Journal of Solid Mechanics

and Materials

Engineering

Vol. 5, No. 12, 2011
921
Influences of Loading Rates on Stress-
Strain Relations of Cured Bulks of Brittle and
Ductile Adhesives*
Toru SUGAYA**, Tatsuya OBUCHI** and Chiaki SATO***
**Graduate School, Tokyo Institute of Technology,
4259 Nagatsuta, Midori-ku, Yokohama, Kanagawa 226-8503, Japan
***Precision and Intelligence Laboratory, Tokyo Institute of Technology,
4259 Nagatsuta, Midori-ku, Yokohama, Kanagawa 226-8503, Japan
E-mail: csato@pi.titech.ac.jp


Abstract
Influences of loading rates on the stress-strain relations of cured adhesive were
experimentally investigated. A brittle epoxy adhesive and a ductile epoxy adhesive
modified with rubber particles were examined. Concave specimens of the cured
adhesives were made, and strain gages for very large strain were bonded on the
specimens. The specimens were tested in static conditions with a material testing
machine and in dynamic condition with a drop-weight impact testing machine. The
influences of loading rates on the stress-strain relations of the adhesives were
identified. For the brittle adhesive, the modulus was constant in both the static and
dynamic conditions, and the tensile strength and total strain increased with the
increase of loading rates. For the ductile adhesive, large plastic deformation
occurred in the static condition, and the tensile strength was 37 MPa and the total
strain was 14%. In contrast, in the condition of high loading rate, the ductile
adhesive became brittle, and the ultimate stress increased and the maximum strain
decreased.
Key words: Adhesive, Impact Strength, Stress-Strain Relation, Strain Gage, Plastic
Deformation

1. Introduction
Adhesive bonding has been widely used in many fields such as automotive and aircraft
structures nowadays because it is lighter, more cost effective, and has lower stress
concentration than other joining methods such as mechanical fasteners. For automotive
structures, impact resistance of adhesively bonded joints is required from a standpoint of
crash safety. Thus, many researches have been conducted on the topic, especially for the
impact strength of joints bonded adhesively
(1)-(14)
. In these works, specimens of bonded joints
were prepared, tested both in static and dynamic conditions, and the strengths were compared
each other. Stress analyses and strength predictions have been also carried out
(15)-(28)
.
However, the most basic and important information for the analyses, i.e. mechanical
properties of adhesives in dynamic conditions are rarely investigated so far, although they,
especially the stress-strain relations, are indispensable for the stress analyses. Goglio and
Peroni have investigated the stress-strain relations of a ductile epoxy adhesive using the
split Hopkinson bar method, and carried out tensile impact tests of the cured adhesive to
obtain the stress-strain relations
(29)
. However, the method has a weak point in tensile tests
because it is originally invented for compression tests. For tensile impact tests, there are
*Received 4 July, 2011 (No. 11-0376)
[DOI: 10.1299/jmmp.5.921]
Copyright 2011 by JSME



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difficulties such as fixing of specimens, etc.
This paper presents a method to obtain the stress-strain relations of cured adhesives
subjected to an impact load. A type of specimen called concave specimen is used. The
concave specimens of a brittle epoxy adhesive and a ductile epoxy adhesive were prepared
and tested in static and impact conditions to obtain the stress-strain relations in a range of
loading rates : 4.010
-4
- 7.010
1
s
-1
.
2. Specimens
2.1 Specimen configurations
Dog born specimens such as JIS Type 2 specimen (JIS K 7113:1995, repealed in 2010)
were widely used for the tensile tests of plastic materials. Since the specimens have a
parallel part in the middle, the strain of the specimens can be calculated from the
displacement of the crosshead of a testing machine if the parallel part deforms uniformly.
However, unstable local deformation called necking may occur for bulks of ductile
adhesives, and the strains are not calculated precisely from the crosshead displacements.
Use of strain gages is an alternative method, but the strain cannot be measured when the
gage was not adhered on the position of necking, as shown in Fig. 1. Therefore,
conventional dog born configuration is not suitable for the measurement of ductile
adhesives. Takahashi and Sato have presented a novel configuration for this problem
(30)
.
The specimen configuration is shown in Fig. 2.

