieve the surface energy which results in the lowest ice adhesion possible,
laboratory experiments were done. Experiments by Matsumoto confirm the primacy of
surface energy influence in ice adhesion and show a proportionality between surface energy
of the solid substrate and ice adhesion, measured by shear stress, both in micro [ 31 ] and
nano [ 37 ] scale. However, conclusions of the experiments developed by [ 19 ] could not find
a real correlation between surface energy and work of adhesion and the ice adhesion observed
in the samples, but roughly stating than ice adhesion is lower when surface energy is lower.
3.3.2 Contact angle and wettability.
The importance of contact angle measurement in ice adhesion study was already
justified before, because its involvement in surface energy calculation. Contact angle of a
Ice adhesion.
Page 12
drop of water over a substrate is the main parameter in wettability, ability of a liquid to keep
contact with a solid determined by a balance between adhesive and cohesive forces previously
defined. Good wettability conditions between both phases is required for adhesion, as well
bad wettability results in bad adhesion [ 35 ]. Next chapter will deal with the subject of
hydrophobicity, which is another parameter closely related to contact angle.
Most of studies consulted about ice adhesion use contact angle as a parameter of study
in order to determine an univocal relationship between both magnitudes, but none of them has
achieved this relationship. Andersson [ 25 ] states that there is an experimental correlation
between ice adhesion and rubber substrate wettability. For these kind of surfaces, shear
strength of ice decreases linearly with incresing contact angle below 90. Above this value,
shear stregth remains practically the same. Bascom and others [ 26 ], as far as they are
concerned, found no correlation between minor contact angle variations and shear strength of
ice in their experiments in search of icephobic substrates including several polymer coatings
over clean brass plates and highly polished stainless steel plates, despite having mentioned a
theory by Raraty and Tabor that agrees the statement of Andersson in the decrease of shear
strength with increasing contact angle over this kind of substrates. However, experiments with
different coatings over a polycarbonate substrate made by Dotan [ 20 ] result in a very good
linear correlation between contact angle of water over the surfaces and shear strength using
the centrifuge ice adhesion test, so it is stated that the higher the contact angle the lower is the
ice adhesion [ 20 ].
Finally, studies of water contact angle over ice by Knight [ 27 ] denied the common
prediction that this value is zero. It was shown through three different experiments that this
contact angle is higher than 0.
3.3.3 Hydrophobicity.
The relationship between hydrophobicity and contact angle exists by definition, since
hydrophobicity is defined: property of a surface that results in a contact angle higher than 90
[ 20 ]. By the way, there is another term related to hydrophobicity. Ultrahydrophobicity or
superhydrophobicity requires the contact angle to be as close to 180 as possible, being over
150 and the sliding angle, the angle at which a liquid drop of certain properties begin to slide
down the surface over it is placed, approaches 0, being lower than 10 [ 20 ] [ 22 ] [ 23 ]
[ 24 ]. Many possibilities of achieving superhydrophobicity are mentioned by Sarkar [ 21 ]
and Andersson [ 25 ] relates this characteristic to air trapping between the substrate and the
water drop or flow.
On the other hand, hydrophilicity exists and is related to a contact angle over a surface
that is lower than 90. Zwieg [ 19 ] found that in hydrophobic surfaces, adhesive forces are
involved in the fracture of the ice-substrate bond while in hydrophilic ones are cohesive ones
who act.
Many authors have experimented with hydrophilic and hydrophobic surfaces in order to
predict ice adhesion over a wide range of surface characteristics. For example, Bascom et al.
[ 26 ] studied both hydrophilic and hydrophobic surfaces finding a rough correlation between
high hydrophobicity and low ice adhesion, but this correlation was not found in surfaces that
Ice adhesion.
Page 13
have a contact angle between 80-120. It is also mentioned that 150 is the value of contact
angle from a decrease in ice adhesion is observed. Nevertheless, Andersson [ 25 ] defined the
hydrophilicity number , depending on contact angle of water and diiodmethan over several
rubber materials, and found that low adhesion was observed in these surfaces when was
lower than 0,2, corresponding to contact angles higer than 90. For higher than 0,2 ice
adhesion strength increased linearly.
Therefore, no fixed correlation can predict relationship between hydrophobicity of a
surface and ice adhesion over the surface, despite Sarkar [ 21 ] states that there is a direct
relationship between hydrophobicity and icephobicity basing on experimental practice. Zwieg
[ 19 ] concludes basing on an experiment by Jellinek, that hydrophobicity is a necessary
condition for low ice adhesion, but it is not sufficient.
3.3.4 Surface roughness.
Later on, a description of practical parameters of surface roughnes can be found
(page 20), but here a discussion basing on experimental and analytical conclusions from
different authors is going to be made.
A deep conceptual description of the roughness factor can be found in [ 9 ] by D.E.
Packham, comparing the theoretical influence of the classical roughness factor by Wenzel
1
,
used when surface roughness is not great, with the much more complex fractal approach to
surface roughness. In the reference, more information about this comparison and its
implications can be found.
It is commonly accepted the relationship between variable surface roughness and
resulting contact angle and there are two mathematical models which try to explain it [ 21 ].

Wenzel model (Figure 7) is expressed by the following equation:
cos 0
i
= r . cos 0 ( 7 )
Where:
: contact angle of the water over the surface considering the roughness.
: contact angle of the water over the surface if it is considered perfectly plane.
r: ratio of areas as in footnote 1.

1
r = AA
0
; where A represents the real area of a surface and A
0
the nominal area [ 9 ].
Figure 7 Wenzel model [ 42 ].
].
Figure 6 Cassie-Baxter model [ 42 ].
].
Ice adhesion.
Page 14
On the other hand, model by Cassie-Baxter (Figure 6):
cos 0
i
=
1
. cos 0
1
+
2
. cos 0
2
( 8 )
Where:
: contact angle of the water over the surface considering the roughness.
f1: area fraction of the solid surface.
f2: area fraction of the air surface.
1,2: contact angle corresponding to each solid-air fraction.
This equation entails high hydrophobicity when a rough surface with high air
entrapment is involved, because f
1
+ f
2
= 1 and
2
= 180 and ( 8 ) can be expressed as:
cos 0
i
=
1
. (cos 0
1
+1) -1 ( 9 )
Dotan [ 20 ] stated that lowest ice adhesion values were obtained over
superhydrophobic surfaces, a surface finishing achieved using a combination of low surface
energy and micro- and nano-roughness, emphasizing that crystallisation is probably affected
by surface roughness. Zhang [ 23 ] also states that formation of a microscaled structure
enhances hydrophobocity and experiments by Guo [ 22 ] with superhydrophobic coatings
over copper substrates show that surface roughness improves water repellency.
Experiments over rubber substrates by Andersson [ 25 ] show that for contact angles
higher than 90 (hydrophobic surface) on a smooth surface, contact angle increased with
increasing surface roughness parameter, reaching values of 160, but results of the study of
the relationship between hydrophobicity and ice adhesion were described above and no
correlation was found. Otherwise, experiments by Bascom [ 26 ] over abraded steel show that
surface roughness can increase adhesion shear stress values.
Finally, studies from Faucheux over aluminium and nickel substrates were focused to
find a quantitative correlation between the surface roughness and the degree of supercooling,
which is closely related to crystallisation. Both [ 34 ] and [ 38 ] present equations relating
these magnitudes basing on experimental evidences.
3.3.5 Polarity.
Importance of surface energy on ice adhesion was already described before and, as well,
relationship of the surface energy with polarity and the intermolecular forces involved in
adhesion.
According to Zwieg [ 19 ], the polarity of the surface has a great influence on the
formation of the ice binding because of the orientation of water molecules over the surface
varies. Thus, icing over polar surfaces is enhanced by the H-bonds of the water and the
hydrolised surface similar to ice structure (Figure 8). Otherwise, molecules ordered over a
non-polar surface have a structure very different from that of the ice and adhesion of ice over
this kind of surfaces requires additional energy to vary the structure, therefore lower
temperature over the surface. Hence, lower ice adhesion over non-polar surfaces can be
predicted.
Ice adhesion.
Page 15
Besides, de Bruynes principle is quoted by Wu [ 32 ] stating that two materials which
have great disparity between their polarities can not form a strong joint. That means that the
greater this disparity between polarities, the lower wettability of the surface will be.

Figure 8 Different orientation of water molecules over a polar/non-polar surface [ 19 ].
3.3.6 Other parameters.
The most influential parameters in ice adhesion were already explained, but others are
also mentioned by different studies, especially to compare its influence with the influence of
the ones above.
3.3.6.1 Cooling heat flux.
On his Fundamental study of ice adhesion to cooling solid surface [ 31 ], Matsumoto
compares the influence of the cooling heat flux and the surface energy of the substrate on the
shear strees at the interface between ice and solid. Experimental results show that surface
energy is proportional to ice adhesion forces rather than the cooling heat flux.
3.3.6.2 Supercooling.
Defined as the difference between the freezing temperature of intial concentration
minus the temperature of the liquid near the cooling surface, supercooling is a way to achieve
supersaturation (metastability) of a solution basing on temperature. Before, the importance of
supercooling on crystallisation process was mentioned. Experiments by Matsumoto [ 39 ]
show that supercooling has a great influence in ice structure near the surface and, therefore, in
scraping force needed to remove ice from the cooling solid. Scraping force have a tendency to
decrease with the increase of supercooling degree because ice formed over the cooling solid
seemed sparse instead of dense (for lower supercooling degrees).
Ice adhesion.
Page 16
Additionally, Faucheux found a correlation between the surface roughness of the
substrate and the recommended degree of supercooling [ 34 ] [ 38 ].
3.3.6.3 Oxide layer.
Great variations of the measured contact angle/surface energy on surfaces with similar
roughness parameters show that not only roughness affects ice adhesion but composition of
the external layer of the substrate.
Matsumoto [ 6 ] studied (re)formation and composition of the oxide layer when
different methods of removing it are applied. Time dependancy on its (re)formation was also
analysed. It was found that buffing was not a valid method to the removal because the heat
transmitted to the plate helps in the reformation and the surface is immadiately oxidised. For
other removal methods was found that reformation occurs during a 90 days process, starting
in the same moment the removal had been done. The removal and the oxidation time were
also proposed as important factors in ice adhesion variation.
The difference in shear stress observed between different oxidation layers is caused by
difference in ratios of Cu and Cu
2
O. Thickness of the oxide layer was also determined and,
since it was tens of ngstroms, influence of the whole quantity of existing oxide in acting
intermolecular forces was suggested.
Okawa [ 40 ] suggests basing on freezing of supercooled water over a metallic surface
(comparing a non oxidised gold plate with a polished copper plate) experiments that oxidation
of the surface prevents the crystallisation of the supercooled water on the surface.
3.3.6.4 Additive concentration.
Adding additives of high surface energy is some of the points mentioned by Andersson
[ 25 ] for enhacing adhesion over rubber surfaces. A deep study of effects of different
additives included in aqueous solutions in ice adhesion is also made by Zwieg [ 19 ].
3.3.6.5 Contact area.
Sarkar [ 21 ] proposes a different way to understand relationship between
hydrophobicity and low ice adhesion. Surface area in contact with water in case of a
hydrophobic substrate is very low comparing it with a hydrophilic substrate and contact area
of ice will be lower as well. Therefore, intermolecular forces and mechanical interlockings
between ice and the substrate will be lower and so ice adhesion.
3.3.6.6 Dielectric constant.
Present importance of electrostatic theory in ice adhesion understanding was stated
before. Sarkar [ 21 ] relates adhesion of ice over a substrate with the dielectric constant of the
substrate material, stating that a low dielectric constant would reduce ice adhesion as the
electrostatic interaction between ice and the substrate is reduced.
Ice adhesion.
Page 17
3.3.6.7 Homogeneity.
Experiments by Zwieg [ 19 ] mentioned in [ 2 ] used a heterogeneus surface with
predetermined nucleation points. The heat released by crystallisation constantly avoid the
solution to reach the supercooling degree. Therefore, homogeneity of the surface is important
to avoid this problem.
3.3.6.8 Micro- and nanostructure.
The formation of a micro- or nanostructure plays an important role in achieving
(super)hydrophobicity, as it has been mentioned before [ 21 ] [ 23 ].
Besides, influence of the surface energy in shear strees between ice and a metallic
substrate was confirmed also at micro- and nanoscale by Matsumoto [ 37 ].
3.3.6.9 Glass transition temperature.
Experiments by Andersson over rubber substrates also showed a correlation between ice
adhesion and glass transition temperature of the substrate. When the glass transition
temperature was below the test temperature, the interfacial shear stress was also lower.
Surfaces: materials and coatings.
Page 18
4 Surfaces: materials and coatings.
Ice adhesion over different surfaces is, as it has been told before, one of the main topics
of this Master Thesis. Throughout the following pages, different methods of surface treatment
are described and their final behavior will depend on the parameters achieved, as explained in
the previous chapter.
Main interest on the different surface treatments put into practice lies on a combination
of hydrophobicity (contact angle), surface energy, polarity, homogeneity and roughness that
could lead to an ideal scenario of no ice adhesion, or less adhesion as possible, in the new
prototype-like ice slurry generator.
In most of the cases considered, copper based plates are used due to its huge high
thermal conductivity and its affordability. This decision can be easily justified comparing this
coefficient with others at 20 C (despite our experiments will be developed below 0 C):

Despite mentioning them in each subchapter below, a summary including a brief
description and some observations of every sample which is going to be used in further
experimental procedures in order to analyse its suitability for its application in the IS
generator can be found in page 34.
4.1 Non-coated copper plates.
For the common development of the project, long copper plates are available to work
with. At first, plates of copper were cut from these long ones with 50 mm x 40 mm, but
additional requirements made necessary some copper plates of 100 mm x 40 mm. Ageing of
these copper plates, dirt and heterogeneity caused by oxidising at ambient conditions and
Material Thermal conductivity [W m
-1
K
-1
]
Aluminum 200-250
Copper 385-400
Glass 1
Gold 315
Iron 70-80
Lead 35
Silver 410-420
Stainless steel 16
Table 1 Different thermal conductivity coefficientes [ 5 ].
Page 19
achieving different experimental conditions require a different surface treatment before an
experimental approach to the topic of ice adhesion could start. The objective is getting a
surface as homogeneus as possible so as to study the properties in any area of it without
problems of repeatability. Moreover, a codename is given to each different plate in order to
simplify.
4.1.1 Procedure.
Basic treatment received for the plates are the one done with denatured alcohol -ethanol
mixtured with hazardous additives- to clean any possible dirt and Sidol Metallpolitur to
remove the surface oxide layer -further information over this topic can be found later on. Both
products are applied with a soft cloth reserved for such purpose in order to not damage the
surface. Besides, plates were carried in a closed box wrapped with a piece of paper.
This basic plate is used as a reference for future measurements and studies, as it
represents the raw material conditions and its codename is REF. As can be seen on Sidol
webpage, the Metallpolitur used contains cleaning components as soap and other non-public
components which remove the oxide layer and remains on the surface protecting it.
Another way to remove the oxide layer is by buffing the surface with different
sandpapers trying to achieve different roughnesses that are goint to be studied as a main part
of this work. In this case, four kind of sandpapers were hand used with the aim of obtaining
roughness parameters of 0,4/0,8/1,6/3,2 m.
Different sandpapers mean different grit sizes involved. Standard ISO6344 [ 7 ] show
the main dimensions of these grit sizes and this classification are shown in Appendix C:
Datasheets. This parameter is measured by letter P and a number, the lower this number is the
rougher the grit size is and the final result would be.
In our case, the sandpapers used were the following ones:
VSM KK114F based in cotton and coated with aluminium oxide grain. P400.
o Codename of the copper plate: R04(q).
VSM KK114F based in cotton and coated with aluminium oxide grain. P280.
CF Schrder AJ25 based in J-cloth and coated with aluminium oxide. P150
Feldmhle Schleifmittel C100 P895
2
. No additional data was found.
Two ways of buffing were made. First of all, oriented lenghtwise and another time with
non-oriented buffing -represented by q in the codename- to check the influence of this
parameter on the experimental approach.

2
This P may not refer to the previously defined P parameter of grit size as this paper is the roughest of the four
considered and the value offered for P should correspond to the finest one.
Page 20
4.1.2 Oxide layer.
It seems important to make clear some aspects relating to oxide layer (re)formation.
This reformation starts just after the removal process finish and lasts for around 90 days when
removal process is not mechanical buffing. Buffing is presented as an ineffective method to
remove oxide layer, as the heat involved in the process helps in the re-oxidisation of the plate.
Complete study at this point can be found on reference [ 6 ] by Matsumoto, where it is
supposed that oxide layer is instantly back to the surface due to the this transferred heat.
4.1.3 Roughness.
All the process was hand made, so checking the real roughness became necessary with
additional roughness measurements. Some basic points over surface roughness may need to
be explained first.
Surface roughness is a measure of the texture of a surface by determining the vertical
deviations of the real surface from its ideal form represented by its mean line. It is a very
important parameter in the quality of a metallic part, but it needs a standardisation in order to
evaluate the different existing textures: [ 8 ] and ISO4287.
Following the described standard and the catalog in Appendix D: Catalogs, it can be
defined:
- R
a
: Arithmetical mean deviation.
Arithmetic mean roughness value from the
amounts of all profile values (Figure 9). R
a

makes no difference between peaks and
valleys.
R
u
=
1
I
m
]
|Z(x)| Jx
I
n
0
( 10 )
- l
m
: Evaluation length.
- l
r
: Sampling length.
l
=
I
n
5
( 11 )
- R
z
: maximum height of profile
Average value of the five R
zi
, maximum for each sampling lenght, l
r
.
- R
t
: total height of profile from the highest peak to the deepest valley.
In the measurements, R
a
was taken as the parameter to determine the surface roughness,
despite there are more models to understand and study this magnitude from a theoretical point
of view. For example, Wenzel roughness factor or the more complex fractal approach by
Mandelbrot [ 9 ].
Since the Institute of Materials and Processes (IMP) of HsKA owns a roughness
measurement machine at the university, two measurements were made to evaluate roughness
Figure 9 R
a
graphical description from
Hommel-etamic catalog
Page 21
itself and influence of oxide layer in it two weeks later and these measurements for the
abovementioned plates are presented in Table 2.

Roughness measurements Ra (m)
REF R04 R04q R08 R08q R16 R16q R32 R32q
#1
0,10,05 0,460,04 0,360,03 0,610,13 0,590,06 0,870,17 1,090,09 1,250,41 1,560,06
#2
0,480,04 0,590,14 0,860,27 1,410,45
Table 2 Roughness measurements of copper non-coated plates.
The machine used was a Hommel-etamic Hommelwerke T800C with a Hommelwerke
TKU300/600 needle resulting in a minimum resolution of 50 nm. Surface roughness
measurements were done under the conditions and requirements presented in DIN EN 10049
[ 8 ]. Each final measurement consist of six individual back and forth measures, three in
longitudinal direction and three in perpendicular. This could be important in the results
analysis, as oriented plates were buffered lengthwise.
4.1.4 Conclusions
Surface roughness measurements do not show any visible dependance on oxide layer
growth, as in [ 6 ] is said that oxide layer thickness is several orders of magnitude lower than
micrometers -common resolution of surface roughness measurements-, around 20-40 for
the samples considered in that experiment.
The value of surface roughness for the plate REF after it was polished with Sidol is the
lowest one of the measured ones. This range (from REF to R32q) of roughness will be studied
as an important parameter in ice adhesion later on. On the other hand, REF measurement is
very near to the consulted minimum resolution of the device used in surface roughness
measurement (50 nm), despite the results obtained from the company software include more
decimal data. Accuracy at this level could not be as good as at other levels.
In case of oriented plates, great difference was found between lengthwise and
perpendicular measurements, due to its own characteristic, but R
a
was calculated with all the
data obtained just dismissing harsh outliers. These outliers may be because of strong surface
damages on the plates like severe scratches and other similar marks.
Three longitudinal and three transversal measures were made and this result in a
difference between data obtained from oriented and non-oriented plates. Measures done over
oriented plates show greater standard deviation than measures done over non-oriented ones,
precisely due to the method used in measuring and calculating the arithmetical mean surface
roughness parameter.
Nevertheless, no direct relationship but lower standard deviation was found between
oriented and non-oriented measurements and the reason is already explained.
Page 22
4.2 Coated plates.
Different coatings over copper plates were studied in order to achieve different results
to be compared and may lead to the optimum combination of parameters for avoiding ice
adhesion. Especially, hydrophobicity -or even superhydrophobicity- are desired.
These coatings are now described by dividing them en three groups: plastic coatings,
metallic coatings and organometallic coatings.
4.2.1 Plastic coatings.
Available at the laboratory, there are several plastic products whose properties include
adhesion over some surfaces and waterproofness. These properties are going to be used for
the purpose required of coating a copper plate to improve the hydrophobicity of raw material.
The same procedure was used for all of them in order to expand the product over the
plate and achieve some grade of homogeneity. Both borders were covered lengthwise with
adhesive tape and the product were spilled in the middle and spread with a flat surface, i.e.
another similar copper plate, levelling the result using both adhesive tape strips. Previously,
the surface has received a special treatment if necessary (ProbeF) or has been cleaned with
denatured alcohol and Sidol Metallpolitur as described before. When the tape strips are
removed, mid region is covered with the product and ready to let dry at ambient conditions
during a couple of hours or a day, depending on the components.
Most of the plastic coatings are silicone based or even silicone itself. A list of them and
their components and properties are shown below, including the codename of each plate for
further identification:
Normal silicone by quick-mix, white/transparent colored. No composition was
found in the package.
o Codename of the copper plate: ProbeA.
Silicone plus by Probau, grey colored. Safety datasheet in Appendix C:
Datasheets.
o Codename of the copper plate: ProbeB.
Silicone adhesive for aquaria by Hobby, transparent. No composition was found.
o Codename of the copper plate: ProbeC.
Hochtemperatur silicone by Probau, red colored. Safety datasheet in Appendix
C: Datasheets.
o Codename of the copper plate: ProbeD.
Anaerobic pipe thread sealing SWAK by Swagelock, white colored. Containing
resin (methacrylic ester) and PTFE (Teflon) particles.
o Codename of the copper plate: ProbeE.
Sikaflex 295UV by Sika. White colored. 1-C Polyurethane based adhesive.
o Codename of the copper plate: ProbeF.

Pretreatment over the copper plate in ProbeF sample was very different from the
previously described procedure as it was found in the Sika catalog. At first, Sika Aktivator
were spread over the copper surface. Then, 15 minutes have passeda and 206 G+P Primer also
by Sika were applied. Finally, 10 minutes after, Sikaflex product were spread and let dry.
Page 23
Results of plastic coatings were
uneven, as some of them worked and other
did not. Silicone coatings worked perfectly
over the copper plate. ProbeA, B, C and D
showed great adhesion, uniformity of the
external layer and homogeneity. It seems
that worths continuing with further
experiments with these samples. Though,
ProbeE and ProbeF did not show either
great adhesion or homogeneity to the
surface.

