Laminated safety glass and adhesives : A literature survey on experimental techniques and experimental data

SP Technical Research Institute of Sweden

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Abstract

This literature survey presents some of the available information in the literature regarding experimental methods and experimental data for mechanical testing of laminated safety glass and windscreen adhesives for the automotive industry.

When testing laminated safety glass several methods exist that involve dynamic loading. The evaluation of these tests does not normally involve acquisition of loads or

displacements but do only include evaluation of the fracture appearance. Some methods, like split Hopkinson bar test, do include acquisition and analysis of loads and strains. The literature survey indicates that there is a lack in windscreen adhesive data for higher strain rates. Articles describing testing at high strain rates exists regarding structural adhesives. Methods for high strain rate testing, both in compression and tension, have thus been used for testing of structural adhesives. Data from adhesive suppliers are mainly limited to low strain rates.

Key words: Windscreen adhesives, polyurethane adhesive, laminated safety glass,

experimental methods, experimental data, crash, high strain rate

SP Sveriges Tekniska Forskningsinstitut

SP Technical Research Institute of Sweden SP Arbetsrapport Nr 2012:25

ISBN 978-91-87017-40-7 ISSN 0284-5172

Contents

Abstract 3

 

Contents 5

 

Summary 7

 

1

 

Introduction 9

  1.1  Delimitations 9 

2

 

Glass 9

  2.1  Glass in general 9 

2.2  Laminated safety glass 10 

2.3  Experimental methods 10 

2.3.1  Mandatory test methods for laminated safety glass 10 

2.3.2  Other test methods 12 

2.4  Experimental data 14 

2.4.1  PVB experimental data 14 

2.4.2  Laminated safety glass data 15 

3

 

Adhesives 18

 

3.1  Adhesives for automotive glass 18 

3.2  Experimental methods 19 

3.2.1  Test methods used by the adhesive manufacturers 20 

3.2.2  Other test methods 22 

3.3  Experimental data 24 

3.3.1  Sikaflex-256 FC experimental data 24 

3.3.2  High strain rate test of structural adhesive 28 

4

 

References 31

 

5

 

Appendices 33

 

5.1  Appendix 1. Standard methods for mechanical testing of adhesives 33  5.2  Appendix 2. Standards for mechanical testing of adhesives 38 

5.2.1  ISO STANDARDS - Number/Title 38 

Summary

This literature survey presents some of the available information in the literature regarding experimental methods and experimental data for mechanical testing of laminated safety glass and windscreen adhesives for the automotive industry.

When testing laminated safety glass several methods exist that involve dynamic loading. The evaluation of these tests does not normally involve acquisition of loads or

displacements but do only include evaluation of the fracture appearance. Some methods, like split Hopkinson bar test, do include acquisition and analysis of loads and strains. The literature survey indicates that there is a lack in windscreen adhesive data for higher strain rates. Articles describing testing at high strain rates exists regarding structural adhesives. Methods for high strain rate testing, both in compression and tension, have thus been used for testing of structural adhesives. Data from adhesive suppliers are mainly limited to low strain rates.

1

Introduction

This literature survey aims to presents available information in the literature regarding experimental methods and experimental data for mechanical testing of laminated safety glass and windscreen adhesives for the automotive industry.

1.1

Delimitations

The literature survey will focus on laminated safety glass and windscreen adhesives in crash, i.e., experimental data and methods at high strain rates.

The literature survey does not present how adhesives should be applied and used for best performance but focuses on mechanical properties and test methods of adhesives and laminated safety glass.

Although the focus is on high strain rates corresponding to crash, static and quasi-static test methods will be presented together with methods covering higher strain rates. Typical strain rates in the base material at crash simulations are about 300 s-1 (Carlberger, Biel and Stigh 2009).

2

Glass

2.1

Glass in general

In EN 1288-1:2000 (CEN, EN 1288-1:2000 Glass in building - Determination of the bending strength of glass - Part 1: Fundamentals of testing glass 2000) glass is described as given below.

Glass is a homogeneous isotropic material having almost perfect linear-elastic behaviour over its tensile strength range.

Glass has a very high compressive strength and theoretically a very high tensile strength, but the surface of the glass has many irregularities which act as weaknesses when glass is subjected to tensile stress. These irregularities are caused by attack from moisture and by contact with hard materials (e.g. grit) and are continually modified by moisture which is always present in the air.

Tensile strengths of around 10 000 MPa can be predicted from the molecular structure, but bulk glass normally fails at stresses considerably below 100 MPa.

The presence of the irregularities and their modification by moisture contributes to the properties of glass which need consideration when performing tests of strength. Because of the very high compressive strength, glass always fails under tensile stress. Further information on glass properties can be found in manufacturer’s manuals where e.g. Saint-Gobain Sekurit presents some of the data given in Table 1.

Table 1. Mechanical and thermal properties of glass (Saint-Gobain Sekurit - Glazing manual 2012, Larcher, et al. 2012).

Density (kg/m3) Knoop Hardness (HK) Compression resistance (MPa) Modulus of Elasticity (GPa) Bending strength (MPa) Poisson’s ratio 2500 470 800 – 1000 70 45 0.22 Failure strain (%) Failure Stress (MPa) Softening temp. (°C) Specific heat (J/gK) Thermal cond. (W/mK) Thermal exp. (K-1) 0.12 84 Approx. 600 0.8 0.8 9×10-6

The compression strength/resistance defines the ability of a material to resist a load applied vertically to its surface. The bending strength given in Table 1 is determined from ring-on-ring test (described in section 2.3.2).

2.2

Laminated safety glass

According to Pilkington and Saint-Gobain Sekurit the surface area of glazing per vehicle has increased vastly during the last 35-40 years. Pilkington says that the glazing area has increased by 50 % in 35 years and Saint-Gobain Sekurit says that it has been doubled in the last 40 years. Partly these glazed areas consist of laminated safety glass.

