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Contents lists available at ScienceDirect

**International Journal of Adhesion & Adhesives
**

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

Development of a constitutive hyperelastic material law for numerical simulations of adhesive steel–glass 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 Façade Engineering, Rue Coudenhove-Kalergi L-1359, Luxembourg Université de Lorraine, LEMTA, UMR 7563, Vandœuvre-lès-Nancy F-54500, France c CNRS, LEMTA, UMR 7563, Vandœuvre-lès-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 façades 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 artiﬁcially aged specimens. Furthermore, the softening due to low cyclic loading (Mullins' effect) has been considered and quantiﬁed by comparison to quasi-static loading for all test series. The developed hyperelastic model has been implemented into the ﬁnite 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 façades is mainly based on two independent structural connection methods, i.e. mechanical ﬁxings 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 ﬂaws on the panel edges, which appear critical for the glass strength [1]. Because of the fully linear stress–strain behaviour without any plastic range, the stress peaks due to the ﬂaws 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

n

Corresponding author. Tel.: þ 352 46 66 44 5722; fax: þ 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 façades 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 [2–4]. 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

until constant stiffness is reached. is detailed after highlighting the inadequacy of the existing laws to represent the strong nonlinear behaviour at small-strains. Therefore. In façades. Hence. whose coefﬁcients should be obtained by experiments. whose validity varies regarding the different materials [9]. namely SSGS and IGU. linking at their extremities two glass plates and ensuring the mechanical stability of the unit. The consideration of adhesives ageing and related changes in material behaviour have to complete the characterisation. The uniaxial tension/compression. Review of material laws Hyperelastic silicone materials may exhibit nonlinear large deformations up to 700%. 2. B.8]. However. The inﬂuences of the loading rate. It has to be mentioned that. As examples. sealants are also subjected to several environmental condition variations. The validation of the developed law. the few researches [7. UV-radiation and humidity on the material must be evaluated based on experimental investigations on aged test specimens. A convenient way to describe their behaviour is therefore to postulate the existence of a strain energy function frequently referred as “W”. who postulated a phase change between the initial hard phase toward a soft one observed after several load applications. the design and approval of both assemblies. may be subjected to spatial rearrangements at the molecular scale. compression and shear. the form of W depends essentially on network assumptions. achieved with numerical simulations in which the quasi-incompressible hyperelastic model has been implemented in Abaquss software via a developed UHYPER subroutine. conducted to ﬁt the coefﬁcients of the proposed law. Therefore. depend on the results of relatively costly experiments. The application of IGUs in façades requires carrying out beforehand tests. a common method consists in splitting the deformation into an isochoric part and a volumetric part. which could affect their behaviour. In this way. Under temperature ﬂuctuations. regarding the durability of the edge seals [6]. The validation of the so ﬁtted constitutive model. N (–) Polynomial coefﬁcients W Amin (MPa) Strain energy potential proposed by Amin W Ogden (MPa) Strain energy potential proposed by Ogden λi (–) Deviatoric principal stretches μi (MPa) Constant shear moduli of the Ogden model αi (–) 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 TrðÞ (–) Trace of the matrix detðÞ (–) Determinant of the matrix λ (–) Uniaxial elongation s (MPa) Uniaxial stress A. The joint dimensions of insulating glass systems are essentially based on experience and tests. so far. has to be achieved with numerical simulations. the inﬂuence of temperature. for both studies. representing . humidity and UV-radiation) and on repeated cyclic action (Mullin's). information on the effect of environmental factors on the behaviour of two-component structural silicone sealants are lacking. the softening of the materials stiffness due to repeated load cycles. led on the optimisation of IGU edge bonds and based on numerical simulations. possibly dependent on external factors (e. the quantiﬁcation of the effect of compressibility should be detected from experimental investigations and assessed for relevance. the hyperelastic material properties were not derived from experimental values and thus were incomplete. elastomers. regrouping the three environmental factors and simulating ﬁve years of external conditions. Dias et al. But. largely employed in structural glass façades. was conducted on UV-cured acrylics and polyurethanes and showed changes in behaviour [12]. the adhesives act as a secondary seal. where the latter depends only on the third invariant deformation tensor J [10]. 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 parallel. two different theories exist to deﬁne this function: the ﬁrst one is based on statistical mechanics of molecular chains/networks and the second relies on the continuum mechanics. appropriate constitutive modelling approaches providing the possibility to implement the compressibility needs to be identiﬁed. A possible explanation for this phenomenon was given for the ﬁrst time by Mullins and Tobin [11]. The development of a new quasi-incompressible hyperelastic constitutive model for the two-component Dow Corning silicone elastomer DC 993©. In this case.g. Further. First of all. the resistance against several uniaxial loadings. To properly model and evaluate the durability of structures involving adhesives. are described hereafter. An artiﬁcial ageing procedure. such as the Gaussian theory. the objective of the work presented in this paper is to ﬁt these gaps in current knowledge for silicone elastomers and to propose a constitutive material law describing their quasiincompressible behaviour. constituted of long cross-linked polymer chains. repeated load cycles as well as environmental conditions according to [12] are considered in these tests series and discussed. The majority of the phenomenological developed constitutive models are based on the assumption of incompressibility. demonstrated the inﬂuence on the stresses of the geometry and of the dimensions of the inner steel/aluminium spacer and of the secondary sealant. e. is ﬁnally presented. uniaxial tension. shear and oedometric tests.g. With the ﬁrst method. The so called Mullins' effect needs to be quantiﬁed for silicone elastomers and accounted for in the material description. C . has to be assessed. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 195 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 . To include volume changes in hyperelastic models. Damages to the adhesive may also be engendered by UVradiation or humidity absorbed and re-ejected by the material. the exact description of the materials properties and their time-depending changes constitutes a fundamental basis. ﬁnite element analysis could represent a method allowing reducing the number of large-scale tests and optimising the aforementioned parts. combination of temperature. At this step.V. needs to be characterised.

