International Journal of Adhesion & Adhesives 48 (2014) 194 209

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International Journal of Adhesion & Adhesives

journal homepage: www.elsevier.com/locate/ijadhadh

Development of a constitutive hyperelastic material law for numerical simulations of adhesive steelglass connections using structural silicone
V. Dias a,n, C. Odenbreit a, O. Hechler a, F. Scholzen a, T. Ben Zineb b,c
a

University of Luxembourg, ArcelorMittal Chair of Steel and Faade Engineering, Rue Coudenhove-Kalergi L-1359, Luxembourg Universit de Lorraine, LEMTA, UMR 7563, Vanduvre-ls-Nancy F-54500, France c CNRS, LEMTA, UMR 7563, Vanduvre-ls-Nancy F-54500, France
b

art ic l e i nf o
Article history: Accepted 12 September 2013 Available online 5 October 2013 Keywords: Hyperelastic material laws Silicone elastomers Quasi-incompressibility Mullins' effect Non-linear numerical simulations

a b s t r a c t
Silicone elastomers are amongst others employed in glass faades as structural connection materials. They are known to be durable adhesives, able to transfer forces under variable loading and atmospheric conditions during their design life. For the dimensioning of adhesive joints, numerical simulations are often used, especially for joints which exhibit large deformations and/or for complex geometries. However, silicones have strong non-linear material behaviour already at small strain deformations, are slightly compressible and show a time-depending behaviour. The current existing material laws do not allow for considering these effects properly in simulation, particularly for combined loading. Therefore a hyperelastic material law for silicones has been developed and validated, based on a strain energy function. For this purpose, test series have been carried out to determine all relevant material parameters needed to describe the strain energy potential, namely tension, compression, shear and multi-axial oedometric test series on non-aged and articially aged specimens. Furthermore, the softening due to low cyclic loading (Mullins' effect) has been considered and quantied by comparison to quasi-static loading for all test series. The developed hyperelastic model has been implemented into the nite element software Abaquss for validation and the results of numerical simulations have been compared to experimental results and existing laws. The comparison showed that the proposed model better matched the real behaviour of silicone elastomers and led to an increase in exactness of the numerical simulations of adhesive joints. & 2013 Elsevier Ltd. All rights reserved.

1. Introduction The construction of fully transparent glass faades is mainly based on two independent structural connection methods, i.e. mechanical xings and adhesive connections. The mechanical connections, except for the classical installations for which the glass panes are placed in a metallic frame, require some machining of the glass, e.g. drilling of holes. The machining procedures often generate aws on the panel edges, which appear critical for the glass strength [1]. Because of the fully linear stressstrain behaviour without any plastic range, the stress peaks due to the aws cannot be redistributed and crack propagation may be initiated. Therefore, the adhesive assemblies are widely increasing. These connection types present several advantages like the uniform distribution of the stresses along the jointed parts and the possibility to bond dissimilar adherents in terms of mechanical

Corresponding author. Tel.: 352 46 66 44 5722; fax: 352 46 66 44 5200. E-mail address: vincent.dias@uni.lu (V. Dias).

and thermal properties. With the recent innovations, adhesives have acquired the capacity to transfer high loads between the joined elements, enabling the realisation of structural systems. The most commonly employed adhesives in existing glass faades are silicone elastomers. They are in particular used to build Structural Sealant Glazing Systems (SSGS), in which they connect the edges of the glass panes to a secondary steel sub-structure. These sealants allow on one hand redistributing the loads acting on the outer glass elements to the steel supporting frame and, on the other hand, compensate the different thermal expansions of the bonded components. Consequently, they appear as determining parts of the system. The choice of the structural sealants and a short design rule concerning the adhesive dimensions, based on the trapezoidal load distribution theory, are provided by European Technical Approvals and Standards [24]. However, the application of out-of-plane loads, such as wind loads, which create up-lifting forces in the corner, are not considered in these design guides [5]. Due to the complexity of the load distribution, the assessment of such structures under combined loadings is accomplished with the help of mock-up tests simulating real conditions.

0143-7496/$ - see front matter & 2013 Elsevier Ltd. All rights reserved. http://dx.doi.org/10.1016/j.ijadhadh.2013.09.043

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Nomenclature W (MPa) Strain energy function W iso (MPa) Isochoric part of the strain energy function W vol (MPa) Volumetric part of the strain energy function J () Third invariant deformation tensor I 1 () First invariant of the left Cauchy-Green Tensor I 2 () Second invariant of the left Cauchy-Green Tensor C i (MPa) Material constant of the Amin model M ; N () Polynomial coefcients W Amin (MPa) Strain energy potential proposed by Amin W Ogden (MPa) Strain energy potential proposed by Ogden i () Deviatoric principal stretches i (MPa) Constant shear moduli of the Ogden model i () Material constant of the Ogden model F () Deformation gradient tensor

F () Volume-preserving deformation tensor B () Left Cauchy-Green tensor B Deviatoric left Cauchy-Green tensor I 1 () First deviatoric strain invariant I 2 () Second deviatoric strain invariant I 3 () Third deviatoric strain invariant Tr () Trace of the matrix det () Determinant of the matrix () Uniaxial elongation s (MPa) Uniaxial stress A; B; C ; D (MPa) Material constants of the strain energy function E () Material constant of the developed strain energy function K (MPa) Material constant of the developed volumetric strain energy function

The insulating glass units (IGU) represent another connection type assembled with elastomers. In this case, the adhesives act as a secondary seal, linking at their extremities two glass plates and ensuring the mechanical stability of the unit. The application of IGUs in faades requires carrying out beforehand tests, regarding the durability of the edge seals [6]. The joint dimensions of insulating glass systems are essentially based on experience and tests. In this way, the design and approval of both assemblies, namely SSGS and IGU, depend on the results of relatively costly experiments. However, nite element analysis could represent a method allowing reducing the number of large-scale tests and optimising the aforementioned parts. As examples, the few researches [7,8], led on the optimisation of IGU edge bonds and based on numerical simulations, demonstrated the inuence on the stresses of the geometry and of the dimensions of the inner steel/aluminium spacer and of the secondary sealant. It has to be mentioned that, for both studies, the hyperelastic material properties were not derived from experimental values and thus were incomplete. To properly model and evaluate the durability of structures involving adhesives, the exact description of the materials properties and their time-depending changes constitutes a fundamental basis. First of all, the resistance against several uniaxial loadings, e.g. uniaxial tension, compression and shear, needs to be characterised. The majority of the phenomenological developed constitutive models are based on the assumption of incompressibility, whose validity varies regarding the different materials [9]. To include volume changes in hyperelastic models, a common method consists in splitting the deformation into an isochoric part and a volumetric part, where the latter depends only on the third invariant deformation tensor J [10]. Therefore, appropriate constitutive modelling approaches providing the possibility to implement the compressibility needs to be identied. In parallel, the quantication of the effect of compressibility should be detected from experimental investigations and assessed for relevance. Further, the softening of the materials stiffness due to repeated load cycles, until constant stiffness is reached, has to be assessed. A possible explanation for this phenomenon was given for the rst time by Mullins and Tobin [11], who postulated a phase change between the initial hard phase toward a soft one observed after several load applications. The so called Mullins' effect needs to be quantied for silicone elastomers and accounted for in the material description. The consideration of adhesives ageing and related changes in material behaviour have to complete the characterisation. In faades, sealants are also subjected to several environmental condition variations, which could affect their behaviour. Under temperature