Laminated safety glass is basically two panes of glass joined by an interlayer of polyvinyl butyral (PVB). During an accident, the glass will crack but it will stick together due to the PVB layer. Apart from keeping the windscreen intact the PVB layer also decreases the noise and improves the acoustic comfort inside the car. Saint-Gobain Sekurit has an acoustic PVB, dBCONTROL®, which consists of three layers; two outer layers of normal PVB and an inner layer made of a material with high damping properties. How this inner layer affects the mechanical properties and modelling of the laminated safety glass is not presented on Saint-Gobain Sekurit’s web page apart from stating that the PVB layers provide the mechanical properties of the laminated glass as requested by existing norms such as R43 (Saint-Gobain Sekurit - Glazing manual 2012).

A typical laminated safety glass has a thickness of 5 mm of which the two glass panes and the PVB interlayer have thicknesses of 2.1 mm and 0.76 mm, respectively. Typical properties of PVB layer are given in Table 2.

Table 2. Mechanical properties of PVB layer (Xu, Sun, et al. 2011, Larcher, et al. 2012).

PVB Density (kg/m3) 870 – 1100

Elastic limit (MPa) 11

Modulus of Elasticity (GPa) 0.100 – 0.220

Failure stress (MPa) 28

Failure strain (%) 200

Poisson’s ratio 0.48 – 0.495

2.3

Experimental methods

When performing mechanical testing of glass there exist methods that involve dynamic loading. The evaluation of these tests does not normally involve acquisition of loads or displacements but do only include evaluation of the fracture. Other methods involve acquiring of load and deformation. Some of these methods are described in the sections below.

2.3.1

Mandatory test methods for laminated safety glass

The mandatory mechanical test methods for laminated safety glass for vehicles are described in a UN regulation as given in this section.

Mechanical tests according to ECE R43

The performance of laminated safety glass is regulated in United Nations ECE R43, Rev. 2 (Regulation ECE R43 n.d.) and presents mainly two different tests for mechanical strength; ball impact test and headform test.

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the glazing w eight of frag mm thick gla ment at ball

Figure 1. S

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assess the ad ll test is to as verify the co of injury in t pecified weig wo frames. Th nt heights dep ndscreen glas ve given a sa econds after valuated and mum 15 g. rm tests is sho

ball tests (Reg

with differen es a 227 g ba dhesion of th ssess ball-pe ompliance of the event of i ght is droppe he 2260 g ba pending on th ss the drop h atisfactory re the moment should not e own in Figs. gulation ECE nt weight of t all and one u

he interlayer netration res f glazing with impact of the ed to a 300x3 all is dropped he thickness height is 10 m esult if the ba of impact. F exceed a spec 1-2. E R43 n.d.).

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2007), stand r of laminated also describe building - De ported at two point bending and the actu

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f the glass fra s used in com on 2012). By mbination wit ure in glass i rify calculatio aphy is of int ) for which o kinson pressu 2011). By us age of the SH gram of split l double ring nding strengt with small te standard tes acture there a mbination wit using high-s th acquisition s achieved. T ons regardin terest for e.g only the appe

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nt bending te ). The tested 6.72 mm of w micro cracks glass in four ng test (as als sson ratio of safety glass f laminated s shows high med at each s opkinson pre d from quasi on rates (Xu st in which t d specimen h which the PV s of the cut ed r-point bendi so shown in F 0.23 and a fa is shown in safety glass i strain rate d strain rate. Th essure bar tes

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urves obtaine rates (X in Figs. 8-9 th fety glass the 1). The MFO or cracks and g. 8 is engine deformation from wave pr namic strain of different f safety glas w a nonlinear nonlinear phe PVB interlay te increases, ns nearly the uasi-static) si d (ii) glass is et al. 2011). ed from dyna Xu, Li, et al. the authors st e failure strai O strain was d d a drop in lo eering values n rate is give ropagation th n (Xu, Li, et a failure strain ss (Xu, Li, et r characterist enomenon is yer and progr the major fa same. The m ituation, the o s a rate-indep amic SHPB e . 2011). tate that, whe in will be dis defined as th ad is observe s. No inform n in the pape heories in sol al. 2011). ns at various t al. 2011). ic in mechan probably cau ressive micro ailure onset (M major respons outer glass p pendent mate experiments en changing scontinuous a e strain at wh ed. ation regardi er. In Fig. 9 t lids. Thus, th strain rates o nical behavio aused by both o-crack grow MFO) strain sible reasons panel plays a erial whereas at high strain the strain ra as shown in hich the

ing the numb the stress-he data in Fig of laminated our h wth n s s n te ber g.

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mat and Deng al]. Therefore Xu, Li, et al. 2

agation with Xu, Sun, et a ges of crack lculated as d m/s. The sta mpeding the elocity and ac strain rates. I ultimate stra he contrary, i haviour beco k load of the g [referred to e, the ultimat 2011). 1 kg of drop al. 2011). growth, as s epicted in Fi able crack gr crack propag cceleration (X In both quasi ain to increas n the domain mes more br impact. Thi o by Xu, Li e te strain’s dis p weight and shown in Fig ig. 12. The st owth occurs gation (Xu, S Xu, Sun, et a i-static and se before n where quas rittle, shown is phenomeno et al], and scontinuity a 1 m of drop g. 11, the crac teady-state due to Sun, et al. al. 2011). si-on at ck

3

Adhesives

3.1

Adhesives for automotive glass

There are several adhesive manufacturers worldwide who produce automotive direct-glazing adhesive systems. The manufacturers often differentiate between adhesives for OEM (original equipment manufacturer) and after-market adhesive system although both are polyurethane based adhesives. Some manufacturers and their adhesive systems for direct-glazing are given in Table 3 below.

Table 3. Some important adhesive manufacturer and examples of their systems for direct-glazing.

Manufacturer System name Adhesive type Bostik ISR (Industry

Special Range)

Silyl Modified Polymer (SMP)

DOW BETASEAL™ 1 component

polyurethane

Henkel TEROSTAT 1 component polyurethane

Sika SikaTack Sikaflex

1 component polyurethane

As seen in Table 3 the adhesives for direct-glazing are mostly polyurethanes but other adhesive types exist. Polyurethanes are used for most materials but is especially good for plastics and metals.