Derivation of the adopted constitutive model 3. 1). I 2 ( I 3 constant) as: W ðF Þ ¼ W ðBÞ ¼ W iso ðB Þ þ W vol ðJ Þ 2μ i i¼1 αi 2 ðλ1 þ λ2 þ λ3 À 3Þ αi αi αi ð2Þ ¼ W iso ðI 1 ðB Þ. 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 ¼ F F . I2 and I3. The basis of many well-known continuum mechanical laws. has to be adopted. by assuming isotropy of the material. Moreover other laws.and 8-chain”. The deformation gradient tensor F is written as follows: F ¼ J 1=3 F 1=3 ð3Þ account for the volume-changing deformations. However. Descent of the polynomial model for incompressible material. it cannot be used if the calculated exponents are negative. postulates that the strain energy potential could directly be expressed in function of the principal stretches. it has been decided to develop a customised constitutive law of polynomial form for the hyperelastic material behaviour of silicone elastomers. (1). 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. depending solely on the deformation gradient tensor F. The simple determination of the coefﬁcients with a linear least square method constitutes an advantage of this formulation. but requires a large amount of data with at least uniaxial and equibiaxial experiments due to the existence of multiple optimal sets of material coefﬁcients [20]. see Eq. In spite of their physical interpretation. the idea proposed by Flory [21]. However. the phenomenological description was investigated. J being where J the Jacobian of the deformation tensor F (J ¼ detðF Þ) and F corresponding to the volume-preserving deformation tensor. the “3-chain” model. This law demonstrates its capacity to simulate the behaviour of the material under large deformations. These exponents have to be determined with a non-linear least square method. Eq. constituted of a linear combination of monomial functions expressed in term of the ﬁrst and second invariants (Fig. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 Fig. most of the constitutive laws in literature and implemented in ﬁnite element codes present this characteristic. Dias et al. the involved coefﬁcients in the equation of the aforementioned models have to be determined by testing. need complicated test setups. mi. especially to represent the strong nonlinear effects at low deformations. The assumption of isotropy allows expressing the strain energy potential W in terms of the strain invariants I1. Mooney-Rivlin or Yeoh. Thus. αi material parameters to be evaluated from testing. they are inadequate to represent the strong nonlinearity at low deformations. As both ways to deﬁne the strain energy function. Another well-known model. relied on the ﬁtting of experimental results. The phenomenological models. I 2 ðB ÞÞ þ W vol ðJ Þ ð5Þ .196 V.1. W Ogden ¼ ∑ N With the large deformation theory [10]. Fundamental theory The strain energy function W. consisting in the decomposition of deformation into a volumetric part and an isochoric part. or the non-Gaussian theory for large deformations [13]. derivate from the ﬁtting of experimental results. when the material can undergo some volume changes. Even if this function ﬁts better to the experimental data. due to Ogden [19]. (3) becomes: W ðF Þ ¼ W iso ðF Þ þ W vol ðJ Þ ð4Þ with M and N material parameters and C2 to C5 constants to be determined with tests. The decoupled form of the strain energy function W based on the kinematic assumption of Eq. relatively well the material behaviour under small deformations. based on either the statistical mechanics or the continuum mechanics. such as Neo-Hookean. which are built with the continuum mechanics. 1. the assumption of incompressibility is invalid and a new deﬁnition of the strain energy potential W has to be formulated. as it will be demonstrated farther. Therefore. is the polynomial form. (2). The most well-known non-Gaussian models were developed by Wang and Guth [14] requiring two parameters. the function W can be described in terms of the deviatoric strain invariants I 1 . 3. An exhaustive list of phenomenological hyperelastic laws is presented by Hoss and Marczak [17]. W Amin ¼ C 5 ðI 1 À 3Þ þ C3 C4 ðI 1 À 3ÞN þ 1 þ ðI 1 À 3ÞM þ 1 þ C 2 ðI 2 À 3Þ N þ1 Mþ1 ð1Þ with λi the deviatoric principal stretches and N. Finally. 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. as the Ogden form. Therefore. The widely employed polynomial model and the Amin model were unﬁt to reproduce test results for combined loading. allows the full description of the behaviour of incompressible hyperelastic materials.

At this step. 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. (a) Uniaxial tests i¼1 ∑ iAi ðI 1 À 3Þi À 1 dI 1 þ N M Z j¼1 ∑ jBj ðI 2 À 3Þj À 1 dI 2 ð12Þ N ¼ ∑ A i ðI 1 À 3Þi þ ∑ Bj ðI 2 À 3Þj i¼1 j¼1 with Ai and Bj material constants and M and N integers. for which the strain energy potential vanishes in the reference conﬁguration. (10) was employed to evaluate the stresses corresponding to the experiments and.g. (6) and (7) explicitly depend on the deviatoric left Cauchy-Green strain tensor. i. the function W becomes Z W iso ¼ M VolumeÀpart where λ corresponds to the one-dimensional elongation. a simple polynomial relation can be established " # s12 ¼ 2γ ∑ iAi γ 2i À 2 þ ∑ jBj γ 2j À 2 ¼ C 0 γ þ C 1 γ 3 þ C 2 γ 5 i¼1 j¼1 M N ð13Þ (b) Shear tests λ1 B F ¼F ¼@0 0 0 B B¼B ¼B @0 0 λ2 1 0 0 λ2 0 0 À1 λ1 0 0 λ1 B C 0 0 A¼B @ λ3 0 1 0 0 À1 λ1 0 À 1 =2 λ1 0 0 À 1 =2 λ1 1 C C A 0 1 B F ¼F ¼@0 0 0 0 γ 1 0 0 1 C 0A 1 γ 1 0 1 0 C 0A 1 1 C C A 0 1 þ γ2 B B¼B ¼@γ 0 À1 þ λ1 2 I 1 ¼ I1 ¼ 2λ1 I 2 ¼ I2 ¼ λ1 À 2 þ 2λ1 I1 ¼ I2 ¼ I1 ¼ I2 ¼ 3 þ γ 2 I3 ¼ I3 ¼ 1 I3 ¼ I 3 ¼ 1 h i W δW s11 ¼ 2ð1 À λ1 À 3 Þ λ1 δ δ I 1 þ δI 2 s12 ¼ 2γ h δW δW δI 1 þ δ I 2 i . compression and shear tests. (12). uniaxial tension. 3. were carried out. Dias et al. some assumptions on the form of the strain energy function had to be made. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 197 with I 1 ðB Þ ¼ TrðB Þ 1 2 I 2 ðB Þ ¼ ½TrðB Þ2 À TrðB Þ 2 I 3 ðB Þ ¼ detðB Þ ¼ 1 ð6Þ ð7Þ ð8Þ Several experimental investigations carried out by Obata [22] and Kawabata [23] allowed to demonstrate the respective dependency of δW =δI 1 and δW =δI 2 to I 1 and to I 2 . for which mixed terms are eliminated. Therefore. (12) corresponds to a particular case of the well-known polynomial form. Eq. The reduced polynomial form and the Mooney–Rivlin form can still be extracted from the equation Eq. so that it was conceivable to write J ¼ detðF Þ ¼ 1 and F ¼ F .V. the volume variation was considered as non-existent. Additionally Eq. a major problem arises concerning the representation of the shear behaviour which exhibits a strong non-linearity at small strains and at least one inﬂection point. their expressions are based on the related types of experiments. i. Table 1 Derivation of the stresses related to experiments.2. Formulation of the isochoric part The deviatoric strain invariants given in Eqs. tension or compression) can be invoked ∂W ¼ s ∂λ with s¼ ∂ W ∂W ∂I 1 ∂ W ∂I 2 ∂W ∂J ¼ þ þ ∂J ∂λ ∂λ ∂I 1 ∂λ ∂I 2 ∂λ |ﬄﬄﬄ{zﬄﬄﬄ} |ﬄﬄﬄﬄﬄﬄﬄﬄﬄﬄﬄﬄﬄ{zﬄﬄﬄﬄﬄﬄﬄﬄﬄﬄﬄﬄﬄ} Isochoric part ð9Þ ð10Þ 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. the number of constants to be determined depends on the degrees of the polynomials. two categories stood out: (a) the uniaxial tests either tension or compression and (b) the shear tests. which are rarely higher than 3 in order to avoid the identiﬁcation of too many parameters. the principle of virtual work applied in the case of an uniaxial action (e. By injecting Eq. exposed in Table 1. With this deﬁnition.e. The ﬁnal forms of the stresses. Besides the unknown degrees of the polynomials. regarding the form of the deformation gradient tensor F . In the consequence. W ðF ¼ I Þ ¼ 0 with I the identity matrix. the following equations are established ∂W ∂I 1 ¼ f 1 ðI 1 Þ ∂W ∂I 2 ¼ f 2 ðI 2 Þ ð11Þ where Tr is the trace of the tensor and det the determinant. have been expressed in function of the longitudinal and shear deformations and of the derivatives of the strain energy potential W by the ﬁrst and second invariants. Based on this approach. (12) into the formulae of the shear stress given in Table 1. To determine the form of the strain energy functions.e. To derivate the stress s from the strain energy potential W. With the introduction of two functions f 1 and f 2 . three basic tests. see data from Treloar [24] and Amin [18].

