Archimer
Archimer
Archimer
Archimer
http://archimer.ifremer.fr
Abstract :
The modelling of the non-linear behaviour of ductile adhesives requires a large experimental database
in order to represent accurately the strains which are strongly dependent on the tensile-shear loading
combination. Various pressure-dependent constitutive models can be found in the literature, but only a
few experimental results are available, for instance, to represent accurately the initial yield surface
taking into account the two stress invariants, hydrostatic stress, and von Mises equivalent stress. This
paper presents the possibility of combining the use of tests on bulk specimens and tests on bonded
assemblies, which strongly limit the influence of the edge effects, with a pressure vessel especially
designed to study the influence of hydrostatic stress. The latter allows pressures up to 100 MPa to be
applied during mechanical testing. For a given strain rate of the adhesive, experimental results using
various stress paths are presented in order to analyse the influence of the hydrostatic stress on the
mechanical behaviour of an adhesive. The analysis of the results focuses herein on the modelling of
the initial yield surface, but such results are also useful for the development of the flow rules in the
case of 3D pressure-dependent models.
Keywords : Adhesive testing ; Finite element analysis ; Hydrostatic stress ; Modelling ; Non-linear
behaviour ; Yield surface
1. Introduction
Adhesive bonding is nowadays a well established technique in different engineering fields [1-2].
Simple design rules exist for designing simple joints such as single lap joints which just rely on the
adhesive elastic constants [3] or yielding stress [4]. However, for a more precise joint strength
prediction, more information is needed about the adhesive constitutive behaviour. There are several
types of tests available to generate test data for constitutive modelling. The tensile stress-strain curve
on bulk specimens is generally the most common test used. This is sufficient if the yield behaviour of
the adhesive is assumed to be of the von Mises type. However, it is known that adhesive yielding is
better described by more complex yielding criteria [5-7] for which an additional test under a different
loading condition is required. Shear tests are usually preferred because the compressive test is more
difficult to perform. There are many test methods for the determination of failure strength data.
Basically, they can be divided into two main categories: tests on bulk specimens and tests in a joint or
in-situ. Tests in the bulk form are easy to perform and follow the standards for plastic materials. Tests
in-situ more closely represent reality, but there are some difficulties associated with accurately
measuring the very small adhesive displacements of thin adhesive layers. Moreover, the adhesive stress
distribution is not perfectly uniform and the failure mode may not be the same as that found in real
joints. Another important point is that the adhesive strength measured in a joint depends on the surface
preparation. This is not only critical for the short-term strength but even more so for the long-term
strength, especially if aggressive environments are present. There has been intense debate about the
most appropriate method and whether the two methods (bulk and in-situ) can be related. Some argue
that the properties in the bulk form may not be the same as in a joint because the cure in the bulk form
and the cure in a joint (thin film) may not be identical. In effect, the adherends remove the heat
produced by the exothermic reaction associated with cure and prevent overheating. However, many
studies have shown that the relation is reasonable taking into account all the differences associated to
each method [8-10]. Adhesive properties in tension, compression and shear are well correlated
provided a model that takes into account the hydrostatic stress component is used. However, the
prediction of the shear strain to failure does not compare well with the experimental value. The shear
strain to failure is the most difficult parameter to obtain both in terms of accuracy and precision. It is
highly dependent on the type of loading and quality of the specimen. The adhesive has a different
behaviour when loaded in shear and in tension in the presence of defects such as voids. In tension, once
a crack is triggered next to a void, the specimen fails due to the high stress concentration. In shear, even
if a crack is triggered, the remaining area is capable of further deformation, especially if the adhesive is
ductile. For example, in bulk tension, a small void will cause a premature failure whereas in the thick
adherend shear test (TAST) for example, the presence of a void is not as critical. There have been
recent advances in this area where the same type of specimen is used for all loadings giving very good
results up to the failure strain [11-12]. The work presented here is a step further in the determination of
a test that can provide reliable data for the adhesive constitutive modelling, taking into account the
effect of hydrostatic stress. Two types of joints with reduced edge effects were studied: modified TAST
and modified Arcan. These specimens were loaded in a jig that enables to apply mixed tension and
shear loadings. An hydrostatic pressure was also applied through a pressure vessel filled with water in
order to provide additional information regarding this important variable. Bulk specimens were also
tested in tension and compression with hydrostatic pressure to relate bulk and in-situ properties.