These adhesives are often abbreviated to PU or PUR, and are chemically reactive formulations that may be one-component or two-component systems and can be fast curing. A fast cure usually necessitates applying the adhesives by machine. They are often used with primers.

The single-component formulations that are available, are partially polymerised and stable until cure is initiated by the action of absorbed atmospheric moisture. Their reaction rate is slower because it takes time to absorb the necessary water. Polyurethanes can be supplied as reactive chemicals, solvent solutions, pastes or hot melts.

The single-component polyurethanes provide strong, resilient joints which are impact resistant and have good low-temperature strength compared with many other adhesives. Polyurethanes find major uses in the bonding of glass fibre reinforced plastics (GRP), direct-glazing of automobiles and lamination of both insulation panels and flexible packaging materials (Adhesive Toolkit 2012).

Table 4. Mechanical data for some adhesive manufacturers adhesive systems. Bostik ISR 70-08 AP DOW BETASEAL 1943 Henkel TEROSTAT Sika SikaFlex-252 Density (kg/m3) 1.5 1.25 – 1.30 1.27 1.20 Tensile strength (MPa) 2.9 (DIN 53504/ISO 37) > 5 (DIN 53504) 8 (DIN 53504) 4 (ISO 37) Stress at 100% (MPa) 2.3 (DIN 53504/ISO 37) Not given 2 (DIN 53504) Not given Elongation at break (%) 250 (DIN 53504/ISO 37) ca. 300 400 (DIN 53504) >300 Shear strength (MPa) 2.4 (Alu-Alu, 2 mm, 50 mm/min) (DIN 53283/ASTM D1002) Min. 5 (after 7 d 23°C/50% rh, 2 mm adhesive height) (EN 1465) 1.5 (@ 24 h, DIN EN 1465) 5 (fully cured, 5 mm, DIN 53283) 2.5 (ISO 4587) Tear strength (N/mm) 16 (Type C, 500 mm/min) (DIN 53515/ISO 34)

Not given Not given 9 (ISO 34) Modulus of elasticity (10%) (MPa) 5.5 (DIN 53504/ISO 37)

Not given Not given Not given

Based on the shear strength of an adhesive the adhesives can be divided into; structural, semi-structural and sealant. Structural adhesives have a shear strength higher than 15 MPa, semi-structural 8 – 15 MPa and sealant less than 8 MPa (Albinsson 2012). Based on this, the windscreen adhesives should be considered as sealants.

3.2

Experimental methods

As an overview of test methods the division of methods found on Adhesive Toolkit webpage (Adhesive Toolkit 2012) is given in Appendices 1-2. The test methods are given in Tables A1 – A4 presented in Appendix 1. Each of the test methods is specified in different standards. The name of the ISO and ASTM standards is given in the tables as well as listed with their full title in Appendix 2. The tables in Appendix 1 also specify relative costs associated with the different methods and other useful information regarding the methods. All tables are adopted from Adhesive Toolkit (2012).

Due to the focus on windscreen adhesives and crash in this literature survey all of the methods given in the appendices should be seen as a general overview of adhesive test methods.

In the main part of the report the methods presented are thus methods used for testing of windscreen adhesives or methods used for high strain rate testing. For the higher strain rate testing other adhesives might be reviewed due to a lack of high strain rate testing of non-structural adhesives.

3.

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Other test

re a large am tioned in sect ds used in re ain rates are perimental da

e and dimens shall result in ant rate of loa te. hould be expr tress, in meg is calculated metres. p shear test is ptimized sing o limit the in 2011). This k rlberger, Priv 11003-2:200 art 2: Tensile

t methods

mount of meth tion 3.2.1 are esearch, invo presented. S ata. sions (in mm n fracture wi ading is used ressed as the gapascals, of by dividing s the thick ad gle lap shear nfluence of st kind of test m vate commun 02 - Adhesiv e test method

s

hods are desc e the ones us olving other a Some test me m) of test pan ithin a period d, apply the s e mean of the f the valid spe

the breaking dherend she r test, since th tress singula method is also nication 201 ves - Determ d using thick cribed when sed by the ma adhesives tha thods are als

nel and specim d of 65 s ± 20

shear load at

e breaking fo ecimen. The g force, in ne

ear test (TAS

hick substrat arities (Cogna o suitable to 2). The TAS ination of sh k adherends 2 testing adhe anufacturers. an windscree so mentioned men. 0 s. If a t a rate of 8.3 orce, in lap shear ewtons, by th ST). The

tes and a sma ard, use for ST is describe hear behaviou 2002). esives. The . In the prese en adhesives, d in the sectio 3 he all ed ur ent , on

Pe To (C en Th im 20 F Th Th tem gi Fr Sh Pu Bi be co Fr eel Strength o achieve pu Carlberger, B nergy can thu he principle mage showing 009). a) Double c Figure 17. Pri he crosshead his crosshead mperature. T iven strain ra rom the DCB hear strengt

ure shear can iel and Stigh ending and d onsidered as

Figure rom the ENF

h and Fractu

ure peel defor Biel and Stigh us be determi of loading an g how the lo cantilever be inciple of do d speed in the d speed resul The strain rat ate was determ B test the stra

th

n be achieved h 2009). As s due to the occ

a crack (as in

e 18. End no F test the stra

ure Energy rmation the d h 2009). From ined. The me nd the test sp ading might eam specime ouble cantilev e experiment lted in a strai te varies duri mined when ain energy re d by using en hown in Fig currence of th n the figure), tch flexure s ain energy rel

double cantil m this kind o ethod is desc pecimen are be achieved en.

ver beam tes ts performed in rate aroun ing the test d n half of the f elease rate (J nd notched fl . 18 the spec he unbounde , shear will ta specimen (Ca lease rate (J, lever beam (D of test the pe cribed in AST shown in Fig d is depicted b) Loading ting (Carlber d by Carlberg nd 1.5·10-3 s-1 due to softeni fracture energ , given in J/m flexure (ENF cimen is subj ed part of the ake place at arlberger, Bi given in J/m DCB) can be el strength an TM D 3433 ( g. z a). In Fig (Carlberger, of the DCB s rger, Biel and ger et al was

1

when testin ing of the adh gy was consu m2) can be de ) specimens ected to thre e specimen, w the end of th el and Stigh m2) can be de e used and fracture (ASTM 199 g. 17 b) an

Biel and Sti

specimen. nd Stigh 2009 100 mm/s. ng at room dhesive. The umed. etermined. (Carlberger, ee-point which can be he crack. 2009). etermined. 9). igh 9). , e

H Th 20 on ba Fo hy F A we sp

3

3.