see Fig. 2. 2. Bj and C0.596158 C1 0. (15).009606 C2 0.5 1 (-) 1. except one for the introduction of the load.5 2 2. the weighting of the coefﬁcient C0 becomes so important that the other terms can be neglected.005776 Fig. " # M N 2Dγ s12 ¼ 2γ ∑ iAi γ 2i À 2 þ ∑ jBj γ 2j À 2 þ ð15Þ ðγ 2 þ EÞ2 i¼1 j¼1 The only difference between the last equation and Eq.3. Curve ﬁtting of experimental data for High Damping Rubber (HDR) with Eq. (13) represents the slope of the initial tangent of the curve.5 C0 0. It is important to note that. due to Table 2 Derivation of the stresses related to oedometric tests.5 1 2 λ1 6 F ¼40 0 3 0. Dias et al.03677 E 0. The ﬁrst term C0 of Eq. (13). (15). the representation of the sum of the last terms presents a horizontal tangent at the origin and. This term thus introduce the missing non-linearity of the existing hyperelastic models. the experimental inﬂection appearing for very small strains at about 0. Hence. (13) comes from the fraction term. even employed by the ﬁnite element software Abaquss. (13) Several forms of the volumetric part depending on the Jacobian of the deformation J were proposed and listed [25]. A standard linear least square method has to be carried out to evaluate these coefﬁcients. Eq.2 cannot be taken into account. By suppressing the ﬁrst term in γ . while the other terms C1 and C2 are reﬂecting the “non-linearity” at higher strains.5 HDR-Amin-Experiments 2 Estimation Eq. 3. Curve ﬁtting of experimental data for HDR with Eq. where a comparison between the experimental data of Amin [18].5 HDR-Amin-Experiments 2 Estimation Eq. (15) σ12 (MPa) 1. were adapted to this purpose.498301 B 0. (14) and (16). the sample is constraint in all directions.4. This phenomenon could be observed on Fig. Final constitutive model The complete form of the strain energy potential. therefore. One of the most common functions. Therefore. see Table 2. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 where Ai. The shear stress arising from this last formulation is provided in Eq.059097 D 0. frequently used in rock mechanics.5 J ¼ detðF Þ ¼ λ 2 2 =3 λ 0 6 1 À 1 =3 60 λ1 F ¼6 4 0 0 0 0 λ1 À 1 =3 3 7 7 7 5 I 1 ðBÞ ¼ λ4=3 þ 2λ À 2=3 I 2 ðB Þ ¼ λ À 4=3 þ 2λ2=3 Fig.5 0 1 0 0 1 7 05 0 0 0. 3. The oedometric tests. C1.207839 1. was established by Sussman and Bathe [26] and is detailed as K W vol ðJ Þ ¼ ðJ À 1Þ2 2 ð16Þ 12 (MPa) 1. The determination of this constant K has to be realized with the help of experiments in which a change in volume could be observed. 2. and the analytic results of Eq. 3.5 2 2. To compensate the poor ﬁtting at low strains. which is equal to zero in the absence of deformation and tends to zero at large shear strains. results from the sum of the Eqs. two further “non-linear” terms were added to Eq. Formulation of the volume-part 2. C2 are material constants. (12) in conformity to the normalisation condition: W iso ¼ ∑ Ai ðI 1 À 3Þi þ ∑ Bj ðI 2 À 3Þj À i¼1 j¼1 M N D D þ ðI 2 À 3 þ EÞ E ð14Þ with D and E ﬁtting material constants to be obtained out of tests. 3.198 V. to describe the relation between the stress and the strain. (14) constitutes the ﬁnal potential form employed in this paper to model the isochoric deformations.5 1 0. presenting an inﬂection point at very small strains similar to the ones expected for the tested silicone.5 where K is a material constant.5 1 γ (-) A 0. In this test. (13) was exposed. 0 0 0. with an experimental curve ﬁtting. .