2.1. Materials
In the present study, the adhesive is the epoxy resin Huntsman, Basel, Switzerland, Araldite 420
A/B, cured at 50C for 4 hours after 12 h at 20C. Bonded assemblies were studied using aluminium
substrates with a simple surface preparation (abrasion with 120 grade paper and acetone degreasing).
For the bonded assemblies, the adhesive thickness was 0.2 mm. As adhesives often show large viscous
effects, in order to facilitate the comparison between the different experimental results, a constant strain
rate in the adhesive was applied (of about 0.12 minute-1).
assemblies [12] and the details of this vessel have been presented previously [14-15]. Figure 1(a) shows
the CHEM pressure vessel mounted on a standard tensile testing machine. View-glasses can be used to
see inside the pressure vessel up to a pressure of 60 MPa which allow a non-contact measurement
system by image correlation (Fig. 1(a)). It is important to note that measuring displacements in the
CHEM pressure vessel through the view-glass with a digital camera is a difficult task, and requires
great care with calibration and lighting. Above this pressure of 60 MPa, metallic closures have to be
used instead of the view-glasses (Fig. 1(b)). After positioning the specimen in the tensile testing
machine, the vessel is closed. During the closure of the vessel (descent of the upper part, Fig. 1(b)),
some small movements of the upper part of the vessel can occur. Therefore, special fixing systems
compatible with those movements were used in order to limit the preloading of the specimens. The
screw-nut system presented in Fig. 1(b) was used to complete the vessel closure. The vessel was then
filled with tap water and the required pressure was applied using a special pump. While the pressure
increased, a specific two-chamber equilibrium system ensured no other preloading of the specimen.
Thus, during this phase, the only loading of the specimen was due to the hydrostatic pressure. Then, a
mechanical test, imposed by the tensile testing machine, can be performed at a given pressure in the
vessel. The result is the superposition of two loadings: a hydrostatic pressure and a mechanical loading.
All the tests presented below were performed by controlling the displacement of the crosshead of the
tensile testing machine in order to have a strain rate of about 0.12 minute-1.
A pressure of 0.5 MPa (noted as 0 in the following) corresponds to a very low hydrostatic pressure
loading of a specimen simply immersed in water. Tests were performed for hydrostatic pressures of: 0,
30, 60 and 90 MPa.
metallic
closure
pressure
vessel
view-glass
screw
motion
during the
closure of
the vessel
digital
camera
experimental
device
Screw-nut
(a)
(b)
FIGURE 1 CHEM system description. (a) CHEM system with the use of a digital camera and (b)
closing system (screw-nut) of the pressure vessel and positioning of the experimental device inside the
pressure vessel.
without porosity was used [10]. The specimens for tensile tests were machined from the plates to a dogbone geometry with a useful rectangular section of 10 mm x 4 mm and a useful length of 40 mm. The
system designed for the modified thick adherend shear test (TAST) was used to load the specimen [16].
The bulk specimen was fixed on two supports using clamping systems with bolts. In order to prevent
parasitic loadings, connections allowing rotations were used (Fig. 2(a)): a universal joint ensures the
radial positioning of the support in the vessel and the axial load is transmitted by a pin in order to
control the geometrical constraints. For these tests, the crosshead displacement rate of the tensile
testing machine was 5 mm/minute.
For compression tests, cylindrical specimens were used (diameter of 12.75 mm and length of 25.4
mm). Specimens were machined from plate specimens. A specific device was used in order to ensure a
precise compression loading (Fig. 2(b)). For these tests, a displacement rate of the crosshead of the
tensile testing machine of 3 mm/minute was used.
