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FUNDAMENTALS OF LAMINATING PROCESS AND

QUALITY REQUIREMENTS
Dr. Gérard F. Savineau

Monsanto Chemicals Europe S.A.


Avenue de Tervuren, 270-272, B 1150 Brussels

ABSTRACT glass in building - Construction Products Directive


(CDP) 89/106/EEC: Official Journal L 40,
Abstract: Fundamentals of Laminating Process 11.2.1989, p.12 - and to the six Essential
and Quality Requirements. Requirements - Interpretative Documents (ID’s):
Official Journal C 62, 28.2.94, p.1 - laid down in the
As we review the previous decades, we are CDP. This clearly indicates that the evaluation of
impressed with the technological conformity, including initial type testing of the
accomplishments of the worldwide laminated essential characteristics, initial type of testing if the
architectural glass manufacturers especially in product belongs to the intended product group, and
the areas of product diversification. Keeping up the organization of the factory production control, is
with it has been challenging for all of us and, as in line with the attestation of conformity. To achieve
we are entering a new century, we see even more this objective, an in-depth knowledge of the
diversifications and greater challenges for PVB- laminating process (es) and product requirements
based laminated glass. is essential. The following will give you an overview
As might be expected, past diversification and on how to master the laminating processes to fulfill
growth have led up to some confusions and, to a the expected quality requirements.
lesser extent, some misunderstandings in the
market place about laminated glass products and 2. PRODUCT DESCRIPTION
performances.
From the CEN/TC129/WG3 “Glass in Building” The prEN ISO 12543-1 defines terms and
prEN 12543-1 to 7 draft documents, we are getting describes component parts for laminated glass
a clear understanding of what is laminated glass and laminated safety glass for use in building.
and laminated safety glass, as well as, what is
expected of these products in terms of 2.1 Laminated glass:
performances, overall visual quality and durability. An assembly consisting of one sheet of glass
An in-depth knowledge of the laminating glass with one or more sheets of glass and/or plastics
process fundamentals combined with the legen- glazing sheet material joined together with one or
dary “know-how” of the professionals should mini- more interlayers.
mize or better eliminate industry wide problems and 2.2 Laminated glass with fire resistant properties:
assess definitively the credibility of these products. Laminated glass which does not achieve its
fire resistance by means of interlayers which
1. INTRODUCTION react to high temperatures.
2.3 Fire resistant laminated glass:
Laminated glass and laminated safety glass - Laminated glass where at least one interlayer
with or without fire resistant properties - are reacts to high temperature to give the product its
covered by several European Standards drafts fire resistance
and, in particular, by prEN 12543-1 to 7. They 2.4 Laminated safety glass:
incorporate by dated or undated reference, Laminated glass where in case of breakage
provisions from other publications. These the interlayer serves to retain the glass
standards are interrelated and unable the user to fragments, limits the size of opening, offers
find out which glass product or test method residual resistance and reduces the risk of cutting
standards should be referred to when considering or piercing injuries.
a particular product property related to the use of

154 GLASS PROCESSING DAYS, 13–15 Sept. ‘97


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Laminated glass can be made from most Nr Performances
combinations of all types of glass, plastics 1 Fire resistance
glazing sheet material (polycarbonate or acrylic) 2 Reaction to fire
and interlayers in solid form (film) or liquid form 3 Light transmittance and reflection S
(resins) such as: 4 Solar energy characteristics E
◆ Film: - polyvinylbutyral (PVB) 5 Wind, snow and:or permanent load resistance S
- ethylvinylacetate (EVA) 6 Human impact resistance S
- polyurethane (PU) 7 Explosion resistance
◆ Liquid: - one-component resins 8 Sound reduction
I
- multi-component resins 9 Energy saving O
- intumescent gels 10 Bullet resistance N
11 Burglar/vandalism resistance
3. PROCESS DESCRIPTION 12 Release of dangerous substances 2
One can distinguish two main lamination For each of above performances there do exist a
processes corresponding National and/or European Standard.