only four tests are needed. i. The samples manufactured with this injection procedure were exempt of any edge-ﬂaws and air bubbles. the Taguchi table is given in Table 3. The “softness” of silicone elastomers. namely temperature. to then form the shape with cutting dies described in the ISO 23529 [27].V. A common method to determine the factors inﬂuencing the behaviour of the silicone consists in drawing up an Ishikawa diagram. The force–displacement data were converted in stress–strain curves by dividing the force by the tested section area and the displacement by the initial testing length of 60 mm. is based on listing the possible causes around six main points: material. Fig. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 199 the change in volume. these materials are subjected to several climate changes and load variations.1. Tensile tests Standard polymer “dog-bone” samples can be obtained by three main processes. Mold for dog-bone samples and vacuum pump. 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. moudling. As silicone elastomers are mainly employed in structural sealant glazing systems to bond the glass and the steel together. I 2 Þ þ W vol ðJ Þ ¼ ∑ Ai ðI 1 À 3Þi þ ∑ Bj ðI 2 À 3Þj À i¼1 j¼1 M N D ðI 2 À 3 þ EÞ D K þ þ ðJ À 1Þ2 E 2 ð17Þ The material parameters Ai. especially the one of the selected structural silicone Dow Corning DC 993. the moudling procedure was employed to produce the “dog-bone” samples. but in reality interactions between these exist. This diagram. considering one factor at a time. was selected. which allows the determination of the degree of adhesion after exposure to heat. D and E are determined with the help of curve ﬁttings of the tensile. According to this standard. 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. Lower part of the mold for dog-bone samples. . 6. humidity and UV-radiation.e. see Fig. aged and non-aged and 50 mm/min and 500 mm/min. see Fig. With regards to the high deformations of the silicone and to the tested length of 60 mm. 4. two tests series were conducted. Experimental investigations 4. while the parameter K is obtained with oedometric tests. but to have a better variance. i. (17) constitutes the ﬁnal form of the strain energy W ¼ W iso ðI 1 . cutting or manufacturing. makes the cutting and the manufacturing way of fabrication almost impossible. as expected Table 3 Taguchi design of experiment for tensile tests. With this listing method. These two factors were considered with the help of the Taguchi design of experiments (DOE) method. Bj.e. Eq. two different loading rates were regarded: 50 mm/min (relatively slow) and 500 mm/min (high). which generally introduces air bubbles. For two factors with two levels. 5. described in EN ISO11431 [29] and recommended in the ETAG 002. the loading rate. and an upper part in Plexiglas connected to a vacuum pump to inject the silicone at ambient temperature and humidity. To evaluate the impact of these three parameters. manpower. In contrary to the artiﬁcial ageing procedure. the possible factors inﬂuencing the strength and strain at breakage of the silicone were extracted and divided in two classes: The “environmental” factors. The preparation of a plate presenting parallel surfaces entails the use of a machine to compress a predeﬁned amount of silicone. 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 ¼ 1). compression and shear tests. 8. machining and environment. an artiﬁcial ageing procedure could be undertaken. see Fig. The latter enables minimising the number of tests to be carried out by not necessarily changing one factor at a time. also called ﬁsh-bone diagram. methods. In consequence. i. The test results conﬁrmed the strong non-linear behaviour with a full-recovery of the dimensions after unloading. The “testing” factor. 4. The inﬂuences of each factor or of their interactions on the experimental results can be evaluated with a variance analysis. 5. 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.e. Standard test no Factors A ¼ Ageing 1 2 3 4 No aged No aged Aged Aged B ¼ Loading rate (mm/min) 50 500 50 500 Fig. A 10 kN force sensor was installed to measure the applied loads. The curing process of the selected two component silicone started in the mold in spite of its air-tightness. Dias et al. 4. measuring methods. Therefore a detailed procedure. see Fig. 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 manufacturing method consists in the rectiﬁcation of rectangular pieces with a milling machine. UV-light and water. Thus. The cutting process needs the realisation of a large plate of adhesive with constant thickness. this factor has to be taken into account during the testing phase. Accordingly.

200 V. However. complex stress distributions involving all the types of loadings arise in real systems. 7. Tensile stress-strain diagram 1. mostly relies on the curve ﬁtting of uniaxial tensile experimental data. This result was visible on the surface plot of the initial stiffness results exposed in Fig.6) and then subjected to sinusoidal loading of 40 mm of amplitude and controlled in displacement. The evoked test set-up for the quasi-static tests was conserved for these experiments. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 for hyperelastic silicone material. Tensile dog-bone test. 4. Stress–strain diagram for silicone dog-bone samples under uniaxial quasistatic tension. Indeed. . In addition to these quasi-static tests. A typical stress–strain diagram issued from one sample is provided in Fig. All the curves.25 MPa occurs at a strain of 0. after the ﬁrst cycle.5 Fig. for which no tendency could be extracted in reason of the observed roof shape.6. Two different frequencies were applied on non-aged specimens in spite of the independence on loading rate found for the quasi-static tests. were relatively well superposed. 8 for the extremum curves. To ensure the stability of the silicone properties even at small strain. 9. To model silicone joints subjected to solely tensile loading. Average Max 1 1. for non-aged specimens the stiffness increased with the loading rate. Compression tests The description of hyperelastic materials in numerical ﬁnite element codes.4 Min 0. see Fig. Compared to the ﬁrst cycle.8 (MPa) 0. see Fig. 7. the most important loss in stress of about 0. 6. this stress softening becomes smaller with the increase of the number of cycles and disappears almost completely after ﬁve cycles. the curve ﬁtting of tensile data allowing the calculation of material constants. The results also showed the independence of the silicone properties towards the artiﬁcial ageing and the loading rate. this deﬁnition could be sufﬁcient. the ﬁve cyclic curves being almost superimposable. such as Abaquss. a second test series of ﬁve “dog-bone” samples was subjected to a low number of cyclic loadings with the aim to probe the Mullin’s effect. However.2 0 0 0. Dias et al. Hence.2. 8. Again results showed no dependency to the frequency. The specimens were initially elongated to 40 mm (equivalent to a strain of 0. for aged or non-aged specimens tested at low and high loading rate.6 0. A variance analysis based on the ANAVAR method [30] was carried out on these calculated values and veriﬁed the independence of the tensile stress–strain data with respect to the “environmental” and loading rate factors. It is to be noted that. the stiffness at the origin was calculated according to the linearization of the strain proposed in ETAG 002. Three samples were tested at a low frequency of 0. 9. while the opposite occurred for aged specimens.2 1 0. Surface plot of the stiffness at the origin K0 according to the ageing and the loading rate – Tension tests.5 (-) Fig.1 Hz and two samples were tested at 1 Hz. the stress shows an important loss in all the strain range. Fig.

8 1 1. Stress–strain diagram for silicone dog-bone samples under uniaxial cyclic tension. one adherent is generally ﬁxed while either a force or a displacement is applied onto the other. a Teﬂon spray was pulverised on the steel plates before proceeding to each test. The samples were let for 24 h in the mould to achieve a complete curing and then stored for one month. The conducted ANAVAR method validated the invariance of the material. This method has proved to be insufﬁcient as the lateral expansion of the specimen was restricted. The artiﬁcial ageing procedure. described previously. The curves with minimum. the adhesives are subjected to elevated short. (a) Before test and (b) during test. 13. The real shearbehaviour of silicone elastomer has to be assessed before undertaking numerical simulations or design. a low frequency of 1 Hz and a high frequency of 10 Hz. In these experiments. 11. a Taguchi design of experiments was drawn up. The stabilisation of the stress took place after ﬁve cycles. at ambient temperature and humidity. 4. The measured displacement corresponded to the displacement of the machine and the force was recorded with the help of a 10 kN sensor. maximum and mean values are represented in Fig. . Fig. 14 for a specimen tested at 1 Hz. the global geometry selected for the shear tests series was the double-lap 0. Once unloaded. As for the tension.6 (-) Fig. i. 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. 5 mm/min as lower limit and 50 mm/min for high Cyclic stress-strain diagram 1. and no effect of the frequency was noticed.6 0. Two frequencies were comprehended in the test program. a sinusoidal loading of 6 mm of amplitude was applied on a pre-compressed sample to a displacement of 6 mm. Thus. A typical curve is shown in Fig. 12.4 0. The test specimens were manufactured in a Teﬂon mould of 45 mm of diameter and 20 mm of height cut out of a circular standard silicone cartridge. Only the loading rate was adapted to the size of the compression specimens. as exposed on Fig. is generally insufﬁcient to appraise the compressive behaviour of hyperelastic elastomers. As for the “dog-bone” samples.2 1. the specimens recovered immediately their initial dimensions even after a compression of 70% of the height. shielded from light. 10. the stress–strain diagrams in compression were highly non-linear. To complete the evaluation of Mullin's effect.2 0.2 1 0. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 201 corresponding to the selected material model. The realisation of quasi-static and cyclic compression tests appears indispensable. see Fig.4 0. regarding the two factors “environmental” and “loading rate”. 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 most shear tests found in literature are based on single lapjoint tests. 9. Therefore. like for the tensile tests. The stiffness at origin was calculated according to ETAG 002 for all specimens. 11.3.8 (MPa) 0. SC28 -1Hz 5th exp. loading slope speed tests. Compression silicone sample. arising from the self-weight of the glazing element and from the transfer of wind loads to the steel supporting structure. presented the same behaviour demonstrating one more time the invariance of the silicone properties towards both factors.2 0 0 0. see Fig. Aged and non-aged specimens. Dias et al. where only two adherents are bonded via the adhesive joint. Pilot tests were ﬁrst carried out with Teﬂon plates disposed at the extremities of the samples to avoid the friction between the silicone and the steel. cyclic compression tests have been carried out. which is a characteristic of hyperelastic material. The silicone was simply poured inside the mould and the surplus was evacuated by closing the free extremities with Teﬂon plates and applying pressure.4 Fig. Test set-up with Teﬂon spray on the steel surface. For that reason. 10. remained identical.and long-term shear forces.V. subjected to different loading rates.e. Shear tests In the majority of actual steel–glass constructions. like for example the structural sealant glazing systems.

