Documentos de Académico
Documentos de Profesional
Documentos de Cultura
List of Papers
I On the role of tribofilm formation on the alumina drive
components of an ultrasonic motor
J. Olofsson, F. Lindberg, S. Johansson, S. Jacobson, Wear, 267
(2009) 1295-1300
II The influence of grain size and surface treatment of the tribofilm
formation on alumina components
J. Olofsson, S. Jacobson, submitted to: Journal of American
Ceramic Society
III Influence from humidity on the alumina friction drive system of
an ultrasonic motor
J. Olofsson, S. Johansson, S. Jacobson, Tribology International,
42 (2009) 1467-1477
IV Tribofilm formation of lightly loaded self mated alumina contacts
J. Olofsson, U. Bexell, S. Jacobson, submitted to Wear
V On the influence from micro topography of PVD coatings on
friction behaviour, material transfer and tribofilm formation
J. Olofsson, J. Gerth, H. Nyberg, U. Wiklund, S. Jacobson, Wear
271 (2011) 2046-1057
VI Evaluation of silicon nitride as a wear resistant and resorbable
alternative for total hip joint replacement
J. Olofsson, T. M. Grehk, T. Berlind, C. Persson, S. Jacobson, H.
Engqvist, submitted to: Journal of Biomaterials Research part B
VII Fabrication and evaluation of Si
x
N
y
coatings for total joint
replacements
J. Olofsson, M. Pettersson, N. Teuscher, A. Heilmann, K.
Larsson, K. Grandfield, C. Persson, S. Jacobson, H. Engqvist,
submitted to: Journal of Materials Science Materials in
Medicine
Reprints were made with permission from the publishers.
Authors Contribution to the Publications
Paper I Major part of planning, major part of experimental work
excluding TEM analyses, major part of evaluation and
writing.
Paper II Major part of planning, experimental work, evaluation and
writing.
Paper III Major part of planning, experimental work, evaluation and
writing.
Paper IV Major part of planning, major part of experimental work
excluding XPS and SIMS analyses, major part of evaluation
and writing.
Paper V Part of planning, part of experimental work excluding coating
deposition and XPS analyses, part of evaluation and major
part of writing.
Paper VI Major part of planning, major part of experimental work
excluding blood plasma incubations XPS, XRD, and ICP-MS
analyses, major part of evaluation and writing.
Paper VII Major part of planning, part of experimental work excluding
DFT calculations, XRD and TEM analyses, major part of
evaluation and writing.
Parts of this thesis have been previously published (Papers I, III and V).
These papers are reprinted with the kind permission from Elsevier.
Contents
Introduction.....................................................................................................9
Aim of the Thesis ................................................................................10
Overview of Tribofilms ................................................................................11
Friction and Wear of Ceramics .....................................................................13
Wear Mechanisms ...............................................................................13
Influence of Atmosphere .....................................................................14
Ceramics .......................................................................................................15
Ceramic Coatings ................................................................................16
Coatings ........................................................................................................17
PVD Sputter Coating........................................................................17
Coating Deposition..............................................................................18
Friction Drive System of an Ultrasonic Motor .............................................20
Tribology in Hip Joint Replacements ...........................................................22
Hip Joint Replacements .......................................................................22
Biotribology.........................................................................................23
Tribological and Mechanical Testing ...........................................................25
Bench Testing......................................................................................25
Ball-on-Disc Test.................................................................................26
Nanoindentaion....................................................................................27
Solubility Tests of Silicon Nitride .......................................................27
Surface Analysis ...........................................................................................28
Surface Characterisation......................................................................28
Chemical Surface Analysis..................................................................29
Tribofilm Formation, Friction and Wear of Alumina against Alumina........31
Tribofilm Formation on Alumina Surfaces .........................................31
Tribofilm Formation in Water and Different Humidity.......................37
Hardness of the Tribofilm....................................................................38
Chemical Composition of the Tribofilm..............................................39
Friction.................................................................................................40
Friction Behaviour and Tribofilm Formation of TaC/a-C Coating...............43
Friction, Wear and Solubility of Silicon Nitride for Total Hip Joint
Replacements ................................................................................................46
Evaluation of Bulk Silicon Nitride ......................................................46
Evaluation of Si
x
N
y
Coatings...............................................................49
Conclusions...................................................................................................53
Sammanfattning p svenska (Summary in Swedish) ....................................55
Acknowledgements.......................................................................................58
References.....................................................................................................60
9
Introduction
Friction, wear and lubrication have to be considered in most everyday situa-
tions where physical movement is of importance. The science and technol-
ogy of interacting surfaces in relative motion, which encompasses friction,
wear and lubrication, is called Tribology [1]. This means that knowledge of
tribology can also be applied for development of sports and sports equip-
ment.