In the first case, ProbeE covered with thread sealing SWAK result was very
heterogeneus and no solid layer of the product was observed at any moment. The product was
easily removed, so no adhesion had existed too.
Instead, Probe F showed good properties of adhesion over the copper surface, but the
result of the external layer was too uneven. There are two reasons that could explain this
behaviour, being a problem of the Sikaflex itself or the little quantity that remained, which
may be was not enough to be spread over the surface.
On the oher hand, samples A, B, C and D, as it was told, showed good properties both
in adhesion and homogeneity. Final result was better for samples A and C, since B and D
showed damaged regions due to an unaccurate spread method. Besides, further experiments
does not show any considerable difference between A or C and B or D. It was decided to
remain just with ProbeA and C and postpone the final decision of which on will show lower
ice adhesion to real experimental phase.
Finally, roughness measurements were also carried out on these silicone samples
following the procedure abovementioned and results are shown here:
REF ProbeA ProbeC
#1 0,10,05 0,240,06 0,450,12
Table 3 Roughness measurements of plastic coatings.
Just one measure were carried out, as oxide layer growth is not involved. Main
conclusion lies on standard deviation of ProbeC, double of the value of ProbeA. This might
be explained by the little holes that ProbeC shows all over the surface and whose origin is
unknown.
Concluding, it is wide known the hydrophobic and waterproof properties of plastic.
Adhesion showed by most of the samples are promising of good results in low ice adhesion,
as both A and C samples were submerged for a week in slush ice machine and no damage or
any unexpected event happened.
Figure 10 ProbeA shows great adhesion and
homogeneity.
Page 24
4.2.2 Metallic coatings.
Many references consulted emphasize silver thin films hydrophobicity and, thus,
suitability for applications which low ice adhesion is required. Many options exist to achieve
a silver coating over different substrates, but just one of them was selected due to its
simplicity and versatility.
Silvering through Tollens reagent is a widespread way to coat and manufacture home-
made mirrors with silver over a glass substrate. As it has been told, it is a very easy method
and materials needed are usually in any chemistry laboratory:
Silver nitrate -AgNO
3
.
Ammonia -NH
3
.
Potasium hydroxide -KOH.
Glucose -C
6
H
12
O
6
.
Distilled water.
Glass container.
Burner or lighter.

Experimental procedure is now described. 10 g of AgNO
3
are diluted in 50 cm
3
of
distilled water (A), 1 g AgNO
3
is diluted in 25 cm
3
of distilled water (B) and 7 g of KOH are
diluted in 50 cm
3
of distilled water (C). AgNO
3
(aq) is reduced with several drops of
ammonia until the solution is completely transparent, removing the silver precipitade formed
at first. Some drops of B are added in order to avoid the excess of ammonia in the mixture and
then C is added slowly while stirring. Now, the Tollens reagent is formed: [Ag(NH
3
)
2
]NO
3
.
This solution of the Tollens reagent is reduced with aqueous glucose in presences of a
heat source and pure silver precipitade is formed:

|Ag(NE
3
)
2
]
(uq)
+
+ c
-

- Ag
(s)
+ 2NE
3

(uq)
( 12 )
The copper plates previously cleaned with denaturalised alcohol were submerged in
this solution and heated both with a burner and inside an oven in order to achieve a silver thin
coating over them. Result are shown in Figure 11, where the left one is the copper plate
heated with the burner and the right one were heated inside an oven at 90 - 100 C.

Figure 11 Copper plates
after the silver
mirror
experiment
Page 25
From Figure 11, adhesion of the silver mirror over copper is shown to be ineffectual, as
the silver layer is inexistent in some areas and non homogeneus where not. Many possibilities
to understand this situation were considered, since the silvering of the recipient happened. It is
known that glass behaves as a catalyst in this kind of silvering and copper does not perform
this role. Another point could be work temperature, which is low and copper surface does not
soften and help to the adhesion. Last considered point is contact angle, which may be not low
enough between the aqueous solution of the Tollens reagent and copper to ensure adhesion.
Any of these reasons or even others related with pre-treatment or compatibility could
be the reason for the results obtained, which are far to be successful. This experiment failed,
further information about this topic was searched and no solution was found. Increasing the
heating temperature could be favorable and another try may under this condition may be
worth it.
4.2.3 Organometallic coatings.
Another different way in order to create a metallic thin film over the copper plates is
basing in the resinates technology. Resinates paste is a soluble metal-organic preparation
which can form a thin layer over a surface through a suitable thermal treatment. The organic
part is usually a natural resin or a long carbonated backbone (carboxylic, alcoholate, ...) and
the metallic part is usually formed by a precious or a base metal.
Three kinds of resinates paste were received from Ferro GmbH. with some safety
datasheets attached, including a DSC
3
analysis. The references on the thermal analysis do not
match up with the reference of the samples themselves. This mismatch suppose a great
problem for the task, as the thermal treatment cannot be determined basing in the components
involved and their thermal behaviour. Further contacts with the company did not solve the
problem and experiments were carried out on our own.
Literature survey was made and references [ 10 ], [ 11 ], [ 12 ] and [ 13 ] were found
over basics on metal resinates. All of them treat resinates coating methods in order to achieve
the best adhesion conditions over ceramic substrates. Usually, this technique is used to create
decorative details in fine pottery or high conductive threads in electronic applications, but
high adhesion is wet conditions is the unique property in which this project is interested. At
this point, information found in reference [ 10 ] was very important because a range of
temperatures was found and could be used as an initial aproximation.
Composition of the three resinates pastes used in this experiment were:
1. HF8013. Metallic part: Cu circa 10 %. Organic part: Octanoate-naphthenate-copper-
complex (50-100 %), xylene (7-10 %), organic salts from acids/bases and aromatic
carbonates.
o Codename: Probe1.
2. HF8007. Metallic part: Cr circa 10 %. Organic part: organic salts from acids/bases,
vegetable oil and/or turpentine oil.
o Codename: Probe2.

3
Differential Scanning Calorimetry: Thermoanalytical technique in which the difference in the amount of heat
needed to increase the temperature of the sample and a reference in measured as a function of the temperature.
Page 26
3. HF8016. Metallic part: Ni circa 3 %. Organic part: organic salts from acid/bases,
vegetable oil, aldehyde/cetone, carboxylic acid/ester/anhydride, turpentine oil
(30-50 %) and cyclohexanone (1-3 %).
o Codename: Probe3.
Further information can be found in each correspondant Appendix. As well, this
information is not very specific and composition is not really clear to carry out the experiment
with reliable data. It was justified the reason to carry out the experimental part without
following any known method because of the absence of reliable data. From now on, using an
available furnace by Heraeus (MR170, 220 V, 14 A, 1000 C mx.), an attemp to create this
thin layer with any of the resinates paste will be developed. Firstly, the heat treating used was
continuously rising basing in the phases and limits found in [ 10 ] and it consists on brushing
with Sidol Metallpolitur the surface and stabilise for 20 minutes the sample, dry the sample at
100 C for 10-15 minutes and heat up to 500 C for 20 minutes. Real treatment is represented
by Graph 1, including the dry period in ambient air.

Graph 1 Heat treating 1: temperature (C) vs. time (minutes).
Results achieved with this heat treating are shown below in Figure 12, Figure 14 and
Figure 13. It can be seen that results are far from being homogeneus and well stuck to the
substrate, apart from some specific zones of the samples.
There are several reasons which can explain this behaviour, from a wrong heat treating,
to an incorrect pre-treatment of the surface or similar. None of them can be ensured to be
right, but further research at this point should be made, as well as contact with the delivery
company, Ferro.
0
50
100
150
200
250
300
350
400
450
500
0 50 100 150
T
e
m
p
e
r
a
t
u
r
e

[
C
]
Time [min]
Real heat treating
Heat treating 1
Page 27

A possibility to understand this behaviour was found in [ 13 ], which is about forming
thick films and their high adhesion to different substrates as well as their high electrical
conductivity. Usually, resinates films are created over glass surfaces which soften at low
temperatures and helps in adhesion. Forming these films over ceramic or metallic substrates
can be because of this reason much harder and may require some additives in the mixture.
Preparing a mixture between the desired metal resinate and finely divided glass powder is a
commonly used solution as seen in Figure 15.
On firing, after the organic mixture has burnt off, the glass softens, wets the ceramic
surface and concentrates at the substrate/film interface whilst the metal powder [ 13 ].
Therefore, it results in a sintered metal layer attached to the substrate by a glassy interface,
which penetrates all over the substrate creating the adhesion and without any chemical
bonding, depending the adhesion on the mechanical links among the materials.
In [ 13 ], some properties of the glass
powder which is needed to improve
adhesion of organometallic coatings. Size
must be as low as possible, of the order of
10 m to achieve sintering of metals at
reasonably low temperatures. Composition is
also determined, because its importance in
fluidity, and lead borosilicate glass with a
low silica content would be the best option. In this moment, contact was made with Schott
GmbH so as to find the suitable glass powder. Two references were selected as the most
appropiated and their properties are shown in Table 4:

Figure 14 Probe2. Figure 12 Probe1. Figure 13 Probe3.
Figure 15 Metal film, glass powder and substrate
William E. St. Clair, J. C. Minor, Ray V. Lawrence.

Page 28
Table 4 Properties of both references considered as suitable for the experiment.

In the reference mentioned no consideration about ratio of each component in the
mixture, so it experiment was done mixing the organometallic component and the glass
powder in 1:1 proportion. Experiments were done following the heat treating shown in the
datasheet of each glass powder (Appendix C) commonly used in glazing applications and the
real treating developed was a bit different from the original one due to the unaccurate control
of the Heraeus furnace. Both are shown in Graph 2 and Graph 3, including cooling down
period inside the oven with open doors.

Graph 2 Ideal and real heat treating for the glass powder 8465.

0
100
200
300
400
500
600
0 100 200 300 400 500
T
e
m
p
e
r
a
t
u
r
e

(
C
)
Time (min)
Ideal vs real heat treating
Ideal treating
Real treating
Property Ref: 8465 Ref: G017-393
Chemical Composition (wt. %)

Li
2
O: 1-10
Al
2
O
3
: 1-10
SiO
2
: 1-10
PbO: >50
B
2
O
3
: 10-50
Al
2
O
3
: 10-50
SiO
2
: 1-10
PbO: >50
B
2
O
3
: 10-50
Grain size (m)
51 31
Transformation temperature
385 C 320 C
Description
Low melting solder glass. Non crystallising low melting solder glass.
Page 29

Graph 3 Ideal and real treating for the glass powder G017-393.
Six different samples were created with these heat treatings and this is the explanation
for each one:
Resinate HF8013 (Cu) + glass powder 8465 following heat treating in Graph 2.
o Codename: Probe1A.
Resinate HF8013 (Cu) + glass powder G017-393 following Graph 3.
o Codename: Probe1B.
Resinate HF8007 (Cr) + glass powder 8465 following Graph 2.
Resinate HF8007 (Cr) + glass powder G017-393 following Graph 3.
Resinate HF8016 (Ni) + glass powder 8465 following Graph 2.
Resinate HF8016 (Ni) + glass powder G017-393 following Graph 3.
Results of this procedure are shown in Figure 16, where visual finishing can be
evaluated and analysed for each sample.

0
50
100
150
200
250
300
350
400
450
0 50 100 150 200 250
T
e
m
p
e
r
a
t
u
r
e

(
C
)
Time (min)
Ideal vs real heat treating
Ideal treating
Real treating
Figure 16.a Probe1A.
Figure 16.b Probe2A.
Figure 16.c Probe3A.
(c) (a) (b)
Page 30
Visual and tactile evaluation of the results determine that both Probe2A and Probe2B
are the most appropiated ones to continue with further experiments. The rest of them show a
non-homogeneus surface, even broken or not completely coating the whole plate. Heat
treating followed was the one which should have been followed by the glass powder itself, not
considering the influence of the mixture with the organometallic resinate because any heat
treating related to each different resinate paste was not found. The heat treating could have
been the reason for each mixture to not coat properly each substrate, but it might not be the
main reason as adhesion depends on other parameters that were not studied for resinate-
copper interface: contact angle, surface energy, surface topography [ 9 ] or different
interfacial forces [ 6 ].
It was told that results for Probe2A and Probe2B were acceptable as they show
homogeneity in their more external surface. As a matter of fact, Probe2B showed some
irregularities at this surface that can be best seen comparing results of roughness
measurements done following the procedure that was described before (Table 5).

REF Probe2A Probe2B
#1 0,10,05 0,780,12 2,240,40
Table 5 Roughness measurements comparing REF, Probe2A and Probe 2B.
It can be seen that roughness is much higher for Probe2B, which is not necessarily a
problem, but could become in problems with determining some properties which are
fundamental for the previous study of ice adhesion. Despite this, further experiments will be
carried out with this plate to check if the initial supposition about its behaviour is real.
4.2.4 Tin/zinc coating.
Apart from the laboratory made coatings, some other copper plates were studied during
the project. In this case, copper plates coated with tin and zinc were delivered by Weinbrecht
& Kcherer.
In the delivery, plates were wrapped without any mention to the identification of each
plate. That was a problem, because both coatings were silver coloured and very similar each
other. The identification of the plates was needed in order to start research about the material
and their properties.
An initial guess was made basing on internet sources ([ 17 ] [ 18 ]) in where some
properties of zinc and tin are mentioned, respectively. Especially, colour of the plates are a bit
different, as one of them has a bluish shine and the other one is completely silver. The
identification was made by direct observation of the colour and comparison with the
references made, where it is mentioned that zinc has bluish shine as one of the plates and tin is
completely silvered like the other.
This identification can not be understood as definitive, because of the obvious problems
related to visual identification: subjectivity, influence of external light and qualitative
determination. Further information or another ways which can be more precise become
Page 31
necessary. Contact was made with the company and the information received confirmed the
initial hypothesis.
Copper plate coated with tin. Silver coloured.
o Codename: Platte1.
Copper plate coated with zinc. Silver coloured with bluish shine.
o Codename: Platte2.
More experiments were made with both plates, but size (1080 mm x 40 mm x 5 mm)
was a great problem so as to transport the plates and place them properly in the laboratory to
make the experiments.

4.2.5 Other coatings.
Interest of the work developed lies on finding a combination of parameters which helps
in achieving low ice adhesion in the ice slurry generator. Many references ([ 19 ] [ 20 ] [ 21 ])
treat the topic of the relationship between hydrophobicity and ice adhesion icephobicity.
Thus, developing a hydrophobic surface over the copper test plates available became an
interesting issue.
It is considered a hydrophobic surface when contact angle of water over the surface is
higher than 90. Besides, superhydrophobicity (or even ultrahydrophobicity) is achieved when
the contact angle is higher than 150 and the sliding angle of the water drop is lower than 10
[ 20 ] [ 22 ]. Many hydrophobic coatings were already studied and described by [ 1 ] [ 19 ]
and other authors already mentioned before to experimental laboratory work. It would be
interesting for the project 3E by Dipl.-Ing. (FH) Susanne Frank to develop one of these
copper coatings or finishings in order to study its effectivity in the industrial-like working
conditions of the IS generator prototype. Most of the hydrophobic surfaces studied in
relationship with ice adhesion are focused on aviation or space engineering applications [ 2 ]
or may require some equipment technology currently not available at the laboratory of HsKA,
thus hydrophobicity will be achieved by buffing at different roughness and plastic or
(organo)metallic coatings. Despite of this, additional information about superhydrophobic
coatings over copper plates were searched and here are some of the ideas found.
Reference [ 22 ] by Guo treats the topic of superhydrophobicity over copper based
plates through wet chemical reaction. Immersion in an aqueous oxalic acid solution during a
week and coating with dimethylsiloxane (PDMSVT) by spinning, curing in oven for a couple
of hours is also needed for finishing the process.
Another method is described by Zhang [ 23 ] that needs sandblasting of the copper
plate, ultrasonic rinse in NaOH and water, surface oxidation with KOH and K
2
S
2
O
8
solution,
autoclave for an hour, rinse in distilled water, submerging in a solution of fluoroalkylsilane,
hexane and acetic H
2
O and churned up for 5 h at 250 C. Zhang also mentions that time
dependence exist on the duration of each process, resulting in different finishing of the
coating and different results in contact angle measurements.
Page 32
Lastly, polymer plating proposed by Kang [ 24 ] is also traced here. It requires
polymerization in an electrochemical cell with an aqueous solution of Na
2
CO
3
, etching in an
acid solution (HNO
3
+ H
2
O
2
) for a couple of minutes and rinse ultrasonically with water.
Kang also mentions time dependence existance in the relationship between the duration of the
processes and the final contact angle measurements.
It can be seen that the three methods found and described require some special
equipment which is not available at the moment, but can be achieved if the interest for
hydrophobicity over copper becomes even greater.
4.3 Summary.
All the plates that will be studied later on with different experimental procedures were
mentioned along this chapter, but a brief description and their codenames appear in Table 6
below. The plates that were dismissed from the beginning because of any reason are not
included in this table, which should be an easy-access guide for references.

Page 33

Codename. Description. Observations.
REF
Copper plate cleaned with alcohol and Sidol
polish.
Taken as a reference for the rest of the
plates.
R04
Copper plate buffed with the aim of R
a
= 0,4 m. Ra 0,5 m. Oriented.
R08
a
R16
a
R32
a
R04q
a
= 3,2 m. Ra 0,4 m. Non-oriented.
R08q
a
R16q
a
R32q
a
ProbeA
Copper plate coated with normal silicone. White-transparent.
ProbeB
Copper plate coated with silicone plus. Grey.
ProbeC
Copper plate coated with silicone based adhesive. Transparent.
ProbeD
Copper plate coated with silicone
hochtemperatur.
Red.
Probe2A
Copper plate coated with resinate HF8007 (Cr) +
glass powder 8465.
Dark silvered with yellow areas.
Homogeneus.
Probe2B
Copper plate coated with resinate HF8007 (Cr) +
glass powder G017-393.
Brown. Non-homogeneus but well stuck to
the substrate.
Platte1
Copper plate coated with tin. Silver coloured. Big size, hard to carry.
Platte2
Copper plate coated with zinc. Silver bluish coloured. Big size, hard to
carry.
Table 6 Codenames of all plates involved in further experiments. Dismissed ones by any reason are not
included.
Experimental procedures.
Page 34
5 Experimental procedures.
During this chapter, the description of experimental procedures which have been carried
out will be dealt with. The main objective of 3E project is finding a range of conditions that
allows the IS generator to work with the lowest ice adhesion. A theoretical description of the
parameters involved in ice adhesion were developed before (cf. page 8) and some of them are
going to be experimentally measured and discussed next.
These parameters that are going to be measured are the contact angle and the surface
energy calculated following different methods. By measuring these parameters over every
different copper plate in Table 6 a prediction about the future ice adhesion behaviour of each
plate is going to be dicussed.
5.1 Contact angle measurements.
Previously, influence of contact angle on ice adhesion was theoretically described
basing on different authors ([ 9 ] [ 19 ] [ 20 ] [ 25 ] - [ 27 ]). These literature mentions are
enough to justify the interest in measuring the contact angle over the sample plates and apply
these experimental values the results in the prediction of ice adhesion over the surfaces
analysed. Besides, determination of the surface free energy is done basing on contact angle
measurements.
Due to this fact DIN standard 55660-2 [ 28 ], which states the description of the rules
for surface free energy measurements by contact angle determination. A summary of the rules
involved in static contact angle measurements are shown below:
Minimum size of the test plates: 100 mm x 100 mm.
Avoid vibrations in the test area.
Avoid strong air flows in the test area.
An external light source can have its influence in contact angle determination.
Measurements should be done in horizontal.
Temperature range: 23 2 C.
Humidity range: 50 5 %.
Test plate must be at these ambient conditions for at least 16 h before the
measurement is done.
The needle used to drop the liquid must be 3-6 mm over the plate.
Drop volume: 2-6 l.
Results are presented with the mean value. Confusing measures caused by
external factors (i.e. dirt or rests of another liquid) can be dismissed from the
mean value.
The same cleaning pre-treatment must be applied to each plate when
comparative measurements are done, even if no dirt is observed.
Electrostatic charge must be avoided.
Page 35
Waiting time between the drop is placed and the measurement is done varies
with the viscosity of the fluid employed and should be always the same for each
comparative measurement.
Following these rules, the standard deviation of the static contact angle
measurements should not exceed 3.

Besides, some additional recomendations for dynamic contact angle measurements and
surface free energy determination are done in the same standard, which will be mentioned
later on.
Contact angle measurements were developed in Forschungzentrum Karlsruhe
(Kalsruher Institut fr Technologie - Campus Nord) under the guide of Agnes Marciniak.
There, a contact angle machine DSA100 by Krss (Figure 17) connected with a computer
where the software DSA3 for Drop shape analysis is installed.

Figure 17 Contact angle measurement equipment.
The equipment has a multi-dosing system which permits several automatic
measurements with liquids stored inside the machine and the possibility of manual dosing by
an additional syringe. Moreover, a camera installed in the left hand side of the machine
transmits the drop shape evolution to the computer where the software determines the contact
angle. Many parameters can be changed, as the measuring method or the time intervals
between each measuring step. For this experiment, static measurements were done using the
sessile drop measuring system. This method provides quick and accurate contact angle
determination which depends on liquid phase, substrate phase and ambient conditions. Further
information about the possibilities and different kind of measurements that can be done with
this equipment are described in [ 29 ] [ 30 ]. As well, [ 30 ] also details necessary
configuration of the software for the required conditions. In the measurements carried out in
FZK, a measuring template (MT) was followed so as to each measurement can be compared
Page 36
with any other one. This MT includes every property the software can customize, apart from
the already mentioned static sessile drop method. Basic physical properties of the liquids used
were selected from the program database, as well as substrate physical properties can be also
selected when pendant drop method is applied. The dosing mode selected as constant
dispensig volume of 3 l and a rate of 20 l/min. The driving mode of the system were set in
Use syringe loader [SL] only and the
deposition mode in Teach-in as
recommended by both Agnes
Marciniak and [ 30 ] due to
measurement requirements. The
distance between the needle and the
surface was hand configurated to
minimise the influence of the impact of
the drop over the test surface, that is
inside the range mentioned by [ 28 ] as
suitable: 3-6 mm. The sequence
followed by the droping system
includes a waiting time of 10 s between
the liquid first contact with the surface
and the start of the measurement. Since
the measurement process by the
software starts, 2 measurements per
second are made till 3 s. The baseline is automatically determined by the software.
For each individual contact angle measurement (see Figure 18), 6 measurements should
have been done during 3 s according to the parameter previously set and the final result
presented is the mean value of these 6 measurements. Sometimes, the DSA3 software is not
able to offer 2 measurements per second because the system does not identify correctly the
drop shape and individual mean contact angle values often are made for less than 6 time
dependent measurements. Likewise, the mean value is calculated and presented as a result for
each contact angle measurement. Besides, this procedure was not done just once for each
sample but at least four times all over the plate surface in order to avoid unique particularities
of any point, especially when irregularities due to the oxide layer distribution exist.
It seemed interesting for the 3E project to evaluate the contact angle not only with water
but with ethanol-water solutions of different ethanol concentrations. In this case, apart from
pure water measurements, they were carried out measurements with 3, 6, 9 and 12 % mass
concentration of ethanol. These can not be done in the same conditions like water
measurements and they have to be done with manually dosing using an additional syringe
placed in one slot of the multidosing system. This results in a variation of the volume droped
each time, being more irregular than with the automatic Syringe Loader system previously
configurated and it may cause inaccuracy in the measurements. Another problem during the
measurements that avoid to strictly follow the DIN 55660-2 [ 28 ] rules is the logistics. FZK
is situated outside the city and transporting the samples there is required, so they do not stay
at the ambient conditions stipulated for 16 h. Besides, some dirt or surface damage can have
Figure 18 Disposition for a contact angle measurement.
Page 37
been produced and their presence can have an influence on the contact angle values
dispersion. This supposed variation is accepted since it is not the material what is going to be
evaluated, but its prototype-like conditions to industrial applications, including damages, dirt
and oxide layer.
Apart from that, the absence neither of external light nor air flow was possible. More
workers were inside the laboratory where the DSA100 machine is placed, so light entered
inevitably through the windows and the door were opened sometimes letting air enter into the
room.
Due to these problems, the results of the contact angle measured may not be as accurate
as the DIN standard regulation states because some of the points mentioned were impossible
to fulfill.
5.2 Surface free energy.
Surface energy is related both with formation of an adhesive bond and with failure of
this adhesive bond. Determination of surface energy of a solid test surface is usually made by
contact angle measurements of a series of liquids and application of Youngs equation or any
other equation (Good-Girifalco, Wu, OWRK). An alternative way to determine the surface
energy is by the surface forces apparatus, measure based in determination of the interfacial
forces between the test surface and a reference surface when both surfaces are separated [ 9 ].
In this project, determination of the surface free energy of the solid test samples
considerated was done by measuring different contact angles resulting from the use of
different test liquids. Experimental rules are defined in abovementioned DIN 55660-2 [ 28 ]
and are also valid here, but specific advices for surface energy determination are presented
here:

At least two liquids must be used to surface energy determination through
contact angle measurements.
At least one of these liquids must have a polar component higher than 0. A
common pair of liquids employed is water and diiodmethan (or ethyl glycol).
Besides, the standard presents a list of mandatory data that should appear in a complet
report of any surface energy measurements.
Development of surface energy determination includes a first stage when contact angle
of two fluids is calculated. A special configuration for the DSA100 machine is required, using
a MT for two contact angle consecutive measurements. The liquids selected are water and
ethylene glycol, because they were already available in the machine. Their properties were
selected in the DSA3 software database. As well, contact angle was measured by static
pendant drop measurements. The dosing mode selected was constant volume with 6 l for
each liquid, with a dosing rate of 40 l/min for ethylene glycol and 20 l/min for water.
Driving mode, deposition mode and distance between needle and sample were configurated as
described before for the contact angle measurements. The sequence followed by the
measurements is quite different from previous one. The waiting time between the drop starts
Page 38
to drop and the start of the measurement is 18 s, because viscosity of ethylene glycol is much
higher than water
4
and it takes more time the drop to form and fall into the surface. Then, the
measurement process starts and 2 measurements per second are made during 15 s more, which
result in 30 independent contact angle measurements. For each measurement, the process
done was the same with one drop per liquid.
Once the contact angle measurements are done, the data obtained is processed by the
DSA3 software in order to calculate surface energy through several relationships between
contact angle, liquid properties (surface tension), Youngs equation ( 4 ) and different
estimations of the surface tension between solid and liquid phase.
Surface free energy calculation process by Fowkes divides it into two parts: polar and
dispersive component. For the dispersive component, an equation for the surface tension
between solid and liquid phase is proposed:
y
sI
= o
s
+ o
I
- 2 . o
s
+ o
I
( 13 )
Where:
sl
: surface tension between solid and liquid interface.
s
: surface energy of the solid.
l
: surface energy of the liquid.
D
: dispersive component of the surface energy solid/liquid.