The two investigated thickness dimensions were nevertheless 3 mm and 6 mm.8 As for the tensile experiments. see Fig. The “environmental” parameters were constituted by temperature.5 2 1. 15. and the bonding thickness. The geometrical factors were split in two categories: the bonding size. 13. equivalent to the solicited glued area.5 0. 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). a Taguchi design of experiments containing four factors with two levels each was drawn up. see Table 4. then calibrated Teﬂon spacers were added. Max Average Min Fig. Cyclic stress-strain diagram 4. The loading rates were chosen in accordance to the both thicknesses.1 0. The ﬁrst glass plate was inserted horizontally into a ﬁxed frame. Crucial tensile stresses were thus not introduced in the glass. the “geometrical”. i.4 (-) 0.5 1 0. two bonding areas were considered.202 V. The ﬁrst procedure. The symmetry of the samples allowed restraining the appearance of peel stress.2 0. i. As it can be noted.3 (-) 0. consisted in a simple pouring process for the both thicknesses of 3 mm and 6 mm. Stress–strain diagram for silicone under uniaxial cyclic compression. i. an Ishikawa diagram was set up to account for the most inﬂuent factors which were classiﬁed into three main categories for the double lap-joint shear tests. 14. 544 cm2. The ﬁnal step corresponded to the positioning of the steel plate on the ﬁrst poured system . 15.5 4 3.e.5 0 0 0.6 0. the “environmental” and the “loading rate”. loading slope Fig.5 3 (MPa) 2. either 2 large strips (544 cm2) or 4 strips (192 cm2): Fig. equivalent to the minimal dimension advised by the adhesive manufacturer.e. the EOTA for structural sealant glazing preconised a minimal thickness of 6 mm. Dias et al. followed by the pouring operation. sixteen experiments were necessary to fulﬁl this DOE.2 0. humidity and UV-radiation and were treated with the cyclic artiﬁcial ageing procedure proposed by EN ISO11431. Stress–strain diagram for silicone under uniaxial quasi-static compression. Two outer fullytempered glass plates measuring 240 Â 200 Â 12 mm and an inner steel plate of 200 Â 200 Â 12 mm were brought together with silicone elastomer.4 0. Surface plot of the stiffness at the origin K0 according to the ageing and the loading rate – Compression tests. 12. equivalent to all the contact area and 192 cm2. was partitioned in 4 silicone strips of 30 mm width each. As the two geometrical factors were investigated independently. 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. joint assembly as investigated by Hart Smith [31]. The realisation of the samples was divided in two parts regarding the size of the bonding. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 Fig. The same procedure was applied on the second glass plate.e. Compressive stress-strain diagram 9 8 7 6 (MPa) 5 4 3 2 1 0 0 0.6 SC-34 -1Hz 5th exp. Concerning the thickness of the joint. Push-out geometry. for large bonded areas.

six external displacement sensors were installed on each push-out specimen.897 0. the lateral displacements of the glass plates during the tests were not restrained. resulting in pure shear loading of the silicone. Finally. see the worst case of test No. The two lateral displacement sensors. 19(b). where only steel to steel contact occurred. 20. As all the samples broke cohesively. and the closure with the second one. This allowed injecting the adhesive in a pre-assembled system. the determination of shear strains was conceivable and realized by dividing the relative displacement by the joint thickness. measured with an image-processing program after breakage. see Fig. Consequently both glass plates remained parallel during testing. for which the appropriate joint dimensions were achieved with the help of Teﬂon spacers.898 0. An aged ﬁnished sample presenting 4 strips was exposed on Fig. 19(a). the calculation of shear stresses was done by dividing the total applied load by the net bonding area. Fig. a control of the “opening” of the tested assembly was undertaken by measuring the displacements perpendicular to the two glass surfaces. the minimal and maximal values are shown in Fig. showed relatively small values. 192 cm2 manufactured sample. The deformation in the silicone.302 1. 22. two lateral steel supports surrounded the push-out sample and a polyamide spacer was introduced in the gap existing between the glass plates. the possible rotation of the glass plates around their supported edges. With this disposition. To ensure transferring only pure shear action in the adhesive.185 0. Only the relative displacement sensors provided noteworthy data. was measured at two opposite sides with the help of polyamide sensor-ﬁxing devices attached to one glass plate and of steel bars bonded on the lower edge of the steel plate. 18. Horizontal displacement sensors measuring the “opening” of the assembly. 19(b) and 18. 19(c).252 1. Injector for small bonded areas. accounting for the strain in glass. Standard test no A Ageing B Bonding size (cm²) 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 τ (MPa) 3 90 3 90 3 90 3 90 3 90 3 90 3 90 3 90 1. the lateral expansion of the glass was also measured at opposite sides with two horizontal in-plane displacement sensors. In addition to the press total displacement measurement. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 Table 4 Taguchi design of experiment for double lap-joint shear tests. Fig.270 1. Dias et al.e. Fig.V. see Fig. 17. 12 of Table 4 on Fig. Thus. 16. As pure shear was expected. adaptable to the cartridge.931 1. 18. 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. The load was introduced through the upper steel part. 12. see Figs. see Fig. recorded insigniﬁcant values. eventual rotations of the inner steel plate were observable. see Fig. i. see Fig. Glass contact with steel was prevented laterally by inserting two Neoprene spacers 3 mm thick and horizontally by disposing a Teﬂon plate of 3 mm under the specimen. assimilated to relative displacement between the glass and steel plates. The tests were carried out displacement-controlled on a 630kN INSTRON mobile hydraulic piston (max. where a large dispersion on the stress–strain . The mean curve. A pressure was applied on the whole assembly to remove the surplus.583 0. A self-designed injector.024 1.6kN). Pre-assembly prepared for the injection of the 4 strip.425 0. 16.919 1. With the latter.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. This objective was achieved by positioning two 10 mm horizontal sensors at the top free glass surfaces. 17. was manufactured.220 1. 21 for the test No.729 1. recorded load of 64.591 0.302 1.