For example, football shoes have studs which control the grip, i.e. the
friction between the shoes and the grass. However, if it rains, water will act
as a lubricant and the friction between the grass and the shoes decreases. If
the grass has dried but not the soil, the soil under the grass is the most easily
sheared material, and then the shearing takes place in the soil and yet another
friction level will apply. In addition, the surface properties could change
over time. Grass and soil could adhere to the shoes, smoothen the surfaces
and thus change the friction behaviour. Further, it should be considered that
the wear of the football field increases when the soil is softer. Contrastingly,
if the field is hard and contains a lot of sand and stones, the studs will be
worn and hence the friction decreases. In conclusion, in order to understand
the friction and wear behaviour it is of high importance to consider the sur-
face properties as they will develop over time due to the tribological contact.
The initial surfaces will always change.
Friction arises as a resistance to motion when a solid surface moves over
another surface. The tangential friction force (F
F
) is proportional to the nor-
mal load (F
N
) by the coefficient of friction (), therefore the friction equation
can be expressed as:
N
F
F
F
(1)
This proportional law is called the First Law of Friction by Amonton 1699
[1]. The coefficient of friction depends on the materials in contact, and will
change with time as the surfaces change. At each point of contact, the softest
material will deform and the material with lowest shear strength ( ) will be
sheared.
However, when the surrounding conditions change, e.g. a lubricant is
added (water on grass), the temperature changes (different shear strength of
10
the soil), and so on, the coefficient of friction will change. The friction is not
only a parameter for the original materials in contact, it is a parameter for the
whole, dynamic system! The materials in contact have to be well adapted to
the system and therefore materials science is essential for tribology. In terms
of football, different types of shoes and materials are used for different
grounds to achieve the optimal friction between the ground and the shoe.
The optimal friction is different for different systems. To reduce the en-
ergy losses in machine elements, the friction should be low. A low friction is
also desired in hip joints to facilitate body movement. However, the optimal
friction is high in an ultrasonic motors friction drive system in order to
transfer movement.
Aim of the Thesis
The aim of this thesis is to improve the function of ultrasonic motors, hip
joint replacements and low-friction applications using ceramic materials and
coatings. The investigations focus on understanding the friction and wear
mechanisms of ceramic surfaces, as well as on acquiring knowledge about
the properties of the new surfaces created during wear. Ultimately, this un-
derstanding can be used to develop ceramic systems offering both high and
low friction, while minimising material losses.
11
Overview of Tribofilms
The surfaces of two bodies that slide against each other are subjected to high
local stresses and pressures. This results in local shear deformation and frac-
ture of the surfaces and locally high temperatures can arise. The high tem-
peratures can accelerate chemical reactions on the surfaces or even melt the
surfaces locally. These conditions are not only destructive to the surface,
they are also necessary for the formation of new surface compounds, i.e.
tribofilms [2]. These compound layers, or tribofilms, give the surfaces new
tribological properties by changing the surface topography, chemistry and
mechanical properties. Jacobson and Hogmark [2] divide the tribofilm for-
mation into two groups: Transformation Type Tribofilms and Deposition
Type Tribofilms. Transformation Type films includes transformation of the
original surface by plastic deformation, phase transformations, diffusion,
etc., without any material transfer, see Figure 1a. In contrast, Deposition
Type films are formed by molecules fed from the counter surface, the envi-
ronment, or by wear debris, exemplified in Figure 1b,c and Figure 2.
Figure 1. Schematic image of tribofilms. The arrows indicate the sliding direction of
the bodies; (a) Transformation Type, the lower surface have transformed, chemically
or mechanically; (b) Deposition Type, wear particles from both surfaces has formed
a tribofilm on the lower surface; (c) Deposition Type, the surface has reacted with
the environment during contact and formed a tribofilm of chemical reaction prod-
ucts.
12
Figure 2. Tribofilm on a steel ball surface, formed by agglomeration and tribo-
sintering of wear debris from the ceramic coating on the counter surface.
Tribofilms often act as protective layers on a surface [3-5]. Therefore, it is
common to design surfaces or lubricants to achieve a certain tribofilm.
The deposition of low-friction coatings (such as diamond like carbon
(DLC) coatings) is one way to control the friction and wear properties by
tribofilm formation. Often one surface is coated and slides against a counter
steel surface. During running in, coating material adheres to the steel sur-
face, i.e. forms a tribofilm. Thereafter, the sliding takes place in the easily
sheared layers between the coated surface and the tribofilm. This decreases
the friction and protects the steel surface from wear, while the wear rate of
the coating reaches a low steady state level [6].
Most of the lubricants used in engines contain additives. Some of these
additives are used in order to form a tribofilm on the steel surface. A tribo-
film can be chemically formed by reactions between the lubricant and the
solid surfaces. The most frequently used additive to preserve the steel sur-
faces from wear is zinc dialkyldithiophosphate (ZDDP) [7,8]. At high pres-
sures, phosphates are formed and adsorb to the steel surface which in turn
protects the surface from wear.
There are also unwanted tribofilms, for example galling on forming tools.
Galling occurs when lumps of work material adhere to the forming tool and
cause damage to the next work material [2,9]. This kind of tribofilm forma-
tion is often prevented by decreasing the surface roughness of the forming
tool [10].