Combining this with Youngs equation, the contact angle can be expressed as:
cos 0 = 2 . o
s
.
1
_c
l
D
- 1 ( 14 )
Where: : contact angle over the surface.
Representing cos against
1
_c
l
D

in a graph as shown in Graph 4 for each
independent contact angle
measurement. The straight line resulting
from the linear regression of the
measurements must go through point
(0, -1). The slope of this line is:
m = 2. o
s
( 15 )
Where the dispersive component of the surface energy,
s
D
is detemined.
For the polar component of the surface free energy, procedure is similar. The expression
proposed for the surface tension between solid and liquid interface is:

4

ethylene glycol
= 1,61 10
-2
Pa s;
water
= 8,9 . 10
-4
Pa s; Source: [ 33 ]
Graph 4 Linear regression to calculate dispersive surface
energy component [ 30 ].

Page 39
y
sI
= o
s
+ o
I
- 2. (o
s
. o
I
+o
s
P
. o
I
P
) ( 16 )
Where:
sl
: surface tension between solid and liquid interface.
s
: surface energy of the solid.
l
: surface energy of the liquid.
D
: dispersive component of the surface energy solid/liquid.
P
: polar component of the surface energy solid/liquid.

The work of adhesion can be also expressed in function of dispersive and polar
components:
w
sI
= w
sI
+w
sI
P
( 17 )
Besides, the equation from Dupr is:
w
sI
= o
s
+o
I
- y
sI
( 18 )
Combining equations ( 16 ), ( 17 ), ( 18 ) and Youngs equation ( 4 ), the polar component
of the work of adhesion can be expressed:
w
sI
P
= o
I
. (cos 0 +1) -2. o
s
. o
I
( 19 )
According to equation ( 16 ) the polar fraction of the work of adhesion is defined by the
geometric mean of the polar fractions of each surface tension involved:
w
sI
P
= 2. o
I
P
. o
s
P
( 20 )
Similarly to the dispersive component, W
sl
P
is represented against 2. o
I
P
in Graph 5,
where linear regression is drawn and the slope from the straight line resulting is:
m = o
s
P
( 21 )
And the polar component of the surface tension of the solis substrate can be
calculated. The total surface tension of the solid will be the sum of both polar and dispersive
components.

Graph 5 Linear regression to calculate polar surface energy component [ 30 ].

Page 40
Very similar to the Fowkes method is the OWRK (Owens, Wendt, Rabel, Kaelble). This
method also divides the surface energy in polar and dispersive component, but it just require
one linear regresion instead of two. Equation proposed for surface tension is ( 16 ) and
applying Youngs equation:
(1+cos0).c
l
2._c
l
D
= o
s
P
. _
c
l
P
c
l
D
+o
s
( 22 )
The equation ( 22 ) is of the form y = mx + b and can be represented like in Graph 6,
where
(1+cos 0).c
l
2._c
l
D
is shown against _
c
l
P
c
l
D
:

Graph 6 Linear regression for the OWRK surface energy determination method [ 30 ].
A linear regression is made with the values of each contact angle measurement and the
slope from the straight line resulting of this regression is:
m = o
s
P
( 23 )
Where the polar component from the surface energy can be calculated. The y-intercept
of the line is:
b = o
s
( 24 )
Where the dispersive component can be calculated.
Last method employed to surface energy calculation is by Wu. Otherwise from OWRK
and Fowkes methods which use harmonic mean value, Wu method use harmonic mean in
determination of the surface tension and it is appropiated to low surface energy systems.
Expression proposed by Wu for surface tension is:
y
sI
= o
s
+ o
I
- 4. (
c
l
D
.c
s
D
c
l
D
+c
s
D
+
c
l
P
.c
s
P
c
l
P
+c
s
P
) ( 25 )

Page 41

Combining this expression with Youngs equation:
o
I
. (cos 0 +1) -4. _
c
l
D
.c
s
D
c
l
D
+c
s
D
+
c
l
P
.c
s
P
c
l
P
+c
s
P
] = u ( 26 )
Estimation of
s
D
and
s
P
requires the solving of equation ( 26 ) for each different liquid
used in contact angle measurements. For two liquids:
(b
1
+c
1
-o
1
). o
s
. o
s
P
+c
1
. (b
1
-o
1
). o
s
+b
1
. (c
1
-o
1
). o
s
P
-o
1
. b
1
. c
1
= u ( 27 )
(b
2
+c
2
-o
2
). o
s
. o
s
P
+c
2
. (b
2
-o
2
). o
s
+b
2
. (c
2
-o
2
). o
s
P
-o
2
. b
2
. c
2
= u ( 28 )
Where:
a
1
:
1
4
. o
I,1
. (cos 0
1
+1)
b
1
:
l,1
D

c
1
:
l,1
P
a
2
:
1
4
. o
I,2
. (cos 0
2
+1)
b
2
:
l,2
D

c
1
:
l,2
P

These methods and three more are described in [ 30 ] and these three were selected
because are commonly the most used ones. The required calculations are made by the DSA3
software after the respective contact angles are measured and filtered with different
confidence levels to avoid measurement errors which can create confusing results.
Results and discussion.
Page 42
6 Results and discussion.
Following the methodology described above, both contact angle measurements and
surface energy evaluation was done.
For each surface and liquid employed, resulting data were processed in Excel building a
table where both individual measurements with its standard deviation and mean value also
including the related standard deviation. For measures clearly out of range (outliers) the
procedure was dismissing them from the mean value calculation but showing them on the
correspondent graph rounded with a red circle. As an example, one of this graphs is shown
here (Graph 7), but the rest can be consulted on the attached documents (CD).

Graph 7 Contact angle measurements of ProbeA plate with ethanol 12 % aqueous solution.
A table like Graph 7 was drawn for every surface and every liquid tested and the mean
value results with its respective standard deviation (SD) are compiled in Table 7, where
Water1 represents the measurements done a day after the previous treatment is applied and
Water2 was done with a two week time interval to study possible influence of oxide layer.
Analysing this compilation table, some conclusions can be drawn. At first, almost every
measure shows a high standard deviation, at least higher than 3 mentioned by DIN 55660-2
[ 28 ]. This can be explained by not having followed this DIN standard for the previously
detailed reasons and it is accepted because interest of these measurements is qualitative in
order to set a comparison among them.
Moreover, plate named 2B, which is resinate coated, showed great heterogeneity in its
external surface but great adhesion of the resinate coating to the substrate due to the glass
powder added. In spite of this fact, contact angle measurements were done so as to analyse the
interest of further research in this kind of coating. This interest was rejected when wetting was
observed over the surface.
75,00
80,00
85,00
90,00
95,00
100,00
1 2 3 4 5 6 7 8 9 10
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Measurement number.
ProbeA (ethanol 12 %)
Mean value
CA measurements
Page 43

Contact angle measurements[]
Water1 Water2 Ethanol 3 % Ethanol 6 % Ethanol 9 % Ethanol 12 %
Sample Mean SD Mean SD Mean SD Mean SD Mean SD Mean SD
REF 78,85 0,26 97,93 1,89 75,52 7,58 88,02 6,2 84,89 8,53 80,8 2,72
ProbeA 105,2 4,12 102 3,67 100,1 3,32 102 5,92 91,94 1,66
ProbeC 110,9 3,54 103,5 3,72 102,3 4,38 99,66 1,93 98,13 3,4
2A 109,7 7,44 104 5,76 96,79 9,28 94,17 3,62 99,59 2,49
2B 77,52 3,99 81,59 8,79 73,43 1,3
R04 73,2 4,46 92,91 6,08 94,74 1,76 94,47 1,81 101,5 1,53 93,48 3,14
R08 89,72 6,32 78,2 4,93 70,38 6,8 94,31 3,85 96,86 2,52 86,07 4,47
R16 106,1 5,51 105,7 5,26 97,78 5,42 95,51 1,84 101,2 3,65 92,64 2,91
R32 111,4 9,4 95,53 7,25 93,07 2,56 94,23 4,71 90,99 7,94 82,68 7,9
R04q 101,6 4,69 87,03 5,48 82,75 3,2 79,24 8,46 76,19 5,11
R08q 104,9 2,17 95,36 4,27 78,38 3,33 78,33 3,08 74,42 4,23
R16q 95,3 6,43 80,92 4,28 90,84 4,82 85,92 5,54 77,88 6,64
R32q 99,28 3,3 86,47 7,11 83,47 3,66 86,14 2,34 80,45 4,42
Table 7 Compilation of contact angle measurements.
Since the interest of this project is studying different plates for a prototype-like setup,
contact angle measurements made over the non-oxidised surfaces were dismissed in the
analysis. Non-oxidised surface refers to the surface one day before the treatment was
applied, when the Water1 contact angle measurements were done, despite the oxide layer
already exists. Some measurements with/without oxide layer, due to lack of time, could not be
repeated and compared. Finally, oxide layer influence were not considered over the plastic
coatings.
Another point that sould be mentioned is the way in which ethanol aqueous solutions
contact angle measurements were made. First, contact angle was determined using the ethanol
3 % m/m and the 12 % m/m aqueous solution to evaluate if ethanol concentration could be a
parameter of interest for contact angle and, therefore, ice adhesion. When these data were
analysed and the influence was observed, measurements with ethanol 6 % m/m and 9 % m/m
were done, that is, two weeks later. Thus, measurements called Water1, ethanol 3 % and
ethanol 12 % were made the same day and Water2, ethanol 6 % and ethanol 9 % were made
two weeks later.
6.1 Discussion on ethanol concentration.
Effect of the ethanol concentration on the contact angle measurement was evaluated for
the different surfaces involved in this project.
For example, for silicone coatings variation of contact angle is shown in Graph 8:
Page 44

Graph 8 Contact angle versus ethanol concentration for silicone coatings.
Clearly, contact angle decreases when ethanol is added to the test solution. Similarly,
for the resinates coating which was considered valid for this application:

Graph 9 Contact angle versus ethanol concentration for resinates coating (plate 2A).
Same correlation between contact angle and ethanol concentration is observed in Graph
9 for the resinate coated plate 2A, but for 12 % ethanol volume concentration. For the REF
plate (raw copper plate polished with Sidol), the same correlation was found, but for 3 %
ethanol volume concentration. No reason for both different behaviours was found.
The same analysis was made for both oriented and non-oriented samples for each
different roughness parameter:
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Ethanol concentration [% v/v]
Average CA vs. Ethanol concentration (Silicone coatings)
ProbeA
ProbeC
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Ethanol concentration [%v/v]
Average CA vs Ethanol concentration (2A, REF)
2A
REF
Page 45

Graph 10 Series of graphs where contact angle is represented against ethanol concentration.
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Ethanol concentration (% v/v)
R04
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
R04q
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
R08
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
R08q
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
R16
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
R16q
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
R32
60
70
80
90
100
110
120
0 3 6 9 12
C
o
n
t
a
c
t

a
n
g
l
e

[
]
R32q
Page 46
The abovementioned correlation between contact angle and ethanol concentration is
observed in any of the non-oriented plates for any of the roughnesses considered, but some
individual measurements which can be considered as exceptions or values out of range. For
the oriented plates, conclusion is more difficult to achieve. For the plates with higher
roughness parameter studied, contact angle decreases with increasing ethanol volume
concentration. For the plates with lower roughness parameter, results were confusing. R04
shows no real influence of ethanol concentration in contact angle. R08 shows a great
dispersion of the measures that leads to no conclusion. It has been stated that roughness
parameter for R08 plate is not 0,8 m, as it was the initial intention, but around 0,6 m.
Maybe by chance but it is worth mentioning that Faucheux [ 34 ] in the study of degree of
supercooling for different surface roughness parameters found that measurements for 0,8 m
showed as well great dispersion.
6.2 Discussion on the effect of oxide layer.
Two different contact angle measurements over some of the plates were done in order to
evaluate influence of the oxide layer reformation, measurements separated for two weeks.
In case of plate named REF, an increase of about 20 was found between both
measurements and no changes in colour are seen. It was demonstrated by Matsumoto [ 6 ] that
buffing results in an immediate reformation of the oxide layer. Polishing with Sidol has an
abrasive effect over the surface and that would create again the oxide layer within the period
of time between the polishing and the contact angle measurement (one day). Another possible
reason that was considered is the remaining time of the polish material over the surface,
which could have affected the first contact angle measurement. Therefore, its absence in the
second measurement has caused the so told mean contact angle difference.
Results for plate R04 were very similar in values to REF but not in surface finishing.
Oxidising over this plate has create areas of different colouring and even the drops which
were used to measure contact angle have created a ring of different colour over the surface as
can be seen in Figure 20. This plate and oriented ones were submerged for a week in an ice
slurry storage vessel for accelerating the oxide layer reformation process. Adhesive tape was
used to keep them fixed to the vessel and the right hand side of the plate in Figure 20 was
contaminated with adhesive substances. All over the rest of the surface, the different coloured
areas can be observed. The great standard deviation exisiting in R04 contact angle
measurements can be explained by this fact.
R08 results shows a little decrease between the first and the second measurement. In
Figure 19 oxidation of the surface can be observed. However, no considerable influence of the
oxide layer reformation was found in R16 contact angle measurements one day and two
weeks after the treatment was applied. As well, no considerable change in surface colour is
observed neither for R16 plate (Figure 21) nor R32 (Figure 22), but the rests of the adhesive
tape in R16 and some damaged regions or small regions affected by oxidation. A similar
decrease to R08 mean contact angle values is observed in R32 values too, very influenced by
high values of standard deviation which avoid finding a conclusion.
Page 47

Therefore, no direct correlation between oxide layer and contact angle measurements
could be found with the experimental data acquired. Further research at this point and
additional experiments may be required.
6.3 Discussion on the effect of surface roughness.
In this case, just oriented and non-oriented plates will be analysed, since information for
set conclusions for plastic or organometallic coatings is not enough. Like in the previous
discussions, contact angle measurements with pure water and several ethanol aqueous
solutions can be graphically seen below in Graph 11. As well, measurements of surface
roughness described during chapter 4 (page 18) are considered here in order to evaluate
different contact angle measurements.

Figure 20 Plate R04 after oxidising. Figure 19 Plate R08 after oxidising.
Figure 21 Plate R16 after oxidising. Figure 22 Plate R32 after oxidising.
Page 48

60,00
70,00
80,00
90,00
100,00
110,00
120,00
0,00 0,50 1,00 1,50 2,00 2,50
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Surface roughness Ra [m]
CA vs Roughness (water)
REF
Oriented
Non-oriented
60
70
80
90
100
110
120
0,00 0,50 1,00 1,50 2,00 2,50
C
o
n
t
a
c
t

a
n
g
l
e

[
]
CA vs Roughness (ethanol 3 %)
Oriented
Non-oriented
REF
60
70
80
90
100
110
120
0,00 0,50 1,00 1,50 2,00 2,50
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Oriented
Non-oriented
REF
Page 49

Graph 11 Series of graphs where contact angle is represented against surface roughness for both oriented
and non oriented copper plates.
From the graphs above, no direct correlation was found between contact angle and
surface roughness but a rough relationship involving ethanol concentration and oriented/non-
oriented copper plates. The evolution of the points in the whole series of graphs shows that
oriented plates have higher contact angles than non-oriented when ethanol concentration is
higher than when this concentration is lower for any surface roughness parameter.
This different behaviour both depending on orientation and on roughness itself may be
explained by the wetting transition. This process occurs during the stability of the drop over
the surface, starting like in the Cassie-Baxter model and changing to the Wenzel model as the
air pockets become thermodynamically unstable. Nucleation of the liquid in air holes is
produced and the drop spreads from a mushroom-like state to the final result. This process is
complex and requires time, resulting in irregularities in the measurement of contact angle
when surface roughness is considered as the main parameter. As well, surface roughness
60
70
80
90
100
110
120
0,00 0,50 1,00 1,50 2,00 2,50
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Oriented
Non-oriented
REF
60
70
80
90
100
110
120
0,00 0,50 1,00 1,50 2,00 2,50
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Oriented
Non-oriented
REF
Page 50
(oriented or non-oriented) was made manually over the surface and homogeneity of the result
is not ensured.

Finally, in the following graph, not a conclusion but a curiosity is set out:

Graph 12 Contact angle vs surface roughness for every oriented plates measuring conditions.

Representing every copper plate over which contact angle was measured in the same
graph and including (false)
5
lines that go from one point to another results in an interesting
result. Every line drawn over the graph in Graph 12 have almost the same tendency at the
same roughness value. In fact, lines can be paired up by most similar shape: OrientedWATER
and OrientedE3, OrientedE9 and Oriented E12; remaining OrientedE6 unpaired. An
explanation to this behaviour has not been found by the author and interest of this graph is
mainly proposing this explanation as subject for further experimental research.
Comparison with non-oriented plates is also made at this point. In Graph 13 can be seen
that no every liquid droplet creates the same shape as it was created in oriented copper plates.
However, the pairs abovementioned also have similar shape in this case.

5
The autor is aware that these lines do not strictly exist as intermediate values have not been measured.
69,00
74,00
79,00
84,00
89,00
94,00
99,00
104,00
109,00
0,00 0,20 0,40 0,60 0,80 1,00 1,20 1,40 1,60
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Oriented plates at different ethanol concentrations
OrientedWATER
OrientedE3
OrientedE6
OrientedE9
OrientedE12
Page 51

Graph 13 Contact angle vs surface roughness for every non-oriented plates measuring conditions.

6.4 Surface energy results.
It was detailed the three methods that were used to calculate surface energy: Fowkes,
OWRK and Wu. The calculation of the final value is made by the DSA3 software itself when
the static contact angle is measured and a report can be obtained for filing the results.
Results of each report, including the contact angles measured with water (CA_W) and
ethylene glycol (CA_EG) are shown in Table 8, including the division made between polar
and dispersive component.
In this table, it can be checked the different results obtained with both OWRK and Wu
methods and the results obtained by Fowkes. Recommendations by the manufacturer, Krss,
shows that OWRK method is considered to be accurate for surfaces with moderate polarity,
which is the case of this project. Wu and Fowkes are highly recommended for applications in
which substrates with high surface energy are involved.

70
75
80
85
90
95
100
105
110
0 0,2 0,4 0,6 0,8 1 1,2 1,4 1,6 1,8
C
o
n
t
a
c
t

a
n
g
l
e

[
]
Non-oriented plates at different ethanol concentrations
Non-orientedWater
Non-orientedE3
Non-orientedE6
Non-orientedE9
Non-orientedE12
Page 52
Surface free energy [mN/m]
Sample OWRK method Wu method Fowkes method
CA_W CA_EG
Polar Disp Total Polar Disp Total Polar Disp Total
REF 3,7 20,3 24 7,7 21 28,7 9 8,1 17,1 92,7 87,9
ProbeA 0 27,1 27,1 0 27,2 27,2 1,6 10,8 12,4 109,5 78,6
0,3 24,1 24,4 1,9 24,4 26,3 2,9 9,6 12,5 105,5 82,6
Mean 0,15 25,6 25,75 0,95 25,8 26,75 2,25 10,2 12,45
ProbeC 0,8 24,4 25,2 3,4 24,7 28,1 4,3 9,7 14 101 82,1
1,4 29,1 30,5 4,7 29,1 33,8 6,1 11,6 17,7 94,5 76,1
Mean 1,1 26,75 27,85 4,05 26,9 30,95 5,2 10,65 15,85
2A 0,1 30,8 30,9 1,4 30,8 32,2 2,8 12,3 15,1 103 73,9
1 18,3 19,3 3,6 19,2 22,8 4,2 7,3 11,5 104,7 90,9
Mean 0,55 24,55 25,1 2,5 25 27,5 3,5 9,8 13,3
R04 1,4 13,7 15,1 4,3 15,3 19,6 4,4 5,5 9,9 106,8 98,5
3,9 8,1 12 7,6 10,5 18,1 7,1 3,2 10,3 104,3 110,2
Mean 2,65 10,9 13,55 5,95 12,9 18,85 5,75 4,35 10,1
R08 0,1 38,8 38,9 1,8 39,6 41,4 3,4 15,5 18,9 97,7 64,3
4,9 15,7 20,6 9 17,1 26,1 10,1 6,3 16,4 93,2 95
Mean 2,5 27,25 29,75 5,4 28,35 33,75 6,75 10,9 17,65
R16 2,3 14,6 16,9 5,6 16,1 21,7 5,9 5,8 11,7 102,4 96,9
1,4 16,9 18,3 4,2 18 22,2 4,7 6,7 11,4 104,1 93,1
Mean 1,85 15,75 17,6 4,9 17,05 21,95 5,3 6,25 11,55
R32 0,2 30 30,2 1,6 30 31,6 2,9 12 14,9 102,7 74,9
R04q 1,6 29,1 30,7 5 29,2 34,2 6,5 11,6 18,1 93,6 76
R08q 1,8 57,8 59,6 6,8 67,9 74,7 10,1 23 33,1 76,2 41,5
7,3 36,8 44,1 12,5 37,2 49,7 17,3 14,7 32 72,1 66,7
Mean 4,55 47,3 51,85 9,65 52,55 62,2 13,7 18,85 32,55
R16q 0 42,6 42,6 1,3 44,2 45,5 3,1 17 20,1 97,3 59,9
1,2 22,4 23,6 4,1 22,8 26,9 4,9 8,9 13,8 100,4 84,9
Mean 0,6 32,5 33,1 2,7 33,5 36,2 4 12,95 16,95
R32q 2,3 22,3 24,6 5,9 22,8 28,7 7 8,9 15,9 95,7 85
Table 8 Compilation of surface energy values.
When two measurements have been done and accepted as valid (considering previous
results for contact angle), the mean value was calculated and highlighted in Table 8.
It is interesting to represent surface energy of copper plates against surface roughness to
evaluate the relationship between both magnitudes as it has been done with contact angle.
This graph is shown in Graph 14. Again, no direct correlation was found between surface
energy and surface roughness parameter. For measurements over plates with a surface
Page 53
roughness parameter between 0,5 m and 1 m, the standard deviation obtained was very
high.