With the injection method.01 Hz was regarded. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 Fig. the importance of the manufacturing process and the control of the thickness to enhance the properties of steel–glass connections using structural silicone subjected to shear. A typical cyclic stress–strain diagram and the curve extracted at the 5th cycle. Additional tests should be performed to appraise to which extend these factors affect the shear material strength and to provide representing mathematical functions. 22. versus Time 0. A statistical ANAVAR study was carried out on the calculated shear strengths given in Table 4.1 -0. versus time for test No.2 op (mm) opening 10mm front Breakage Test No.6 0.2 -0.6 Time (s) Fig.8 1 Fig. disp. it emerged that the artiﬁcial ageing and the loading rate had no impact on the silicone properties regarding shear. From this analysis. Double lap-joint shear (a) set-up.2 -0. The test set-up and the data acquisition system of the static tests. For all the tests. a frequency of 0. were re-used for the cyclic tests.1 lat (mm) lateral 10mm right lateral 10mm left Breakage Test No. Glass lat. which were responsible of the large strength variations. for which the silicone was either injected (192 cm2) or poured (544 cm2).4 -0.25 mm of amplitude. 12. on the other hand. 21. composed by six external displacement sensors. 12. 20. 5 10 15 20 0 0.3 Time (s) Fig.2 0. the strength was found slightly higher than for the poured process. the strength decreased with an increasing of the joint thickness. 12 0 0 -0.2 0. on one hand. due to the difﬁcult pouring manufacturing process of the samples. 5 10 15 20 data.4 (-) 0. 19.3 0. The samples were initially subjected to a displacement of 2. 12 1 0.2 Min Average Max 0. This study allows demonstrating. Dias et al. in contrary to the “geometrical” factors.64) and then subjected to a sinusoidal displacement of 2.2 0 0 0 -0. Opening versus Time 0. (b)relative displacement sensors and (c) opening displacement sensors. To account for unfavourable cases. The better results were thus obtained for the small injected bonded area with a narrow joint thickness. The stress softening corresponding to the Mullin's effect was investigated with the help of cyclic tests carried out on “push-out” samples. Stress–strain diagram for silicone double-lap joint samples under quasistatic shear loading. Largest opening disp. where a . Glass lateral disp. the largest dimensions of the bonding area were associated to a thickness of 3 mm.25 mm (strain of about 0.4 0.204 V. the non-dependency of the material to loading rate and ageing and. The dependency between strength and bonding area can be explained with the difference in the realisation of the samples.6 0. can be noticed. Additionally.6 opening 10mm back Shear stress-strain diagram 1. versus time for test No.4 0.8 (MPa) 0.

the evaluation of the volume-part of the strain energy potential.6 which has to be considered in design. the 10kN INSTRON mobile hydraulic cylinder was used displacement-controlled. Silicone elastomers are presented in literature as quasi-incompressible and exhibiting almost no deformation on elevated loads.03 0. 23.1 mm/min and 1 mm/min. was feasible. see Eq. the size of the sample must ﬁt perfectly the size of the rigid frame.V. as described in Section 3. (17). Oedometric tests To determine the properties of silicone under a multiaxial stress state.1 MPa was observed until a strain of 0. are shown in Fig. Therefore. Dias et al. air can be trapped. 24.4 0. To obtain a good reproducibility. the ageing had no impact on the properties of the silicone and only the loading rate was chosen for the oedometric tests as possible inﬂuence criterion. holes had to be drilled to evacuate the air.4. Stress–strain diagram for oedometric tests on silicone.2 0. i. the method used for the realisation of the compressive samples could not be considered in this case. whose dimensions had to be identic and of the same size than the ones of the frame. 24. The last difﬁculty came from the manufacture of the circular samples.5 0. Oedometric test (a) schematisation and (b) test set-up.4. Cyclic stress-strain diagram 1 0.3 0. According to this test.2 10 8 6 4 2 0 0 0. Stress–strain diagram for silicone under cyclic shear loading. Fig. After the ﬁrst cycle a global loss of 0. Identiﬁcation of the material law coefﬁcients The characterisation of the silicone elastomer was analytically derived in the chapters 3.3 and is based on a combined strain energy potential of an isochoric. 25 in which the maximum and minimum encountered stresses were close to the average ones.8 1 1.6 (-) 0. A new method was created to inject the silicone into a Teﬂon mold to produce bubble-free specimens with 30 mm of diameter and 15 mm of height.and a volume-part. 0. With the help of the test results derived from the four experiment types. To conduct the oedometric tests. 23. loading slope Oedometric stress-strain diagram 16 14 12 (MPa) 0.7 (MPa) M-2 -0. otherwise a slight uniaxial compression adulterates the results. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 205 stabilisation of the stress was found. With these experiments. The determination of the coefﬁcients was carried out in two steps. ﬁrst the evaluation of the isochoric-part coefﬁcients.e. The obtained stress–strain diagram was more “linear” than the ones of the other tests and presented a very low dispersion in stress for a given strain. Fig.1 to 3.02 (-) 0. i.6 0. see Fig. During the installation of the specimen into the frame. see Fig. chapters 4.8 0. The loading rate did not inﬂuence the results and high stresses were reached under very low deformations.9 0.01Hz 5th exp. 5.2 0.4 0.3. Consequently. . which led to the selection of two very low loading rates. for which the Jacobian of the deformation tensor F was equivalent to unity. 25.1 0 0 0.e. a circular sample is inserted into a rigid steel frame and is loaded from the top through a piston.04 Min Average Max Fig. it is now possible to determine the material coefﬁcients of this equation. the oedometric test layout was employed. As it was demonstrated previously for the uniaxial compression tests. and then the estimation of the unique volume-part coefﬁcient K.01 0. Force and displacement were respectively recorded by an external force sensor and by the machine. 4.1 to 4.