In po po hi elo is Ac ad A sta pr Se po an Fi High speed te

here are exam 011). These t ne componen ar test was us or low and in ydraulic mac Figure 19. Sp s seen in Fig ere used for pecimen teste

.3

E

.3.1

S

n a study (Lo olyurethane) olyurethane a igher strength ongation at b an aftermark ccording to L dhesive joint thicker adhe ates that a th roperties. everal interes olyurethane a nd loaded the ig. 20. esting mples in the tests are perf nt epoxy. To sed with diff ntermediate s chine. lit Hopkinso g. 19 the tests 3D digital im ed.

Experim

Sikaflex-2

ureiro, et al. and compar adhesive it is h and elonga break 400 % ket grade for Lennart Nyst

(0.2 mm) is esive thickne hicker elastom

sting data are adhesive. In em statically literature on formed on a s achieve the ferent setups strain rates (0 on test in tens s were filmed mage correla

ental da

56 FC exp

2010) Sikaf ed with an ep s chemically ation at break and tensile l r automotive tedt at Sika, suitable for ess is suitable meric adhesiv e presented r the study the , in fatigue a n high strain r structural ad high strain r for tension a 0.1 – 53 s-1) sion (upper) 2011). d with high s ation analysis

ata

periment

flex-256 FC w poxy adhesiv identical to k. The tensile

lap shear stre glass replac Sweden (Ny the epoxy ad e for the elas ve joint wou regarding the e authors use and with an im rate testing o dhesive BETA rates (100 – 5 and compres Morin et al. and compres speed camera s to achieve a

tal data

was tested (a ve. Accordin Sikaflex-252 e strength is ength 5 MPa ement busin ystedt 2012) t dhesive but n stomeric type uld improve t e mechanical ed T-peel join mpact. The s of adhesives ( AMATE 149 5000 s-1), spl sion as show used a high s ssion (lower)

as. The acqu a full strain f a one-compon ng to the data 2 but has a so approximate a. The Sikafle ess. the thickness not the Sikafl e of adhesive the measured l properties o nts and singl specimens ar (Morin, et al 96V which is lit Hopkinson wn in Fig. 19 speed ) (Morin, et a uired images field of the onent

asheet for the omewhat ely 7 MPa, ex-256 grade s of the flex adhesive e. Nystedt d Sikaflex of this le lap joints re shown in l. s a n . al. e e e.

In jo is Fr ha su F in A in de Figure 2 n a single lap int the loadin

introduced ( rom the static as a much low ummary of th igure 21. Fai n SLJs and T s seen in Fig ncreases. A co eformation ra 20. Single lap shear joint ( ng is directly (Loureiro, et c (quasi-stati wer stiffness he failure loa ilure loads fo T-joints tested g. 21 a slight omparison o ates are show

p joint geome Dim (SLJ) the maj y through the al. 2010). ic) tests it is s compared to ads in the stat

or the epoxy d in quasi-sta increase in f f the load-di wn in Fig. 22 etry (top) an mensions in m ajor stress co e adhesive al

seen that the o the epoxy tic tests are s

adhesive (A atic condition et al. 2010). failure load i isplacement c 2. d T-peel join mm. mponent is s lthough a ben e SLJ is non-SLJ). All joi shown in Fig AV138) and t ns under 1 an . is observed a curves for th nt geometry ( shear and in t nding momen -linear from t nts failed co g. 21. he polyureth nd 100 mm/m as the deform he SLJ test at (bottom). the T-peel nt and rotatio

the start (and ohesively. A hane (Sikafle min (Loureir mation rate t different on d ex) ro,

F Fa da Th lo re fa te th co a f Figure 22. Lo atigue tests w ata are shown

he fatigue lo ads determin esults are som atigue resistan sting which m he epoxy (Lou ohesively in t frequency of oad-displacem

were also per n in Figs. 23 Figure 23. F ad in Figs. 2 ned for 1 mm mewhat surpr nce. A possib might have s ureiro, et al. the fatigue te f 10 Hz. ment curves o rformed for t -24. Fatigue life c 3-24 are nor m/min deform rising since e ble cause for stronger influ 2010). As w ests. The fati

of SLJs for t al. 2010). the two joint

curve of SLJ rmalized to th mation rate). elastomeric m r the results t uence on the was the case f

igue tests we the polyureth geometries a Js (Loureiro, he average st According to materials are the adhesive elastomeric for the static ere performed hane adhesiv and adhesive et al. 2010). tatic failure l o the authors known for t heating duri adhesive in tests, all spe d with a load

ve (Loureiro,

es. The fatigu

load (failure s the fatigue their improve ing fatigue comparison ecimens faile d ratio R=0.1 et ue ed to ed at

Th At sp de In F he two geom Figure t impact test pecimen (T-jo eformation ra n Fig. 26 the Figure 24. Fa metries were a e 25. Inertial ing an impac oint or SLJ t ate of 1.8·10 static failure

atigue life cur also impact t wheel impac ctor on the in type). The im 5 mm/min. e load at 1 mm rves of T-joi tested with th ct testing equ nertial wheel mpact velocit m/min are co ints (Loureiro he test set up uipment (Lo l hits an anvi ty was 3 m/s ompared with o, et al. 2010 p shown in Fi ureiro, et al. l at the end o which is equ h the impact 0). ig. 25. 2010). of the uivalent to a t loads.

F In le al sta

3.