13
Friction and Wear of Ceramics
Ceramics are used in a wide range of applications, both in lubricated and
unlubricated contacts. Due to their hardness and high wear resistance,
ceramics are often used in applications such as water pump bearings, ball
bearings, cutting tools, etc. [11,12]. Ceramics are relatively inert and are
therefore suitable in harsh chemical environments as well as in medical ap-
plications. Alumina (Al
2
O
3
), zirconia (ZrO
2
), silicon carbide (SiC) and sili-
con nitride (Si
3
N
4
) are some of the most common sintered bulk ceramics
used for engineering applications. To overcome the low ductility of bulk
ceramics, ceramics are commonly deposited as thin coatings on more ductile
materials. The ductile bulk withstands high mechanical stresses while the
coatings improve the hardness and wear resistance of the surface.
One of the main advantages of using ceramics against ceramics in unlu-
bricated contacts is that the chemical bonds between the surfaces are easier
to break than the metallic bonds that form between clean metal surfaces.
When metal slides against metal, oxides normally cover the surfaces, which
often decreases the coefficient of friction. However, if the oxides become
worn off, strong metallic bonds form between the exposed metal surfaces.
Further sliding will require shearing of the metallic interface, which
increases the coefficient of friction [1]. Typically, in tribological contacts
between ceramics and metals, the metal adheres to the ceramic surface and
then the sliding takes place in the created metal-metal interface [13].
Wear Mechanisms
Wear of ceramics are dominated by cracking and chemically induced surface
transformations. Plastic deformation does occur but more rarely [14]. There
are typically two wear regimes for ceramics, mild and severe wear. In sliding
under low contact pressures the wear is mild, the surfaces become polished,
the roughness decreases and the wear rate is low [12,15]. Smooth surfaces
and low pressures give lower coefficients of friction [16,17]. Conversely,
severe wear takes place under higher contact pressures where stresses exceed
the tensile strength of the material and grain fracture lead to formation of
wear debris and an increased wear rate [12,15]. At very high pressures,
whole grains will chip out from the ceramic matrix and the surface rough-
ness increases drastically [18]. The size of wear debris typically increases
with contact pressure. Severe wear is typical during running and as the
14
surfaces become smoother, the wear regime transforms to mild wear.
Further, the sliding speed has an influence on the wear of ceramics. The
wear normally increases with increasing sliding velocity [17]. It has also
been demonstrated that an increased grain size increases the wear rate in
sliding contacts [19].
In repeated contact, the wear debris that is formed in the contact will be
ground to smaller sizes. In case of ceramic sliding against ceramic, the wear
debris is usually generated from both surfaces [20]. In dry contacts (i.e.
without any lubricant) the wear debris formed may fill up cavities and create
agglomerates on the surfaces. The local pressures and temperatures in a
tribological contact are high enough to sinter the agglomerated particles to a
solid tribofilm. This phenomenon is called tribo-sintering [21]. This type of
tribofilm has been shown to smoothen surface topography and may have a
thickness up to 6 m [5].
Influence of Atmosphere
The friction and wear properties of ceramics strongly depend on the
surrounding atmosphere [22]. The ability to form a sintered tribofilm on
alumina decreases with increasing humidity. The hydrophilic alumina wear
particles are less prone to agglomerate since they adsorb water which leads
to lower adhesive forces [23]. It is claimed that aluminium hydroxides
(AlOOH, Al(OH)
3
) are formed on the alumina surfaces in water and humid
air [4,24,25]. This hydroxide is said to have lower shear strength than alu-
mina and therefore contributes to a lower friction.
Silicon nitride sliding against silicon nitride demonstrates a similar behav-
iour of tribochemical wear. Silicon nitride reacts with water and forms silica
(SiO
2
) [26]. This silica layer contributes to very low coefficients of friction
and low wear rates [27]. However, Xu et al. [27] have also shown that when
the silica layer has reached a critical thickness, it delaminates from the sili-
con nitride surface and a new layer of silica builds up on the surface. The
chemical reactions with water will continue to dissolve the silica, creating a
reaction product consisting of silicon hydroxide (Si(OH)
4
). The majority of
crystalline wear particles are produced at an early stage of the test, whereas
with increased sliding distance the wear particles produced are amorphous or
consist of silica or silicon hydroxide. However, Tomizawa et al. [26] claim
that no solid wear particles are generated from the contact of silicon nitride
against silicon nitride in water.
15
Ceramics
Ceramics are a large group of materials exhibiting a wide range of proper-
ties. Ceramic materials can be defined as compounds of metallic and non-
metallic elements as well as non-metallic, non-organic materials [28].
The characteristic properties of ceramics include high melting point, low
density, high corrosion resistance, high hardness and low thermal expansion.
Further, they are much stronger in compression than in tension and their
main disadvantage is brittleness.