Graph 14 Study of the influence of surface roughness of oriented and non-oriented copper plates on
surface energy determined by measurements of the contact angle.
As well, results were classified from lowest surface energy to highest:

Surface free energy
R04 13,55 2,19 [mN/m]
R16 17,6 0,99 [mN/m]
REF 24 0,00 [mN/m]
R32q 24,6 0,00 [mN/m]
2A 25,1 8,20 [mN/m]
ProbeA 25,75 1,91 [mN/m]
ProbeC 27,85 3,75 [mN/m]
R08 29,75 12,94 [mN/m]
R32 30,2 0,00 [mN/m]
R04q 30,7 0,00 [mN/m]
R16q 33,1 13,44 [mN/m]
Platte1 46,2 0,00 [mN/m]
R08q 51,85 10,96 [mN/m]
Table 9 Surface energy values from lowest to highest.

0,00
10,00
20,00
30,00
40,00
50,00
60,00
70,00
0,00 0,20 0,40 0,60 0,80 1,00 1,20 1,40 1,60 1,80
S
u
r
f
a
c
e

e
n
e
r
g
y

[
m
N
/
m
]
Surface roughness [m]
Surface energy vs surface roughness
REF
Oriented
Non-oriented
Page 54
6.5 Polarity results.
Polarity of a surface can be calculated as:
_
P
=
y
s
P
y
s
( 29 )
Polarity was evaluated basing on the data obtained from the OWRK surface energy
measurements. A comparison between the polarity values for each plate and their surface
roughness parameter is done in Graph 15 below:

Graph 15 Polarity vs surface roughness for oriented and non-oriented copper plates.
A rough correlation between decreasing polarity and increasing surface roughness can
be determined in case of oriented copper plates, but no other conclusion can be observed.
Similarly, comparing polarity with the resulting water contact angle measured for the surface
energy calculation (CA_W in Table 8):

Graph 16 Contact angle measurements compared with polarity for every surface studied.
0,00
0,05
0,10
0,15
0,20
0,25
0,00 0,50 1,00 1,50 2,00 2,50
P
o
l
a
r
i
t
y
Surface roughness [m]
Polarity vs surface roughness
REF
Oriented
Non-oriented
60
65
70
75
80
85
90
95
100
105
110
0,000 0,050 0,100 0,150 0,200 0,250
C
o
n
t
a
c
t

a
n
g
l
e
Polarity
Contact angle vs Polarity
REF
Plastic coatings
Organometallic coatings
Oriented plates
Non-oriented plates
Page 55
Highest contact angle values are those related with lowest polarity values,
corresponding to those plates which would have lowest ice adhesion following study of
polarity made by Zwieg [ 19 ].
6.6 Supercooling degree.
Faucheux [ 34 ] [ 38 ] found that just influence of surface roughness can be considered
when degree of supercooling is analysed in a freezing process of an ethanol aqueous solution
over both nickel and aluminium surfaces. Other parameters were found as negligible and a
quantitative correlation was determined for evaluating the mean degree of supercooling for
both materials. These correlations are going to be used here to predict an initial degree of
supercooling that may be useful to start experimentation on the test rig with real conditions:
For nickel plates, experimental equation for the supercooling degree is [ 34 ]:
AI1 (C) = 12,67S . R
u
-0,047
( 30 )
Where:
T1: Degree of supercooling over nickel plates.
Ra: Arithmetical mean deviation of the surface roughness.
For aluminium copper plates [ 38 ]:
AI2 (C) = 7,1S . R
u
-0,196
( 31 )
Where:
T2: Degree of supercooling over aluminium plates.
Ra: Arithmetical mean deviation of the surface roughness.
For the studied copper plates, the results are shown in :
Reference
Surf.
Roughn.
[m]
T1
[C]
T2
[C]
REF
0,1 14,12 11,23
R04
0,48 13,12 8,26
R08
0,59 12,99 7,93
R16
0,86 12,77 7,36
R32
1,41 12,47 6,68
R04q
0,36 13,30 8,74
R08q
0,59 12,99 7,93
R16q
1,09 12,62 7,03
R32q
1,56 12,41 6,55
Table 10 Supercooling degree calculated according to Faucheux.
Despite none of the plates considered were from nickel or aluminium, these
supercooling degree values can be assumed as a rough approximation when starting
measurements in the test rig, not as a prediction because of the obvious difference in each
substrate material.
Conclusions.
Page 56
7 Conclusions.
Developing an IS generator which can improve reliability and decrease in both
investment and operational costs is the main objective of 3E doctoral thesis by
Dipl.-Ing. (FH) Susanne Frank. Demonstrating that there is a combination of flow conditions,
heat exchanger surface, ice and additives content and degree of supercooling which result in a
controllated process of crystallisation inside a heat exchanger could lead to the development
the mentioned IS generator. This kind of generator would boost the expansion of IS
technology, since it avoid the main disadvantages of its industrial application, preserving
current advantages.
In particular, this project has dealt with the study of different surfaces which can be
employed in the abovementioned HX. That means both achieving the desired surface
finishings and coatings and predicting the future behaviour of each plate basing on determined
experimental parameters, which are considered as fundamental in (ice) adhesion study.
At first, some tasks were made in the test platform where the heat exchanger-IS
generator is placed. Existing leakage in the HX leads to a basic redesign of it and some
additional ideas (stirrer, cover, valves) were proposed for future development. As well, a new
heat exchanger was designed and its manufacturing was not completed. Other laboratory
works as insulating or study of a handheld refractometer were done. These tasks are important
in order to improve the general working conditions of the test platform.
Then, modifying the surface finishing of the test plates was tried. Different surface
roughness states were achieved over copper substrates by abrasive polishing (sandpapers).
Despite a predetermined roughness parameter was set, measurements of it showed a
difference between the initial supposition and the real values of it for each plate. The results
of the measurements are presented throughout this project. As well, trying to achieve that
different coatings stuck to the copper substrate was one of the works done. Four different
plastic coatings were successfully stuck to the substrate, but two failed. Besides, these plastic
coatings were submerged in ice slurry flowing to evaluate its resistance to a constant flow and
no problem was observed during a week. A metallic coating was also tried by covering the
copper substrate with a silver layer using the silver mirror experimental deposition (Tollens
reaction). Experiment failed and no homogeneity adhesion of silver to the substrate was
observed as it exist when the experiment is done over glass. Organometallic coatings were
also studied by trying to coat the substrate with different metal powders dissolved in organic
rosins. At first, the needed procedure was found by a literature survey but no correlation
between the predicted and actual results occured. Addition of glass powders to the organic
mixture helped in achieving a better degree of adhesion of the metallic layer to the substrate,
but heterogeneity of the external surface was not suitable for the requirements, except in one
case.
As well, literature search for achieving a superhydrophobic surface finishing over
copper substrate was made, but procedures and materials required were not easy to find and
every process was dismissed. However, further research at this point is recommended in the
future.
Conclusions.
Page 57
According to the literature survey made about crystallisation and ice adhesion over
different surfaces, both surface energy [ 31 ] and polarity [ 19 ] are the most relevant
parameters in ice adhesion prediction. As well, contact angle is also found as importat
because of its relationship in surface energy determination. Besides, some authors [ 20 ] [ 21]
found a correlation between high contact angle values, that is (super)hydrophobicity, and low
ice adhesion observed or even low shear stress between ice and substrate despite adhesion
exists.
An opportunity for measuring contact angle existed and experimental procedure for
these measurements is explained in this project. As well, data obtained are presented
throughout this document.
Influence of ethanol concentration in contact angle measured is discussed along the
project, resulting in an experimental correlation between increasing ethanol concentration and
decreasing contact angle. Not every result confirms that correlation, as copper plates with
lowest surface roughness parameter that had been buffed following the same direction did not
fulfill it. No apparent reason was found for this behaviour, but irregulaties in the formation of
the oxide layer over these two plates (references R04 and R08 in Table 6, which can be seen
in Figure 20 and Figure 19, respectively) was supposed to be closely related to it.
It was read in reference [ 6 ] that the oxide layer has a great influence as pure copper Cu
of the substrate becomes Cu
2
O, which affect directly to the intermolecular forces that are
involved in ice adhesion. This influence means a change in surface energy and, therefore, in
contact angle measured before, meanwhile and after the oxide layer formation process. The
same reference states that buffing a surface is an invalid way to remove oxide layer, since the
heat transferred to the plate during the process helps in oxide layer reformation, which occurs
almost immediately, contrasting with the 90 days that may last the reformation when removal
of the oxide layer is done by other methods. However, most of the buffed plates studied in
this project showed a difference in contact angle measurements between the moment in which
the buffing was done and two weeks later. This difference was also observed in the colour that
surface of the plates got. No explanation was found for this behaviour which do not agree
statements by Matsumoto over oxide layer reformation over copper substrates. Besides, areas
of different colours (related to oxide reformation) were observed in low roughness oriented
plates R04 (Figure 20) and R08 (Figure 19) without no apparent explanation. Possible
reasons that were considered are related to the presence of some external compound that
could vary the oxide layer formation in these areas. As well, these different coloured areas are
seen as a reason for the dispersion in contact angles measurements that led to not fulfilling the
correlation ethanol concentration and contact angle.

Contact angle was also evaluated in relation to surface roughness arithmetical average
value R
a
. No direct correlation between both magnitudes was found for each of the liquids
employed (aqueous solutions of different ethanol concentration). However, some interesting
conclusions can be extracted of the graphs (Graph 11). Increasing ethanol concentration, non
oriented plates are more affected in their contact angle measurements than oriented plates. It
can be seen in Graph 12 the particularities on the results obtained with oriented plates and all

Page 58
the range of ethanol concentrations in contact angle measurements. Intermediate
measurements would be required to evaluate if this relationship is incidental or not.
Following different methods and basing in individual contact angle measurements with
water and ethylene glycol, surface energy was evaluated, both polar and dispersive
component. It should be mentioned that contact angle measurement of each plate (at least for
water) does not always correspond to the mean value previously determined. For its interest in
the range of this project (low surface energy), OWRK method was selected as the most valid
for the analysis of the results. A classification from the lowest to the highest value of surface
energy was made and also a graph comparing several values with its correspondant surface
roughness and obtaining no clear correlation. Most of the copper plates whose roughness was
modified have similar surface energy, but some exceptions.
Basing on this measurements, polarity was calculated and represented in two graphs
agains surface roughness and contact angle. No correlation was found between surface
roughness and polarity of each surface, but there is a coincidence between lowest values of
polarity determined by OWRK method and highest values of water contact angle measured
over the plates, except from two plates (R04 and R16).
Finally, a possible degree of supercooling for future experimental procedures was
estimated using equations proposed by Faucheux [ 34 ] [ 38 ] for nickel and aluminium plates
basing in arithmetical average of surface roughness, R
a
. Copper plates differ from both
mentioned materials, but this step should be understood as a first approach to experimental
tests on the IS generator.
From the experimental tests done, it is not clear which conditions will fulfill better IS
generator requirements, so further research is needed.
Both plastic coatings results were good enough to consider its study in prototype
conditions as they have shown high contact angle (hydrophobicity), good sticking to the
substrate, low polarity and acceptable values of surface roughness. Visually, little holes can
be seen over ProbeC, so ProbeA may have better homogeneity, but ProbeC showed higher
experimental hydrophobicity.
Despite experimental results for resinate coated plate 2A were more than acceptable, the
coating generated still has some problems as the sticking over the surface presents
irregularities. Another heat treating may be necessary to achieve better adhesion of the
chromium layer.
Oriented and non-oriented plates showed a high variability in their properties. None of
the plates measured present homogeneous results for contact angle, surface energy and
polarity tests, as many deviations have been produced. Dismissing polarity, plate R16 showed
a great behaviour in the other fields, but the author of this project cannot be sure of the
influence of the polarity comparing it with surface energy. As a rough recommendation
observing experimental data obtained during this project, a copper plate with a surface
roughness parameter R
a
1 m should lead to the best results in avoiding ice adhesion, but
this prediction may not be right due to the low correlation found in every test.

Bibliography
Page 59
8 Bibliography
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and engineering. Paris: International Institute of Refrigeration (IIR guides), 2005.

[ 2 ] S. Frank, M. Kind, M. Kauffeld. Optimization of ice slurry production with the right
heat transfer surface. Hochschule Karlsruhe, 2010.

[ 3 ] M. Domnguez Prez. Determinacin de propiedades fsicas a 25 C para los sistemas:
propanoato de propilo + hexano + etilbenceno, + o-xileno, + m-xileno, + p-xileno,
dissertation. A Corua, enero 2006.

[ 4 ] Carl L. Yaws, Thermophysical properties of chemicals and hydrocarbons, William
Andrew Inc., Norwich, New York, 2008.

[ 5 ] http://www.engineeringtoolbox.com, values of thermal conductivity coefficient of some
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[ 6 ] K. Matsumoto, M. Morohoshi, Y. Teraoka, Fundamental study of adhesion of ice to
cooling solid surface: discussion on influence of copper oxide layer on ice adhesion force,
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[ 7 ] International Organization for Standardization. Coated abrasives Grain size
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[ 8 ] Deutsches Institut fr Normung. Measurement of roughness average Ra and peak
count RPc on metallic flat products, DIN EN 10049:2005.

[ 9 ] D.E. Packham. Surface energy, surface topography and adhesion. International Journal
of Adhesion and Adhesives, 23 (6), pp. 437-448, 2003.

[ 10 ] Deram, V., Turrell, S., Darque-Ceretti, E., Aucouturier, M. Study of "liquid gold"
coatings: Thermal decomposition and formation of metallic thin films. Thin Solid
Films, 515 (1), pp. 254-259, January 2006.

[ 11 ] J. N. Borglin, P. R. Mosher, H. A. Elliott. Fused Metal Resinates. Ind. Eng.
Chem., 36 (8), pp 752756, August 1944.

[ 12 ] William E. St. Clair, J. C. Minor, Ray V. Lawrence. Fused Metal Resinates from
Aldehyde-Modified Rosin. Ind. Eng. Chem., 46 (9), pp 19731976, September 1954.

[ 13 ] B. Walton. Principles of thick film materials formulation. IERE Conference on Hybrid
microelectronics, Canterbury, September 1973.

[ 14 ] Trelleborg group. Trelleborg O-rings catalog. 2008.
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[ 15 ] http://www.misco.com/traditional.php: Description of a traditional HR.

[ 16 ] World Health Organization. Methyl Ethyl Ketone: enviromental health criteria.
Geneva, 1993.

[ 17 ] http://www.periodic-table.org.uk/element-zinc.htm: Properties of zinc.

[ 18 ] http://www.periodic-table.org.uk/element-tin.htm: Properties of tin.

[ 19 ] T. Zwieg. Biomimetical ice nucleating coatings, dissertation. Dresden, april 2006.

[ 20 ] A. Dotan, H. Dodiuk, C. Laforte, S. Kenig. The relationship between water wetting
and ice adhesion. Journal of Adhesion Science and Technology, vol. 23, pp. 19071915,
2009.

[ 21 ] D.K. Sarkar, M. Farzaneh. Superhydrophobic Coatings with Reduced Ice Adhesion.
Journal of Adhesion Science and Technology, Volume 23, Number 9, 2009 , pp. 1215-1237
(23).

[ 22 ] Zhiguang Guo, Jian Fang, Libo Wang, Weimin Liu. Fabrication of
superhydrophobic copper by wet chemical reaction. Thin Solid Films 515 (2007) 71907194.

[ 23 ] Youfa Zhang, Xinquan Yu, Quanhui Zhou, Feng Chen, Kangning Li. Fabrication
of superhydrophobic copper surface with ultra-low water roll angle. Applied Surface Science
256 (2010) 18831887.

[ 24 ] Zhixin Kang, Qi Ye, Jing Sang, Yuanyuan Li. Fabrication of super-hydrophobic
surface on copper surface by polymer plating. Journal of Materials Processing Technology
209 (2009) 45434547.

[ 25 ] L.-O. Andersson. Ice Adhesion to rubber materials. J. Adhesion Sci. Technol., vol. 8,
pp. 117-132, 1994.

[ 26 ] W.D. Bascom, R.L. Cottington, C.R. Singleterry. Ice adhesion to hydrophillic and
hydrophobic surfaces. J. Adhesion, Vol. 1, No. 10, 246-263, 1969.

[ 27 ] C.A. Knight. Experiments on the contact angle of water on ice. Philosophical
Magazine, 23:181, 153165, 1971.

[ 28 ] Deutsches Institut fr Normung. Wettability Part 2:Determination of the free
surface energy of solid surfaces by measuring the contact angle, DIN 55660-2.
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[ 29 ] Krss GmbH. DSA100 Handbook.

[ 30 ] Krss GmbH. DSA3 Handbuch: Software zur Tropfenkonturanalyse. Hamburg, 2009.

[ 31 ] K. Matsumoto, T. Kobayashi. Fundamental study on adhesion of ice to cooling solid
surface. International Journal of Refrigeration, vol. 30, pp. 851-860, August 2007.

[ 32 ] S. Wu. Polar and nonpolar interactions in adhesion. The Journal of Adhesion, vol. 5,
pp. 3955, 1973.

[ 33 ] www.wolframalpha.com. Viscosity values for ethylene glycol and water.

[ 34 ] M. Faucheux, M. Havet, A. LeBail. Impact of the roughness of a nickel metallic
surface in the supercooling degree of a water-ethanol aqueous solution. 7th Conference on
Phase-Change Materials and Slurries. Dinan, France, September 2006, Paris: International
Institute of Refrigeration.

[ 35 ] Henning Gleich. Zusammenhang zwischen Oberflchenenergie und
Adhsionsvermgen von Polymerwerkstoffen am Beispiel von PP und PBT und deren
Beeinflussung durch die Niederdruck-Plasmatechnologie, dissertation. Duisburg-Essen, 2004.

[ 36 ] Seiji Okawa, Akio Saito, Tatsuyuki Matsui. Nucleation of supercooled water on solid
surfaces. International Journal of Refrigeration, 29, 134-141, August 2005.

[ 37 ] Koji Matsumoto, Yuya Daikoku. Fundamental study on adhesion of ice to solid
surface: discussion on coupling of nano-scale field with macro-scale field. International
Journal of Refrigeration, 32, 444-453, 2009.

[ 38 ] M. Faucheux, G. Muller, M. Havet, A. LeBail. Influence of surface roughness on the
supercooling degree: Case of selected water/ethanol solutions frozen on aluminium surfaces.
International Journal of Refrigeration, vol. 29, pp. 12181224, November 2006.

[ 39 ] K. Matsumoto, T. Akimoto, Y. Teraoka. Study of scraping force of ice growing on
cooling solid surface. International Journal of Refrigeration, vol. 33, pp. 419427, March
2010.

[ 40 ] S. Okawa, A. Saito, H. Suto. The experimental study on freezing of supercooled water
using metallic surface. International Journal of Refrigeration, vol. 25, pp. 514520, August
2002.

[ 41 ] ke Melinder. Thermophysical Properties of Aqueous Solutions Used as Secondary
Working Fluids, dissertation. Stockholm, 2007.