In str Ho an 4 Th vi re F Figure 26. Fa nterestingly it ss pronounce so concluded atic loading,

.3.2

H

n a study (Mo rain rates ran opkinson bar nd when man MPa, respec he tensile tes isco-elastic p espectively. igure 27. Ev ailure loads o t can be obse ed under imp d that the join

especially fo

High strai

orin, et al. 20 nging from 0 r test equipm nufacturing th ctively) to stu sts performed phenomenon volution of th of specimens at 1 mm/min erved that the pact loading

nt strengths w for the polyur

in rate tes

011) a structu 0.1 to 5000 s -ment. The adh

he test specim udy the influe d at low and as depicted i he tensile elas s under impa n (Loureiro, e differences conditions c were much h rethane adhe

st of struc

ural adhesive -1 using a hig hesive was te mens these w ence of both intermediate in Fig. 27. T stic modulus et al. 2011). ct loads, alon et al. 2010). s between the compared to s higher under esive (Lourei

ctural adh

e, BETAMA gh speed hyd ested in both were cured at h strain rate a e strain rates The strain rate

s as a functio . ng with static e two adhesiv static loading impact loadi ro, et al. 201

hesive

ATE 1496V, w raulic machi h tension and t different pr nd curing pr showed a no es were 5.3·1 on of the strai c failure load ves become g. The study ding than und

10). was tested at ine and a spl d compression ressures (1 an ressure. on-negligible 10-3 and 53 s in rate (Mori ds der t it n nd e s-1, in,

Re in F Si str co F egarding pla n Fig. 28. Figure 28. Tr imilarly, Figs rain rates and ompression.

Figure 29. E

sticity for th

rue tensile str

s. 29-30 show d thus the vis

volution of t an e tensile test ress-true plas w the elastic sco-elastic an the compress nd curing pre ts a visco-pla stic strain cu al. 2011). modulus an nd visco-pla sive elastic m essure (Mori astic behavio urves at diffe nd the stress-s astic behaviou modulus as a in, et al. 2011

our was obser

rent strain ra strain curves ur observed i function of t 1). rved as show ates (Morin, s at different in

the strain rat wn

et

F Fi Fi co Figure 30. Tr igure 31. Tru ig. 31 shows ompressive te rue compress curin ue compressi The strain the influenc esting at a str sive stress-tru g pressure w ive stress-tru n rate at testi ce of curing p rain rate of 5 ue plastic str was 4 MPa (M ue plastic stra ing was 53 s pressure on t 53 s-1. rain curves at Morin, et al. 2 ain curves at -1 (Morin, et he stress lev t different str 2011). different cur al. 2011). els observed rain rates. Th uring pressure d at he es.

4

References

Adhesive Toolkit. April 17, 2012. www.adhesivetoolkit.com (accessed April 17, 2012).

Albinsson, Ola, interview by Torsten Sjögren. Discussion on adhesives (March 16, 2012). ASTM. "ASTM D 3433–99: Standard Test Method for Fracture Strength in Cleavage of

Adhesives in Bonded Metal Joints." ASTM, 1999.

Bennison, S, J Sloan, D Kristunas, P Buehler, T Amos, and C Smith. "Laminated glass for blast mitigation: Role of intrelayer properties." Glass processing days. 2005. Carlberger, Thomas. "Private communication." Gothenburg, May 9, 2012.

Carlberger, Thomas, Anders Biel, and Ulf Stigh. "Influence of temperature and strain rate on cohesive properties of structural epoxy adhesive." International Journal of

Fracture, 155 2009: 155-166.

CEN. ”EN 1288-1:2000 Glass in building - Determination of the bending strength of glass - Part 1: Fundamentals of testing glass.” European Committee for Standardization, 2000.

—. "EN 1288-3:2000 Glass in building - Determination of the bending strength of glass - Part 3: Test with specimen supported at two points (four point bending)."

European Committee for Standardization, 2000.

—. "EN 1288-5:2000 E - Glass in building - Determination of the bending strength of glass - Part 5: Coaxial double ring test on flat specimens with small test surface areas." European Committee for Standardization, 2000.

Cognard, JY, R Créac´hcadec, and Laurent Sohier. "Strategies for the analysis of the behavior of an adhesive in bonded assemblies." Journal of Engineerin Materials

and Technology, Transactions of the ASME, July 2011.

ISO. "ISO 11003-2:2002 - Adhesives - Determination of shear behaviour of structural adhesives - Part 2: Tensile test method using thick adherends." ISO, 2002. —. "ISO 34-1:2010 - Rubber, vulcanized or thermoplastic - Determination of tear

strength - Part 1: Trouser, angle and crescent test pieces." ISO, 2010.

—. ”ISO 4587:2003 - Adhesives - Determination of tensile lap-shear strength of rigid-to-rigid bonded assemblies.” ISO, 2003.

Iwasaki, R, JL Lataillade, och P Viot. ”Experimental study on the interface fracture toughness of PVB (polyvinyl butyral)/glass at high strain rates.” International

Journal of Crashworthiness, 2007: 293-298.

Larcher, Martin, George Solomos, Folco Casadei, and Norbert Gebbeken. "Experimental and numerical investigations of laminated glass subjected to blast loading."

International Journal of Impact Engineering, 18 2012: 42-5.

Loureiro, AL, LFM da Silva, C Sato, and MAV Figueiredo. "Comparison of the Mechanical Behaviour Between Stiff and Flexible Adhesive Joints for the Automotive Industry." The Journal of Adhesion, 2010: 765-787.

Mattiasson, Kjell. ”Private communication.” Chalmers Tekniska Högskola, den 2 April 2012.

Morin, D, G Haugou, B Bennani, and F Lauro. "Experimental characterization of a toughened epoxy adhesive under a large range of strain rates." Journal of

Adhesion Science and Technology, 2011: 1581-1602.

Morison, C, M Zobec, and A Frenceschet. "The measurement of PVB properties at high strain rates, and their application in the design of laminated glass under bomb blast." ISIEMS 2007, International symposium on interaction of the effects of

munitions with structures, 17-21 September. Orlando, USA, 2007.

Nystedt, Lennart. ”Private communication.” Sika Sverige AB, den 9 May 2012.