The plastic deformation of crystalline ceramics and metals takes place by
dislocation motions. The atomic bonding in ceramics is of a covalent or ionic
character. With these bonding types there are a limited number of slip
planes, along which dislocations can move [29]. For ionically bonded atoms,
the repulsive forces of the electrically charged atoms restrict the slip of the
atoms. For covalently bonded atoms, the strength of the covalent bonds pre-
vents the slip. The ions in metallic bonding share electrons and therefore no
electrostatic forces prevent slip of atoms. Due to the restricted slip and there-
fore restricted dislocation motion, plastic deformation is limited for ceramics
and they often fracture before plastic deformation can occur. Also due to the
restricted number of slip systems, the strength of ceramics in tension is lim-
ited by the defects within the material. A defect in a ceramic material weak-
ens the structure by creating a stress concentration from which the crack
propagation starts. Therefore, bulk ceramics should not be subjected to high
tensile stresses. For non-crystalline ceramics, there is no regular atomic
structure and consequently plastic deformation does not occur by dislocation
motion. These materials deform by viscous flow [29]. Applied shear forces
cause the atoms to slide past each other, by breaking and reformation of
interacting bonds, without a favourable sliding direction.
Bulk ceramics are produced by the compaction of powder and a subse-
quent densification of the same through sintering/firing at high temperatures.
Due to high hardness and brittleness, any following treatment such as shap-
ing is complicated and often requires diamond cutting tools and abrasives.
Sharp edges and corners should be avoided due to concentrations of tensile
stresses.
Ceramics are often used in applications that are too hot for metals, such as
ovens and heat engines. They are also used as electrical insulators and heat
barriers. Moreover, ceramics can have semiconducting character (for exam-
ple silicon carbide) and can also be used for heat transfer [28].
16
The most common bulk ceramics in tribological use are based on alumina
(Al
2
O
3
), silicon carbide (SiC), silicon nitride (Si
3
N
4
), zirconia (ZrO
2
) or
boron nitride (B
4
N). To exemplify, silicon nitride may be used in bearings
and metal cutting tools, alumina in cutting tools and hip joints, silicon
carbide in mechanical seals, zirconia in dies and hip joints and boron nitride
is mainly used in cutting and abrasive applications.
Ceramic Coatings
Ceramic coatings are deposited to give surfaces the beneficial properties of a
ceramic material while maintaining the strength and ductility of the underly-
ing bulk material. Ceramic coatings, only a few micrometres thick, are
enough to improve the life of cutting tools, which need to withstand extreme
stresses and temperatures.
17
Coatings
Many engineering components can be improved with a coating. The coating
can act as a protective layer on top of a bulk material or a brittle, wear resis-
tant material can be improved by the support of a more ductile bulk material.
This makes it possible to focus specific properties where they are most
needed. It is also possible to combine several material properties within a
coating, for example combining a hard phase with a lubricious phase. The
hard phase is usually a carbide or nitride and the lubricious phase is often
amorphous carbon (a-C) that can reduce adhesion and sticking to the counter
surface. These low-friction wear resistant coatings are frequently used in
various machine elements to reduce energy losses.
There are several deposition techniques for the production of coatings,
where PVD (physical vapour deposition) is a common method for applying
thin coatings (1-10 m) aimed for low friction and/or wear resistance. PVD
is often chosen due to the possibility to produce high quality coatings of
variable composition at relatively low substrate temperatures. Further, the
technique allows combination of several materials to fabricate multilayer
structures. PVD can be achieved by either evaporation or sputtering of a
solid source in vacuum. In both cases, the vapour can form a coating either
with the same composition as the evaporated material or in an altered form
after reaction with a gas introduced into the deposition chamber (such as TiN
formed from sputtered Ti reacted with N
2
gas).
PVD Sputter Coating
The purpose of sputter coating is to generate free atoms from a solid target
such that these emitted atoms collide with a substrate surface, condense and
form a coating. The process begins with evacuation of the chamber, followed
by introduction of a working gas (usually Ar) and application of an electric
potential between the target and a shield around the target. The electric field
accelerates ions towards the target, which in turn creates more ions and elec-
trons upon bombardment with gas molecules, thereby a plasma is formed.
The positively charged ions in the plasma are accelerated towards the target
and upon impact eject atoms which are finally deposited as a coating on the
substrate.
To increase the ionization and hence the deposition rate, magnetron sput-
tering is an alternative [30]. In magnetron sputtering, a magnetic field per-
18
pendicular to the electron current is utilised to obtain a helical path for the
electrons. The secondary electrons released from the target by the ionic bom-
bardment are trapped by the magnetic field and move in the same pattern as
the other electrons. This concentration in electron density leads to a locally
increased ionisation and thus a higher sputter rate of the target in this area,
forming the so-called racetrack.
In the simplest sputter methods, the substrates are earthed. A negative
potential (bias) can be applied to the substrates to accelerate positive ions
also towards the substrate, to generate a mild sputtering. This controls the
coating growth and could also improve adhesion of the coating. A negative
bias can also be used for sputter cleaning of the substrate prior to deposition,
in order to get rid of oxides and surface contaminations. However, it has
been revealed that sputter cleaning may also roughen the surfaces. One im-
portant example of this is tool steels, where the sputter rate of the carbides is
lower than that of the matrix [31,32].
If the potential applied between the shield and target is constant over
time, it is termed as direct current (DC) sputtering. However, this potential
can be pulsed and if the frequency is sufficiently high, it is referred to as
radio frequency (RF) sputtering. RF sputtering is preferable to avoid charg-
ing if the target material does not have sufficient conductivity.
To deposit more complex coating compositions, sputtering can be made
from two targets simultaneously, so called co-sputtering.