uctuations, elastomers, constituted of long cross-linked polymer chains, may be subjected to spatial rearrangements at the molecular scale. Damages to the adhesive may also be engendered by UVradiation or humidity absorbed and re-ejected by the material. Hence, the inuence of temperature, UV-radiation and humidity on the material must be evaluated based on experimental investigations on aged test specimens. An articial ageing procedure, regrouping the three environmental factors and simulating ve years of external conditions, was conducted on UV-cured acrylics and polyurethanes and showed changes in behaviour [12]. But, so far, information on the effect of environmental factors on the behaviour of two-component structural silicone sealants are lacking. Therefore, the objective of the work presented in this paper is to t these gaps in current knowledge for silicone elastomers and to propose a constitutive material law describing their quasiincompressible behaviour, possibly dependent on external factors (e.g. combination of temperature, humidity and UV-radiation) and on repeated cyclic action (Mullin's). The validation of the developed law, whose coefcients should be obtained by experiments, has to be achieved with numerical simulations. The development of a new quasi-incompressible hyperelastic constitutive model for the two-component Dow Corning silicone elastomer DC 993, largely employed in structural glass faades, is detailed after highlighting the inadequacy of the existing laws to represent the strong nonlinear behaviour at small-strains. The uniaxial tension/compression, shear and oedometric tests, conducted to t the coefcients of the proposed law, are described hereafter. The inuences of the loading rate, repeated load cycles as well as environmental conditions according to [12] are considered in these tests series and discussed. The validation of the so tted constitutive model, achieved with numerical simulations in which the quasi-incompressible hyperelastic model has been implemented in Abaquss software via a developed UHYPER subroutine, is nally presented.

2. Review of material laws Hyperelastic silicone materials may exhibit nonlinear large deformations up to 700%. A convenient way to describe their behaviour is therefore to postulate the existence of a strain energy function frequently referred as W. At this step, two different theories exist to dene this function: the rst one is based on statistical mechanics of molecular chains/networks and the second relies on the continuum mechanics. With the rst method, the form of W depends essentially on network assumptions, such as the Gaussian theory, representing

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Fig. 1. Descent of the polynomial model for incompressible material.

relatively well the material behaviour under small deformations, or the non-Gaussian theory for large deformations [13]. The most well-known non-Gaussian models were developed by Wang and Guth [14] requiring two parameters, the 3-chain model, the 8-chain established by Arruda and Boyce [15] and the Wu and Van der Giessen [16] corresponding to a weighted combination of the 3- and 8-chain. In spite of their physical interpretation, the involved coefcients in the equation of the aforementioned models have to be determined by testing. The phenomenological models, which are built with the continuum mechanics, derivate from the tting of experimental results. The assumption of isotropy allows expressing the strain energy potential W in terms of the strain invariants I1, I2 and I3. Thus, most of the constitutive laws in literature and implemented in nite element codes present this characteristic. An exhaustive list of phenomenological hyperelastic laws is presented by Hoss and Marczak [17]. The basis of many well-known continuum mechanical laws, such as Neo-Hookean, Mooney-Rivlin or Yeoh, is the polynomial form, constituted of a linear combination of monomial functions expressed in term of the rst and second invariants (Fig. 1). The simple determination of the coefcients with a linear least square method constitutes an advantage of this formulation. However, as it will be demonstrated farther, they are inadequate to represent the strong nonlinearity at low deformations. A polynomial strain energy function with non-integer exponents M and N has been proposed by Amin [18] in order to represent rubbers in compression and shear, see Eq. (1). These exponents have to be determined with a non-linear least square method. Even if this function ts better to the experimental data, it cannot be used if the calculated exponents are negative. W Amin C 5 I 1 3 C3 C4 I 1 3N 1 I 1 3M 1 C 2 I 2 3 N 1 M1 1

with i the deviatoric principal stretches and N, mi, i material parameters to be evaluated from testing. As both ways to dene the strain energy function, based on either the statistical mechanics or the continuum mechanics, relied on the tting of experimental results, the phenomenological description was investigated. The widely employed polynomial model and the Amin model were unt to reproduce test results for combined loading, especially to represent the strong nonlinear effects at low deformations. Moreover other laws, as the Ogden form, need complicated test setups. Therefore, it has been decided to develop a customised constitutive law of polynomial form for the hyperelastic material behaviour of silicone elastomers.

3. Derivation of the adopted constitutive model 3.1. Fundamental theory The strain energy function W, depending solely on the deformation gradient tensor F, allows the full description of the behaviour of incompressible hyperelastic materials. However, when the material can undergo some volume changes, the assumption of incompressibility is invalid and a new denition of the strain energy potential W has to be formulated. Therefore, the idea proposed by Flory [21], consisting in the decomposition of deformation into a volumetric part and an isochoric part, has to be adopted. The deformation gradient tensor F is written as follows: F J 1=3 F
1=3

account for the volume-changing deformations, J being where J the Jacobian of the deformation tensor F (J detF ) and F corresponding to the volume-preserving deformation tensor. The decoupled form of the strain energy function W based on the kinematic assumption of Eq. (3) becomes: W F W iso F W vol J 4

with M and N material parameters and C2 to C5 constants to be determined with tests. Another well-known model, due to Ogden [19], postulates that the strain energy potential could directly be expressed in function of the principal stretches, Eq. (2). This law demonstrates its capacity to simulate the behaviour of the material under large deformations, but requires a large amount of data with at least uniaxial and equibiaxial experiments due to the existence of multiple optimal sets of material coefcients [20]. W Ogden
N