"Regulation ECE R43." n.d. http://www.unece.org/trans/main/wp29/wp29regs/43rv2e.pdf (accessed April 17, 2012).

"Saint-Gobain Sekurit - Glazing manual." April 17, 2012. http://www.saint-gobain-sekurit.com/en/index.asp?nav1=GC&fn=sgs_auto_glazing.html (accessed April 17, 2012).

SIS. "SS-ISO 37:2012 - Rubber, vulcanized or thermoplatsic - Determination of tensile stress-strain properties." Swedish Standard Institute, 2012.

Timmell, M, S Kolling, P Osterrieder, and P.A. Du Bois. "A finite element model for impact simulation with laminated glass." Internation Journal of Imact

Engineering, 2007: 1465-1478.

Xu, Jun, et al. "Experimental and macroscopic investigation of dynamic crack patterns in PVB laminated glass sheets subjected to light-weight impact." Engineering

Failure Analysis, 2011: 1605-1612.

Xu, Jun, Yibing Li, Bohan Liu, Mengyi Zhu, and Dongyun Ge. "Experimental study on mechanical behavior of PVB laminated glass under quasi-static and dynamic loadings." Composites: Part B, 2011: 302-308.

5

5

Ta Te Pr sp se M Pr Ob M Re sp Ty Di M fo Co Fa at Co Te Sp Fa Eq Re Sp In Re Te an Re

5

A

.1

A

t

able A1. Ten

est Method rinciple imag pecimen or te t-up Mechanical roperties btained Material Quan equirements pecimen ypical Specim imensions (m Materials Suita r Testing ost of Specim abrication/Pr tion ost of esting/Specim pecimen abrication quipment equirements pecimen nstrumentatio equirements est Equipmen nd Fixture equirements

Append

Appendi

esting of

nsile and pee

Tensi Joint ge of st Tensi streng ntity per Low men mm) Diam Adhe thickn able 1—6 men repar Low men Low Surfa prepa on Exten nt Unive mach grips

dices

x 1. Stan

f adhesiv

l test method ile Butt t ile gth/modulus meter 15–25 erend ness 12–15 ace ation nsometer ersal test hine + end

ndard m

ves

ds for adhesi T-Peel Peel strength Low Bond length Width 25 Adherend thickness 0. Arm length 1, 4 and 6 Flexible-flex adherend Low-moder Low Surface preparation Bonding+Bo jig None Universal te machine + e grips

methods f

ves. Clim h Pee stiff Hig h 150 5–1.0 50 Lon Sho Wid Adh 0.5– xible Flex adh 1— stru ate Hig Low onding Sur Bon jig Non est end Spe Uni mac grip

for mech

mbing Drum l strength/skin fness gh ng adherend 3 ort adherend 2 dth 25 herend thickne –5.0 xible-rigid herend —6 + sandwich uctures gh w—moderate face preparati nding+Bondin ne

ecial test fixtur iversal test chine + end ps

hanical

m Floatin Method n Peel str Low 00 240 ess Flexible 250 Rigid ad Width 2 Adheren 0.5–1.6 h Flexible adheren 1—6 Low—m Low—m ion ng Surface Bonding jig Extenso off) re Special Univers machine grips g Roller d ength e adherend dherend 200 25 nd thickness e-rigid nd moderate moderate preparation g+Bonding ometer (2 test fixture sal test e + end

Fa pe Cr Pe En su Da Ac (E St M 1 = 6 = Ta Te Pr of tes M Pr Ob M Qu Re ec Ty Di M Su Te Co Fa ar atigue erformance reep erformance nvironmental uitability ata Reduction ccuracy Estimated) tandard Test Methods Avail = metal-metal = composite-c able A2. Cle

est Method rinciple imag f specimen or st set-up Mechanical roperties btained Material uantity equirements/ cimen ypical Specim imensions (m Materials uitable for esting ost of Specim abrication/Pr ration Limit Suitab l Suitab n Straig To be determ lable ASTM ASTM l; 2 = metal-pl composite. avage and M Wedge ge r Fractur /Sp Low men mm) Length Width 2 Adhere thickne 1 men rep Low ted ble ble ghtforward e mined M D 897 M D 2095 lastic; 3 = met Mode I fractur e Cleavage re energy h 200 25 end ess 2 Unsuitable Possibly Suitable Straightforw Large uncer (> 30%) ISO 8510: P ISO 11339 ASTM 1876 tal-composite ure toughness Compact Tension Cleavage stre high Length 25 Width 25 Adherend thickness 12 1—6 Low-modera Uns Uns Uns ward Stra rtainty To b Part 2 6 AST e; 4 = plastic-p s test method DCB (Dou Cant Beam ength Mode tough Low Leng Width Adhe thickn 1—6 ate Low suitable suitable suitable aightforward be determined TM D 3167 plastic; 5 = pla ds for adhesiv ble tilever m) e I fracture hness th 356 h 25 erend ness 6.35 Unsuita Unsuita Unsuita Straight d To be d ASTM astic-composi ves. TDCB (Tapered D Cantilever Beam) Mode I frac toughness High Length 240 Width 25 Adherend thickness 1 1 and 6 Moderate— able able able tforward determined D 3167 te; Double r cture 0 2.8 —High