Each test on a bulk specimen requires nearly an hour, taking into account the preparation phases, the
closure of the vessel, increasing the pressure, the mechanical test and the opening of the vessel.
support
fixing
system
of the
specimen
Fixing
support
joint
tensile
bulk
pin with
universal
joint
compression
bulk specimen
(a)
(b)
FIGURE 2 Bulk tests in the pressure vessel. (a) Device and specimen used for tensile loading and (b)
device and specimen used for compression loading.
used to connect the modified TAST fixture to the tensile testing machine in order to prevent parasitic
loads during the different phases of the test. The main parameters which define the geometry of the
bonded specimen are: 2e = 0.2 mm, h = 0.2 mm, d = 0.5 mm, = 1.5 e, = 60 (Fig. 3c). For these
tests, the displacement rate of the crosshead of the tensile testing machine was 0.024 mm/minute.
Each test on a bonded assembly requires nearly two hours, taking into account the preparation phases,
closure of the vessel, increasing of the pressure, and the mechanical loading at a slow crosshead
displacement rate of the tensile testing machine, followed by opening of the vessel.
(3)
(2)
(1)
pin with
universal
joint
(4)
(b)
Fixing
support
(1)
(a)
(c)
FIGURE 3 Modified TAST in the pressure vessel. (a) Mounting of the device, (b) fixing of the bonded
specimen and (c) geometry of the small bonded specimen with beaks all around the substrates.
In order to choose the geometry of the bonded specimens, 3D models were used to analyze the
influence of the hydrostatic pressure on the stress distribution in the adhesive. To limit the size of the
numerical model, the calculation was made on a quarter of the TAST specimen, using adequate
boundary conditions (Fig. 4a). Figures 4a-b present geometries of two bonded specimens for the
modified TAST device. The first one has a rectangular shape and the adhesive free edges are straight
(Fig. 4a). The second one has a round shape, with beaks all around the substrates and the adhesive free
edges (borders of the joint) are cleaned by wiping off excess adhesive (Fig. 4b). In fact, as the
computations were performed under elastic assumptions for the different parts, the influence of the
hydrostatic pressure on the stress distribution in the adhesive can be seen as the superposition of two
loadings. The first is associated with pressure on the substrate surfaces whose normal direction is
parallel to the normal of the joint mean plane (coordinate z, Fig. 4a). Such loading leads to a
compression of the joint between the two substrates. Therefore the numerical results obtained for the
modified Arcan system under tensile loading can be used; they underline that beaks all around the
substrates are necessary to limit the influence of edge effects [19]. The second loading component is
associated with pressure on the other surfaces of the bonded joint (surfaces presented in grey in Fig.
4a). For such loadings, numerical simulations have been performed using aluminium substrates (Young
modulus: Ea = 75 GPa, Poisson's ratio: a = 0.3) and the elastic material parameters for the studied
5
adhesive were such that: Ej = 2.0 GPa, j = 0.42 (results obtained from tensile and compression bulk
tests). Results are only presented for a small part of the adhesive (close to a so-called corner: circle on
Fig. 4a-b). Figure 4c presents the distribution of the von Mises equivalent stress in the adhesive for a
pressure of 1 MPa for a joint thickness of 0.2 mm. It can be noted that only a small part of the adhesive
close to the joint free edges is loaded, and such a geometry leads to quite large stress concentrations
close to the substrate-adhesive interface. Figures 4d-f present the distribution of the von Mises
equivalent stress in the adhesive for geometry b for a pressure of 1 MPa and for joint thicknesses of
0.2, 0.4 and 0.8 mm. Under each drawing, the minimal and maximal values of the von Mises equivalent
stress is written. This indicates that in order to limit the stress concentrations, it is necessary to use thin
joints. Experimental tests were performed using an adhesive thickness of 0.2 mm in order to facilitate
the measurement of the adhesive deformation in the pressure vessel through the view-glass. Moreover,
the use of thin beaks and joint edges from which spew fillets are removed give good results for the
loading associated with the hydrostatic pressure and for the mechanical loading.
substrate
analysed
zone
adhesive
hydrostatic
pressure
analysed
zone
antisymmetry
symmetry
(a)
(b)
y
substrate
Adhesive
u
x
(b)
support
fixing
system
Loading
pin
adhesive
x
substrate
Loading
pin
test with = 90
test with = 0
test with = 45
(a)
(c)
FIGURE 5 Modified Arcan device in the pressure vessel. (a) Test under tensile-shear loading = 45,
(b) presentation of the bonded specimen & close-up view of the beak and (c) test under tensile loading
= 0 and test under shear loading = 90.
following a simplified approach is used in order to determine different points of the initial yield
function.