With the large deformation theory [10], the measure of the deformation can be introduced with the help of the deviatoric stretch tensor B similar to the left Cauchy-Green strain tensor T B F F . Finally, by assuming isotropy of the material, the function W can be described in terms of the deviatoric strain invariants I 1 , I 2 ( I 3 constant) as: W F W B W iso B W vol J

2 i

i1

1 2 3 3

W iso I 1 B ; I 2 B W vol J

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with I 1 B TrB 1 2 I 2 B TrB 2 TrB 2 I 3 B detB 1 6 7 8

Several experimental investigations carried out by Obata [22] and Kawabata [23] allowed to demonstrate the respective dependency of W =I 1 and W =I 2 to I 1 and to I 2 . With the introduction of two functions f 1 and f 2 , the following equations are established W I 1 f 1 I 1 W I 2 f 2 I 2 11

where Tr is the trace of the tensor and det the determinant. To derivate the stress s from the strain energy potential W, the principle of virtual work applied in the case of an uniaxial action (e.g. tension or compression) can be invoked W s with s W W I 1 W I 2 W J J I 1 I 2 |{z} |{z}
Isochoric part

10

The strain energy potential W is written as the sum of the integrals of these two functions f 1 and f 2 and the assumptions on the form of W are reported on these two functions. Therefore, by respectively associating f 1 and f 2 to sums of polynomial terms of I 1 and I 2 and by respecting the normalisation condition, for which the strain energy potential vanishes in the reference conguration, i.e. W F I 0 with I the identity matrix, the function W becomes Z W iso
M

Volumepart

where corresponds to the one-dimensional elongation. 3.2. Formulation of the isochoric part The deviatoric strain invariants given in Eqs. (6) and (7) explicitly depend on the deviatoric left Cauchy-Green strain tensor. In the consequence, their expressions are based on the related types of experiments. To determine the form of the strain energy functions, three basic tests, i.e. uniaxial tension, compression and shear tests, were carried out. Based on this approach, the volume variation was considered as non-existent, so that it was conceivable to write J detF 1 and F F . Additionally Eq. (10) was employed to evaluate the stresses corresponding to the experiments and, regarding the form of the deformation gradient tensor F , two categories stood out: (a) the uniaxial tests either tension or compression and (b) the shear tests. The nal forms of the stresses, exposed in Table 1, have been expressed in function of the longitudinal and shear deformations and of the derivatives of the strain energy potential W by the rst and second invariants. At this step, some assumptions on the form of the strain energy function had to be made.
Table 1 Derivation of the stresses related to experiments. (a) Uniaxial tests

i1

iAi I 1 3i 1 dI 1
N

j1

jBj I 2 3j 1 dI 2 12

A i I 1 3i Bj I 2 3j
i1 j1

with Ai and Bj material constants and M and N integers. Eq. (12) corresponds to a particular case of the well-known polynomial form, for which mixed terms are eliminated. The reduced polynomial form and the MooneyRivlin form can still be extracted from the equation Eq. (12). With this denition, the number of constants to be determined depends on the degrees of the polynomials, which are rarely higher than 3 in order to avoid the identication of too many parameters. Besides the unknown degrees of the polynomials, a major problem arises concerning the representation of the shear behaviour which exhibits a strong non-linearity at small strains and at least one inection point, see data from Treloar [24] and Amin [18]. By injecting Eq. (12) into the formulae of the shear stress given in Table 1, a simple polynomial relation can be established " # s12 2 iAi 2i 2 jBj 2j 2 C 0 C 1 3 C 2 5
i1 j1 M N

13

(b) Shear tests

1 B F F @0 0 0 B BB B @0 0 2 1

0 2 0 0
1 1

0 1 B C 0 0 AB @ 3 0 1 0 0
1 1

0
1 =2 1

0 0
1 =2 1

1 C C A

1 B F F @0 0 0

1 0

C 0A 1 1 0 1 0 C 0A 1

1 C C A

1 2 B BB @ 0

1 1 2 I 1 I1 21 I 2 I2 1 2 21

I1 I2 I1 I2 3 2 I3 I3 1

I3 I 3 1 h i W W s11 21 1 3 1 I 1 I 2 s12 2 h
W W I 1 I 2

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where Ai, Bj and C0, C1, C2 are material constants. A standard linear least square method has to be carried out to evaluate these coefcients. The rst term C0 of Eq. (13) represents the slope of the initial tangent of the curve, while the other terms C1 and C2 are reecting the non-linearity at higher strains. By suppressing the rst term in , the representation of the sum of the last terms presents a horizontal tangent at the origin and, therefore, the experimental inection appearing for very small strains at about 0.2 cannot be taken into account. Hence, with an experimental curve tting, the weighting of the coefcient C0 becomes so important that the other terms can be neglected. This phenomenon could be observed on Fig. 2, where a comparison between the experimental data of Amin [18], presenting an inection point at very small strains similar to the ones expected for the tested silicone, and the analytic results of Eq. (13) was exposed. To compensate the poor tting at low strains, see Fig. 3, two further non-linear terms were added to Eq. (12) in conformity to

the normalisation condition: W iso Ai I 1 3i Bj I 2 3j

i1 j1 M N

D D I 2 3 E E

14

with D and E tting material constants to be obtained out of tests. The shear stress arising from this last formulation is provided in Eq. (15). " # M N 2D s12 2 iAi 2i 2 jBj 2j 2 15 2 E2 i1 j1 The only difference between the last equation and Eq. (13) comes from the fraction term, which is equal to zero in the absence of deformation and tends to zero at large shear strains. This term thus introduce the missing non-linearity of the existing hyperelastic models. Therefore, Eq. (14) constitutes the nal potential form employed in this paper to model the isochoric deformations. 3.3. Formulation of the volume-part

2.5
HDR-Amin-Experiments

Estimation Eq. (13)

Several forms of the volumetric part depending on the Jacobian of the deformation J were proposed and listed [25]. One of the most common functions, even employed by the nite element software Abaquss, was established by Sussman and Bathe [26] and is detailed as K W vol J J 12 2 16

12 (MPa)

1.5

0.5

where K is a material constant. The determination of this constant K has to be realized with the help of experiments in which a change in volume could be observed. The oedometric tests, frequently used in rock mechanics, were adapted to this purpose. In this test, the sample is constraint in all directions, except one for the introduction of the load, see Table 2. 3.4. Final constitutive model The complete form of the strain energy potential, to describe the relation between the stress and the strain, results from the sum of the Eqs. (14) and (16). It is important to note that, due to
Table 2 Derivation of the stresses related to oedometric tests.