Co Te Sp Fa Eq Re Sp In Re Te an Re Fa pe Cr Pe En su Da Ac (E St M Av 1 = 6 = Ta Te Pr sp M Ob M Re Ty Di ost of esting/Specim pecimen abrication quipment equirements pecimen nstrumentatio equirements est Equipmen nd Fixture equirements atigue erformance reep erformance nvironmental uitability ata Reduction ccuracy Estimated) tandard Test Methods vailable = metal-metal = composite-c able A3. She

est Method rinciple imag pecimen or te Mechanical Pr btained Material Quan equirements/ ypical Specim imensions (m men Low Surface prepara on Travell microsc video c nt Self-str Not sui Possibl l Suitabl n Straigh To be d ASTM l; 2 = metal-pl composite. ear test metho

ge of st set-up roperties ntity /Specimen L men mm) L W A t O 2 e ation ling cope or camera ressed itable ly le htforward determined D 3762 lastic; 3 = met

ods for adhes

Single-Lap Shear strength Low Length 100 Width 25 Adherend thickness 2 Overlap lengt 25 Low-modera Surface preparation Bonding + bonding jig Extensomete crack openin displacement Universal tes machine + loading fixtu Suitable Suitable Suitable Straightforw To be determ ASTM D 106 tal-composite sives. Double-h SDouble-hear st Low th Length Width 2 Adheren thicknes Overlap 25 ate Low-Surfa prepa er for ng t Trave micro video st ure Univ mach loadin Suita Unsu Suita ard Straig mined Large 62 ASTM e; 4 = plastic-p -Lap V-trength Sh str Lo 100 25 nd ss 12 length Le W No Ad thi -moderate ace aration elling oscope or o camera ersal test hine + ng fixture ble uitable ble ghtforward e uncertainty M D 3433 plastic; 5 = pla -Notched Bea hear ength/modulu ow ength 76 idth 20 otch width 12 dherend ickness 5 Low-mode Surface preparation Bonding + Bonding jig Travelling microscope video came Universal t machine + loading fix Suitable Unsuitable Suitable Straightfor Moderate ASTM D 3 astic-composi am Arcan us Shear s Low Length Width 4 Notch w Adhere erate n g e or era test ture ward 3433 te; strength/modu 52 40 width 12 end thickness ulus 6

Materials Suitable for Testing

1, 3 and 6 1, 3 and 6 1, 3 and 6 1, 3 and 6

Cost of Specimen Fabrication/Preparation

Low Low-moderate Moderate Moderate

Cost of

Testing/Specimen

Low Low-moderate Low-moderate Low-moderate

Specimen Fabrication Equipment Requirements Surface preparation Bonding + bonding jig Surface preparation Bonding + bonding jig Surface preparation Bonding + Bonding jig Surface preparation Bonding + Bonding jig

Specimen Instrumentation Requirements

None None Shear extensometer Strain gauges

Shear extensometer Strain gauges

Test Equipment and Fixture Requirements Universal test machine + loading grips Universal test machine + loading grips Universal test machine + loading fixture

Universal test machine + loading fixture

Fatigue performance Limited Suitable Unuitable Suitable

Creep Performance Suitable Possibly Unsuitable Unsuitable

Environmental suitability

Suitable Suitable Suitable Suitable

Data Reduction Straightforward Straightforward Straightforward Straightforward

Accuracy (Estimated) Moderate Low (30%) Low—moderate

(10–20%)

Low—moderate (10– 20%)

Standard Test Methods Available BS 5350: Part C5 BS EN 1465 BS EN ISO 9664 ASTM D 1002 ASTM D 3166 BS 5350: Part C5 BS EN ISO 9664 ASTM D 1002 ASTM D 3166 No adhesive standard ASTM D 5379— PMCs None

1 = metal-metal; 2 = metal-plastic; 3 = metal-composite; 4 = plastic; 5 = plastic-composite; 6 = composite-composite.

Ta Te Pr sp M Ob M Re Ty Di M Te Co Fa Co Te Sp Eq Re Sp In Re Te Fi Fa Cr En su Da Ac St Av 1 = 6 =

able A4. She

est Method rinciple imag pecimen or te Mechanical Pr btained Material Quan equirements/ ypical Specim imensions (m Materials Suita esting ost of Specim abrication/Pr ost of esting/Specim pecimen Fabr quipment equirements pecimen nstrumentatio equirements est Equipmen ixture Requir atigue perfor reep Perform nvironmental uitability ata Reduction ccuracy (Esti tandard Test vailable = metal-metal = composite-c

ear and Mode

T ge of st set-up roperties ntity /Specimen L men mm) L W A 2 O able for men reparation L men L rication B j on E o nt and rements mance N mance P l n imated) T Methods I A l; 2 = metal-pl composite. e II fracture t Thick Adher Shear strength/modu Low Length 110 Width 5 Adherend thic 26 Overlap lengt 1- 6 Low-moderat Low Surface prepa Bonding = bo jig Extensometer off) Self-stressed Not suitable Possibly Suitable Straightforwa To be determi ISO 11003 ASTM D 316 lastic; 3 = met toughness te rend To Jo ulus Sh str Lo ckness th 5 Di Ad thi 1— te Lo Lo aration onding Su pre Bo jig rs (2 Ro ext Un ma fix Su Su Su ard Str ined To 65 No tal-composite st methods f orsion Butt int hear ength/modulu ow ameter 15–25 dherend ickness 12–15 —6 ow-moderate ow-moderate urface eparation onding + bond g otary tensometer niversal test achine + loadi xture uitable uitable uitable raightforward o be determine one e; 4 = plastic-p for adhesives Napkin us Shear st Low Length Width 2 Adhere thickne 1—6 Modera Low-m ding Surface prepara Bondin bonding Rotary extenso ng Torsion machin loading Suitable Unsuita Suitable Straight ed To be d ASTM plastic; 5 = pla s. n Ring strength 356 25 end ess 6 ate-high moderate e ation ng + g jig ometer n test ne + g fixture e able e htforward determined E 229 astic-composi ENF (End-Notche Flexure) Mode II fracture energies Low 1 and 6 Low Low-moderat Surface preparation Bonding + Bonding jig Travelling microscope o video camera Universal test machine + flexure fixtur Suitable Unsuitable Suitable Straightforwa Large uncertainty (30%) None te; ed te or a t e ard

5.2

Appendix 2. Standards for mechanical testing of

adhesives

5.2.1

ISO STANDARDS - Number/Title

Cleavage Tests

ISO 10354 (1992): Adhesives—Characterization of Durability of Structural-Adhesive-Bonded Assemblies—Wedge Rupture Test

ISO 11343 (2003): Adhesives—Determination of Dynamic Resistance to Cleavage of High-Strength Adhesive Bonds Under Impact Conditions—Wedge Impact Method Peel Tests