60 MPa
30 MPa
F (kN)
1.6
0 MPa
1.2
0.8
0.4
0.0
0
10
hydrostatic stress on the mechanical behaviour of the adhesive (initial elastic limit for a given strain
rate).
0
-2 0
50
100
150
200
-25
250
-20
-15
-10
-1 0
-3
-6
-8
0 MPa
30 MPa
-10
-12
F (kN)
F (kN)
-4
-5
-5
30 MPa
0 MPa
-7
60 MPa
-14
-9
60 MPa
-16
90 MPa
-18
-11
Time (s)
Axial strain (%)
(a)
(b)
FIGURE 7. Experimental results for compression tests on bulk specimens for a crosshead displacement
rate V = 3 mm/min. (a) Load-time diagram for pressures p = 0, 30, 60 and 90 MPa and (b) load-strain
diagram for pressures p = 0, 30 and 60 MPa.
80
: Bulk-tensile
: Bulk-compression
60
hydrostatic
pressure
compression
-120
-100
p =90 MPa
-80
20
tensile
-60
p =60 MPa
-40
40
p =30 MPa
p =0 MPa
0}
-20
20
40
3.2. Experimental results for shear tests with the modified TAST
For the modified TAST, the term DT denotes the relative displacements of both ends of the adhesive in
the tangential direction. FT represents the applied load in the tangential direction in the mean plane of
the adhesive.
Figure 9 presents results for three hydrostatic stress loads (0, 30 and 60 MPa) in the load-displacement
(FT-DT) diagram and indicates the influence of the hydrostatic stress on the behaviour of the adhesive
in a bonded assembly under shear loadings. For a given hydrostatic pressure, two specimens were used.
These tests are associated with quite low variability; other results can be found in [13].
9
10
60 MPa
FT (kN)
30 MPa
6
0 MPa
4
2
0
0
0.1
0.2
0.3
DT (mm)
FIGURE 9 Load-displacement curves for shear tests using the modified TAST for a crosshead
displacement rate V = 0.024 mm/min and for pressures p = 0, 30 and 60 MPa.
substrate
Compression
loading
adhesive
shear
loading
antisymmetry
symmetry
(a)
(b)
stress
(MPa)
(c)
(d)
FIGURE 10 Stress distribution in the mean plane of the TAST joint for compression and shear loadings. (a)
Quarter of the bonded specimen with a round shape, beaks all around the substrates and the adhesive
free edges cleaned, (b) shear stress in the mean plane of the adhesive for an average shear stress of 1
MPa, (c) tensile stress in the z direction in the mean plane of the adhesive for an average tensile stress
of 1 MPa associated with compression in the z direction, and (d) tensile stress in the y direction in the
mean plane of the adhesive for an average tensile stress of 1 MPa associated with compression in the z
direction.
An analysis of the stress distribution in the adhesive, for this shear test in the pressure vessel, requires
two main mechanical loadings to be taken into account. A compression of the bonded joint associated
with the hydrostatic pressure, and a shear loading associated with the mechanical loading. Figure 10a
presents the geometry of the modified TAST bonded specimen with a round shape, beaks all around the
10
substrates and the adhesive free edges cleaned. For the two computations under elastic assumptions, a
quarter of the specimen can be used using adequate boundary conditions (Fig. 10a). Figure 10b shows
the shear stress on half of the mean plane of the adhesive for an average shear stress equal to 1 MPa.
The shear stress is represented on the z-axis and the maximal value of the shear stress is equal to 1.16.