[ 42 ] Wikimedia Commons.
Appendixes
Page 62
9 Appendixes

9.1 Appendix A: Refractometer
9.1.1 Introduction
Hand refractometers (HR from now on) are often used to measure percentage of
volume/volume concentration on a wide variety of mixtures knowing the fact that refractive
index varies proportionally with the variation of molar fraction of each component. Each
refractometer suits each use, as refractive index variation depends not only on concentration
but also on the temperature and components involved.
The measuring of the refractive index of a mixture with a HR is based on evaluating
total internal reflection angle, the angle formed by the ray of light approaching a surface with
respect to the normal to the surface when no refraction occurs. A measuring prism and a
reticle are passed through by the reflected ray, which is projected over a graduated scale,
related to the components involved. HR often have a bi-metallic strip acting as a temperature
auto-calibration, moving the lens proportionally to temperature changes. If not, calibration
tables are provided by manufacturer [ 15 ].
At the present day, on our laboratory, a hand refractometer is employed in order to
measure ethanol concentration in aqueous solutions (carrier fluid of ice slurry mixtures)
running in several experiments. From experience at this field it is shown that refractometer
measurements are not reliable at all right now and a simple test can prove this statement at
any time. As well, ethanol used in experiments is not pure ethanol, but ethanol with additives
for laboratory use only.
Aim of this report is trying to find a reason which can explain this wrong behaviour, as
well as getting to a solution to ease quick and practical ethanol concentration measurements.
9.1.2 Theoretical approach
As refractive index is a physical property of each pure substance, hand refractometers
used in measuring mixture concentrations work with the variation of this property in a
determined mixture to evaluate determined concentrations in the mixture, under determined
ambient conditions.
It has been said that a hand-held refractometer is used in our laboratory to measure
ethanol concentration in aqueous solutions. Despite of the fact that it was made to measure
sugar content, measuring ethanol concentrations up to 25 % is also possible and the
measurements should be quite accurate only at 20 C, since temperature calibration tables for
sugar content are no good for ethanol mixtures.
Also, because of higher taxes for ethanol used in spirituous beverages, ethanol commercially
obtained for laboratory work contains a unhealthy [ 16 ] component called methyl ethyl
ketone (MEK from now on) in low concentrations: around 1 % v/v. Despite this low
Appendixes
Page 63
concentration, presence of methyl ethyl ketone is also pointed as a possible part of the wrong
HR measurements.
Thus, studying refractive index variations in ternary systems (ethanol, MEK in aqueous
solution) becomes necessary. Literature survey over this topic proves that this theoretical
study, especially with organic compounds involved, is too complex for dealing with it deeply
in this report, as its objective is mainly practical.
Finding a valid reference for the components involved was not possible, as well as
facing the problem in its complexity, so following the reference [ 3 ] main aspects of it will be
exposed below:
9.1.2.1 Refractive index variation in ternary systems:
Most of the literature references consulted (for example, reference [ 3 ]) develops the
study about the topic comparing the results obtained by experimental measurements in
laboratory with theoretical results provided by prediction equations, evaluating which one fits
better the conditions under focus.
Due to complexity in liquid state analysis, study of physical properties in liquid
mixtures is made by the determination of the deviation between physical properties under
study and ideal values of them, excess functions, whose general expression in a mixture is
developed below:
AH
mx
R
= H- _ n

. H
m
( 32 )
Where:
M
R
mix
: function for the real mixture
M: function for the solution
M
i
m
: function for each pure substance
n
i
: number of moles
Similarly, for each ideal property, function of the ideal mixture can be calculated:
AH
mx
I
= H
I
- _
. H
m
( 33 )
Where:
M
I
mix
: function for the ideal mixture
M: function for the solution
M
i
m
: function for each pure substance
i
: number of moles
Consequently, the general expression for the excess function of each physical property:
H
L
= AH
mx
R
- AH
mx
I
= H-H
I
( 34 )
Where:
M
E
: excess function of a mixture
M
R
mix
: variation of the function for the real mixture
M
I
mix
: variation of the function for the ideal mixture
M: real value of the physical property
M
I
: value of the physical property following Raoult law
Appendixes
Page 64
Great algebraic complexity involves applying directly the equation to a mixture (it
requires calculating an activity coefficient) and, often, results are not accurate enough.
Usually, empirical methods are used to ease the process. Particularly, for refractive index:
n
L
= n
mx
R
- n
mx
I
= n
mx
R
- _ _
. n

( 35 )

Where:
n
R
mix
:refractive index for the real mixture
n
I
mix
: refractive index for the ideal mixture
i
: molar fraction
n
i
: refractive index of the pure component

Whenever no chemical reaction between the components has occurred, deviation of real
values obtained from the ideal ones is justified by the existence of intermolecular forces:
electrostatic forces (van der Waals), induction forces (polarity), London dispersion forces and
specific chemical forces (hydrogen bond). A deeper chemical approach at this point would be
necessary to understand completely the already mentioned deviation.
Even so, theoretical prediction of a physical property of a mixture is nowadays
impossible, but with empirical prediction equations by different authors. The error committed
using one of these equations should not be significant until third or four decimal, which is
accurate enough for most of the applications.
In particular, for prediction of refractive index in ternary systems, equations are based in:
n
123
L
= n
bn
L
+ n
tc
L
= n
12
L
+ n
13
L
+ n
23
L
+ n
tc
L
( 36 )
Where:
n
E
123
: refractive index of the mixture
n
E
bin
: refractive index associated at the binary mixtures
n
E
ter
: refractive index associated at the ternary mixture
n
E
ij
: refractive index of each binary mixture
Prediction empirical equations are divided in symmetrical and asymmetrical, but there
is no valid criterion in order to choose among them but compare several results with
experimental ones. The difference between symmetrical and asymmetrical prediction
equations lies on the order in which components are added to the solution (asymmetrical) or
randomly added and considering no influence at this point (symmetrical).
Parameters which affect directly to numerical evaluation of most of the typical
prediction equations are density of pure substances and of the mixture itself, acentric factor,
molar fraction, molar weight and ambient conditions.
9.1.3 Experimental approach
In order to define the error committed when using the laboratorys hand-held
refractometer, a simple experiment was prepared using the following material:
- Hand-held refractometer by Greiner Glasinstrumente GMBH.
Appendixes
Page 65
- Ethanol 70 % v/v provided by Carl Roth.
- Ethanol 99 % v/v provided by Scharr.
As the work developed in the laboratory does not exceed 12 % v/v of ethanol and the
ethanol is provided both 70 % v/v concentration (with 29 % water and 1 % MEK,
approximate values as many additives appear on the component list) and 99 % v/v (with 1 %
MEK and no additives). This volume composition was changed to mass composition using
the following formula:
%
m
i
m
=
%
. M
i
_ %
. M
] ]
( 37 )
Where:
% m
i
/m: mass concentration of component i
% v
i
/v: volume concentration of component i
M
i
: molar mass of component i
% v
j
/v: volume concentration of each component j
M
i
: molar mass of each component j

Thus, mass composition of each ethanol solution used is:

Solution composition v/v

Solution composition m/m
70,00 % ethanol

84,43 % ethanol
29,00 % water

13,68 % water
1,00 % MEK

1,89 % MEK
Table 11 Volume to mass concentration change of ethanol 70 % by Carl Roth.
Solution composition v/v

Solution composition m/m
99,00 % ethanol

98,44 % ethanol
0,00 % water

0,00 % water
1,00 % MEK

1,56 % MEK
Table 12 Volume to mass concentration change of ethanol 99 % by Scharr.

Six samples of 15 g of solution were prepared with each solution in order to evaluate
the relationship between the real ethanol concentration known from the solution preparation
and the ethanol concentration measured by the HR. For the preparation of the samples, the
precision balance PG5002-S by Mettler Toledo was used with a minimum resolution of
0,01 g. At first, needed mass of each solution was determined basing in Table 11 or Table 12
to achieve 2, 4, 6, 8, 10, 12 % of pure ethanol volume concentration in each sample. Then,
water was added until 15 g were reached in each case. Finally, the masses used for each
sample are presented and explained in the following Table 13 and Table 14, representing the
data employed for the experiment done with ethanol 70 % by Carl Roth and ethanol 99 % by
Scharr, respectively:

Appendixes
Page 66
#
Mass
solution
(g)
Mass
MEK
(g)
Mass
ethanol
(g)
Mass water
(total)
(g)
1 0,43 0,008 0,36 14,63
2 0,86 0,016 0,73 14,26
3 1,29 0,024 1,09 13,88
4 1,71 0,032 1,44 13,52
5 2,14 0,040 1,81 13,15
6 2,57 0,048 2,17 12,78
Table 13 Samples prepared with ethanol 70 % solution by Carl Roth.

#
Mass
solution
(g)
Mass
MEK
(g)
Mass
ethanol
(g)
Mass water
(total)
(g)
1 0,30 0,004 0,29 14,70
2 0,61 0,009 0,60 14,39
3 0,91 0,014 0,90 14,09
4 1,21 0,019 1,19 13,79
5 1,52 0,024 1,50 13,48
6 1,83 0,028 1,80 13,17
Table 14 Samples prepared with ethanol 99 % by Scharr.
Where:
Mass solution: mass of the ethanol solution used in the preparation of each sample. It
contains pure ethanol, MEK and water (in case of Carls Roths).
Mass MEK: Mass concentration m
MEK
/m * Mass solution
Mass ethanol: Mass concentration m
ethanol
/m * Mass solution
Mass water (total): mass of water including water of the ethanol solution used (in case of Carl
Roths).
The experiment was executed and results were graphically analysed in order to achieve
an equation relating real ethanol concentration in the prepared solution and the value
measured by the HR. As HR measures concentration, we need to evaluate concentration of
ethanol on the mass already prepared solutions:
Appendixes
Page 67
Conccntrotion
=
voIumc o] thc componcnt
1otuI oIumc o] thc mxtuc
j
l
l
, [ ( 38 )
Since volumetric composition of the ethanol solution used and total mass involved is
known, as well as molecular masses and density of pure substances (reference [ 4 ]). From
now on, concentration of a component will be named by the name of the component in
between of square brackets:

|Etbonol] =
1otuI cthunoI muss noIcd
cnst o] puc cthunoI
,
1otuI muss o] thc mxtuc
cnst o] thc mxtuc
,
( 39 )
Experiments were carried out at ambient temperature, that is 20 C. Tables by ke
Melinder [ 41 ] shows the variation of the density solution with ethanol mass concentration in
aqueous solutions:

2 %
ethanol
4 %
ethanol
6 %
ethanol
8 %
ethanol
10 %
ethanol
12 %
ethanol
Density
of the
solution
(g/cm
3
)
0,995 0,99 0,988 0,985 0,982 0,98
Table 15 Densities at several ethanol mass concentrations at 20 C [ 41 ].
Hand-held refractometer only measures with a 0,2 % resolution, so three measurements
of each 15 g mixture were made and the mean value is presented in tables as definitive
measurement. Following, results of the measurement experiment done with ethanol 70 %:

Table 16 Experimental results with ethanol 70 % solution by Carl Roth.
[ethanol]
real
[ethanol]
measured

3,05 % 0,60 %
6,07 % 1,20 %
9,09 % 2,00 %
12,02 % 2,73 %
14,99 % 3,73 %
17,97 % 4,40 %
Appendixes
Page 68

Graph 17 Relationship between real ethanol concentration and measured ethanol concentration done with
ethanol 70 % by Carl Roth.

And the resulting equation due to a linear regresion made in Graph 17 to calculate real
ethanol concentration by measuring ethanol concentration using the HR is:

|ctbonol]
cuI
= S,7998 . |ctbonol]
mcusucd
+u,u12S ( 40 )

Similarly, for the 99 % ethanol solution, same process is made and the results:

Table 17 Experimental results with ethanol 99 % solution by Scharr.
y = 3,7998x + 0,0125
R = 0,9955
0%
2%
4%
6%
8%
10%
12%
14%
16%
18%
20%
0% 1% 2% 3% 4% 5%
[
e
t
h
a
n
o
l
]

r
e
a
l
[ethanol] measured
Real mass concentration vs. measured values
Measures
Lineal (Measures)
[ethanol]
real
[ethanol]
measured

2,48 % 0,73 %
5,02 % 1,47 %
7,48 % 2,33 %
9,91 % 3,13 %
12,42 % 4,00 %
14,92 % 5,07 %
Appendixes
Page 69

Graph 18 Relationship between real ethanol concentration and measured ethanol concentration done with
ethanol 99 % by Scharr.

So that, the equation relating real ethanol concentration with the ethanol concentration
measured by the HR is obtained by linear regression and:

|ctbonol]
cuI
= 2,877S . |ctbonol]
mcusucd
+ u,uu68 ( 41 )

9.1.4 Conclusions
Under the point of view of real laboratory work, theoretical approach is not useful in our
case. Its complexity and the possibility of carrying out different experimental tests with
simplicity turn analytic calculation into a not practical process.
Results on this experiment shown in the graphs and the equations resulting were proved
under working conditions with the ethanol-water mixture used in a test rig. Following the
outcome of this checking test done with ethanol 70 %:

Table 18 Analysis of the results with ethanol 70 %
by Carl Roth
Where:

Value: volume/volume concentration known
[e]
m
: ethanol concentration measured by the
refractometer
[e]
c
: ethanol concentration calculated using (40)
Error: ([e]
r
desired value)/[e]
r

y = 2,8775x + 0,0068
R = 0,9969
0,00%
2,00%
4,00%
6,00%
8,00%
10,00%
12,00%
14,00%
16,00%
18,00%
0,00% 1,00% 2,00% 3,00% 4,00% 5,00% 6,00%
[
e
t
h
a
n
o
l
]

r
e
a
l
[ethanol] measured
Real mass concentration vs. measured values
Measures
Lineal (Measures)
Value [e]
m
[e]
c
Error
3,00 % 1,00 % 5,05 % 40,59 %
6,00 % 2,00 % 8,85 % 32,20 %
9,00 % 3,00 % 12,65 % 28,85 %
12,00 % 4,10 % 16,45 % 27,05 %
Appendixes
Page 70
As seen, error committed decreases with ethanol concentration increase and is around
25-40 %. This error can be justified by several reasons, mainly by temperature influence on
refractive index variation, since density of liquid components and the mixture itself has a
strong dependence on temperature. Experiments were run in ambient conditions (around
20 C) and check test were measured with liquid near 0 C.
Lack of homogeneity in the mixture, as well as low accuracy in mixture preparation
could be explanations for the error committed, as well as the influence of the range of
substances which the ethanol 70 % used has as an additive. Unknown chemical reactions
probably take its part on the error. A list of this additive involved follows: Acetaldehyd,
Acetic acid, Fuselol, Methanol and Isopropanol. Order in which this components and the main
ones are mixture is unknown, something strongly related with refractive index variation as the
literature mentioned states.
Checking test done with ethanol 99 % at the same working temperature (near 0 C)
produces the following results, where [e]
c
represents the ethanol volume concentration
calculated using ( 41 ):

It can be seen that error in results are
significantly lower and the equation employed
seems to be quite applicable to working
conditions. Error also decreases with increasing
ethanol concentration, as in 70 % experiment, but
in this case is between 0 - 15 %.

Table 19 Analysis of the results with ethanol 99 % by Scharr.

These results compared with the ones of ethanol 70 % show that there is/are a
difference(s) between their compositions, not only in ethanol concentration proportion, but in
the additives added. Despite their low concentration, additives may play an important role on
chemical reactions involving main components. Experience in working mixtures preparations
shows that when ethanol-water mixture is prepared with 99 % commercial ethanol, resulting
total volume of the mixture is higher than the used for the same ethanol concentration
prepared with 70 % commercial ethanol, proving the existence of these unknown chemical
reactions.
Summarising, employ of the hand-held refractometer used in our laboratory lead to a
bad accuracy in ethanol concentration measurement, but HR should be used just as a rough
way to determine ethanol concentration in an aqueous mixture, using equations ( 40 ) or ( 41 )
for it. Besides, HR should not be used when ethanol 70 % by Carl Roth is employed, as the
analytical results obtained have bad accuracy.
Value [e]
m
[e]
c
Error
3,00 % 1,00 % 3,56 % 15,67 %
6,00 % 2,00 % 6,44 % 6,76 %
9,00 % 3,00 % 9,31 % 3,36 %
12,00 % 4,00 % 12,19 % 1,56 %
Appendixes
Page 71
9.2 Appendix B: Redesigning of the heat exchanger.

9.2.1 Introduction
As it has been told before, one of the critical points in ice slurry systems is the ice slurry
generator. This part works as a connector between the primary circuit filled with a comercial
refrigerant and the secondary circuit in where the ice slurry flows and works as HTF.
This part -IS generator- is basically a heat exchanger where heat flows from the
supercooled ice slurry to the low temperature refrigerant, controlling IS temperature and
forcing the crystallisation. Therefore, usual parameters involved in this kind of equipment
should be studied in detail as heat exchange surface, mass flow of both fluids, temperature
gradient, thermal resistance of the materials and state of the fluids involved.
A commonly accepted solution nowadays for this heat exchanger is by using a heat
exchanger, where the plate in between of the fluids becomes the critical point in order to study
and control the crystallisation, especially its external surface. Further study of this plate is
necessary, especially surface contacting with the HTF. Besides, this plate is changed
occasionally and should be easily reachable.
The heat exchanger used in 3E Project
by Dipl.-Ing. (FH) Susanne Frank is a plate
heat exchanger which has some problems
in its daily running, mainly in sealing.
Some leaks were observed along the fluid
path that should be removed with a
redesign of the heat exchanger sealing
system.
Currently, sealing is re-made each
time the plate is changed with silicone. As
this method is effective, is not ideal and the
fact that it is not working correctly made
the decision of the redesign unavoidable.

9.2.2 Objectives.
Three main aspects of the heat exchanger are considered to be revised: joint between test
plate and the polycarbonate cover, sealing in the limits of the heat exchanger and
reconsidering the heat exchanger assembly.

9.2.3 Steps followed.
Firstly, a study of the sealing were carried out in order to evaluate the possibilities.
Due to the special features of the application, temperature lower than 0 C and water-ethanol
Figure 23 Current sealing between copper test plate
and polycarbonate cover (aluminium
strenghtened)
Appendixes
Page 72
mixtures, searching further and choosing carefully materials involved in sealing is obliged.
Sealing chosen will be directly related with the design proposed, and viceversa. Many steps
were thought and developed in a 3D model made with CATIA V5 R19 software.
In Figure 24, the final 3D model solution proposed is shown. Following, the main
aspects of this solution are explained. Intermediate solutions reached are also mentioned
throughout this report.

External appearance of the heat exchanger hardly changes with the new design, because
most of the changes proposed are in normally hidden areas. So, focus in these areas will
follow:

Joint between the test plate and the polycarbonate cover:
The sealing between the test plate and the
polycarbonate cover is made by a flat seal, which needs
help from another person to be placed. Additionally, as
the polycarbonate parts are not tight together, silicone has
been put in between. This solution result in some fluid
losses, unavoidable condensation over the silicone and,
above all, the impediment of dismantling to be easy.
In fact, current solution base its effectivity in two
lines of screws that create the needed force to press the
flat sealing and make it watertight. In the same way,
proposed solution is based in this fact since replacing the
flat sealing for an extended O-ring will result in an easier
placement of the sealing and a more effective sealing
solution.

Figure 24 Heat exchanger CATIA 3D model
Figure 25 Fluid inlet view (detail).
Appendixes
Page 73
Limits of the heat exchanger:
The problem is now transferred to the place where test plate, polycarbonate cover and
fluid inlet meet together. As there are three solids in a point, sealing would need to be double.
The abovementioned solution solves the problem between the test plate and the polycarbonate
cover, but another solution need to be proposed between the inlet and the test plate or the
polycarbonate cover.
Final decision at this point result in merging the inlet and the polycarbonate cover in
the same piece and placing a flat seal in between this piece and the test plate using the force
created by the screws and avoiding sealing in transverse direction which would need
additional forces to achieve watertightness.
This solution may have a problem, as it would exist a step between the polycarbonate
fluid inlet and the copper test plate. This step must be avoided under any circumstances, since
it was suggested by people already working on the platform that this step could work as a
possible heterogeneus nucleation point due to the possibility of the appeareance of a
turbulence caused by the step.
Another point which should be redefined is the joint between the inlet and the piping
system. Nowadays, the pipe is placed inside the inlet and the seal is made by glue. The most
suitable and effective possibility is threading the polycarbonate inlet and installing a fitting
which is compatible with the pipe. More details are mentioned later on.

Assembly and fixing:
Making the assembly of the heat exchanger easier is another important point of the
redesign. Besides, the HX plate should be easily removed from the HX and should be
completely fixed to the structure too.
The easiness of the assembly is achieved by removing the silicone sealing and
changing it to the previous mentioned seal system. The fixing is achieved by placing two
guidance pieces using the pressuring screws for the right placement.

9.2.4 Other proposed steps:
Development of the previously explained final idea for the HX redesign has been
complicated, since some intermediate ideas were dismissed. First global idea included
longitudinal forces applied by screws placed in aluminium flanges situatued in both ends of
the heat exchanger. This force made the needed pressure over a flat sealing to achieve
watertightness in the HX. Flanges would be connected to the polycarbonate parts by several
slots in where the flanges could be glued or just placed.
Appendixes
Page 74
This solution was dismissed because of some constructive difficulties. Mainly, these
difficulties are the inaccuracy of the lenght of the copper test plates, which is a problem in
order to assure the sealing between the plate and the inlet. Besides, a better solution was
found, which lastly is the final solution proposed.

Figure 26 First scheme of the heat exchanger.
9.2.5 Development.
Despite the practical process were not completely done, some important aspects of it
were developed and they are mentioned here.
Concerning the sealing, the material used is the most important issue. The requirements
considered include low working temperatures and resistance to ethanol and other possible
alcoholic compounds. Consulting the Trelleborg catalog [ 14 ] (selection of the most
interesting pages in Appendix D), the materials which have the required chemical
compatibilty are: chloroprene rubber (neoprene), ehtylene propylene (EPDM) and nitrile
(HNBR).

Figure 27 Main dimensions in O-ring installations [Trelleborg catalog].
Based on the information found in the same Trelleborg catalog, dimensions of the
O-ring chosen were determined (named according to Figure 27):
Appendixes
Page 75
d
2
= 2,62 [mm]
t = 2,00+0,05 [mm]
r
1
= 0,3+0,2 [mm]
b
4
= 3,8+0,2 [mm]
These dimensions should be appropiate to cope with the pressure under the O-ring
would be. Availiability of the O-ring considered should be consulted with the company, as
well as the length required.
Besides, a slot should be made either in the test plate or in the polycarbonate. As the
test plate is going to be replaced every so often, the slot will be made in the polycarbonate
cover as can be seen on the drawings attached later on.
Finally, as nowadays a flat sealing is already used and it works well, finding a new
commercial reference should not be necessary.
Another point where some changes were decided to be
made is the connection between the fluid inlet and the piping
system. Threading the polycarbonate inlet in order to find a
fitting which can solve the connection was the solution accepted
at first. Searching for the mentioned fitting, the most suitable
one seems to be the one in Figure 28 by Swagelok, whose
interesting pages of the catalog used could be found in
Appendix D. Additional sealing with an O-ring or Teflon may
be required. This requirements lead to selecting the reference
2507-810-1-6ST in the mentioned catalog.
The redesign proposed needs an important change in the polycarbonate cover. As it has been
told before, inlet-outlet and cover would be merged in the same piece to avoid the possible
leaks between their joints. Another point of importance in this redesign is the step between the
test plate and the polycarbonate inlet, which should be avoided under any circumstances
manufacturing the slope as close to the edge as possible. Contact were made with company
Heinz-Fritz but no answer were received, so the work should be taken further at this point.
Last point in the changes proposed were the guidance to make easier the mounting and
dismantling of the HX. As can be seen in the plans attached, they are small and quite simple
pieces which have not any special requirements. Suitable material could be aluminium and
work could be made in the workshop of HsKA.
Figure 28 Fitting by Swagelok.
Appendixes
9.3 Appendix C: Datasheets.
Content:

- Sandpaper characteristics.
- Grit size table.
- Silicone datasheets:
o Hochtemperatur silicone.
o Silicone plus.
- SWAK datasheet.
- Sikaflex datasheet.
o Pretreatment.
- Surface roughness machine datasheet.
- Glass powder composition and datasheet.
Appendixes
9.3.1 Sandpaper charact
Can be found in:
http://www.vsmabrasives.co
No further information was
9.3.2 Grit size table:
From DIN 69176-1 : 1985-
Series VSM- KK114F
Backing Very flexible c
Grain / Coating Aluminum Oxi
Grit Range P 40 - 240, 320
Abrasive Types (Forms) Rolls, economy
Workpiece Crankshafts, to
Advantages Soft, ultraflex h
Ripping in wef
acteristics:
com/product.php?product=KK114F&guide=s
as found for the other sandpapers used.
-03:
4F
cotton cloth
xide
20, 400
my rolls, sheets, belts, discs
tool parts, car bodies, aeronautics
x hand sanding material of high performance
eft direction
stainless
Seite: 1/4
Sicherheitsdatenblatt
gem 91/155/EWG
Druckdatum: 23.01.2006 berarbeitet am: 10.11.2005
DR
* 1 Stoff-/Zubereitungs- und Firmenbezeichnung
Angaben zum Produkt
Handelsname: PROBAU HOSI Hochtemperatursilikon
Verwendung des Stoffes/der Zubereitung: Abdichtungsmasse
SDB-Nr.: 20668b
Hersteller/Lieferant:
BAHAG AG
Postfach 100561
D-68005 Mannheim
Auskunftgebender Bereich:
Abteilung: Technische Beratung
Tel +49(0)541 601-643
Notfallauskunft: Tel. (0180) 3000462
* 2 Zusammensetzung/Angaben zu den Bestandteilen
Chemische Charakterisierung
Beschreibung:
Zubereitung auf der Basis von Polydimethylsiloxanen, Siliciumdioxid und Vernetzern vom Acetoxylsilan-Typ
Gefhrliche Inhaltsstoffe:
CAS: 4253-34-3
EINECS: 224-221-9
Methyltriacetoxysilan < 5%
CAS: 17689-77-9 Ethyltriacetoxysilan
C; R 34
< 5%
* 3 Mgliche Gefahren
Gefahrenbezeichnung: entfllt
Besondere Gefahrenhinweise fr Mensch und Umwelt: entfllt
Klassifizierungssystem:
Die Klassifizierung entspricht den aktuellen EG-Listen, ist jedoch ergnzt durch Angaben aus der Fachliteratur und
durch Firmenangaben.
Zustzliche Angaben: Das Produkt ist brennbar
* 4 Erste-Hilfe-Manahmen
Allgemeine Hinweise: Keine besonderen Manahmen erforderlich.
nach Hautkontakt:
Bei andauernder Hautreizung Arzt aufsuchen.
Mit dem Produkt getrnkte Kleidung unverzglich wechseln
nach Augenkontakt: Augen bei geffnetem Lidspalt mehrere Minuten mit flieendem Wasser splen.
nach Verschlucken: rztlicher Behandlung zufhren.
nach Einatmen:
Den betroffenen an die frische Luft bringen und ruhig lagern.
Bei Beschwerden Arzt aufsuchen.
Folgende Symptome knnen auftreten: Symptomatische Behandlung vornehmen.
* 5 Manahmen zur Brandbekmpfung
Geeignete Lschmittel: Feuerlschmanahmen auf die Umgebung abstimmen.
Aus Sicherheitsgrnden ungeeignete Lschmittel Wasser im Vollstrahl.
Besondere Gefhrdung durch den Stoff, seine Verbrennungsprodukte oder entstehende Gase:
Das Produkt wird ausschliesslich in Kleingebinden vertrieben. Eine Gefhrdung durch das Produkt bei Brand ist daher
wenig wahrscheinlich. Die hauptschliche Gefahr im Brandfall ergibt sich aus der Entzndbarkeit der Verpackung. Bei
der Verbrennung des Produktes werden Kohlenmonoxid, Kohlendioxid und Siliciumdioxid gebildet. Bei der thermischen
Zersetzung/Verbrennung des Produktes werden giftige und leichtentzndliche Dmfe/Gase freigesetzt.
Besondere Schutzausrstung:
Atemschutzgert anlegen.
Die dem Feuer ausgesetzten Behlter mit Wasser im Sprhstrahl khlen. Im Brandfall umluftunabhngiges
Atemschutzgert und dichtschliessenden Schutzanzug anlegen. Kontaminiertes Lschwasser nach Mglichkeit
auffangen und entsorgen (siehe auch Punkt 13).
6 Manahmen bei unbeabsichtigter Freisetzung:
Personenbezogene Vorsichtsmanahmen: Nicht erforderlich.
(Fortsetzung auf Seite 2)
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(Fortsetzung von Seite 1)
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Umweltschutzmanahmen:
Mit viel Wasser verdnnen.
Nicht in die Kanalisation, Grundwasser, Oberflchenwasser oder Erdreich gelangen lassen.
Verfahren zur Reinigung/Aufnahme:
Mit flssigkeitsbindendem Material (Sand, Kieselgur, Surebinder, Universalbinder, Sgemehl) aufnehmen.
Unbeschdigte Kleingebinde (Dosen, Tuben, Kartuschen) aufnehmen und an einem geschtzten Ort sichern. Den
Gefahrenbereich mechanisch lften. Produktdmpfe nicht einatmen. Bei Austritt grsserer Mengen die weiter
Ausbreitung durch Eindmmen verhindern. Verschttetes, viskoses Produkt mit einem inerten Material berdecken und
in gekennzeichnente, bestndige Container aufnehmen. Das Produkt anschlieend wie in Punkt 13 beschrieben
entsorgen. Den Boden grndlich mit einem selbstemulgiernenden Lsungsmittel und viel Wasser reinigen.
Zustzliche Hinweise: Es werden keine gefhrlichen Stoffe freigesetzt.
* 7 Handhabung und Lagerung
Handhabung:
Hinweise zum sicheren Umgang:
Freiwerdende Produktdmpfe direkt am Entstehungsort wirksam absaugen. Whrend der Verarbeitung des Produktes
freiwerdende Dmpfe nicht einatmen. Produkt nicht mit inkompatiblen Substanzen mischen (siehe Punkt 10). Die
Anwendungsvorschriften beachten. Am Arbeitsplatz Augenwaschflasche bereitstellen. Am Arbeitsplatz nicht rauchen.
Hinweise zum Brand- und Explosionsschutz: Keine besonderen Manahmen erforderlich.
Lagerung:
Anforderung an Lagerrume und Behlter:
Produkt nur in dichtverschlossenen Originalgebinden an einem gut belfteten Ort vor Feuchtigkeit und Frost geschtzt
khl und trocken lagern.
Zusammenlagerungshinweise: Getrennt von Lebensmitteln lagern.
Weitere Angaben zu den Lagerbedingungen: Unter Verschlu und fr Kinder unzugnglich aufbewahren.
Lagerklasse: VCI-Lagerklasse: 10 Brennbare Flssigkeiten soweit nicht LGK 3A bzw. 3B
Klassifizierung nach Betriebssicherheitsverordnung (BetrSichV): -
* 8 Expositionsbegrenzung und persnliche Schutzausrstung
Zustzliche Hinweise zur Gestaltung technischer Anlagen:
Bei der professionellen Dauerverarbeitung des Produktes fr eine effiziente Absaugung sorgen.
Bestandteile mit arbeitsplatzbezogenen, zu berwachenden Grenzwerten:
64-19-7 Essigsure
MAK Kurzzeitwert: 25 mg/m, 10 ml/m
Essigsure
Zustzliche Hinweise: Als Grundlage dienten die bei der Erstellung gltigen Listen.
Persnliche Schutzausrstung:
Allgemeine Schutz- und Hygienemanahmen:
Von Nahrungsmitteln, Getrnken und Futtermitteln fernhalten.
Beschmutzte, getrnkte Kleidung sofort ausziehen.
Vor den Pausen und bei Arbeitsende Hnde waschen.
Berhrung mit den Augen und der Haut vermeiden.
Bei der Arbeit nicht essen, trinken, rauchen, schnupfen.
Atemschutz:
BGR 190 "Regeln fr den Einsatz von Atemschutzgerten" ist zu beachten (BGR: Berufsgenossenschaftliche Regel)
Atemschutzfiltergert mit Gasfilter DIN 3181 AX
bei mangelnder Belftung whrend der Vulkanisation/Vernetzung.
Tragezeitbegrenzung fr Atemschutzmasken nach der TRgA 415 einhalten.
Handschutz:
Handschuhe aus PVC/Gummi.
BGR 195 "Regeln fr den Einsatz von Schutzhandschuhen" ist zu beachten (BGR: Berufsgenossenschaftliche Regel)
Augenschutz:
Schutzbrille.
BGR 192 " Regel n f r di e Benut zung von Augen- und Gesi cht sschut z" i st zu beacht en ( BGR:
Berufsgenossenschaftliche Regel)
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Krperschutz:
Arbeitsschutzkleidung.
BRG 189 "Regeln fr den Einsatz von Schutzkleidung" ist zu beachten (BGR: Berufsgenossenschaftliche Regel)
* 9 Physikalische und chemische Eigenschaften
Allgemeine Angaben
Form: pasts
Farbe: verschiedene
Geruch: suerlich
Zustandsnderung
Schmelzpunkt/Schmelzbereich: nicht bestimmt
Siedepunkt/Siedebereich: nicht bestimmt
Flammpunkt: > 150C
Zndtemperatur: 427C
Selbstentzndlichkeit: Das Produkt ist nicht selbstentzndlich.
Explosionsgefahr: Das Produkt ist nicht explosionsgefhrlich.
Dampfdruck bei 20C: 15 hPa
Dichte bei 20C: ca. 1,08 g/cm
Lslichkeit in / Mischbarkeit mit
Wasser: nicht bzw. wenig mischbar
* 10 Stabilitt und Reaktivitt
Thermische Zersetzung / zu vermeidende Bedingungen:
Bei Einwirkung von feuchter Luft bei Raumtemperatur vernetzt das Produkt (Bildung von max. 2,8 Gew.-% Essigsure,
bezogen auf eingesetztes Produkt).
Zu vermeidende Stoffe:
starke Oxidationsmittel
Kontakt mit Suren vermeiden.
Gefhrliche Zersetzungsprodukte:
Bei der Verbrennung des Produktes werden Kohlenmonoxid, Kohlendioxid, Siliciumdioxid und Stickoxide gebildet. Bei
der thermischen Zersetzung des Produktes werden reizende und entzndliche Dmpfe/Gase freigesetzt.
* 11 Angaben zur Toxikologie
Akute Toxizitt:
Primre Reizwirkung:
an der Haut: Reizwirkung mglich.
am Auge: Reizwirkung mglich
Sonstige Angaben (zur experimentellen Toxikologie):
Bei Beachtung der blichen Vorschriften der industriellen Arbeitshygiene beinhaltet der Umgang mit dem Produkt kein
besonderes Risiko fr die Gesundheit. Die einzelnen Komponenten der Zubereitung beinhakten ein nur geringfgiges,
toxikologisches Potential bei oraler bzw. percutaner Applikation. Essigsuredmpfe knnen die Augenschleimhute
und die oberen Atemwege reizen. Das Produkt wirkt schwach reizend auf die Augen, die Atemwege und die Haut. [Lit]
Zustzliche toxikologische Hinweise:
Bei sachgemem Umgang und bestimmungsgemer Verwendung verursacht das Produkt nach unseren
Erfahrungen und den uns vorliegenden Informationen keine gesundheitsschdlichen Wirkungen.
Der Stoff ist nicht kennzeichnungspflichtig aufgrund der EG-Listen in der letztgltigen Fassung.
* 12 Angaben zur kologie
Allgemeine Hinweise:
Wassergefhrdungsklasse 1 (Selbsteinstufung): schwach wassergefhrdend
Nicht unverdnnt bzw. in greren Mengen in das Grundwasser, in Gewsser oder in die Kanalisation gelangen
lassen.
* 13 Hinweise zur Entsorgung
Produkt:
Empfehlung:
Kleinere Mengen knnen gemeinsam mit Hausmll deponiert werden.
Nicht ausgehrtetes Produkt in einem brennbaren Lsungsmittel verdnnt in einer hierfr genehmigten Anlage
verbrennen. Ausgehrtetes Produkt als festen Rckstand in einer hierfr genehmigten Anlage entsorgen.
Europischer Abfallkatalog
08 04 99 Abflle a. n. g.
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gem 91/155/EWG
DR
Ungereinigte Verpackungen:
Empfehlung:
Kleingebinde (Dosen, Tuben, Kartuschen) grndlich restentleeren und dem Recycling zufhren. Die verschiedenen
Verpackungsmaterialien voneinander trennen und getrennt entsorgen.
* 14 Angaben zum Transport
Landtransport ADR/RID und GGVS/GGVE (grenzberschreitend/Inland):
ADR/RID-GGVS/E Klasse: -
Seeschiffstransport IMDG/GGVSee:
Marine pollutant: Nein
15 Vorschriften
Kennzeichnung nach EWG-Richtlinien:
Die beim Umgang mit Chemikalien blichen Vorsichtsmanahmen sind zu beachten.
Der Stoff ist nicht kennzeichnungspflichtig nach EG-Listen oder sonstigen uns bekannten Literaturquellen.
Das Produkt ist nach EG-Richtlinien/GefStoffV nicht kennzeichnungspflichtig.
R-Stze: keine
S-Stze:
29 Nicht in die Kanalisation gelangen lassen.
Nationale Vorschriften:
Technische Anleitung Luft: Kohlenwasserstoffgemisch, entaromatisiert (< 20%) Klasse III
Wassergefhrdungsklasse: WGK 1 (Selbsteinstufung): schwach wassergefhrdend.
* 16 Sonstige Angaben:
Die Angaben sttzen sich auf den heutigen Stand unserer Kenntnisse, sie stellen jedoch keine Zusicherung von
Produkteigenschaften dar und begrnden kein vertragliches Rechtsverhltnis.
Wortlaut der in Kapitel 2 angegebenen R-Stze (Keine Einstufung der Rezeptur, sondern Einstufung der
Rohstoffe)
34 Verursacht Vertzungen.
Datenblatt ausstellender Bereich: Abteilung F&E
* Daten gegenber der Vorversion gendert
Seite: 1/4
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* 1 Stoff-/Zubereitungs- und Firmenbezeichnung
Angaben zum Produkt
Handelsname: PROBAU SIPLUS
Verwendung des Stoffes/der Zubereitung: Dichtungsmittel
SDB-Nr.: 20670b
Hersteller/Lieferant:
BAHAG AG
Postfach 100561
D-68005 Mannheim
Auskunftgebender Bereich:
Abteilung: Technische Beratung
Tel +49(0)541 601-643
Notfallauskunft: Tel. (0180) 3000462
2 Zusammensetzung/Angaben zu den Bestandteilen
Chemische Charakterisierung
Beschreibung:
Zubereitung auf der Basis von Polydimethylsiloxanen, inerten Fllstoffen und Vernetztern vom Oximsilan-Typ.
Gefhrliche Inhaltsstoffe:
CAS: 22984-54-9
EINECS: 245-366-4
Butan-2-on-O,O',O''-(methylsilylidyn)trioxim
Xn; R 21
CAS: 2224-33-1
EINECS: 218-747-8
Butan-2-on-O,O',O''-(vinylsilylidyn)trioxim
Xi; R 36-43
CAS: 64742-46-7
EINECS: 265-148-2
Destillate (Erdl), mit Wasserstoff behandelte mittlere
Xn; R 65
< 20%
CAS: 37858-57-7 Methyltris(methylisobutylketoxim)silan
Xn; R 22-36-48
zustzl. Hinweise:
Der Wortlaut der angefhrten Gefahrenhinweise ist dem Kapitel 16 zu entnehmen.
Die in Punkt 2 gelisteten Oxime sind in einer Gesamtkonzentration < 5 % enthalten
3 Mgliche Gefahren
Gefahrenbezeichnung: entfllt
Besondere Gefahrenhinweise fr Mensch und Umwelt:
Das Produkt ist kennzeichnungspflichtig auf Grund des Berechnungsverfahrens der "Allgemeinen Einstufungsrichtlinie
fr Zubereitungen der EG" in der letztgltigen Fassung.
Klassifizierungssystem:
Die in Punkt 2 angegebene Kennzeichnung der reinen Kohlenwasserstoff-Fraktion weicht von der ursprnglichen EU-
Einstufung ab, da die Anmerkungen zu der EU-Einstufung erfllt sind.
Zustzliche Angaben:
Das Produkt ist brennbar.
Es sind exotherme Reaktionen mglich mit best. chem. Substanzen. Whrend der Verarbeitung des Produktes werden
gefhrliche Gase / Dmpfe freigesetzt ( 2-Butanononoxim, CAS 96-29-7)
4 Erste-Hilfe-Manahmen
Allgemeine Hinweise: Es sind keine allgemeinen Hinweise notwendig
nach Hautkontakt:
Sofort mit Wasser und Seife abwaschen und gut nachsplen.
Bei andauernder Hautreizung Arzt aufsuchen.
nach Augenkontakt:
Augen mehrere Minuten bei geffnetem Lidspalt unter flieendem Wasser splen. Bei anhaltenden Beschwerden Arzt
konsultieren.
nach Verschlucken: Bei verschlucken sofort rztlichen Rat einholen und Verpackung oder Etikett vorzeigen.
nach Einatmen: Reichlich Frischluft und sicherheitshalber Arzt aufsuchen.
5 Manahmen zur Brandbekmpfung
Geeignete Lschmittel:
CO2, Lschpulver oder Wassersprhstrahl. Greren Brand mit Wassersprhstrahl oder alkoholbestndigem Schaum
bekmpfen.
Aus Sicherheitsgrnden ungeeignete Lschmittel Wasser im Vollstrahl.
Besondere Gefhrdung durch den Stoff, seine Verbrennungsprodukte oder entstehende Gase:
Das Produkt wird ausschlielich in Kleingebinden vertrieben. Eine Gefhrdung durch das Produkt bei Brand ist daher
wenig wahrscheinlich. Die hauptschliche Gefahr im Brandfall ergibt sich aus der Entzndbarkeit der Verpackungen.
Bei der thermischen Zersetzung des Produktes werden reizende und entzndliche Dmpfe/Gase freigesetzt.
Seite: 2/4
gem 91/155/EWG
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Besondere Schutzausrstung: Atemschutzgert anlegen.
6 Manahmen bei unbeabsichtigter Freisetzung:
Personenbezogene Vorsichtsmanahmen:
Fr ausreichende Lftung sorgen.
Haut und Augenkontakt vermeiden.
Umweltschutzmanahmen:
Nicht in den Untergrund/Erdreich gelangen lassen.
Nicht in die Kanalisation, Grundwasser, Oberflchenwasser oder Erdreich gelangen lassen.
Verfahren zur Reinigung/Aufnahme:
Mit flssigkeitsbindendem Material (Sand, Kieselgur, Surebinder, Universalbinder, Sgemehl) aufnehmen.
Zustzliche Hinweise:
Erhrtetes Material kann als Abfall nach Punkt 13 entsorgt werden.
Informationen zur Entsorgung siehe Kapitel 13.
7 Handhabung und Lagerung
Handhabung:
Hinweise zum sicheren Umgang: Fr gute Belftung/Absaugung am Arbeitsplatz sorgen.
Hinweise zum Brand- und Explosionsschutz:
Zndquellen fernhalten - nicht rauchen.
Lagerung:
Anforderung an Lagerrume und Behlter:
Nur im ungeffneten Originalgebinde aufbewahren.
Behlter dicht geschlossen halten.
Erwrmung ber 40C vermeiden.
Zusammenlagerungshinweise: Getrennt von Lebensmitteln lagern.
Weitere Angaben zu den Lagerbedingungen: Vor Luftfeuchtigkeit und Wasser schtzen.
Lagerklasse: VCI-Lagerklasse: 10 Brennbare Flssigkeiten soweit nicht LGK 3A bzw. 3B
* 8 Expositionsbegrenzung und persnliche Schutzausrstung
Zustzliche Hinweise zur Gestaltung technischer Anlagen: Keine weiteren Angaben, siehe Punkt 7.
Bestandteile mit arbeitsplatzbezogenen, zu berwachenden Grenzwerten:
64742-46-7 Destillate (Erdl), mit Wasserstoff behandelte mittlere
MAK Kurzzeitwert: 1000 mg/m, 200 ml/m
Zustzliche Hinweise: Als Grundlage dienten die bei der Erstellung gltigen Listen.
Persnliche Schutzausrstung:
Allgemeine Schutz- und Hygienemanahmen:
Nach der Arbeit und vor den Pausen fr grndliche Hautreinigung sorgen.
Vorbeugender Hautschutz durch Hautschutzsalbe.
Nach der Arbeit eine rckfettende Hautcreme verwenden.
Von Nahrungsmitteln, Getrnken und Futtermitteln fernhalten.
Beschmutzte, getrnkte Kleidung sofort ausziehen.
Bei der Arbeit nicht essen, trinken, rauchen, schnupfen.
Atemschutz: Atemschutzfiltergert mit Gasfilter DIN 3181 AX
Handschutz:
undurchlssige Schutzhandschuhe aus Kunststoff oder Gummi ( nicht obligatorisch, wird aber empfohlen)
Augenschutz:
Dichtschlieende Schutzbrille.
Krperschutz: Arbeitsschutzkleidung.
9 Physikalische und chemische Eigenschaften
Allgemeine Angaben
Form: pasts
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Farbe: verschieden, je nach Einfrbung
Geruch: schwach, charakteristisch
Zustandsnderung
Schmelzpunkt/Schmelzbereich: nicht bestimmt
Siedepunkt/Siedebereich: nicht bestimmt
Flammpunkt: 140C
Zndtemperatur: 435C
Selbstentzndlichkeit: Das Produkt ist nicht selbstentzndlich.
Explosionsgefahr: Das Produkt ist nicht explosionsgefhrlich.
Dampfdruck bei 20C: <1 hPa
Dichte bei 20C: 1,2 g/cm
Lslichkeit in / Mischbarkeit mit
Wasser: unlslich
in den gebruchlichsten org. Lsungsmitteln teilweise lslich
10 Stabilitt und Reaktivitt
Thermische Zersetzung / zu vermeidende Bedingungen:
Bei Einwirkung von feuchter Luft bei Raumtemperatur vernetzt das Produkt (Bildung von Methanol).
Zu vermeidende Stoffe:
starke Oxidationsmittel
Feuchtigkeitszutritt
Gefhrliche Zersetzungsprodukte: keine, bei sachgemer Handhabung und Lagerung
11 Angaben zur Toxikologie
Akute Toxizitt:
Primre Reizwirkung:
an der Haut: Reizwirkung mglich
am Auge: Reizwirkung mglich
Sensibilisierung: keine Daten bekannt
12 Angaben zur kologie
Allgemeine Hinweise:
Wassergefhrdungsklasse 1 (Selbsteinstufung): schwach wassergefhrdend
Nicht unverdnnt bzw. in greren Mengen in das Grundwasser, in Gewsser oder in die Kanalisation gelangen
lassen.
Das Produkt hydrolisiert langsam bei Kontakt mit Wasser. Das Produkt ist nur wenig biologisch abbaubar.
13 Hinweise zur Entsorgung
Produkt:
Empfehlung: Fr die Entsorgung sind die behrdlichen Vorschriften zu beachten.
Europischer Abfallkatalog
Di e Abfal l schl ssel nummern si nd sei t dem 01. 01. 1999 ni cht nur produkt- sondern i m wesentl i chen
anwendungsbezogen. Die gltige Abfallschlsselnummer kann dem Europischen Abfallkatalog entnommen werden.
08 04 99 Abflle a. n. g.
Ungereinigte Verpackungen:
Empfehlung: Entsorgung gem den behrdlichen Vorschriften.
14 Angaben zum Transport
Landtransport ADR/RID und GGVS/GGVE (grenzberschreitend/Inland):
ADR/RID-GGVS/E Klasse: -
Ziffer/Buchstabe: kein Gefahrgut
Seeschiffstransport IMDG/GGVSee:
Marine pollutant: Nein
15 Vorschriften
Kennzeichnung nach EWG-Richtlinien:
Das Produkt ist nach EG-Richtlinien/GefStoffV eingestuft und gekennzeichnet.
S-Stze:
29 Nicht in die Kanalisation gelangen lassen.
Nationale Vorschriften:
Seite: 4/4
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Wassergefhrdungsklasse: WGK 1 (Selbsteinstufung): schwach wassergefhrdend.
16 Sonstige Angaben:
Die Angaben sttzen sich auf den heutigen Stand unserer Kenntnisse, sie stellen jedoch keine Zusicherung von
Produkteigenschaften dar und begrnden kein vertragliches Rechtsverhltnis.
Wortlaut der in Kapitel 2 angegebenen R-Stze (Keine Einstufung der Rezeptur, sondern Einstufung der
Rohstoffe)
21 Gesundheitsschdlich bei Berhrung mit der Haut.
22 Gesundheitsschdlich beim Verschlucken.
36 Reizt die Augen.
43 Sensibilisierung durch Hautkontakt mglich.
48 Gefahr ernster Gesundheitsschden bei lngerer Exposition.
65 Gesundheitsschdlich: kann beim Verschlucken Lungenschden verursachen.
Datenblatt ausstellender Bereich: Abteilung F&E
Ansprechpartner:
* Daten gegenber der Vorversion gendert
Leak Detectors, Lubricants, and Sealants 3
Features
Cures to a bond that resists vibration
or shock
Lubricates threads, preventing costly
thread damage due to galling and
seizing during assembly
Allows low breakaway torque for
easy-to-break connections, even
after fully cured
Is compatible with a wide range of
chemicals
Applies quickly and easily
Clings to threads and will not shred
or tear on assembly
Ordering Information
Tube Size Ordering Number
0.2 fl oz (6 cm
3)
MS-PTS-6
1.69 fl oz (50 cm
3
) MS-PTS-50
8.45 fl oz (250 cm
3)
MS-PTS-250
Some uids and materials are NOT
compatible with SWAK. While not
intended to be a complete list, they
include the following:
Plastic pipe or valve components
other than PTFE
Halogens
Freon
Pure oxygen
Ozone
Hydrazine
Nitrogen dioxide
High concentrations of strong acids
or bases
Food, cosmetic, drug, or water
systems for human consumption
Vacuum systems where any
hydrocarbon outgassing will affect
performance
Material Safety Data Sheets are available from your
authorized Swagelok representative or at swagelok.com.
Pipe Thread Sealants
Swagelok pipe thread sealants are compatible with a wide range of chemicals,
enabling leak-tight sealing in a variety of applications.
Technical Information
Composition: Resin (containing
methacrylic ester) and PTFE particles
Cure time: At room temperature,
allow 24 h minimum before
pressurizing
.
Pressure rating: To pipe or ftting
working pressure up to 10 000 psig
(689 bar), based on proper thread
engagement
Temperature rating: 65 to 350F
(53 to 176C)
Viscosity: Greater than 100 000 cP, in
accordance with ASTM D1824
Storage temperature: 45 to 85F (7
to 29C)
Shelf life: Five years at
recommended storage temperature
Cure time and sealing are dependent on
many variables, such as storage conditions,
cleanliness of threads, quality of threads,
temperature, materials of construction, proper
assembly, specific gravity of system media,
and system operating pressures.
SWAK Anaerobic Pipe Thread Sealant
Features
Material conforms
to Commercial Item
Description A-A-58092
Temperatures up to 450F
(232C)
Ordering Information
Male Tapered
Pipe Size
Tape
Size
Ordering
Number
1/8, 1/4, and 3/8 in.
1/4 by 576 in.
(6.4 mm by 1463 cm)
MS-STR-4
1/2 in. and up
1/2 by 288 in.
(12.7 mm by 732 cm)
MS-STR-8
Applications
Plastics Chemicals
Aluminum Corrosives
Stainless steel Hydraulic fluids
Ceramic Refrigerants
Synthetic rubber Aromatic fuels
Carbon steel and special alloys
Caution: Tape should be used only on male tapered
pipe threads. Do not use on ared, coned, or tube
tting ends.
PTFE Tape Pipe Thread Sealant
!
Sikaex
-200 and SikaTack
Series - Adhesives and Sealants