26.010 0.490 K (MPa) 377.044 0. Finite element analysis of (a) uniaxial tension. 27. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 Table 5 Material parameters for the developed strain energy potential including compressibility. Isochoric strain energy potential W versus the deviatoric invariants for the quasi-static case.009 0. Test type Quasi-static (Instantaneous property) 5th cyclic loading (End of Mullin's effect) A (MPa) 0.021 C (MPa) 0.206 V.221 Fig.221 377.057 B (MPa) À 0.075 D (MPa) 0. .259 0.041 E (-) 0.186 0. Dias et al. (b) uniaxial compression and (c) shear tests – User models. Fig.

multiplied by a positive coefﬁcient. The implicit method of resolution 1. the invariance of the coefﬁcient K towards cyclic actions. the strain-energy function W must always increase with growing deformations. While the displacements at the bottom were restrained.3 0.5 (MPa) 1 6. 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. Uniaxial tension and compression as well as shear tests.1 0. (b) uniaxial compression and (c) shear tests.2 0. The differences observed between both quasi-static and cyclic sets of coefﬁcients arose from the consequent loss in stresses between the ﬁrst and ﬁfth experimental loading curves.4 0. As the compressive tests were performed on cylindrical specimens. given by Eq. Other cyclic oedometric experiments were performed exposing the invariance of the stress–strain data and.5 COMPRESSION-User COMPRESSION-NeoHooke COMPRESSION-Mooney COMPRESSION-Yeoh COMPRESSION-Poly2ndO Experimental Data 0 0 0.3 0.4 (-) 0. compression and shear tests data. Bj. D K W ¼ AðI 1 À 3Þ þ BðI 1 À 3Þ2 þ C ðI 2 À 3Þ À þ þ ðJ À 1Þ2 ðI 2 À 3 þ E Þ E 2 D ð18Þ section of 10 Â 4 mm) and applying corresponding symmetry boundary conditions. This implies that this term is always positive. consequently. while for the cyclic behaviour at the end of the Mullin's effect. To compare the developed law with the existing models exposed in Section 2 and the experimental results. this demonstrates the correctness of the evaluated coefﬁcients for the proposed constitutive model.9 Uniaxial tension was modelled by considering only one fourth of the straight tested length of the dog bone sample (cross Fig. and the cyclic case. where a damping factor is added to control the speed of the convergence.4 0. This method corresponds to the iterative Gauss-Newton least square method. with a non-linear least square method. despite the presence of a negative coefﬁcient for the quasi-static representation.3 (-) 0.4 0. .8 0. Comparison of material model for (a) uniaxial tension.2 0 0 0. 8. the Jacobian of the deformation tensor is raised to the second power. The non-linear least square method of LevenbergMarquardt [32] was inevitable due to the two last terms linking the coefﬁcients D and E. 14 and 23 were regarded.8 (MPa) 0. see Fig. (18) and Table 5. Quadratic hybrid elements C3D20H were employed to solve the problem under Abaqus/ Standard. in this case the strain energy potential.2 1 0. These both methods are based on a linear approximation of the searched function.6 0.2 0. that the function is always positive. an axisymmetric representation was envisaged. only the 5th experimental loading curves exposed on Figs.1 0 0 0. see Fig.4 2.8 1 TENSION-User TENSION-NeoHooke TENSION-Mooney TENSION-Yeoh TENSION-Poly2ndO Experimental Data 1.6 SHEAR-User SHEAR-NeoHooke SHEAR-Mooney SHEAR-Yeoh SHEAR-Poly2ndO Experimental Data (MPa) 0. the material parameters Ai.7 0. Dias et al.5 2 1. they allowed the prediction of the shear. In the volume-part. Veriﬁcation and numerical simulations A ﬁrst veriﬁcation prior to numerical approval of the form and coefﬁcients of the strain energy potential.4 0. were numerically modelled as follows to ensure of the correctness of the written subroutine: 0.5 0. the average curves of Figs. Once the coefﬁcients calculated. The material parameter K. 0.1 0.6 (-) 0.5 0.6 For the quasi-static isochoric set of coefﬁcients. 27. 28. (18).2 0. the loading was introduced on the sample via the upper edge of the model by imposing a displacement.V. consists in ensuring. 13 and 22 were considered. was then calculated with the help of the oedometric experimental average data and of Eq. (18). the related material parameters are listed in Table 5. to be compared to the test data.2 0. Indeed. Therefore. True stresses and true strains were converted to engineering stresses and strains. the average uniaxial stress–strain tension and compression experimental data were regrouped in only one set of data to identify. the coefﬁcient K was determined with a simple linear curve ﬁtting.2 1. D and E associated to a chosen form of the strain energy potential. This procedure was repeated for different polynomial degrees of M and N until ﬁnding a form able to ﬁt as close as possible the tension. As the isochoric coefﬁcients were already known.6 0. which was then compared to the averaged experimental curve. A simple displacement was applied on the upper face of the silicone part. Table 5 gives the material parameter representing the instantaneous and the characteristic behaviour after several cycles of quasi-incompressible silicone elastomer.7 0. accounting for the volume-change. The retained form of the strain energy potential with the respective coefﬁcients to model the quasi-static and the stress– strain behaviour at the end of the Mullin's effect is given in Eq. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 207 Therefore. a UHYPER subroutine in FORTRAN was implemented in the numerical software Abaquss. From the physical point of view.5 0. 26. 9.