For the compression loading in the z direction, Figure 10c-d present respectively the tensile stress in the
z and y directions for an average tensile stress in the z direction equal to 1. The ratio of the maximal and
the average zz component of the tensile stress is equal to 1.30. In the middle of the joint the ratio of the
xx or yy component and the zz component stress is equal to 0.70. In the following, a simplified analysis
of such tests is proposed using the stress state in the middle of the adhesive.
It can be noted that such geometries of the bonded specimens limit the stress state close to the free
edges of the adhesive, even using hydrostatic pressure. The normal components of the stress are very
low all around the free edge of the joint; but the shear stress is only very low on two of the free edges of
the bonded joint.
Figure 11 presents the elastic part of the results in the von Mises equivalent stress-hydrostatic stress
diagram. The dashed lines represent, under elastic behaviour, the loading path in the pressure vessel.
For such tests, starting with an unstressed specimen, increasing the hydrostatic pressure leads to
compression of the bonded specimen which can be described using the previous numerical results.
Such a loading is presented in Figure 10 with a grey arrow for a hydrostatic pressure of 60 MPa. For a
given hydrostatic pressure, the mechanical shear loading is associated with an increase of the von
Mises equivalent stress (shown using a black arrow for a pressure of 60 MPa). The different points of
the elastic limit are presented in Figure 10 using the following marks c.
80
c: TAST-shear
60
40
shear loading
p =90 MPa
hydrostatic
pressure
20
p =60 MPa
p =30 MPa
-120
-100
-80
-60
-40
-20
0}
0
p =0 MPa
20
40
3.3. Experimental results for tensile-shear tests with the modified Arcan device
For each given hydrostatic pressure, and for each configuration of the Arcan device studied ( = 0, 45,
90 and 135) only one specimen was used, as each test requires nearly 2 hours. The scatter in the
results are very low for the modified Arcan tests as for this test the influence of edge effects is strongly
limited using beaks and cleaning of the adhesive free edges [11, 17]. For the Arcan tests, the terms DN
and DT denote the relative displacements of both ends of the adhesive in the normal (direction y,
11
Figure 5) and tangential direction (direction x, Figure 5). FN and FT represent the normal and
tangential components of the applied load in the normal and tangential directions.
50
60 MPa
40
FN (kN)
30 MPa
30
0 MPa
20
10
0
0
0.025
0.05
0.075
0.1
DN (mm)
FIGURE 12 Experimental results for tensile tests with the modified Arcan device ( = 0) for pressures
p = 0, 30 and 60 MPa for a crosshead displacement rate V = 0.024 mm/min.
20
20
16
16
60 MPa
12
30 MPa
FT (kN)
FT (kN)
60 MPa
30 MPa
0 MPa
8
4
12
0 MPa
8
4
0
0
0.1
0.2
0.3
0.1
0.2
0.3
DT (mm)
DT (mm)
(a)
(b)
FIGURE 13 Experimental results for tests with the modified Arcan device for pressures p = 0, 30, 60
and 90 MPa for a crosshead displacement rate V = 0.024 mm/min. (a) Results for tensile-shear ( =
45), and (b) results for shear loadings ( = 90).
Experimental results using the modified Arcan fixture are presented for three hydrostatic stress levels
(0, 30 and 60 MPa) in Figures 12-14. Figure 12 presents results of tensile tests ( = 0) in the loaddisplacement (FN-DN) diagram (results in the normal direction). Figure 13 shows results from tensileshear ( = 45) and shear tests ( = 90) on the load-displacement (FT-DT) diagram (results in the
tangential direction). Results under tensile shear loadings ( = 135) are presented in Figure 14 on a
load-time diagram; for these tests the load F measured by the tensile testing machine is presented
(combination of FN and FT).
Figure 15 presents the elastic part of the results in the von Mises equivalent stress-hydrostatic stress
diagram. The elastic limits obtained for the tensile and shear loadings are presented using respectively
the following marks z and z. For the two tests the initial loading with the hydrostatic pressure is
represented as a compression of the bonded assembly as for the modified TAST. For shear tests the
stress path is similar to the one obtained with the modified TAST specimen. However, for tensile tests,
the loading of the tensile testing machine leads first to a reduction in the compression of the bonded
12
assembly, and secondly to a tensile loading of the specimen. The arrows indicate the loading path of
the bonded joint for a pressure of 30 MPa.