0 0 0.5 1 (-) 1.5 2 2.5

C0 0,596158

C1 0,009606

C2 0,005776

Fig. 2. Curve tting of experimental data for High Damping Rubber (HDR) with Eq. (13).

2.5 HDR-Amin-Experiments 2 Estimation Eq. (15)

12 (MPa)

1.5

1
2 1 6 F 40 0 3

0.5

0 1 0

0 1

7 05

0 0 0.5 1 (-) A 0,498301 B 0,059097 D 0,03677 E 0,207839 1.5 2 2.5

J detF 2 2 =3 0 6 1 1 =3 60 1 F 6 4 0 0

0 0 1
1 =3

3 7 7 7 5

I 1 B 4=3 2 2=3 I 2 B 4=3 22=3

Fig. 3. Curve tting of experimental data for HDR with Eq. (15).

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the change in volume, the isochoric part of the strain energy function has to be written in terms of the deviatoric invariants to preserve the unity of the third invariant (I 3 1). In consequence, Eq. (17) constitutes the nal form of the strain energy W W iso I 1 ; I 2 W vol J Ai I 1 3i Bj I 2 3j
i1 j1 M N

D I 2 3 E

D K J 12 E 2

17

The material parameters Ai, Bj, D and E are determined with the help of curve ttings of the tensile, compression and shear tests, while the parameter K is obtained with oedometric tests.

4. Experimental investigations 4.1. Tensile tests Standard polymer dog-bone samples can be obtained by three main processes, i.e. moudling, cutting or manufacturing. The cutting process needs the realisation of a large plate of adhesive with constant thickness, to then form the shape with cutting dies described in the ISO 23529 [27]. The manufacturing method consists in the rectication of rectangular pieces with a milling machine. The softness of silicone elastomers, especially the one of the selected structural silicone Dow Corning DC 993, makes the cutting and the manufacturing way of fabrication almost impossible. The preparation of a plate presenting parallel surfaces entails the use of a machine to compress a predened amount of silicone, which generally introduces air bubbles. Thus, the moudling procedure was employed to produce the dog-bone samples. The mold was composed of two parts: a non-adhesive lower part in Pom C (copolymer Polyoxymethylene) in which three identical shapes according to dog-bone type 1B of the ISO 527-2 [28] were machined, see Fig. 4, and an upper part in Plexiglas connected to a vacuum pump to inject the silicone at ambient temperature and humidity, see Fig. 5. The curing process of the

selected two component silicone started in the mold in spite of its air-tightness. The specimens were unmolded 24 h after the injection and then stored for a period of one month at ambient temperature and humidity shielded from light. The samples manufactured with this injection procedure were exempt of any edge-aws and air bubbles. As silicone elastomers are mainly employed in structural sealant glazing systems to bond the glass and the steel together, these materials are subjected to several climate changes and load variations. A common method to determine the factors inuencing the behaviour of the silicone consists in drawing up an Ishikawa diagram. This diagram, also called sh-bone diagram, is based on listing the possible causes around six main points: material, manpower, methods, measuring methods, machining and environment. With this listing method, the possible factors inuencing the strength and strain at breakage of the silicone were extracted and divided in two classes:

 The environmental factors, namely temperature, humidity

and UV-radiation. To evaluate the impact of these three parameters, an articial ageing procedure could be undertaken, considering one factor at a time, but in reality interactions between these exist. Therefore a detailed procedure, described in EN ISO11431 [29] and recommended in the ETAG 002, which allows the determination of the degree of adhesion after exposure to heat, UV-light and water, was selected. According to this standard, a cyclic exposure has to be carried out for 3 weeks (504 h) in which the samples are placed in water at 25 7 3 1C for 5 h a day and in an oven at 65 7 5 1C under UV-light the rest of the time. The testing factor, i.e. the loading rate. In contrary to the articial ageing procedure, this factor has to be taken into account during the testing phase. With regards to the high deformations of the silicone and to the tested length of 60 mm, two different loading rates were regarded: 50 mm/min (relatively slow) and 500 mm/min (high).

Fig. 4. Lower part of the mold for dog-bone samples.

These two factors were considered with the help of the Taguchi design of experiments (DOE) method. The latter enables minimising the number of tests to be carried out by not necessarily changing one factor at a time. The inuences of each factor or of their interactions on the experimental results can be evaluated with a variance analysis. For two factors with two levels, i.e. aged and non-aged and 50 mm/min and 500 mm/min, the Taguchi table is given in Table 3. Accordingly, only four tests are needed, but to have a better variance, two tests series were conducted. The tensile tests were realized on a 10 kN INSTRON mobile hydraulic press with self-closing wedge clamps having a large number of teeth at their surface to avoid any sliding, see Fig. 6. A 10 kN force sensor was installed to measure the applied loads. The forcedisplacement data were converted in stressstrain curves by dividing the force by the tested section area and the displacement by the initial testing length of 60 mm, see Fig. 8. The test results conrmed the strong non-linear behaviour with a full-recovery of the dimensions after unloading, as expected
Table 3 Taguchi design of experiment for tensile tests. Standard test no Factors A Ageing 1 2 3 4 No aged No aged Aged Aged B Loading rate (mm/min) 50 500 50 500

Fig. 5. Mold for dog-bone samples and vacuum pump.

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for hyperelastic silicone material. The results also showed the independence of the silicone properties towards the articial ageing and the loading rate. All the curves, for aged or non-aged specimens tested at low and high loading rate, were relatively well superposed, see Fig. 8 for the extremum curves. To ensure the stability of the silicone properties even at small strain, the stiffness at the origin was calculated according to the linearization of the strain proposed in ETAG 002. A variance analysis based on the ANAVAR method [30] was carried out on these calculated values and veried the independence of the tensile stressstrain data with respect to the environmental and loading rate factors. This result was visible on the surface plot of the initial stiffness results exposed in Fig. 7, for which no tendency could be extracted in reason of the observed roof shape. Indeed, for non-aged specimens the stiffness increased with the loading rate, while the opposite occurred for aged specimens. In addition to these quasi-static tests, a second test series of ve dog-bone samples was subjected to a low number of cyclic loadings with the aim to probe the Mullins effect. The evoked test

set-up for the quasi-static tests was conserved for these experiments. The specimens were initially elongated to 40 mm (equivalent to a strain of 0.6) and then subjected to sinusoidal loading of 40 mm of amplitude and controlled in displacement. Two different frequencies were applied on non-aged specimens in spite of the independence on loading rate found for the quasi-static tests. Three samples were tested at a low frequency of 0.1 Hz and two samples were tested at 1 Hz. Again results showed no dependency to the frequency, the ve cyclic curves being almost superimposable. A typical stressstrain diagram issued from one sample is provided in Fig. 9. It is to be noted that, after the rst cycle, the stress shows an important loss in all the strain range. However, this stress softening becomes smaller with the increase of the number of cycles and disappears almost completely after ve cycles. Compared to the rst cycle, the most important loss in stress of about 0.25 MPa occurs at a strain of 0.6, see Fig. 9.