1 2
Pr econdi t i on:
Surfaces have to be dry, oil, fat and dust free. Soiled
substrates can be cleaned with Sika
Remover-208.
According to the nature of soiling, other methods such
as Sika
Cleaner P or water based cleaners, steam

washer etc. may be used. It is recommended to verify
compatibility with the cleaning products.
Levels
M
e
c
h
a
n
i
c
a
l
C
l
e
a
n
i
n
g
/
A
c
t
i
v
a
t
i
n
g
P
r
i
m
e
r
M
e
c
h
a
n
i
c
a
l
C
l
e
a
n
i
n
g
/
A
c
t
i
v
a
t
i
n
g
P
r
i
m
e
r
Aluminium (AlMg3, AIMgSi1)
SVF
SVF
SA
205
SVF
SVF
205
205
210
204 N

C
o
n
t
a
c
t

T
e
c
h
n
i
c
a
l

S
e
r
v
i
c
e
Aluminium (anodized) SA
205
SA
204 N
206 GP
Steel (St37 etc.)
205
SA
204 N
206 GP
SVF
SVF
205
SA
204 N
206 GP
Steel (Stainless steel)
205
SA
SVF
SVF
205
205
210
204 N
Steel (hot-dipped, galvanized)
SA
205
SVF
SVF
SA
205
206 GP
210
2-Component top coat (PUR, acrylic)
SA
SCA
SA 206 GP
Powder coated
(PES, EP/PES)
SCA
SA SVF
SCA
SA 206 GP
2-Component water-based paint primer and top
coats (PUR, acrylic)
SA
SCA
SA 206 GP
Cathode dip coating
SA
SA
SA 206 GP
Coil coating
205
SCA
SVF 205
SCA 206 GP
GRP /unsaturated polyester) gelcoat side or SMC SA
SVF SA
SA 206 GP
GRP (unsaturated polyester) lay-up side SA 206 GP
S80
S80
SA
205
206 GP
215
ABS
215
206 GP
205
SA
215
206 GP
Hard PVC 215 205 215
PMMA/PC (without anti scratch coating) SA 209 D
SVF
SVF
SA
SA
209 D
206 GP
Glass SA
SA
SA 206 GP
Ceramic screen print SA
SA
SA 206 GP
Plywood unnished

215
3
Levels Description
1
a) General sealing applications, small components where joint movement capabilities are not required
b) Non-strucutural interior bonding applications, no exposure to short term temperature extremes, and no contact with water
2
a) Sealing applications involving large components where joint movement capabilities are required
b) Interior and exterior bonding applications under normal environmental conditions
3
Exterior applications where certain levels of chemical resistance required
Applications to prevent liquid ingress where corrosion could occur
Please also consult additional information, such as General Guidelines Bonding and Sealing with Sikaex
, actual Product Data Sheets, etc.

Adhesion test are based on DIN 54457 and Internal Standard CQP 033-1
1 to 9 see last page Explanatory Notes on Substrate Preparation and Treatment
1
st
Process = Recommendation
2
nd
Process = Alternative
For bonding/sealing process no surface preparation (mechanical, cleaning/activating, primer) are required
1
2
3
4
5
9 6
9 6
7
8
9
9

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Technical Data Sheet
Version 08 / 01 / 2006
Sikaflex
-295 UV
UV Resistant Adhesive/Sealant
Technical Product Data (typical values)
Chemical base 1-C polyurethane
Color Black, White
Cure Mechanism Moisture-curing
Density (uncured) 10.8 lbs/gal
VOC Content 0.11 lbs / gal
Non-sag properties Good
Application temperature product 50F - 95F (10C - 35C)
Tack free time
1
60 minutes
Curing speed (see diagram 1)
Shrinkage 1%
Shore A-hardness (ASTM D 2240) 35
Tensile strength (ASTM D 412) 160 psi
Elongation at break (ASTM D 412) 500%
Tear propagation resistance (ASTM D 624) pli 5N/mm
Service temperature permanent -40F -195F (-40C - 90C)
Short term 4hours
1hour
248F (120C)
302F (150C)
Shelf life (storage below 80F (25C)) Cartridge & UniPac
Drum & Pail
12 months
6 months
1)
73F (23C) / 50% r.h.

Description
Sikaflex
-295UV is a one-component
polyurethane adhesive/sealant
specifically formulated for bonding acrylic
and polycarbonate windows and
hatches. It is also an excellent color
stable, non-chalking sealant for general
marine sealing.

Product Benefits
- UV resistant, no cracking or chalking
- Salt water resistant
- Fast tack-free time
- Paintable and sandable
- Stable
- Bonds and seals in one step
- Initial load bearing capacity
- High thixotropy/good gap filling
properties
- Non yellowing
- Non chalking

Areas of Application
Sikaflex
-295 UV black is intended to be

used as an adhesive and/or sealant in
bonding applications for polycarbonate
windows and acrylic (PMAA) windows.
Black: Use in conjunction with Sika
-
Cleaner 226 and Sika
Primer 209N.
Prior to use, always refer to installation
guide available at www.sikaindustry.com/
ipd-marine-window-295.

Sikaflex
-295 UV white is intended to be

used as a sealant in open joints between
glass, ceramics, metals, many plastics,
fiberglass and many types of paint.
Use in conjunction with Sika
-Cleaner
226 or Sika
-Aktivator. Refer to the

Surface Preparation Guidelines for
further information. It is not intended to
bond mineral glass.

S
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Further information available at:
www.sikaindustry.com

Sika Corporation
Industry Division
30800 Stephenson Highway
Madison Heights, MI 48071
USA
Tel. 248 577 0020
Fax 248 577 0810
Cure Mechanism
Sikaflex
-295 UV cures by reaction with

atmospheric moisture. At low
temperatures the water content of the air
is lower and the curing reaction proceeds
more slowly (see diagram).

Time (days)
0
0 2 4 6
23C / 50% r.h
10
8
12
10C / 50% r.h
4
T
h
i
c
k
n
e
s
s

o
f

c
u
r
e

(
m
m
)

Diagram 1: Curing speed Sikaflex
-295 UV
Chemical Resistance
Sikaflex
-295 UV is resistant to fresh

water, seawater, aqueous, chlorine free
cleaning solutions and sewage effluent
as well as diluted acids and caustic
solutions; temporarily resistant to fuels,
mineral oils, vegetable and animal fats
and oils; not resistant to organic acids,
alcohol, concentrated mineral acids,
caustic solutions or paint thinners. The
above information is offered for general
guidance only. Advice on specific
applications will be given on request.
Method of Application
Surface preparation
Surfaces must be clean, dry and free
from all traces of grease, oil, dust, and
standing moisture. As a rule the faces
must be prepared in accordance with the
instructions given in the current Sika

Primer Chart for Marine Applications.
Keep the work area shielded from direct
sunlight and temperature extremes.
Advice on specific projects is available
from the Technical Service Department
of Sika Industry 888-832-7452.
Application
Cartridges: Pierce cartridge membrane.
Unipacs: Place unipac in the sealant
gun and snip off the closure clip. Cut off
the tip of the nozzle to suit the joint and
apply the adhesive with a suitable hand-
operated or pneumatic gun. Once
opened, cartridges or packs should be
used up within a relatively short space of
time. To ensure a uniform thickness of
adhesive bead, we recommend that the
adhesive be applied as a triangular bead
(see illustration). The nozzle cut
dimensions and the number of beads
applied, are dependent upon the
required width and thickness of the
adhesive bead in the final assembly.
Correct joint design is essential when
bonding plastic glazing materials and
must take into account the special
properties of these substrates. Do not
apply at temperatures below 10C or
above 35C. The optimum temperature
for substrate and adhesive is between
15C and 25C. For advice on selecting
and setting up a suitable pump system,
as well as on the techniques of pump
operated application, please contact the
System Engineering Department of Sika
Industry at 888-832-7452.

b b
h
2h

Figure 1: Recommended bead
configuration

Tooling and finishing
Tooling and finishing must be carried out
within the tack-free time of the adhesive.
We recommend the use of Sika
Slick.
Other finishing agents or lubricants must
be tested for suitability/compatibility.

Removal
Uncured Sikaflex
-295 UV may be
removed from tools and equipment with
Sika
Remover-208 or another suitable

solvent. Once cured, the material can
only be removed mechanically. Hands
and exposed skin should be washed
immediately using a suitable industrial
hand cleaner and water. Do not use
solvents!

Overpainting
Sikaflex
-295 UV may be overpainted

when tack-free. The paint and paint
process must be tested for compatibility
by carrying out preliminary trials.
Sikaflex
-295UV should not be exposed

to baking temperatures until it has
attained full cure. It should be
understood that the hardness and film
thickness of the paint might impair the
elasticity of the sealant and lead to
cracking of the paint film with time.

Limitations
- Do not apply on frozen surface or
through standing water or under water.
- Do not apply over silicones or in the
presence of curing silicones.
- Avoid contact with alcohol and alcohol
containing solvents during cure.
- Allow minimum of 1-week full cure prior
to total water immersion situations.
- Maximum chlorine exposure 2.5 ppm.
- Do not use as a deck seam sealant.
- Do not use for bonding glass.

Important Considerations:
When applying sealant, avoid air
entrapment. Protect from action of water
during curing period.

WARNING:
IRRITANT, SENSITIZER.
Contains Polyisocyanate Prepolymer
(Mixture). Causes eye irritation. May
cause skin/respiratory irritation. May
cause skin and/or respiratory
sensitization after prolonged contact.
May be harmful if swallowed. Use only
in well ventilated areas. Deliberate
misuse by inhalation of vapors may
be harmful or fatal. Strictly follow all
usage, handling and storage
instructions.
HMIS
Health *2
Flammability 1
Reactivity 0
Personal Protection C
First Aid Measures
Eyes Hold eyelids apart and flush
thoroughly with water for 15 minutes.
Skin Remove contaminated clothing.
Wash skin thoroughly for 15 minutes with
soap and water. Inhalation Remove
to fresh air. Ingestion Do not induce
vomiting. Dilute with water. Contact
physician. In all cases contact a
physician immediately if symptoms
persist.
Further Information
Copies of the following publications are
available on our homepage
www.sikaindustry.com:
-Material Safety Data Sheets
-Technical Data Sheet
-Sika Primer Chart
-General guidelines for bonding and
sealing with Sika products

S
i
k
a
f
l
e
x

-
2
9
5

U
V

3

/

3

Further information available at:
www.sikaindustry.com

Sika Corporation
Industry Division
30800 Stephenson Highway
Madison Heights, MI 48071
USA
Tel. 248 577 0020
Fax 248 577 0810
In case of emergency call:
Chemtrec: 800-424-9300
International: 700-527-3887

For further information and advice
regarding transportation, handling,
storage and disposal of chemical
products, users should refer to the actual
Material Safety Data Sheets containing
physical, ecological, toxicological and
other safety related data. It is highly
recommended to read the actual Material
Safety Data Sheet before using the
product.

-KEEP OUT OF REACH OF CHILDREN
-NOT FOR INTERNAL CONSUMPTION
-FOR INDUSTRIAL USE ONLY
-KEEP CONTAINER TIGHTLY CLOSED

Packaging Information
Cartridge 10.5 fl. oz.
UniPac
Drum
Handling and Storage
Avoid direct contact. Wear personal
protective equipment (chemical resistant
goggles/gloves/clothing) to prevent direct
contact with skin and eyes. Use only in
well ventilated areas. Open doors and
windows during use. Use a properly
fitted NIOSH respirator if ventilation is
poor. Wash thoroughly with soap and
water after use. Remove contaminated
clothing and launder before reuse. Store
below 77F (25C) in a cool dry place
away from sunlight.
Clean Up
Use personal protective equipment
(chemical resistant gloves/
goggles/clothing). Without direct contact,
remove spilled or excess product and
placed in suitable sealed container.
Dispose of excess product and container
in accordance with applicable
environmental regulations.
Warranty
All information provided by Sika
Corporation (Sika) concerning Sika
products, including but not limited to, any
recommendations and advice relating to
the application and use of Sika products,
is given in good faith based on Sikas
current experience and knowledge of its
products when properly stored, handled
and applied under normal conditions in
accordance with Sikas instructions. In
practice, the differences in materials,
substrates, storage and handling
conditions, actual site conditions and
other factors outside of Sikas control are
such that Sika assumes no liability for
the provision of such information, advice,
recommendations or instructions related
to its products, nor shall any legal
relationship be created by or arise from
the provision of such information, advice,
recommendations or instructions related
to its products. The user of the Sika
product(s) must test the product(s) for
suitability for the intended application
and purpose before proceeding with the
full application of the product(s).

Sika reserves the right to change the
properties of its products without notice.
All sales of Sika product(s) are subject to
its current terms and conditions of sale,
which are available at www.sikacorp.com
or by calling 201-933-8800.

Prior to each use of any Sika product,
the user must always read and follow the
warnings and instructions on the
products most current Technical Data
Sheet, product label and Material Safety
Data Sheet, which are available at
www.sikaindustry.com. Nothing
contained in any Sika materials relieves
the user of the obligation to read and
follow the warnings and instruction for
each Sika product as set forth in the
current Technical Data Sheet, product
label and Material Safety Data Sheet
prior to product use.

Limited Material Warranty:
SIKA warrants this product for one year
from date of installation to be free from
manufacturing defects and to meet the
technical properties on the current
Technical Data Sheet if used as directed
within shelf life. User determines
suitability of product for intended use and
assumes all risks. Buyers sole remedy
shall be limited to the purchase price or
replacement of product exclusive of labor
or cost of labor. NO OTHER
WARRANTIES IMPLIED OR EXPRESS
SHALL APPLY INCLUDING ANY
WARRANTY OF MERCHANTABILITY
OR FITNESS FOR A PARTICULAR
PURPOSE. SIKA SHALL NOT BE
LIABLE UNDER ANY LEGAL THEORY
FOR SPECIAL OR CONSEQUENTIAL
DAMAGES. SIKA SHALL NOT BE
RESPONSIBLE FOR THE USE OF
THIS PRODUCT IN A MANNER TO
INFRINGE ON ANY PATENT OR ANY
OTHER INTELLECTUAL PROPERTY
RIGHTS HELD BY OTHERS.
T8000
7
HOMMEL-ETAMIC C8000 inductive
Application example: measurement of penetration
radii of crankshafts.
HOMMEL-ETAMIC T8000 C200-400
High performance contour evaluation with digital
scales in Z and X direction.
Options
full CNC functionality with motorized tilting
device and CNC software
certied qs-STAT
interface (AQDEF)
wavecontrol basic control panel
KN8 contour standard
GTR instrument table
System components
evaluation computer with 19 TFT at screen,
color printer, CD/DVD writer, and evaluation
software for contour measurement
motorized wavelift 400 measuring column
with automatic probing
waveline C120/C200 traverse unit
with incremental linear measuring system
tilting device for traverse unit with swivel
range of 45
inductive or digital contour probe incl. 2 probe arms
with carbide tip or ruby ball
granite plate with 10 mm T groove
MT1 XYO measuring table for holding the
workpieces (also available without)
calibration set
HOMMEL-ETAMIC C8000 / T8000 C
C8000 inductive C8000 digital T8000 C120-400 T8000 C200-400
Art. no. 1001 7064 Art. no. 1001 7065 Art. no. 1001 7066 Art. no. 1003 6457
Measuring range 20 mm 60 mm 60 mm 60 mm
Min. resolution 68 nm 50 nm 50 nm 50 nm
Vertical measuring principle inductive digital digital digital
Measuring range/horizontal res. 120 mm/0.1 m 120 mm/0.1 m 120 mm/0.1 m 200 mm/0.01 m
Vertical travel measuring column 400 mm 400 mm 400 mm 400 mm
Granite plate 780 x 500 mm 780 x 500 mm 780 x 500 mm 1000 x 500 mm
1000 x 500 mm Art. no. 1003 6585 Art. no. 1003 6585 Art. no. 1003 6585
granite plate upgrade
800 mm measuring Art. no. 1003 6584 Art. no. 1003 6584 Art. no. 1003 6584 Art. no. 1003 6584
column upgrade
Roughness measurement upgrade Art. no. 1004 7700 Art. no. 1004 7699
8465
Glass No.:
Date of Print
Page 1 of 2
02/03/2011
SCHOTT Electronic
Packaging GmbH
Christoph-Dorner-Strae 29
84028 Landshut Germany
Phone +49 (0)871 826 708
Fax +49 (0)871 826 710
www.schott.com/epackaging
Preliminary Data Sheet
Other grain size distributions available upon request.
The glass will be supplied as powder.
375 C
*10
Low melting Lead-Alumo-Borosilicate solder glass. Good match to materials
with a thermal expansion of 8,5 ...9,5 ppm/K.
-4
Temperature for viscosity (ISO 7884-6) of
10 566
10 460
4
7,6
C
C
dPas
dPas
Form of supply:
8,2 D
20 - 300
Transformation temperature (ISO 7884-8) 385 C
Density 5,4
Dielectric constant ( , 25C) 14,9
tan ( , 25C) 27
t
K100
Thermal expansion coefficient (ISO 7991)
g*cm
-3
*10
-6 -1
K
G
Physical properties:
d 12
50 d m Powder in standard grain size:
d 63
99 d m
(Mean values of specified tolerance ranges)
1MHz
1MHz
8465
Glass No.:
Date of Print
Page 2 of 2
02/03/2011
SCHOTT Electronic
Packaging GmbH
Phone +49 (0)871 826 708
Fax +49 (0)871 826 710
Preliminary Data Sheet
Firing Conditions: Burn out binder and Pre-Glazing
Firing Conditions: Vitreous seals and glazings
0
100
200
300
400
500
600
0 100 200 300 400
Time [min]
T
e
m
p
e
r
a
t
u
r
e

[
C
]
0
100
200
300
400
500
600
0 50 100 150 200
Time [min]
T
e
m
p
e
r
a
t
u
r
e

[
C
]
( In case of paste )
( In case of powder or preglazed material )
1. heating up: <10 K/min to 520C
2. holding time at 520C ; 30 min
3. cooling down: <5 K/min to 25C
Supplementary Information
Chemical Composition (wt.%)
Al O
2 3
10-50
SiO
2
1-10
PbO >50
B O
2 3
10-50
Date of Print 02/03/2011
SCHOTT Electronic
Packaging GmbH
Phone +49 (0)871 826 708
Fax +49 (0)871 826 710
8465
Glass No:
G017-393
Glass No.:
Date of Print
Page 1 of 2
02/03/2011
SCHOTT Electronic
Packaging GmbH
Phone +49 (0)871 826 708
Fax +49 (0)871 826 710
Data Sheet
Other grain size distributions available upon request.
The glass will be supplied as powder.
Electric volume resistivity
log ( 11,8 U>: cm]) at 150C
305 C
Young's modulus E 58 GPa
*10
Non crystallizing low melting composite solder glass with a lead borate glass
and an inert ceramic filler. The thermal expansion coefficient is well matched
to Alumina.
log ( 9,3
log ( 7,3
U>: cm]) at 250C
U>: cm]) at 350C
-4
Temperature for viscosity (ISO 7884-6) of
10 370
7,6
C dPas
Form of supply:
6,6 D
20 - 300
Transformation temperature (ISO 7884-8) 320 C
Density 4,8
Dielectric constant ( , 25C) 11,6
tan ( , 25C) 15
t
K100
Thermal expansion coefficient (ISO 7991)
g*cm
-3
*10
-6 -1
K
G
Physical properties:
d 12
50 d m Powder in standard grain size:
d 63
99 d m
(Mean values of specified tolerance ranges)
1MHz
1MHz
G017-393
Glass No.:
Date of Print
Page 2 of 2
02/03/2011
SCHOTT Electronic
Packaging GmbH
Phone +49 (0)871 826 708
Fax +49 (0)871 826 710
Data Sheet
Firing Conditions: Burn out binder and Pre-Glazing
Firing Conditions: Vitreous seals and glazings
0
50
100
150
200
250
300
350
400
450
0 50 100 150 200
Time [min]
T
e
m
p
e
r
a
t
u
r
e

[
C
]
0
50
100
150
200
250
300
350
400
450
0 50 100 150
Time [min]
T
e
m
p
e
r
a
t
u
r
e

[
C
]1. heating up: <10 K/min to 420C
Supplementary Information
Chemical Composition (wt.%)
1-10 Li O
2
Al O
2 3
1-10
SiO
2
1-10
PbO >50
B O
2 3
10-50
Date of Print 02/03/2011
SCHOTT Electronic
Packaging GmbH
Phone +49 (0)871 826 708
Fax +49 (0)871 826 710
G017-393
Glass No:
Appendixes
9.4 Appendix D: Catalogs.
Contents:

- Trelleborg O-rings catalog.
- Swagelok fittings catalog.
Temperature range
-100 -50 0 50 100 150 200 250 300 350
The temperature ranges apply only
in connection with media that are
compatible with the respective
elastomers
Operating temperature
range
Only to be achieved under particular conditions with special
materials
Temperature (C)
Figure 4 Temperature range of various elastomers
General field of application
Elastomer materials are used to cover a large number of
fields of application. Details regarding resistance in special
media are shown in chapter Chemical compatibility,
page 9.
The various elastomers can be characterised as follows:
NBR (Nitrile Butadiene Rubber):
The properties of the Nitrile Rubber depend mainly on the
ACN content which ranges between 18% and 50%. In
general they show good mechanical properties. The
operating temperatures range between -30C and +100C
(for a short period of time up to +120C). Suitable
formulated NBR can be used down to -60C.
NBR is mostly used with mineral based oils and greases.
FKM (Fluorocarbon Rubber)
Depending on structure and fluorine content FKM
materials can differ with regards to their chemical
resistance and cold-flexibility.
FKM is known especially for its non-flammability, low gas
permeability and excellent resistance to ozone, weathering
and aging.
The operating temperatures of the Fluorocarbon Rubber
range between -20C and +200C (for a short period of
time up to +230C). Suitable formulated FKM can be used
down to -35C. FKM is also often used with mineral based
oils and greases at high temperatures.
EPDM (Ethylene Propylene Diene Rubber)
EPDM shows good heat, ozone and aging resistance. In
addition they also exhibit high levels of elasticity, good low
temperature behaviour as well as good insulating
properties.
The operating temperatures of applications for EPDM
range between -45C and +150C (for a short period of
time up to +175C). With sulphur cured types the range is
reduced to -45C and +120C (for short period of time up to
+150C).
EPDM can often be found in applications with brake fluids
(based on glycol) and hot water.
ORing
Latest information available at www.tss.trelleborg.com
8
Edition June 2008
HNBR (Hydrogenated Nitrile Butadiene Rubber)
HNBR is made via selective hydrogenation of the NBR
butadiene groups. The properties of the HNBR rubber
depend on the ACN content which ranges between 18%
and 50% as well as on the degree of saturation. HNBR
shows good mechanical properties.
The operating temperature of HNBR ranges between -30C
and +140C (for a short period of time up to +160C) in
contact with mineral oils and greases. Special types can be
used down to -40C.
VMQ (Silicone Rubber)
VMQ shows excellent heat resistance, cold flexibility,
dielectric properties and especially good resistance to
weather, ozone an UV rays.
Specific VMQ formulations are resistant to aliphatic engine
and gear oils, water up to +100C and high-molecular
chlorinated hydrocarbons. The temperature range is
between -60C and +200C (temporary up to +230C).
FVMQ (Fluorosilicone Rubber)
FVMQ has a good heat resistance, very good low
temperature flexibility, good electrical properties and
excellent resistance to weather, ozone and UV rays.
FVMQ shows a significant better chemical resistance than
standard Silicone especially in hydrocarbons, aromatic
mineral oils, fuel and low molecular aromatic
hydrocarbons e.g. Benzene and Toluene. The temperature
range is between -55C and +175C (temporary up to
+200C).
CR (Chloroprene Rubber)
In general the CR materials show relatively good
resistances to ozone, weathering, chemicals and aging.
Also they show good non-flammability, good mechanical
properties and cold flexibility.
The operating temperatures range between -40C and
+100C (for a short period of time up to +120C). Special
types can be used down to -55C.
CR materials are found in sealing applications such as
refrigerants, for outdoor applications and in the glue
industry.
ACM (Polyacrylate Rubber)
ACM shows excellent resistance to ozone, weathering and
hot air, although it shows only a medium physical strength,
low elasticity and a relatively limited low temperature
capability.
The operating temperatures range from -20C and +150C
(for a short period of time up to +175C). Special types can
be used down to -35C.
ACM-materials are mainly used in automotive applications
which require special resistance to lubricants containing
many additives (incl. sulphur) at high temperatures.
FFKM (Perfluoro Rubber)
Perfluoroelastomers show broad chemical resistance similar
to PTFE as well as good heat resistance. They show low
swelling with almost all media.
Depending on the material the operating temperatures
range between -25C and +240C. Special types can be used
up to +325C.
Applications for FFKM can be mostly found in the chemical
and process industries and in all applications with either
aggressive environments or high temperatures.
Polyurethane (Zurcon
Polyurethane)
Polyurethanes are an exceptionally complex material
group. They are individually designed and fit various
applications needs. Therefore it is not possible to unify
the materials properties.
Zurcon
polyurethane materials from Trelleborg Sealing

Solutions are customized to appropriate applications and
stand out due to their excellent elastic properties and
optimum abrasion resistance. Outstanding tensile strength,
low compression set and good resistance to O
2
and O
3
are
further significant characteristics. Depending on the
individual Zurcon
polyurethane type the application

temperature range from below -50C up to +110C,
temporary even higher, is feasible.
Chemical compatibility
For the pre-selection of a suitable material group a
comprehensive chemical compatibility guide is available.
This can be downloaded from our website
www.tss.trelleborg.com or you can contact your local
Trelleborg Sealing Solutions company for further details.
It is important to recognise that when using this guide, the
ratings shown are based on published data and immersion
tests. These tests are conducted under laboratory
conditions predominantly at room temperature and may
not represent adequately the conditions in the field.
Relative short term laboratory tests may not pick up all
the additives and impurities which may exist in long term
service applications.
Care must be taken to ensure that all aspects of the
application are considered carefully before a material is
selected. For example at elevated temperatures some
aggressive fluids can cause a much more marked effect
on an elastomer than at room temperature.
Physical properties as well as fluid compatibility need to be
considered. Compression set, hardness, abrasion resistance
and thermal expansion can influence the suitability of a
material for a particular application.
It is recommended that users conduct their own tests to
confirm the suitability of the selected material for each
application.
Our experienced technical staff can be consulted for
further information on specific applications.
ORing
Edition June 2008
9
Table IX Material specification for standard HNBR
HNBR 70
Shore A
partially saturated
HNBR 75
Shore A
partially saturated
Hardness DIN 53 505
ASTM D 2240
Shore A 70 5 75 5
Tensile strength DIN 53 504
ASTM D 412
MPa
N/mm
> 15 > 15
Elongation at break DIN 53 504
ASTM D 412
% > 250 > 250
Compression set 24h / 125 C DIN ISO 815B
ASTM D 395B
% < 35 < 35
Heat aging 72h / 150 C DIN 53 508
ASTM D 573
Change of hardness Shore A max +10 max +10
Change of tensile strength % max -30 max -30
Change of elongation at break % max -30 max -30
Resistance in ASTM-Oil # 1 72h / 150 C DIN 53 521
ASTM D 471
Change of hardness Shore A max +10 max +10
Change of volume % max -10 max -10
Resistance in ASTM-Oil # 3 72h / 150 C DIN 53 521
ASTM D 471
Change of hardness Shore A max -15 max -15
Change of volume % max +20 max +20
Temperature range
Maximum and minimum operating temperatures
depend on the specific application criteria.
-30 C to +130 C -30 C to +130 C
Trelleborg Sealing Solutions offers various materials, which
provide additional advantages, in addition to the standard
materials previously described. The advantages include a
wide range of available molds, special operating
temperature range, special media resistance and
institutional approvals for the portable water,
pharmaceutical and beverage industries.
The following table shows preferred materials, which are
characterized by their wide spectrum of use. They can be
used for standard applications as well as for special
industrial applications.
Table X Preferred materials
Material
Type
Hardness
Shore A
( 5)
Color Operating
temperature
range
Material
code
Description
NBR
Nitrile
Butadiene
Rubber
70 black -30 C to
+100 C
N7083 Preferable for sizes acc. to AS 568 B, preferably used for energizing
elements, good overall performance
-50 C to
+100 C
N7T40 Polar, extremely good low temperature properties, preferably
used for static applications in mineral oil and for energizing elements,
preferable for sizes acc. to AS 568 B
-30 C to
+100 C
N7003 Preferable for metric sizes, good overall performance, wide range of
molds available
-30 C to
+100 C
N7024 Good overall performance, preferable for large quantities
-30 C to
+100 C
N7027 Preferable for potable water applications: KTW, ACS, NSF61, NSF51,
DIN EN 549: 0 C / 80 C, W270, FDA, also suitable for use in gas
applications
90 black -25 C to
+100 C
N9002 Good overall performance, wide range of molds available
ORing
18
Edition June 2008
Material
Type
Hardness
Shore A
( 5)
Color Operating
temperature
range
Material
code
Description
HNBR
Hydrogenated
Nitrile
Butadiene
Rubber
70 black -30 C to
+140 C
H7671 Good overall performance, wide range of molds available
-35 C to
+140 C
H7503 Wide range of operating temperature, good resistance to mineral
oil, good overall performance
FKM
Fluorocarbon
Rubber
70 green -20 C to
+200 C
V70GA Preferable for sizes acc. to AS 568 B, preferably used for energizing
elements, good overall performance, DVGW, BAM
-18 C to
+200 C
V70G2 Preferable for sizes acc. to AS 568 B, good overall performance
75 black -20 C to
+200 C
VC009 Preferable for sizes acc. to BS 4518 (metric), standard FKM
80 green -18 C to
+200 C
V80G2 Good overall performance, wide range of molds available
black -18 C to
+200 C
V8003 Good overall performance, wide range of molds available
-20 C to
+200 C
V8605 For pharmaceutical and food and beverage industries, FDA
90 green -15 C to
+200 C
V90G1 Good overall performance, wide range of molds available
black -15 C to
+200 C
V9670 Good overall performance, wide range of molds available
EPDM
Ethylene
Propylene
Diene Rubber
70 black -45 C to
+150 C
E7502 Peroxide cured, for pharmaceutical and food and beverage industries,
KTW, WRAS, FDA, USP Class VI, USP 26, plasticizer content < 3 %
-45 C to
+125 C
E7002 Sulfur cured, standard EPDM, wide range of molds available
-45 C to
+140 C
E7515 Peroxide cured, standard EPDM, wide range of molds available
-45 C to
+150 C
E7T41 Peroxide cured, extremely low compression set in hot water and
steam. Excellent resistance to ozone, can be used in contact with copper
and brass
-45 C to
+140 C
E7518 Peroxide cured, preferable for the use in potable water: KTW, WRAS,
FDA, NSF61, NSF51, W270, W534, EN 681, ACS, USP Class VI,
USP 26, plasticizer content < 1 %
VMQ
Methyl Vinyl
Silicon
Rubber
60 red -50 C to
+200 C
S60R1 Good overall performance, wide range of molds available
70 red -50 C to
+200 C
S70R2 Sulfur cured, good overall performance, wide range of molds
available
The stated operating temperatures exclude any kind of
load. Actual operating temperatures may differ depending
on media and load type.
At time of publication the information contained in this
literature, including availability or institutional approvals,
is believed to be correct and accurate.
Further materials are available on request.
ORing
Edition June 2008
19
ORing as a rotary seal
In some applications, e.g. with short running periods, the
ORing can also be used as a rotary seal for sealing shafts. In
this case, the following points should be observed:
In order to be able to function as a rotary seal, ORings
must be installed in accordance with specific guidelines, the
rotary seal principle.
The rotary seal principle is based on the fact that an
elongated elastomer ring contracts when heated (Joule
effect). With the normal design criteria the ORing inside
diameter d
1
will be slightly smaller than the shaft diameter,
and the heat generated by friction would cause the ring to
contract even more. This results in a higher pressure on the
rotating shaft so that a lubricating film is prevented from
forming under the seal and even higher friction occurs. The
result would be increased wear and a premature failure of
the seal.
Using the rotary seal principle, this is prevented by the seal
ring being selected so that its inside diameter is
approximately 2 to 5% larger than the shaft diameter to
be sealed. The installation in the groove means that the
seal ring is compressed radially and is pressed against the
shaft by the groove diameter. The seal ring is thus slightly
corrugated in the groove, a fact which helps to improve the
lubrication.
Special materials are available for rotary seal applications.
Trelleborg Sealing Solutions does not recommend the use
of ORings as rotary seals. Please contact your local
Trelleborg Sealing Solutions company for further details.
Technical data
ORings can be used in a wide range of applications.
Temperature, pressure and media determine the choice of
appropriate materials. In order to be able to assess the
suitability of the ORing as a sealing element for a given
application, the interaction of all the operating parameters
have to be taken into consideration.
Working Pressure
Static application
- up to 5 MPa for ORings with inside diameter > 50 mm
without Back-up Ring
up to 10 MPa for ORings with inside diameter
- < 50 mm without Back-up Ring
(depends on the material, the cross section and the
clearance)
- up to 40 MPa with Back-up Ring
- up to 250 MPa with special Back-up Ring
Please note the permissible extrusion gaps.
Dynamic application
- Reciprocating up to 5 MPa without Back-up Ring
- Higher pressures with Back-up Ring
Speed
Reciprocating up to 0.5 m/s
Rotating up to 0.5 m/s
Depending on material and application.
Temperature
From -60 C to +325 C
Depending on material and media resistance.
When assessing the application criteria, the peak and
continuous operating temperature and the running period
must be taken into consideration. For rotating applications
the temperature increase due to frictional heat must be
taken into account.
Media
With the wide range of the available materials, each with
different properties, it is possible to seal against practically
all liquids, gases and chemicals. Please note when selecting
the most suitable material the information in chapter
B.1 Materials, and in our ORing Material Guide.
ORing
24
Edition June 2008
Installation recommendations
d2
b3 b2 h
b1
r1
r1
t
1
S
t
S
t
1
b
4
Figure 25 Installation drawing
Radial clearance, see chapter Design Recommendations, page .
Surface specifications, see chapter Design Recommendations, page .
Groove width b2 and b3: When using Back-up Rings the groove is to be widened by the corresponding Back-up Ring
thickness (b2: one Back-up Ring, b3:two Back-up Rings).
Table XV Installation dimensions
Cross section
d2
Radial installation Axial installation Radius
1)
Groove depth Groove width Groove depth Groove width
Dynamic
t1 +0.05
Static
t +0.05 b1 +0.2 h +0.05 b4 +0.2 r1 0.2
0.50 - 0.35 0.80 0.35 0.80 0.20
0.74 - 0.50 1.00 0.50 1.00 0.20
1.00 - 0.70 1.40 0.70 1.40 0.20
1.02 - 0.70 1.40 0.70 1.40 0.20
1.20 - 0.85 1.70 0.85 1.70 0.20
1.25 - 0.90 1.70 0.90 1.80 0.20
1.27 - 0.90 1.70 0.90 1.80 0.20
1.30 - 0.95 1.80 0.95 1.80 0.20
1.42 - 1.05 1.90 1.05 2.00 0.30
1.50 1.25 1.10 2.00 1.10 2.10 0.30
1.52 1.25 1.10 2.00 1.10 2.10 0.30
1.60 1.30 1.20 2.10 1.20 2.20 0.30
1.63 1.30 1.20 2.10 1.20 2.20 0.30
1.78* 1.45 1.30 2.40 1.30 2.60 0.30
1.80 1.45 1.30 2.40 1.30 2.60 0.30
1.83 1.50 1.35 2.50 1.35 2.60 0.30
ORing
28
Edition June 2008
Cross section
d2
1)
Dynamic
t1 +0.05
Static
t +0.05 b1 +0.2 h +0.05 b4 +0.2 r1 0.2
1.90 1.55 1.40 2.60 1.40 2.70 0.30
1.98 1.65 1.50 2.70 1.50 2.80 0.30
2.00 1.65 1.50 2.70 1.50 2.80 0.30
2.08 1.75 1.55 2.80 1.55 2.90 0.30
2.10 1.75 1.55 2.80 1.55 2.90 0.30
2.20 1.85 1.60 3.00 1.60 3.00 0.30
2.26 1.90 1.70 3.00 1.70 3.10 0.30
2.30 1.95 1.75 3.10 1.75 3.10 0.30
2.34 1.95 1.75 3.10 1.75 3.10 0.30
2.40 2.05 1.80 3.20 1.80 3.30 0.30
2.46 2.10 1.85 3.30 1.85 3.40 0.30
2.50 2.15 1.90 3.30 1.85 3.40 0.30
2.62* 2.25 2.00 3.60 2.00 3.80 0.30
2.65 2.25 2.00 3.60 2.00 3.80 0.30
2.70 2.30 2.05 3.60 2.05 3.80 0.30
2.80 2.40 2.10 3.70 2.10 3.90 0.60
2.92 2.50 2.20 3.90 2.20 4.00 0.60
2.95 2.50 2.20 3.90 2.20 4.00 0.60
3.00 2.60 2.30 4.00 2.30 4.00 0.60
3.10 2.70 2.40 4.10 2.40 4.10 0.60
3.50 3.05 2.65 4.60 2.65 4.70 0.60
3.53* 3.10 2.70 4.80 2.70 5.00 0.60
3.55 3.10 2.70 4.80 2.70 5.00 0.60
3.60 3.15 2.80 4.80 2.80 5.10 0.60
4.00 3.50 3.10 5.20 3.10 5.30 0.60
4.50 4.00 3.50 5.80 3.50 5.90 0.60
5.00 4.40 4.00 6.60 4.00 6.70 0.60
5.30 4.70 4.30 7.10 4.30 7.30 0.60
5.33* 4.70 4.30 7.10 4.30 7.30 0.60
5.50 4.80 4.50 7.10 4.50 7.30 0.60
5.70 5.00 4.60 7.20 4.60 7.40 0.60
6.00 5.30 4.90 7.40 4.90 7.60 0.60
6.50 5.70 5.40 8.00 5.40 8.20 1.00
6.99* 6.10 5.80 9.50 5.80 9.70 1.00
7.00 6.10 5.80 9.50 5.80 9.70 1.00
7.50 6.60 6.30 9.70 6.30 9.90 1.00
8.00 7.10 6.70 9.80 6.70 10.00 1.00
8.40 7.50 7.10 10.00 7.10 10.30 1.00
9.00 8.10 7.70 10.60 7.70 10.90 1.50
9.50 8.60 8.20 11.00 8.20 11.40 1.50
ORing
Edition June 2008
29
Cross section
d2
1)
Dynamic
t1 +0.05
Static
t +0.05 b1 +0.2 h +0.05 b4 +0.2 r1 0.2
10.00 9.10 8.60 11.60 8.60 12.00 2.00
12.00 11.00 10.60 13.50 10.60 14.00 2.00
n * Preferred sizes
1) If a Back-up Ring is used the recommended radius r1 should
always be r1=0.25 0.2mm.
The given installation dimensions cannot be used for FFKM
materials (Isolast
). Please use the Isolast
brochure or contact
our specialists for further details.
ORing
30
Edition June 2008
Gaugeable SAF 2507 Super Duplex Tube Fittings 3
Ordering Information and Dimensions
Dimensions are for reference only and are subject to change.
Dimensions are shown with Swagelok tube ftting nuts fnger-tight. For Swagelok nut dimensions, see page 6.
The E dimension is the minimum nominal opening.
CAD templates are available on www.swagelok.com.
Unions
D D
A
E
Tube
OD
in.
Ordering
Number
Dimensions, in. (mm)
A D E
1/4 2507-400-6 1.61 (40.9) 0.60 (15.2) 0.19 (4.8)
3/8 2507-600-6 1.77 (45.0) 0.66 (16.8) 0.28 (7.1)
1/2 2507-810-6 2.02 (51.3) 0.90 (22.9) 0.41 (10.4)
5/8 2507-1010-6 2.11 (53.5) 0.96 (24.4) 0.50 (12.7)
3/4 2507-1210-6 2.11 (53.5) 0.96 (24.4) 0.62 (15.9)
Bulkhead Unions
D D
A
E
F fat F fat F fat
Tube
OD
in.
Ordering
Number
A D E F
Panel
Hole
Size
Max
Panel
Thickness
1/4 2507-400-61 2.27 (57.7) 0.60 (15.2) 0.19 (4.8) 5/8 29/64 0.40 (10.2)
3/8 2507-600-61 2.45 (62.2) 0.66 (16.8) 0.28 (7.1) 13/16 37/64 0.44 (11.2)
1/2 2507-810-61

2.80 (71.1) 0.90 (22.9) 0.41 (10.4) 1 1/16 49/64 0.50 (12.7)
5/8 2507-1010-61 3.11 (78.9) 0.96 (24.4) 0.50 (12.7) 1 3/16 1 1/64 0.66 (16.8)
3/4 2507-1210-61 3.33 (84.5) 0.96 (24.4) 0.62 (15.9) 1 3/8 1 9/64 0.75 (19.0)
Straight Fittings
NPT
D
A
E
F fat
Tube
OD
in.
NPT
Size
Ordering
Number
A D E F
1/4
1/4
1/2
2507-400-1-4
2507-400-1-8
1.49 (37.8)
1.76 (44.7)
0.60 (15.2) 0.19 (4.8)
9/16
7/8
3/8
1/4
3/8
1/2
2507-600-1-4
2507-600-1-6
2507-600-1-8
1.57 (39.9)
1.57 (39.9)
1.82 (46.2)
0.66 (16.8) 0.28 (7.1)
5/8
11/16
7/8
1/2
1/4
3/8
1/2
2507-810-1-4
2507-810-1-6
2507-810-1-8
1.71 (43.4)
1.71 (43.4)
1.93 (49.0)
0.90 (22.9)
0.28 (7.1)
0.38 (9.7)
0.41 (10.4)
13/16
13/16
7/8
5/8 1/2 2507-1010-1-8 1.99 (50.5) 0.96 (24.4) 0.47 (11.9) 1 1/16
3/4
3/4
1
2507-1210-1-12
2507-1210-1-16
1.99 (50.5)
2.25 (57.1)
0.96 (24.4) 0.62 (15.9)
1 3/16
1 3/8
Male Connectors
D
A
E
F fat
O-ring
May be back drilled to larger ID at straight thread end.
Standard O-ring material is 90 durometer fluorocarbon FKM.
Tube
OD
in.
SAE/MS
Thread
Size
Ordering
Number
Uniform
O-ring
Size
A D E
F
1/4
7/16-20
9/16-18
2507-400-1-4ST
2507-400-1-6ST
1.34 (34.0)
1.40 (35.6)
0.60 (15.2) 0.19 (4.8)
9/16
11/16
904
906
3/8 9/16-18 2507-600-1-6ST 1.46 (37.1) 0.66 (16.8) 0.28 (7.1) 11/16 906
1/2
9/16-18
3/4-16
2507-810-1-6ST
2507-810-1-8ST
1.54 (39.1)
1.65 (41.9)
0.90 (22.9)
0.28 (7.1)
0.41 (10.3)
13/16
7/8
906
908
5/8 7/8-14 2507-1010-1-10ST 1.77 (44.9) 0.96 (24.4) 0.50 (12.7) 1 1/16 910
3/4 1 1/16-12 2507-1210-1-12ST 1.93 (49.0) 0.96 (24.4) 0.62 (15.6) 1 3/8 912
SAE/MS Straight Thread (ST)

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Hochschule Karlsruhe Technik und Wirtschaft

Surfaces: materials and coatings.

-200 and SikaTack

Series - Adhesives and Sealants

Cleaner P or water based cleaners, steam

, actual Product Data Sheets, etc.

-295 UV black is intended to be

-295 UV white is intended to be

-Aktivator. Refer to the

-295 UV cures by reaction with

-295 UV is resistant to fresh

Remover-208 or another suitable

-295 UV may be overpainted

-295UV should not be exposed

polyurethane materials from Trelleborg Sealing

polyurethane type the application

). Please use the Isolast

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