contained six material constants and could be used for quasi-static. Guardian Luxembourg and VitrumLux for their support with steel and glass materials as well as Dow Corning and the Kömmerling-Chemie company for structural silicone and their inspiring cooperation. allowing the identiﬁcation of these 6 coefﬁcients. Yeoh and the 2nd order polynomial form for the cases “pure tension”. Therefore. namely “user” law. after the Mullin's effect stress softening. Review of ETAG 002 guideline with focus on glass unit corner loading. only the dimensions of the bonded area. which could be exploited to predict the behaviour of more complex assemblies. compression and shear was executed for the determination of 5 of the coefﬁcients representing the isochoric-part of the foreseen strain energy potential. “pure compression” and “shear”. The strong non-linearity of the material behaviour under small strains ﬁts better with the user model than with the other constitutive laws. only pure shear was investigated and the only difference came from the reduced size of the joint. was compared to the experimental data and results derived with the laws of Neoh Hooke. A displacement was applied on one rigid plate while the other was ﬁxed. The strength of glass. As for the shear push-out tests. based on a combined strain energy potential of an isochoricand a volume-part. Finally. which was estimated less time consuming. [5] Hagl A. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 14 12 10 (MPa) 8 6 4 2 0 0 0. temperature and humidity) and concerning the loading rate was assessed with statistical methods. effect of edge quality. The 6th coefﬁcient was studied with the help of oedometric tests. Glass in building—Structural sealant glazing—Part 1: Glass products for structural sealant glazing systems for supported and unsupported monolithic and multiple glazing. [4] ETAG 002. References [1] Veer FA. Glass Processing Days 2003.04 Oedometric -Experiments FEA -UHYPER -CAX8H Fig.e. ISAAG 2010:45–54. Mooney–Rivlin. Dias et al. 28. Summary and conclusion After a review of the most well-known and employed material laws for hyperelastic material. Zuidema J. a square cross section of 12 mm Â 12 mm and a length of 50 mm. which differ more form the real behaviour. Results of these simulations were compared with the experimental stress–strain curves and a high correlation was established for each test. i. The complete procedure. i. Guideline for European technical approval for structural sealant glazing systems (SSGS). the invariance of the silicone properties concerning ageing (UV-radiation. such as for structural sealant glazing systems or for secondary sealant of insulating glass panes. the long-term behaviour should also be investigated with relaxations tests conducted in uniaxial tension/ compression and shear. Finite element analysis of (a) oedometric tests and (b) results comparison. Injection techniques associated to relatively small thicknesses of the joint of about 3 mm are hence highly recommended to attain higher shear strengths. [3] EN 13022-2:2006.e. whose dimensions were given by the ETAG-002.01 0. EOTA 2001. see Fig. numerical simulations and to reproduce the behaviour of the elastomer after several cycles. Glass in building—Structural sealant glazing—Part 2: Assembly rules. see Fig. a new model was developed and proposed for silicone elastomer to mitigate this difﬁculty. The oedometric tests have also been modelled under Abaquss in an axisymmetric way and subjected to a ﬁnite displacement. Acknowledgements The authors wish to express their deep gratitude to ArcelorMittal. reﬂecting the process of fabrication. Standard stress–strain diagrams were obtained by recording the reaction forces at the ﬁxed rigid plate and the displacement at the opposite plate. Stress–strain diagrams of experimental and numerical analyses were examined and a relatively good concordance was found. The developed constitutive model with the evaluated material coefﬁcients were inserted into the ﬁnite element software Abaquss via a UHYPER subroutine and numerical simulations of the conducted tests were undertaken. C3D8H quadratic and hybrid elements were used to solve with Abaqus/Standard this shear problem. The shear analyses were carried out on parallelepiped samples. the quasi-incompressibility of the material was included too and could be appraised. [2] EN 13022-1:2006. instantaneous.03 0. The numerical investigations proved the validity and the suitability of the proposed constitutive model. of Abaqus was employed in combination to quadratic hybrid CAX8H elements. On two opposite surfaces. This duplicity was achieved by adapting the material coefﬁcients. 29. The developed law. In addition. A complete series of quasi-static and cyclic tests in tension. Further. 7. 29.208 V. analytical rigid plates were tied to the sample and two “reference points” were attached to these rigid plates. and the related tests were detailed in this article. and the joint thickness were found to be of inﬂuence on the strengths of shear tests. The proposed model. . Nevertheless.02 (-) 0. a problem concerning the representation of the strong non-linearity at small strains had been identiﬁed.

Journal of Engineering Mechanics 2006.73:505–23. p. 2004.178:307–16. Journal of Chemical Physics 1952. 1985. [28] ISO 527-2. [23] Kawabata S. On improved 3-D non-Gaussian network models for rubber elasticity. [18] Amin AFMS. Adhesive-bonded Double-Lap Joints. Mechanics Research Communications 1992. Dissertation Texas Tech University.A-28: 903–19. [22] Obata Y. Nonlinear solid mechanics: a continuum approach for engineering. Rubber—General procedures for preparing and conditioning test pieces for physical test method.Computational Mechanics. Advances in Polymer Science 1977. Tobin NR. Holzapfel – England: John Wiley and Sons. Journal of Polymer Science 1970.57:829–38. B.XXIX:2759–73. 209 [20] Ogden RW. Determination of tensile properties of plastics: test conditions for moulding and extruding plastics.74(4):541–59.132(1):54–64.26:357–409. M. Dias et al. dtu. LJ. Informatics and Mathematical Modelling Technical University of Denmark. [8] Panaît A.3.imm. [11] Mullins L. [14] Wang MC. 328.dk/pubdb/views/publication_details. [15] Arruda. vol. 567–83. Kawabata S. Nielsen HB. Pratique des Plans d’Expériences – Méthodologie Taguchi et Compléments. Kawai H. A new constitutive model for rubber-like materials.34(6):484–502. Rubber Chemistry and Technology: March 1957 1957. [32] Madsen K. Theoretical model for the elastic behaviour of ﬁllerreinforced vulcanized rubbers. . Mecánica Computacional 2010. 1973. Glass in building—Insulating glass units—Part 5: Evaluation of conformity. [31] Hart-Smith. IMM Publication (http://www2. 1992. Insulating glass units: the effects of seal stresses and deformations on durability and service life.V. [30] Vigier. [13] Boyce MC. Challenging Glass 2012. Saccomandi R. [10] Holzapfel GA.php?id=3215). Dissertation Massachusetts Institute of Technology. On the development of compressible pseudo-strain energy density function for elastomers – Part 1.19(5):427–33. [26] Sussman T. [21] Flory PJ. http://dx. Computational Mechanics. [29] EN ISO 11431. Glass Performance Days 2007. A ﬁnite element formulation for nonlinear incompressible elastic and inelastic analysis. Madsen – Lecture Note. 2000 ISBN-13:0471823193. / International Journal of Adhesion & Adhesives 48 (2014) 194 –209 [6] EN 1279-5:2005. 2002. Methods for non-linear least squares problems. Bathe KJ. Inﬂuence of various factors on mechanical properties of adhesive joint in glass structures. ISO527-2:1993. Ogden . Rubber Chemistry and Technology: September 2001 2001. EM. Guth E. CEN. Arruda Ellen M. Van der Giessen E. ISO 23529:2004(E). Theory and experiment. Rubber Chemistry and Technology 2000. 2004 . Kawai H. water and artiﬁcial light through glass. November 2004. USA. [27] ISO 23529. Marczak RJ. [9] Bischoff Jeffrey E. [17] Hoss L.30(2):555–71. Constitutive models of rubber elasticity: a review. [16] Wu PD. Paris.24:90–124. Statistical theory of networks of non‐Gaussian ﬂexible chains. [7] Anderson. NASA Technical Report. Strain energy density functions of rubber vulcanizates from biaxial extension.org/10. The structural mechanics behaviour of sealed insulating glass units. 1988. Characterization of the strain hardening response of amorphous polymers. Fitting hyperelastic models to experimental data. Hyperelasticity model for ﬁnite element analysis of natural and high damping rubbers in compression and shear. Series A.20:1144. Grosh Karl. Stress–strain data for vulcanized rubber under various types of deformation. Transactions of the Faraday Society 1944.1007/ s00466-004-0593-y. Journal of Materials Processing Technology 2006. [12] Machalická K. 1575.40:59–70. [24] Treolar LRG. Mechanical properties of natural rubber vulcanizates in ﬁnite deformation. A new constitutive model for the compressibility of elastomers at ﬁnite deformations. Eliášová M. Transactions of the Faraday Society 1961. In: Proceedings of the royal society of London. Thermodynamic relations for high elastic materials. [25] Ghaemi H. Tingleff O. Arruda EM. Sgura I. Jointing products: determination of adhesion/cohesion properties of sealants after exposure to heat. mathematical and physical sciences. Les Editions d’Organisation. Springer-Verlag. Large deformation isotropic elasticity – on the correlation of theory and experiment for incompressible rubber solids.doi. [19] Ogden RW. Computer and Structures 1987.

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