4.2. Compression tests The description of hyperelastic materials in numerical nite element codes, such as Abaquss, mostly relies on the curve tting of uniaxial tensile experimental data. To model silicone joints subjected to solely tensile loading, this denition could be sufcient. However, complex stress distributions involving all the types of loadings arise in real systems. Hence, the curve tting of tensile data allowing the calculation of material constants,

Tensile stress-strain diagram

1.2 1 0.8 (MPa) 0.6 0.4
Min

0.2 0 0 0.5 (-)

Fig. 6. Tensile dog-bone test.

Average Max

1.5

Fig. 8. Stressstrain diagram for silicone dog-bone samples under uniaxial quasistatic tension.

Fig. 7. Surface plot of the stiffness at the origin K0 according to the ageing and the loading rate Tension tests.

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corresponding to the selected material model, is generally insufcient to appraise the compressive behaviour of hyperelastic elastomers. The realisation of quasi-static and cyclic compression tests appears indispensable. The test specimens were manufactured in a Teon mould of 45 mm of diameter and 20 mm of height cut out of a circular standard silicone cartridge, see Fig. 10. The silicone was simply poured inside the mould and the surplus was evacuated by closing the free extremities with Teon plates and applying pressure. The samples were let for 24 h in the mould to achieve a complete curing and then stored for one month, shielded from light, at ambient temperature and humidity. As for the dog-bone samples, a Taguchi design of experiments was drawn up, regarding the two factors environmental and loading rate. The articial ageing procedure, described previously, remained identical. Only the loading rate was adapted to the size of the compression specimens, i.e. 5 mm/min as lower limit and 50 mm/min for high

Cyclic stress-strain diagram

1.2 1 0.8 (MPa) 0.6 0.4 0.2 0 0 0.2 0.4 0.6 (-)
Fig. 9. Stressstrain diagram for silicone dog-bone samples under uniaxial cyclic tension.

SC28 -1Hz 5th exp. loading slope

speed tests. The 10 kN INSTRON press employed for the tensile tests allowed realizing the compression ones by removing the jaws and adapting a system composed by two parallel steel plates. The measured displacement corresponded to the displacement of the machine and the force was recorded with the help of a 10 kN sensor. Pilot tests were rst carried out with Teon plates disposed at the extremities of the samples to avoid the friction between the silicone and the steel. This method has proved to be insufcient as the lateral expansion of the specimen was restricted. Thus, a Teon spray was pulverised on the steel plates before proceeding to each test, see Fig. 11. As for the tension, the stressstrain diagrams in compression were highly non-linear. Once unloaded, the specimens recovered immediately their initial dimensions even after a compression of 70% of the height, which is a characteristic of hyperelastic material. The curves with minimum, maximum and mean values are represented in Fig. 13. Aged and non-aged specimens, subjected to different loading rates, presented the same behaviour demonstrating one more time the invariance of the silicone properties towards both factors. The stiffness at origin was calculated according to ETAG 002 for all specimens. The conducted ANAVAR method validated the invariance of the material, as exposed on Fig. 12. To complete the evaluation of Mullin's effect, cyclic compression tests have been carried out. For that reason, a sinusoidal loading of 6 mm of amplitude was applied on a pre-compressed sample to a displacement of 6 mm. Two frequencies were comprehended in the test program, a low frequency of 1 Hz and a high frequency of 10 Hz. A typical curve is shown in Fig. 14 for a specimen tested at 1 Hz. The stabilisation of the stress took place after ve cycles, like for the tensile tests, and no effect of the frequency was noticed. 4.3. Shear tests In the majority of actual steelglass constructions, like for example the structural sealant glazing systems, the adhesives are subjected to elevated short- and long-term shear forces, arising from the self-weight of the glazing element and from the transfer of wind loads to the steel supporting structure. The real shearbehaviour of silicone elastomer has to be assessed before undertaking numerical simulations or design. The most shear tests found in literature are based on single lapjoint tests, where only two adherents are bonded via the adhesive joint. In these experiments, one adherent is generally xed while either a force or a displacement is applied onto the other. An important drawback of this test is due to the presence of peel stresses which interfere with the shear stresses and which prevent the correct determination of the latter. Therefore, the global geometry selected for the shear tests series was the double-lap

0.8

1.2

1.4

Fig. 10. Compression silicone sample.

Fig. 11. Test set-up with Teon spray on the steel surface. (a) Before test and (b) during test.

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Fig. 12. Surface plot of the stiffness at the origin K0 according to the ageing and the loading rate Compression tests.

Compressive stress-strain diagram

9 8 7 6 (MPa) 5 4 3 2 1 0 0 0.2 0.4 (-) 0.6 0.8
As for the tensile experiments, an Ishikawa diagram was set up to account for the most inuent factors which were classied into three main categories for the double lap-joint shear tests, i.e. the geometrical, the environmental and the loading rate. The environmental parameters were constituted by temperature, humidity and UV-radiation and were treated with the cyclic articial ageing procedure proposed by EN ISO11431. The geometrical factors were split in two categories: the bonding size, equivalent to the solicited glued area, and the bonding thickness. By taking into account the dimensions of the adherent plates of the push-out sample and the positioning of the steel with regard to the glass (free vertical gap of 40 mm), two bonding areas were considered, i.e. 544 cm2, equivalent to all the contact area and 192 cm2, was partitioned in 4 silicone strips of 30 mm width each. Concerning the thickness of the joint, the EOTA for structural sealant glazing preconised a minimal thickness of 6 mm, equivalent to the minimal dimension advised by the adhesive manufacturer. The two investigated thickness dimensions were nevertheless 3 mm and 6 mm. As the two geometrical factors were investigated independently, a Taguchi design of experiments containing four factors with two levels each was drawn up, see Table 4. As it can be noted, sixteen experiments were necessary to full this DOE. The loading rates were chosen in accordance to the both thicknesses. The realisation of the samples was divided in two parts regarding the size of the bonding, i.e. either 2 large strips (544 cm2) or 4 strips (192 cm2):
Fig. 15. Push-out geometry.