Coating Deposition
In this thesis, two types of coatings have been deposited by PVD-sputtering.
The coating of TaC/a-C
*
was produced because it has been shown to give a
low coefficient of friction, about 0.05 in a ball-on-disc apparatus against a
ball of steel [33]. The other coating of Si
x
N
y
was produced in order to
achieve wear resistant bearing surfaces for hip joint replacements, which
case a minimum amount of wear particles that are resorbable in vivo
.
TaC/a-C Coating
The TaC/a-C coating was deposited in the BAI640R PVD coating system by
sputtering from a planar DC magnetron source. In order to simultaneously
sputter tantalum and carbon, the carbon target was partly covered by a tanta-
lum foil, a procedure earlier used by Nilsson et al. [34]. Metallurgical
powder high speed steel ASP 2053
Material composition (wt.): 2.48% C, 5.2% Cr, 3.1% Mo, 4.2% W, 8.0% V, balance Fe
19
cleaning/etching process was performed at an Ar-pressure of 1.5 x 10
-6
bar
and a substrate bias of -200 V. The 240 minute sputtering process was per-
formed using a magnetron power of 1.5 kW at a total chamber pressure of
3.5 x 10
-6
bar. The substrate bias was set to 0 V (floating potential).
Si
x
N
y
Coatings
The Si
x
N
y
coatings were deposited on CoCr, ASTM F1537
*
substrates as
well as on silicon wafers. The coatings were deposited by reactive RF sput-
tering (13.56 Hz), utilising a 4 inch silicon target and an Ar/N
2
gas mixture.
The coating system (Hochvakuum, Dresden, Germany) was not equipped
with a bias control of the substrates and hence no sputter cleaning was per-
formed prior to deposition. In order to optimise the coating composition,
microstructure etc., several coating parameters were varied. The total cham-
ber pressure during coating was 10.5 bar, the target power was in most
cases set to 300 W, the substrate temperature was in most cases set to 280 C
and the gas flow rate was about 40 sccm with various gas compositions. To
avoid overheating of the target, the coating process alternated between 10
min sputtering and 3 min breaks. The total deposition time was 2 hours,
except for the coating sputtered with a target power of 150 W, which had a
deposition time of 3 hours. In two of the coating processes, ethylene (C
2
H
4
)
gas was let into the chamber as a reactive agent in order to dope the coating
with carbon.
*
Material Composition (wt.): 28% Cr, 6 %, Mo, C 0.35%, balance Co
20
Friction Drive System of an Ultrasonic Motor
The demands for portable products with several functions utilising mechani-
cal movements are steadily increasing. Ultrasonic motors are well suited in
systems where miniature size, high speed, good precision and low power
consumption are essential features. The drive mechanisms of ultrasonic
motors are based on the converse piezoelectric effect, where the piezoelec-
tric material elongates when an electric field is applied [35,36].
Traditional electromagnetic motors are typically based on a rotating sys-
tem which needs gear-boxes, lead screws and nuts to accomplish a linear
movement. Miniaturisation of such systems is complicated due to difficulties
in manufacturing and assembling. However, the movement of piezoelectric
elements can give a direct linear motion, requiring only a friction drive sys-
tem which is well adapted to miniaturization. With fewer components, the
size can be considerably reduced. A commercial such ultrasonic motor is
shown in Figure 3 and the main parts of the friction drive system are sche-
matically illustrated in Figure 4. The main function of this motor is to
operate a drive rail back and forth.
Figure 3. The ultrasonic, piezoelectric motor PiezoWave
TM
from PiezoMotor AB.
The orange tail is a part of the flexible printed circuit board and has contact pads for
electricity supply.
The piezoelectric elements are soldered to the flexible printed circuit
board and the drive pads are glued to the piezoelectric elements. The flexible
printed circuit board is folded and assembled into a plastic housing, which
places the elements in their right positions, according to Figure 4. The drive
rail is inserted into the plastic housing and integrated bearings keep the rail
in place. A spring attached to the flexible printed circuit board presses the
elements towards the drive rail and creates a normal force between the drive
21
pads and the drive rail. When electric signals are applied to the elements
they will oscillate. Due to a shift of the electric phase, the middle of the
elements, i.e. the assembled drive pads, will describe a rotating motion. The
drive pads transfer the movement to the drive rail by pushing it in the desired
driving direction during half the cycle of the rotating motion. The rail is
pushed approximately 1-3 m per cycle, at a frequency of 96 kHz. Due to
the high frequency, the continuous motion of the drive rail has a speed of
approximately 100 mm/s. The total stroke of the investigated motor is ap-
proximately 6 mm. This implies that the drive pads push the drive rail
approximately 5000 times per stroke and always with the same area in con-
tact. The average contact pressure between the drive pads and the drive rail
is approximately 10 MPa.
Figure 4. Principle of the friction drive system on an ultrasonic motor (Piezo-
Wave
TM
); (a) Schematic cross section, the black springs indicate the normal force
(1 N) applied between the drive pads and the drive rail; (b) Bending of the piezo-
electric bimorph elements due to elongation of selected layers by an applied electric
field. The drive pads on the elements give the drive rail a linear motion. The arrows
indicate the motion of the drive pads.