3.1 Folio lamination process 4.3 Optical and visual quality


This lamination process is the most widely National and/or European Standard (prEN ISO
used process where the interlayer is a solid film 12543-6) specifies defects of finished sizes and
such as PVB. The process flow diagram is test methods with regard to the appearance when
divided into 4 main steps: looking through the glass.
◆ glass and film preparation
◆ assembly step 4.4 Dimensional tolerances
◆ deairing step either by calendring or under National and/or European Standard (prEN ISO
vaccum 12543-5) specifies dimensions, tolerances and
◆ autoclaving under heat and pressure edge finishes.
For more details, please refer to Mr. Van
Russelt’s paper “How to Make a Good Laminated 5. CONFORMITY
Safety Glass” - Automotive Session 9.

3.2 Cast-in place lamination process The evaluation of conformity is based on:
Commonly used where the interlayer is a
liquid resin. Lamination is done by pouring a 5.1 Factory production control
liquid between the plies of glass or plastics 5.2 Inspection of samples taken at the factory
glazing sheet material. The assembly is then ◆ on-line quality control
chemically, UV-cured to produce the final ◆ off-line quality control
product. The process flow diagram is: 5.3 Continuous monitoring and assessment of
◆ glass and liquid preparation the factory production control
◆ assembly step
◆ curing step It becomes obvious that laminated glass
and laminated safety glass process(es) is an
INDUSTRIAL process carried out by HIGHLY
4. REQUIREMENTS PROFESSIONAL PEOPLE. The fundamentals
4.1 Conformity to the definitions of the laminating glass and quality
Products intended to belong to the product requirements have to be clearly understood
group laminated and laminated safety glass units and are the key success of the product
shall be conform with the definition of laminated performances, durability and credibility.
and laminated safety glass defined by National
and/or European Standards (prEN 12543-1/2/3). 6. FUNDAMENTALS AND
On that basis, the laminated glass shall resist the REQUIREMENTS
durability tests: high temperature, humidity and
radiation tests (prEN 12543-4). Additionally for This part focuses on laminated safety glass
laminated safety glass, it shall be tested and based on PVB interlayers only. Indeed more than
catalogized conform with the human impact 90% of the laminated glass consumption in the
pendulum test (prEN 12600). building industry are PVB-based laminated safety
glass.
4.2 Performances of the characteristics: The importance of accurate record keeping
The performances of the characteristics listed cannot be overstressed when it comes to
below shall be determined when required

GLASS PROCESSING DAYS, 13–15 Sept. ‘97 155


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troubleshooting process or product performance 6.2 Impact performance properties
deviations. The final laminate performance
properties include impact, adhesion and 6.2.1 Deviation
durability/ageing tests. Processing observations ◆ Increase or decrease in tested impact level
include bubbles, trapped air penetration and
delamination. The format for discussion of each 6.2.2 Potential Cause list:
property incorporates: ◆ Change in the glass/PVB adhesion level
◆ Change in the interlayer thickness
◆ Statement deviation ◆ Glass thickness change
◆ Potential cause list ◆ Wrong interlayer product type
◆ Action steps ◆ Change in impact test conditions or
procedure
6.1 BASIC RELATIONSHIPS ◆ Glass treatment

Impact, adhesion to glass, moisture content of 6.2.3 Action steps


the PVB interlayer, thickness of the PVB, float ◆ First check adhesion (see next session)
glass orientation, glass treatment (metal coated, ◆ If OK then check the test conditions,
chemically tempered, color), residual salts on the observe the impacted specimen in terms of
glass surface, glass surface contamination, are dimension, break pattern, interlayer used,
all important variables that control final and laminate thickness.
performance:
6.3 Adhesion performance properties
◆ For a given glass type and thickness, impact
levels will vary inversely with adhesion: 6.3.1 Deviation
 impact = f (1/adhesion) ◆ Increase or decrease in adhesion level
◆ The thicker the PVB the higher the impact:
 impact= f (PVB thickness) 6.3.2. Potential cause list
◆ Moisture in the PVB interferes with the ◆ Change in moisture content of PVB in
glass/PVB bonding mechanism. Thus as laminate
moisture content increases, the adhesion ◆ Different residual salts on the glass
drops and the impact improves: ◆ Change in detergents or glass washing
 Adhesion = f (1/% moisture) conditions
 impact = f (% moisture) ◆ Glass type/composition
◆ Too high moisture content may result in ◆ Float glass orientation (air vs tin)
bubble formation and/or delamination with ◆ Incorrect autoclave cycle
time. ◆ Contamination
◆ The placement of the air side of the float ◆ Change in adhesion test conditions or
glass against the PVB will result in higher procedure
adhesion than the tin side
◆ High residual salt concentration on the glass 6.3.3 Action Steps
surfaces at lamination, interferes with ◆ Identify any water supply changes (glass
bonding and lower the adhesion. washing/rinsing machine)
◆ Adhesion to metal coated glass depends on ◆ Review washer performance and records
the coating and requires to be studied case (changes in detergents, line speed, air blow-
by case. off system, water temperature, brushes worn
◆ Any glass surface contamination at the out)
assembly step may result in unacceptable ◆ Review adhesion tests conditions and
visual and/or optical quality. samples
◆ Unadequate deairing steps and/or autoclave ◆ Review autoclave cycle, probes, gauges
cycle may result in trapped air penetration and recorders for accuracy. Low
and consequently delamination or bubble temperatures and short hold times may not
formation even if not directly visible at the allow for PVB to flow and intimate contact
inspection. with the glass
◆ Check laminates for contamination
These basic relationships are important to ◆ Check PVB type
keep in mind when identifying the cause(s) of
performance deviations and testing the cause(s)