Max Average Min

Fig. 13. Stressstrain diagram for silicone under uniaxial quasi-static compression.

Cyclic stress-strain diagram

4.5 4 3.5 3 (MPa) 2.5 2 1.5 1 0.5 0 0 0.1 0.2 0.3 (-) 0.4 0.5 0.6
SC-34 -1Hz 5th exp. loading slope

Fig. 14. Stressstrain diagram for silicone under uniaxial cyclic compression.

joint assembly as investigated by Hart Smith [31]. Two outer fullytempered glass plates measuring 240 200 12 mm and an inner steel plate of 200 200 12 mm were brought together with silicone elastomer. The symmetry of the samples allowed restraining the appearance of peel stress. A gap of 4 cm between the bottom of the glass plates and the steel plate was inserted with the aim to undertake the test in compression, see Fig. 15. Crucial tensile stresses were thus not introduced in the glass.

 The rst procedure, for large bonded areas, consisted in a

simple pouring process for the both thicknesses of 3 mm and 6 mm. The rst glass plate was inserted horizontally into a xed frame, then calibrated Teon spacers were added, followed by the pouring operation. The same procedure was applied on the second glass plate. The nal step corresponded to the positioning of the steel plate on the rst poured system

V. Dias et al. / International Journal of Adhesion & Adhesives 48 (2014) 194 209 Table 4 Taguchi design of experiment for double lap-joint shear tests. Standard test no A Ageing B Bonding size (cm) C Bonding thickness (mm) 3 3 6 6 3 3 6 6 3 3 6 6 3 3 6 6 D Results Loading rate Shear (mm/min) strength (MPa) 3 90 3 90 3 90 3 90 3 90 3 90 3 90 3 90 1.302 1.583 0.919 1.302 1.024 1.185 0.898 0.931 1.270 1.591 0.729 1.252 1.220 1.425 0.897 0.514

203

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16

No aged No aged No aged No aged No aged No aged No aged No aged Aged Aged Aged Aged Aged Aged Aged Aged

192 192 192 192 544 544 544 544 192 192 192 192 544 544 544 544

Fig. 17. Pre-assembly prepared for the injection of the 4 strip.

Fig. 18. 192 cm2 manufactured sample.

Fig. 16. Injector for small bonded areas.

and the closure with the second one. A pressure was applied on the whole assembly to remove the surplus. The second procedure for the four silicone strips of 30 mm was based on injection for the two bonding thicknesses of 3 mm and 6 mm. A self-designed injector, adaptable to the cartridge, was manufactured, see Fig. 16. This allowed injecting the adhesive in a pre-assembled system, for which the appropriate joint dimensions were achieved with the help of Teon spacers, see Fig. 17. An aged nished sample presenting 4 strips was exposed on Fig. 18.

The tests were carried out displacement-controlled on a 630kN INSTRON mobile hydraulic piston (max. recorded load of 64,6kN). To ensure transferring only pure shear action in the adhesive, two lateral steel supports surrounded the push-out sample and a polyamide spacer was introduced in the gap existing between the glass plates, see Fig. 19(a). Glass contact with steel was prevented laterally by inserting two Neoprene spacers 3 mm thick and horizontally by disposing a Teon plate of 3 mm under the specimen. With the latter, the lateral displacements of the glass plates during the tests were not restrained. The load was

introduced through the upper steel part, where only steel to steel contact occurred. In addition to the press total displacement measurement, six external displacement sensors were installed on each push-out specimen. The deformation in the silicone, assimilated to relative displacement between the glass and steel plates, was measured at two opposite sides with the help of polyamide sensor-xing devices attached to one glass plate and of steel bars bonded on the lower edge of the steel plate, see Figs. 19(b) and 18. With this disposition, eventual rotations of the inner steel plate were observable. As pure shear was expected, a control of the opening of the tested assembly was undertaken by measuring the displacements perpendicular to the two glass surfaces. This objective was achieved by positioning two 10 mm horizontal sensors at the top free glass surfaces, see Fig. 19(c). Finally, the lateral expansion of the glass was also measured at opposite sides with two horizontal in-plane displacement sensors, Fig. 19(b). Horizontal displacement sensors measuring the opening of the assembly, i.e. the possible rotation of the glass plates around their supported edges, recorded insignicant values, see the worst case of test No. 12 of Table 4 on Fig. 20. Consequently both glass plates remained parallel during testing, resulting in pure shear loading of the silicone. The two lateral displacement sensors, accounting for the strain in glass, showed relatively small values, see Fig. 21 for the test No. 12. Only the relative displacement sensors provided noteworthy data. Thus, the determination of shear strains was conceivable and realized by dividing the relative displacement by the joint thickness. As all the samples broke cohesively, the calculation of shear stresses was done by dividing the total applied load by the net bonding area, measured with an image-processing program after breakage. The mean curve, the minimal and maximal values are shown in Fig. 22, where a large dispersion on the stressstrain

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Fig. 19. Double lap-joint shear (a) set-up, (b)relative displacement sensors and (c) opening displacement sensors.

Opening versus Time

0.6
opening 10mm back

Shear stress-strain diagram

1.2
Min Average Max

0.4 0.2
op (mm)

opening 10mm front Breakage

Test No. 12

1 0.8 (MPa) 0.6 0.4 0.2 0

0 0 -0.2 -0.4 -0.6 Time (s)

Fig. 20. Largest opening disp. versus time for test No. 12.

10

15

20

0.2

0.4 (-)

0.6

0.8

Fig. 22. Stressstrain diagram for silicone double-lap joint samples under quasistatic shear loading.

Glass lat. disp. versus Time

0.3 0.2 0.1
lat (mm)

lateral 10mm right lateral 10mm left Breakage

Test No. 12

0 0 -0.1 -0.2 -0.3 Time (s)

Fig. 21. Glass lateral disp. versus time for test No. 12.