The drive pads and the drive rail are made of alumina, due to its relatively
high wear resistance and high coefficient of friction. For some applications it
is of importance that the friction drive system produces a minimal amount of
wear particles so as not to disturb the function of adjacent components.
The driving force of the motor equals the friction force between the drive
pads and the drive rail, thus the driving force of the motor can never exceed
the friction in the friction drive system. Therefore, it is important that the
friction force is relatively stable and on a relatively high level. With higher
friction forces, the motor become stronger and can be suitable for several
applications.
22
Tribology in Hip Joint Replacements
The human body is a complex system with several sensors and actuators.
Whenever something happens to it, e.g. an injury or another kind of compli-
cation, it senses and reacts to it, in purpose to defend itself and stay intact.
When a foreign material is inserted in vivo, i.e. in the body, the involved
tissue will be damaged regardless of implantation method. The reactions the
body sets in motion will attempt to heal the wound or remove the foreign
material. When optimising an implant, the aim is to minimise the foreign
body reactions. The variation in intensity and duration of the inflammatory
response or wound-healing process depends on the size, shape, chemical and
physical properties of the biomaterial. It is important that the biomaterial is
biocompatible, i.e. it is able to perform with an appropriate host response for
its intended function [37]. When it comes to total hip joint replacements, it is
the whole system, rather than the individual materials, that have to be bio-
compatible.
Hip Joint Replacements
Total joint replacements constitute one of the most common and successful
procedures in orthopaedics [38]. In the United States alone, approximately
202 500 primary total hip joint replacements were performed in 2003. By
2030 the number of primary procedures is estimated to grow to 572 000 [39].
Primary procedure refer to the first time the total joint replacement is
performed, while any following procedures are referred to as revisions. To
occupy in the space of the previous replacement, the dimension of each revi-
sion has to be larger than the previous. For example the stem of a first revi-
sion hip is longer than the primary hip stem (Figure 5a).
A total hip joint replacement has an average life span of approximately
15 years before it has to be replaced by a revision [40]. An increasing num-
ber of younger patients are receiving implants and an aging population [41].
It is therefore highly desirable to increase the implant longevity, in order to
reduce the number of revisions.
A total hip joint replacement consists of several parts, see Figure 5. The
stem placed in the thighbone (i.e. femoral bone) is often composed of tita-
nium. The ball (i.e. the femoral head) is often composed of cobalt chromium
(CoCr), alumina (Al
2
O
3
) or zirconia (ZrO
2
). The acetabular cup is positioned
in the pelvis bone and is often composed of CoCr, steel or alumina. If poly-
23
ethylene is used for the cup, it is often used as a liner between the femoral
head and the acetabular cup, as shown in Figure 5a. The diameter of the
femoral heads is typically around 28 mm, with a diameter clearance to the
cup of typically 100-200 m.
Figure 5. Total hip joint replacement. (a) This implant is for the third revision of a
replacement. The stem is of titanium and coated with hydroxyapatite for improved
bone integration, the femoral head is of alumina, the liner of polyethylene and the
acetabular cup is of titanium; (b) X-ray image, the patients left hip has been re-
placed.
Biotribology
Failures of total joint replacements can be due to several factors including
insufficient fixation and positioning, mechanical loosening and infections.
One of the most critical factors is related to tribology, i.e. wear of the cup,
head and liner. It is the produced wear particles rather than the material loss
from the joint surfaces that become the limiting factor. The wear particles
that are accumulated close to the implant may cause inflammation and
osteolysis (degeneration of bone tissue) which eventually leads to implant
loosening [40,42,43]. The most important demands on the material combina-
tion in the implant are high wear resistance and biocompatibility. In addition,
smooth bearing surfaces are important to reduce the generation of wear par-
ticles.
Common material combinations for hip joint bearings include cups of
ultra-high molecular weight polyethylene (UHMWPE) that slide against a
head of CoCr, alumina or zirconia. These material combinations exhibit a
24
low coefficient of friction, but the UHMWPE often wears to produce a rela-
tively large amount of wear particles [44,45]. In order to reduce the genera-
tion of wear particles from the UHMWPE, alternative material combinations
are used, for example CoCr against CoCr, alumina against alumina or zirco-
nia against zirconia. Other metals than CoCr have also been used, including
titanium alloys and stainless steels [40]. Although wear particles from metals
and ceramics have also been shown to cause osteolysis [46,47], wear parti-
cles of UHMWPE are considered to be more biologically detrimental [47].
However, it has been demonstrated that corrosion of metallic wear particles
increases the metal ion content in the body, which is a cause of concern since
Co and Cr ions are known carcinogens [48].
Bulk ceramics (mainly alumina and zirconia) against themselves have
been used for hip joint bearings due to their high corrosion resistance. They
have also been shown to produce less and smaller wear particles than other
material combinations [43,45,49]. However, bulk alumina and zirconia are
brittle in comparison to metals, which can lead to catastrophic failure in vivo
[50]. To improve the ductility of the hip joint implant as well as minimising
the production of metallic wear particles, ceramic coatings of ZrO
2
, TiN,
CrN, CrCN, DLC have been deposited on CoCr alloys and tested in vitro (in
an artificial environment) [51,52]. It has also been reported that TiN, CrN
and hydrogenated amorphous carbon (a-C:H) coatings have been deposited
on titanium alloys, and tested in vitro [53].