156 GLASS PROCESSING DAYS, 13–15 Sept. ‘97


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6.4 Moisture performance properties ◆ Check line for deairing. Look for pockets of
trapped air and premature (or lack of) edge
6.4.1 Deviation sealing. Are there large patches of cloudy
◆ Moisture higher or lower than expected appearance? S
◆ Review autoclave cycle: E
6.4.2 Potential cause List  too fast or too slow pressurisation S
◆ Incoming PVB moisture content level before heat-up can allow edge defects due S
◆ Unsealed PVB storage to air penetration.
◆ Relative humidity storage and lay-up room  Temperature at pressure release
I
◆ Moisture test conditions and procedure point should be at or below 50°C to avoid O
◆ Moisture standards bubbles formation along the edges of the N
laminate.
6.4.3 Action steps  Fast heat-up prior to pressurisation 2
◆ Review production records can expand residual entrapped air
◆ Check incoming PVB moisture  Low temperatures and short hold
◆ Check %RH in lay-up room times reduce adhesion and further may
◆ Check moisture analyser calibration initiate delamination
◆ Check moisture standards  Too high temperature (>160°C)
combined with too long hold time may
6.5 Durability performance properties initiate the degradation of the PVB. The
radiation test will amplify this phenomena
Process conditions have to be set in a such ◆ Measure glass match: does defect align
way that they shall prevent from air penetration, with? Gaps greater than 10% of the PVB
trapped air (inside air posket or bubbles), thickness are suspect
delaminations, edge bubbles, product yellowing ◆ Measure PVB stabiliser content or ask the
or discoloration (PVB degradation) interlayer supplier the quality control data. A
too low UV/anti-oxydant concentration may
6.5.1 Deviation induce the change in light transmittance
◆ Failure during high temperature tests (boil ◆ Review boil/bake/humidity/Radiation test
and/or bake test) conditions
◆ Failure during humidity test (with or without
condensation)
◆ Failure in radiation test CONCLUSIONS
6.5.2 Potential Cause list The above fundamentals in laminating glass
◆ Excessive moisture content thus low and related quality performance requirements are
adhesion based on decades of research experimentation,
◆ Trapped air process troubleshooting and process
◆ Contaminations optimisation. Laminated safety glass based on
◆ Poor edge sealing PVB interlayer has been tested and proven since
◆ Localized interlayer thinning more than 50 years in the automotive industry
◆ Glass flatness (tempered glass) (windscreen) and about 30 years in architectural
◆ Glass mismatch buildings. When manufactured according to the
◆ Premature edge sealing PVB supplier recommendations, the product
◆ Improper autoclave cycle performances characteristics listed above (see
◆ Folded PVB § 4 - requirements) will last, subject to normal
◆ Interlayer heat/light stability maintenance and actions which are foreseeable,
◆ Test conditions and procedure for an economically reasonable working life.
From field experiences we have learned to trust
6.5.3 Action steps in laminated safety glass based on PVB for its
◆ Test moisture content. High moisture reliability in terms of product durability, ageing,
(>0.8%) can create bubbles upon boiling/ and multi-function performances.
baking
◆ Test adhesion level: if below 3 Pummel
units, can cause delamination in conjunction
with glass stresses

GLASS PROCESSING DAYS, 13–15 Sept. ‘97 157


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