10

15

20

data, due to the difcult pouring manufacturing process of the samples, can be noticed. A statistical ANAVAR study was carried out on the calculated shear strengths given in Table 4. From this analysis, it emerged that the articial ageing and the loading rate had no impact on the silicone properties regarding shear, in contrary to the geometrical factors, which were responsible of the large strength variations. The dependency between strength and

bonding area can be explained with the difference in the realisation of the samples, for which the silicone was either injected (192 cm2) or poured (544 cm2). With the injection method, the strength was found slightly higher than for the poured process. Additionally, the strength decreased with an increasing of the joint thickness. The better results were thus obtained for the small injected bonded area with a narrow joint thickness. This study allows demonstrating, on one hand, the non-dependency of the material to loading rate and ageing and, on the other hand, the importance of the manufacturing process and the control of the thickness to enhance the properties of steelglass connections using structural silicone subjected to shear. Additional tests should be performed to appraise to which extend these factors affect the shear material strength and to provide representing mathematical functions. The stress softening corresponding to the Mullin's effect was investigated with the help of cyclic tests carried out on push-out samples. To account for unfavourable cases, the largest dimensions of the bonding area were associated to a thickness of 3 mm. The test set-up and the data acquisition system of the static tests, composed by six external displacement sensors, were re-used for the cyclic tests. The samples were initially subjected to a displacement of 2.25 mm (strain of about 0.64) and then subjected to a sinusoidal displacement of 2.25 mm of amplitude. For all the tests, a frequency of 0.01 Hz was regarded. A typical cyclic stressstrain diagram and the curve extracted at the 5th cycle, where a

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205

stabilisation of the stress was found, are shown in Fig. 23. After the rst cycle a global loss of 0.1 MPa was observed until a strain of 0.6 which has to be considered in design. 4.4. Oedometric tests To determine the properties of silicone under a multiaxial stress state, the oedometric test layout was employed. According to this test, a circular sample is inserted into a rigid steel frame and is loaded from the top through a piston, see Fig. 24. To obtain a good reproducibility, the size of the sample must t perfectly the size of the rigid frame, otherwise a slight uniaxial compression adulterates the results. During the installation of the specimen into the frame, air can be trapped. Therefore, holes had to be drilled to evacuate the air. The last difculty came from the manufacture of the circular samples, whose dimensions had to be identic and of the same size than the ones of the frame. Consequently, the method used for the realisation of the compressive samples could not be considered in this case. A new method was created to inject the silicone into a Teon mold to produce bubble-free specimens with 30 mm of diameter and 15 mm of height. As it was demonstrated previously for the uniaxial compression tests, the ageing had no impact on the properties of the silicone and only the loading rate was chosen for the oedometric tests as possible inuence criterion. Silicone elastomers are presented in literature as quasi-incompressible and

exhibiting almost no deformation on elevated loads, which led to the selection of two very low loading rates, i.e. 0.1 mm/min and 1 mm/min. To conduct the oedometric tests, the 10kN INSTRON mobile hydraulic cylinder was used displacement-controlled. Force and displacement were respectively recorded by an external force sensor and by the machine. The obtained stressstrain diagram was more linear than the ones of the other tests and presented a very low dispersion in stress for a given strain, see Fig. 25 in which the maximum and minimum encountered stresses were close to the average ones. The loading rate did not inuence the results and high stresses were reached under very low deformations. With these experiments, the evaluation of the volume-part of the strain energy potential, as described in Section 3.3, was feasible.

5. Identication of the material law coefcients The characterisation of the silicone elastomer was analytically derived in the chapters 3.1 to 3.3 and is based on a combined strain energy potential of an isochoric- and a volume-part, see Eq. (17). With the help of the test results derived from the four experiment types, chapters 4.1 to 4.4, it is now possible to determine the material coefcients of this equation. The determination of the coefcients was carried out in two steps, i.e. rst the evaluation of the isochoric-part coefcients, for which the Jacobian of the deformation tensor F was equivalent to unity, and then the estimation of the unique volume-part coefcient K.

Cyclic stress-strain diagram

1 0.9 0.8 0.7
(MPa)
M-2 -0.01Hz 5th exp. loading slope

Oedometric stress-strain diagram

16 14 12
(MPa)

0.6 0.5 0.4 0.3 0.2 0.1 0 0 0.2 0.4 0.6 (-) 0.8 1 1.2

10 8 6 4 2 0 0 0.01 0.02 (-) 0.03 0.04

Min Average Max

Fig. 23. Stressstrain diagram for silicone under cyclic shear loading.

Fig. 25. Stressstrain diagram for oedometric tests on silicone.

Fig. 24. Oedometric test (a) schematisation and (b) test set-up.

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Table 5 Material parameters for the developed strain energy potential including compressibility. Test type Quasi-static (Instantaneous property) 5th cyclic loading (End of Mullin's effect) A (MPa) 0.259 0.057 B (MPa) 0.010 0.021 C (MPa) 0.044 0.075 D (MPa) 0.009 0.041 E (-) 0.186 0.490 K (MPa) 377.221 377.221

Fig. 26. Isochoric strain energy potential W versus the deviatoric invariants for the quasi-static case.

Fig. 27. Finite element analysis of (a) uniaxial tension, (b) uniaxial compression and (c) shear tests User models.

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207

Therefore, the average uniaxial stressstrain tension and compression experimental data were regrouped in only one set of data to identify, with a non-linear least square method, the material parameters Ai, Bj, D and E associated to a chosen form of the strain energy potential. The non-linear least square method of LevenbergMarquardt [32] was inevitable due to the two last terms linking the coefcients D and E. This method corresponds to the iterative Gauss-Newton least square method, where a damping factor is added to control the speed of the convergence. These both methods are based on a linear approximation of the searched function, in this case the strain energy potential. Once the coefcients calculated, they allowed the prediction of the shear, which was then compared to the averaged experimental curve. This procedure was repeated for different polynomial degrees of M and N until nding a form able to t as close as possible the tension, compression and shear tests data. The retained form of the strain energy potential with the respective coefcients to model the quasi-static and the stress strain behaviour at the end of the Mullin's effect is given in Eq. (18); the related material parameters are listed in Table 5. D K W AI 1 3 BI 1 32 C I 2 3 J 12 I 2 3 E E 2 D 18

section of 10 4 mm) and applying corresponding symmetry boundary conditions. A simple displacement was applied on the upper face of the silicone part. Quadratic hybrid elements C3D20H were employed to solve the problem under Abaqus/ Standard. True stresses and true strains were converted to engineering stresses and strains, to be compared to the test data. As the compressive tests were performed on cylindrical specimens, an axisymmetric representation was envisaged. While the displacements at the bottom were restrained, the loading was introduced on the sample via the upper edge of the model by imposing a displacement. The implicit method of resolution

1.2

0.8 (MPa)

0.6

For the quasi-static isochoric set of coefcients, the average curves of Figs. 8, 13 and 22 were considered, while for the cyclic behaviour at the end of the Mullin's effect, only the 5th experimental loading curves exposed on Figs. 9, 14 and 23 were regarded. The differences observed between both quasi-static and cyclic sets of coefcients arose from the consequent loss in stresses between the rst and fth experimental loading curves. The material parameter K, accounting for the volume-change, was then calculated with the help of the oedometric experimental average data and of Eq. (18). As the isochoric coefcients were already known, the coefcient K was determined with a simple linear curve tting. Other cyclic oedometric experiments were performed exposing the invariance of the stressstrain data and, consequently, the invariance of the coefcient K towards cyclic actions. Table 5 gives the material parameter representing the instantaneous and the characteristic behaviour after several cycles of quasi-incompressible silicone elastomer.