Alternative ceramics that have shown potential in in vitro tests include
silicon nitride (Si
3
N
4
) and silicon carbide (SiC) [54,55]. Silicon nitride as a
bulk material has been shown to be bioinert and exhibit a good biocompati-
bility [56,57]. When exposed to water, the surface of Si
3
N
4
becomes hydro-
lysed and oxidised, and the silica layer is then leached in the water [27,58].
This in combination with low wear rates suggests that the use of silicon
nitride
bearings would produce less wear particles and those produced would
be biocompatible and degradable. The less body response to the wear parti-
cles, the longer is the life span of the implant.
Even though silicon nitride
is a relatively tough ceramic material, the
bearing component would be more ductile if designed as a silicon nitride
coating on a metallic substrate. CoCr is a good alternative as a substrate
since it has already proven its function as a bearing material for hip joints.
25
Tribological and Mechanical Testing
The ultimate goal of tribological and mechanical testing is to find the best
possible material solution for the specific application with respect to friction
properties and wear resistance. When field tests are complicated and expen-
sive, an alternative test method that mimics the tribological conditions has to
be employed. Fundamental knowledge about tribology is required to choose
the best suited test method. Model tests in the lab are often performed to test
the wear of single components, while other tests measure the tribological
function of a whole system.
Bench Testing
An individual bench test was set up to measure the actual friction force be-
tween the drive pads and the drive rail (Figure 4) of the ultrasonic motor
PiezoWave
TM
, see Figure 6. The drive rail consists of 99% -alumina and
the drive pads consist of 96% - alumina. The contacting surfaces are tested
as sintered, i.e. not further treated after sintering.
Figure 6. Schematic image of the friction force test apparatus for the ultrasonic
motor PiezoWave
TM
. The friction force between the drive pads and the drive rail in
the motor are measured while the motor is turned off.
The friction force measured here was the actual dynamic holding force
of the motor. The normal force of 1 N, applied by the spring, was always
present. The friction force between the drive pads and the drive rail was con-
tinuously monitored while the drive rail was pushed through the motor at a
constant speed of 3 mm/s, using an external operating motor. A position
gauge continuously monitored the position of the drive rail.
26
Ball-on-Disc Test
The ball-on-disc test [59] is a model test that includes a stationary ball slid-
ing against a rotating disc while the friction force is continuously measured,
see Figure 7. The ball-on-disc is used to simulate various sliding, high pres-
sure contact situations, but is best suited for contacts where one surface is
constantly in contact.
Figure 7. Schematic image of the ball-on-disc set up, N is the applied normal force
and F
F
is the measured friction force.
The tribological properties of an alumina drive pad in contact with the
alumina drive rail were simulated with a ball-on-disc apparatus. A polished
-alumina ball of 6 mm was slid against a disc of -alumina. The load and
speed were selected to represent the contact between the drive pads and the
dive rail. The normal load was 1 N and the sliding speed 0.1 mm/s. By
measuring the wear marks on the drive pad and ball after 200 000 passages,
the contact pressure was estimated to approximately 10 MPa.
Also the TaC/a-C coating was tested in the ball-on-disc apparatus and slid
against a ball bearing steel ball of 6 mm in diameter. The setup involving
one uncoated part sliding against a carbon based low-friction coating was
selected since it has become a common technical solution with many advan-
tages [60]. The normal force was 5 N and the sliding speed was 0.005 m/s.
All the tests were performed unlubricated in ambient room conditions with a
relatively humidity of 50 10%. For surface studies of the running-in proce-
dure, tests of three different sliding durations were performed: 5, 20 and
1000 revolutions.
The ball-on-disc has also been utilised for pre-scanning of potential mate-
rials for hip joint replacements. Various material combinations were tested in
this work. Discs of bulk CoCr, silicon nitride, as well as discs coated with
Si
x
N
y
were slid against balls of silicon nitride, and some tests were also exe-
cuted with balls of alumina against CoCr. The balls had a diameter of 6 mm,
the track radius was 2.5 mm and the sliding speed 0.04-0.05 m/s. The tests
have been carried out in a synthetic body fluid PBS (Phosphate Buffered
Saline), which has ion concentrations close to human blood plasma [61].
Tests have also been performed in a solution of 25% bovine serum diluted in
27
deionised water. The sliding speed, track radius and bovine solution was in
accordance with the ASTM standard test [62]. In the long tests, the deionised
water had to be refilled once or twice a day, to make up for evaporation
losses.