ISO 4578 (1997): Adhesives—Determination of Peel Resistance of High-Strength Adhesive Bonds—Floating-Roller Method

ISO 8510 Part 1 (1990) or BS EN 28510–1 (1993): Adhesives—Peel Test for a Flexible-Bonded-to-Rigid Test Specimen Assembly—Part 1: 90 Degree Peel

ISO 8510–2 (1990) or BS EN 28510–2 (1993): Adhesives—Peel Test for a Flexible-Bonded-to-Rigid Test Specimen Assembly—Part 2: 180 Degree Peel

ISO 11339 (2003): Adhesives - T-Peel Test for Flexible-to-Flexible Bonded Assemblies ISO 14676 (1997): Evaluation of the effectiveness of surface treatment techniques for aluminium - Wet-peel test by floating-roller method

Shear Tests

ISO 4587 (2003): Adhesives—Determination of Tensile Lap-Shear Strength of Rigid-to-Rigid Bonded Assemblies

ISO 6237 (2003): Adhesives—Wood-to-Wood Adhesive Bonds—Determination of Shear Strength by Tensile Loading

ISO 9653 (1998): Adhesives—Test method for Shear Impact Strength of Adhesive Bonds ISO 10123 (1990): Adhesives—Determination of Shear Strength of Anaerobic Adhesives Using Pin-and-Collar Specimens

ISO 10964 (1993): Adhesives—Determination of Torque Strength of Anaerobic Adhesives on Threaded Fasteners

ISO 11003 Part 1 (2001): Adhesives—Determination of Shear Behaviour of Structural Adhesives—Part 1: Torsion Test Method Using Butt-Bonded Hollow Cylinders ISO 11003 Part 2 (2001): Adhesives—Determination of Shear Behaviour of Structural Adhesives—Part 2: Tensile Test Method Using Thick Adherends

ISO 13445 (2003): Adhesives—Determination of Shear Strength of Adhesive Bonds between Rigid Substrates by the Block-Shear Method

Tensile Tests

BS EN ISO 527 Part 1 (1993): Plastics—Determination of Tensile Properties—General Principles

ISO 6922 (1987): Adhesives—Determination of Tensile Strength of Butt Joints

BS EN ISO 9664 (1995): Adhesives—Test Methods for Fatigue Properties of Structural Adhesives in Tensile Shear

Mechanical Properties - Other Tests

BS EN ISO 178 (1998): Plastics—Determination of Flexural Properties ISO 604 (2002): Plastics—Determination of Compressive Properties

BS EN ISO 11403 Part 1 (2000): Plastics—Acquisition and Presentation of Comparable Multipoint Data—Part 1: Mechanical Properties

5.2.2

ASTM STANDARDS - Number/Title

Cleavage Tests

ASTM D 1062–02: Standard Test Method for Cleavage Strength of Metal-to-Metal Adhesive Bonds

ASTM D 3433–99: Standard Test Method for Fracture Strength in Cleavage of Adhesives in Bonded Metal Joints

ASTM D 3807–98 (2004): Standard Test Method for Strength Properties of Adhesives in Cleavage Peel by Tension Loading (Engineering Plastics-to-Engineering Plastics) ASTM D 5041–98 (2004): Standard Test Method for Fracture Strength in Cleavage of Adhesives in Bonded Joints

Peel Tests

ASTM D 1781–98 (2004): Standard Test Method for Climbing Drum Peel for Adhesives ASTM D 1876–01: Standard Test Method for Peel Resistance of Adhesives (T-Peel Test) ASTM D 3167–03a (2004): Standard Test Method for Floating Roller Peel Resistance of Adhesives

Shear Tests

ASTM D 905–03: Standard Test Method for Strength Properties of Adhesive Bonds in Shear by Compression Loading

ASTM D 1002–01: Standard Test Method for Apparent Shear Strength of Single-Lap-Joint Adhesively Bonded Metal Specimens by Tension Loading (Metal-to-Metal) ASTM D 3044–94 (2000): Standard Test Method for Shear Modulus of Wood-Based Structural Panels

ASTM D 3163–01: Standard Test Method for Determining Strength of Adhesively Bonded Rigid Plastic Lap-Shear Joints in Shear by Tension Loading

ASTM D 3164–03: Standard Test Method for Strength Properties of Adhesively Bonded Plastic Lap-Shear Sandwich Joints in Shear by Tension Loading

ASTM D 3165–00: Standard Test Method for Strength Properties of Adhesives in Shear by Tension Loading of Single-Lap-Joint Laminated Assemblies

ASTM D 3528–96 (2002): Standard Test Method for Strength Properties of Double Lap Shear Adhesive Joints by Tension Loading

ASTM D 3983–98(2004): Standard Test Method for Measuring Strength and Shear Modulus of Nonrigid Adhesives by the Thick-Adherend Tensile-Lap Specimen ASTM D 4562–01: Standard Test Method for Shear Strength of Adhesives Using Pin-and-Collar Specimen

ASTM D 4896–01: Standard Guide for Use of Adhesive-Bonded Single Lap-Joint Specimen Test Results

ASTM D 5379/D5379M-98: Standard Test Method for Shear Properties of Composite Materials by the V-Notched Beam Method

ASTM D 5648–01: Standard Test Method for Torque-Tension Relationship of Adhesives Used on Threaded Fasteners (Lubricity)

ASTM D 5656–04: Standard Test Method for Thick-Adherend Metal Lap-Shear Joints for Determination of the Stress-Strain Behaviour of Adhesives in Shear by Tension Loading

ASTM D 5649–01: Standard Test Method for Torque Strength of Adhesives Used on Threaded Fasteners

Tensile Tests

ASTM D 897–01: Standard Test Method for Tensile Properties of Adhesive Bonds ASTM D 2095–96(2002): Standard Test Method for Tensile Strength of Adhesives by Means of Bar and Rod Specimens

Mechanical Properties - Other Tests

ASTM D 695–02a: Standard Test Method for Compressive Properties of Rigid Plastics ASTM D 1995–92 (2004): Standard Test Methods for Multi-Modal Strength Testing of Autohesives (Contact Adhesives)

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