25
60 MPa
30 MPa
20
0 MPa
F (kN)
15
10
5
0
0
10
20
30
40
50
Time (s)
FIGURE 14 Experimental results for tests with the modified Arcan device for pressures p = 0, 30 and
60 MPa for a crosshead displacement rate V = 0.024 mm/min - compression-shear tests ( = 135).
=90
=90
=90
z: Arcan-shear
z: Arcan-tensile
40
p =60 MPa
p =30 MPa
-80
-60
tensile loading
(=0)
hydrostatic
pressure
20
p =90 MPa
-100
=90
60
shear loading
(=90)
-120
80
-40
-20
0, 30, 60 MPa
p =0 MPa
0}
0
=0
20
40
13
=135
=135
=135
80
=45
=45
: Arcan-tensile-shear
: Arcan-comp.-shear
=45
60
=45
40
=135
p =90 MPa
20
p =60 MPa
p =30 MPa
-120
-100
-80
-60
-40
-20
0}
0
p =0 MPa
20
40
(1)
where vm is the von Mises equivalent stress and ph is the hydrostatic stress, a, b and pt0 are material
parameters. The results of an identification, taking into account the little over-estimation of the
transmitted load especially for large hydrostatic pressures, are presented in Table 1 and the initial yield
surface is drawn in Figure 17.
14
: Bulk-tensile
: Bulk-compression
c: TAST-shear
z: Arcan-shear
z: Arcan-tensile
: Arcan-tensile-shear : Arcan-comp.-shear
80
60
40
20
0
-120
-100
-80
-60
-40
-20
20
40
pt0 (MPa)
1. E-6
5.05
31.7
4. Conclusion
A pressure vessel combined with a testing tensile machine (the CHEM system) has been used to analyse
the influence of hydrostatic stress on the mechanical behaviour of an adhesive. Various tests have been
used on both bulk adhesive specimens and bonded assemblies (which strongly limit the influence of the
edge effects). This vessel allows pressures up to 100 MPa to be applied during mechanical loading.
Thus, the pressure vessel allows various loading paths to be examined using only one mechanical test,
under hydrostatic pressure up to 100 MPa. For the initial elastic limit and a given strain rate, results
obtained with bulk specimens (under tensile or compression loadings) are quite similar to those
obtained with bonded specimens using the modified TAST and the modified Arcan device. The results,
associated with different loading paths of the adhesive underline a strong influence of the hydrostatic
stress on the mechanical behaviour of the adhesive. Moreover, experimental results using bonded
specimens allow to analyse the non-linear response of an adhesive using various loading paths, and in
particular for large negative hydrostatic stresses. These results constitute a large experimental database,
which is essential in order to define accurate models for the mechanical behaviour of an adhesive in an
assembly using pressure dependent constitutive laws.
In order to increase the precision of experimental results, a loading sensor placed in the pressure vessel
has been developed and is now being evaluated. As the stress state in an adhesive joint is quite complex,
inverse identification techniques using 3D finite element models are necessary to accurately analyse the
experimental results. Moreover, an optimisation of the geometry of the bonded joint can be done to
improve the tests in the pressure vessel: the aim is to limit the stress concentrations close to the free
edges of the joint taking into account the hydrostatic pressure and the mechanical loading.
15
Acknowledgements
The authors wish to acknowledge METRI-2 European project for financial support. The authors are
grateful to Bernard Leilde, Albert Deuff, Christophe Peyronnet and Andr Kerboul from IFREMER for
their collaboration in the experimental tests with the CHEM system. The authors also thank particularly
Herv Trbaol, Pierre Martinat and Bruno Mecucci from ENSIETA/DTN/CMA for their collaboration
in designing and manufacturing the fixing system for bulk tensile tests and the modified Arcan fixture
which have been specially designed to be used in the CHEM pressure vessel.
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16