0.4

0.2

0 0 0.2 0.4 0.6 (-) 0.8 1

TENSION-User TENSION-NeoHooke TENSION-Mooney TENSION-Yeoh TENSION-Poly2ndO Experimental Data

1.2

1.4

2.5

1.5 (MPa) 1

6. Verication and numerical simulations A rst verication prior to numerical approval of the form and coefcients of the strain energy potential, given by Eq. (18) and Table 5, consists in ensuring, that the function is always positive, despite the presence of a negative coefcient for the quasi-static representation. Indeed, the strain-energy function W must always increase with growing deformations. In the volume-part, the Jacobian of the deformation tensor is raised to the second power, multiplied by a positive coefcient. This implies that this term is always positive. Therefore, only the isochoric-part of the strain energy function was checked by plotting the isochoric strain energy potential W versus the deviatoric invariants I 1 and I 2 for the quasi-static case, see Fig. 26, and the cyclic case. From the physical point of view, this demonstrates the correctness of the evaluated coefcients for the proposed constitutive model. To compare the developed law with the existing models exposed in Section 2 and the experimental results, a UHYPER subroutine in FORTRAN was implemented in the numerical software Abaquss. Uniaxial tension and compression as well as shear tests, see Fig. 27, were numerically modelled as follows to ensure of the correctness of the written subroutine:

0.5

COMPRESSION-User COMPRESSION-NeoHooke COMPRESSION-Mooney COMPRESSION-Yeoh COMPRESSION-Poly2ndO Experimental Data

0 0 0.1 0.2 0.3 (-) 0.4 0.5 0.6

0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 0 0.1 0.2 0.3 0.4 (-) 0.5 0.6
SHEAR-User SHEAR-NeoHooke SHEAR-Mooney SHEAR-Yeoh SHEAR-Poly2ndO Experimental Data

(MPa)

0.7

0.8

0.9

 Uniaxial tension was modelled by considering only one fourth

of the straight tested length of the dog bone sample (cross

Fig. 28. Comparison of material model for (a) uniaxial tension, (b) uniaxial compression and (c) shear tests.

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14 12 10
(MPa)

8 6 4 2 0 0 0.01 0.02 (-) 0.03 0.04

Oedometric -Experiments FEA -UHYPER -CAX8H

Fig. 29. Finite element analysis of (a) oedometric tests and (b) results comparison.

of Abaqus was employed in combination to quadratic hybrid CAX8H elements. The shear analyses were carried out on parallelepiped samples, whose dimensions were given by the ETAG-002, i.e. a square cross section of 12 mm 12 mm and a length of 50 mm. As for the shear push-out tests, only pure shear was investigated and the only difference came from the reduced size of the joint, which was estimated less time consuming. On two opposite surfaces, analytical rigid plates were tied to the sample and two reference points were attached to these rigid plates. A displacement was applied on one rigid plate while the other was xed. C3D8H quadratic and hybrid elements were used to solve with Abaqus/Standard this shear problem. Standard stressstrain diagrams were obtained by recording the reaction forces at the xed rigid plate and the displacement at the opposite plate.

The proposed model, namely user law, was compared to the experimental data and results derived with the laws of Neoh Hooke, MooneyRivlin, Yeoh and the 2nd order polynomial form for the cases pure tension, pure compression and shear, see Fig. 28. The strong non-linearity of the material behaviour under small strains ts better with the user model than with the other constitutive laws, which differ more form the real behaviour. The oedometric tests have also been modelled under Abaquss in an axisymmetric way and subjected to a nite displacement. Stressstrain diagrams of experimental and numerical analyses were examined and a relatively good concordance was found, see Fig. 29.

A complete series of quasi-static and cyclic tests in tension, compression and shear was executed for the determination of 5 of the coefcients representing the isochoric-part of the foreseen strain energy potential. The 6th coefcient was studied with the help of oedometric tests. Further, the invariance of the silicone properties concerning ageing (UV-radiation, temperature and humidity) and concerning the loading rate was assessed with statistical methods. Finally, only the dimensions of the bonded area, reecting the process of fabrication, and the joint thickness were found to be of inuence on the strengths of shear tests. Injection techniques associated to relatively small thicknesses of the joint of about 3 mm are hence highly recommended to attain higher shear strengths. The developed constitutive model with the evaluated material coefcients were inserted into the nite element software Abaquss via a UHYPER subroutine and numerical simulations of the conducted tests were undertaken. Results of these simulations were compared with the experimental stressstrain curves and a high correlation was established for each test. The numerical investigations proved the validity and the suitability of the proposed constitutive model, which could be exploited to predict the behaviour of more complex assemblies, such as for structural sealant glazing systems or for secondary sealant of insulating glass panes. Nevertheless, the long-term behaviour should also be investigated with relaxations tests conducted in uniaxial tension/ compression and shear.

Acknowledgements The authors wish to express their deep gratitude to ArcelorMittal, Guardian Luxembourg and VitrumLux for their support with steel and glass materials as well as Dow Corning and the Kmmerling-Chemie company for structural silicone and their inspiring cooperation.

7. Summary and conclusion After a review of the most well-known and employed material laws for hyperelastic material, a problem concerning the representation of the strong non-linearity at small strains had been identied. Therefore, a new model was developed and proposed for silicone elastomer to mitigate this difculty. The developed law, based on a combined strain energy potential of an isochoricand a volume-part, contained six material constants and could be used for quasi-static, instantaneous, numerical simulations and to reproduce the behaviour of the elastomer after several cycles, i.e. after the Mullin's effect stress softening. This duplicity was achieved by adapting the material coefcients. In addition, the quasi-incompressibility of the material was included too and could be appraised. The complete procedure, allowing the identication of these 6 coefcients, and the related tests were detailed in this article.

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