The continuous sliding in the ball-on-disc test is quite far from the com-
plex motion of a hip joint. In addition, the contact pressure is very much
higher than the average pressure in a hip joint. Due to the small ball radius
and the limitation of lowest load for the ball-on-disc apparatus, the maxi-
mum Hertzian pressure [63] of the contact between the silicon nitride ball
and the Si
x
N
y
coated CoCr disc can be estimated to 0.76 GPa
*
, neglecting the
influence from the thin coating. This would correspond to a load of 545 kN
on a hip joint with a diameter of 28 mm and a radial clearance to the cup of
100 m, assuming both head and cup are made of CoCr coated Si
x
N
y
, again
neglecting the small influence from the thin coating on the contact pressure.
Nanoindentaion
For hardness measurements of a surface layer, such as a coating or a tri-
bofilm, the indentation depth should not exceed 1/10 of the layer thickness to
avoid influence from the underlying material [64]. In this thesis, the superfi-
cial hardness measurements were performed with an ultra nano hardness
tester (CSM Instruments UNHT) equipped with a Berkovich tip
. The typical
indent depths range from 30 nm to 250 nm. One advantage with this equip-
ment is that the exact location of the indents can be chosen using an optical
microscope. The indents were analysed in accordance with the Oliver-Pharr
method [65].
Solubility Tests of Silicon Nitride
To estimate the solubility and possible dissolution of silicon nitride wear
particles in the body, a commercial silicon nitride powder (P95H, Akzo
Nobel) was mixed with PBS using three different pH values: 4.8, 6.5 and
7.4. These pH levels were selected to match the pH around an implant,
which has been shown to vary between 4.4-7.7 [66]. PBS has a natural pH of
7.4 so hydrochloric acid was added to decrease the value. 100 mg of Si
3
N
4
powder was mixed with 15 ml PBS. The average grain size of the powder
was approximately 1 m. The PBS/silicon nitride mixtures were stored in
plastic tubes with plastic lids. The tubes were placed on a rocking platform
shaker and stored at 37C during 35 and 75 days respectively. After the stor-
age time, the mixture was filtered through a 0.2 m PTFE membrane using a
syringe. Subsequently to filtration, ICP-MS (Inductively Coupled Plasma
Mass Spectrometry) was used to determine the silicon ion content of the
solutions.
*
Youngs Modulus for Si
3
N
4
320 GPa and for CoCr 241 GPa. Poissons ratio 0.27 for Si
3
N
4
and 0.3 for CoCr.
Serum: I detta fall r det en animalisk produkt som innehller proteiner. Lsningen som
anvndes r en blandning av serum och avjonat vatten.
58
Acknowledgements
Det hr hade varit mycket svrare och inte lika roligt utan all hjlp och std
frn Er andra, ett extra varmt tack till
min handledare Staffan, fr allt du har lrt mig om allt frn tribologi till nya
ord som pepplig och fr att jag ftt sitta p ditt rum och diskuterat ntnings-
mekanismer
min andra handledare Hkan, fr inspiration och fr att du pushat mig i mitt
arbete
min f.d. handledare och chef Stefan, fr att du gav mig chansen att f brja
p ett intressant projekt
Cecilia, fr att du alltid tar dig tid, r snabb p att korrekturlsa och kommer
med bra kommentarer
Thank you Nico Teuscher, for helping me with PVD sputtering, taking care
of me in the lab, as well as inviting me to your home and your family
Thank you Andreas Heilmann, for letting me work in your lab at Fraunhofer
IWM
Mrten Ohlsson, fr all hjlp p PiezoMotor bl.a. med friktionstest-
utrustningen
Maria, fr ett bra samarbete och trevligt sllskap i labbet
Urban, Julia och Harald, fr bra jobb och intressanta diskussioner om tribo-
filmens uppbyggnad under sena kvllar
sa och Sture, fr att ni alltid tar er tid och bidrar med bra diskussioner
Nils, som hjlpt mig med ESCA-underskningar
Frida, fr hjlp med mycket som rrt ESCA, fr trevligt ressllskap, fr
mnga, alltfr lnga tepauser men inte minst fr att du r en bra vn
59
Jonatan, fr att du har fixat alla mina sm och stora dataproblem
Janne, fr all praktiskt hjlp och std i labbet, bde innan och efter att ngot
har gtt snder
Fredric, fr hjlp med diverse analysutrustning
Wei, for always having time to help me with lab work, answering questions,
and with XRD
Kathryn, fr att du tog dig tid att korrekturlsa kappan
Karin och Anja, fr all administrativ hjlp
Peter, Julia, Fredrik, Martina, Harald, Maria, Janna och Petra, fr att ni
har varit som en extrafamilj i ngstrmvrlden och fr alla roliga resor vi
har varit p
MiM:are, MikMek:are, STC:are och JonDeTech:are, fr att ni har varit
med och bidragit till att jag trivts s bra p jobbet, speciellt i fikasoffan
PiezoMotorkollegorna, fr en bra tid p PiezoMotor
vnnerna utanfr ngstrm, fr att det r s roligt att umgs med er
Sala-tjejerna, som har stttat mig i 25 r
Jens och Kristina, fr allt std och skratt bde under plugg och fritid
Mamma och Pappa, fr all krlek och fr att ni alltid stller upp fr mig
min lskade Benny, fr din krlek och fr att ditt tlamod alltid tar vid dr
mitt slutar du r bst!
Uppsala, augusti 2011
60
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