Fig. 1 JIS Type 2 specimen after test (Thickness is 2 mm.)
(30)

Unit: mm
Fig. 2 Configuration of concave specimen
(30)

2.2 Finite element analysis
Stress analysis of concave specimens was carried out to check the stress concentration
using a program (ABAQUS, ver.6.3-1) for the finite element method. Two dimensional
static analysis of the specimen was conducted assuming that the material property was
linear elastic. The modulus used in the analysis was determined by the following
experiment of brittle adhesive A in static condition. The Poissons ratio was assumed as 0.4,
which is a typical value for ordinary plastics. Figure 3 shows the distribution of longitudinal
normal stress in the specimen subjected to a longitudinal tensile load, where the stress is
indicated by normalized value divided by the average stress along the center line. Figure 4
shows the distribution of normal stress concentration factor in the width direction at the
center of the specimen along the right-hand end of Fig.3. Although stress concentrates at the
both sides of the specimen, the maximum concentration factor is only 1.04 that is
negligible. Thus the configuration can be applied to both brittle and ductile adhesives.



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Fig. 3 Normalized stress distribution in concave specimen

Fig. 4 Normalized stress distribution at necked part of concave specimen
2.3 Specimen preparation
A brittle one-part epoxy adhesive (adhesive A) and a ductile one-part epoxy adhesive
(adhesive B) were used for the experiments. Adhesive B includes 7wt% of
carboxyl-terminated liquid butadiene acrylonitrile rubber (CTBN) particles for ductility
enhancement. These adhesives were injected to a mold (Fig. 5), as shown in Fig. 6, and
cured. The cur i ng condi t i on of adhesi ve A was 120 C f or 60 min and that of
adhesive B was 170C for 20 min.

Fig. 5 Mold for concave specimens

Fig. 6 Molding method for concave specimens



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3. Experimental
3.1 Static tests
Static tests of the specimens were carried out using a material testing machine with a
tensile displacement rate of 5 mm/min. The strains of some specimens were measured using
plastic gages for large deformation (KFEM-5-120-C1L1M2R, Kyowa Electronic
Instruments Co., Ltd.,) by which strains up to 30% can be measured. The gage length was 5
mm. The gages were adhered on the specimens using a cyanoacrylate adhesive for large
strains.

3.2 Impact tests
Figure 7 shows the drop-weight impact testing machine used for impact tests of the
specimens. The machine comprises a drop weight, an elevator unit, a release unit, and a
load-cell. By the drop weight with two hammers of the same length that hit an anvil bonded
to the specimen at the bottom, an impact load is applied to the specimen, as shown in Fig.7.
The top part of the specimen was also bonded to a metal fitting connected to the load-cell
using a cyanoacrylate adhesive. The connected areas of specimens to the anvil and the metal
fitting were not broken after the impact test. The impact loads applied to the specimens
were measured with the piezoelectric load-cell (9021A, Kistler Japan Co., Ltd.). The
capacity of the load-cell was 35 kN, and the natural frequency was 2.3 kHz. The
displacement of the drop weight was measured by a laser displacement sensor (LB300,
Keyence Co., Ltd., the measurable displacement range is 200-400 mm.). The velocities of
the drop weight and the elongation of the specimens were calculated from the displacement
measured with the sensor. The weight of the drop weight including the hammer was 25 kg.
When the impact velocity to the specimens was 4 m/s, the kinetic energy of the drop weight
was 200 J, by which the specimens can be broken. For the specimen of adhesive A
subjected to an impact load, a plastic gage (FLA-2-11-5L, Tokyo Sokki Kenkyujo Co., Ltd.,
the gage length is 2 mm.) was used because the maximum strain of the other specimen in
the static test was small enough to be measured by the gage. For the specimen of adhesive B
in the impact test, the plastic gages for large deformation (KFEM-5-120-C1L1M2R) were
used.


Fig. 7 Photos of drop-weight impact testing machine and close-up of specimen and loading part
4. Results and discussion
4.1 Brittle adhesive
Stress-strain curves of adhesive A measured by the static and impact tests are shown in
Fig. 8. The curves are very close and the Youngs moduli are almost the same even in the
static and impact conditions. The maximum stress and strain of the impact test were larger
than those of the static test. Figure 9 shows the specimens after the tests. The specimens



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were simply fractured in a brittle manor without any color change.
The adhesive has the glass transition temperature (Tg) which is much higher than room
temperature, thus is in a glass state in ambient condition. Viscoelastic phenomena of plastics
are not significant in glass states. Therefore, the adhesive does not have the rate dependency
in the modulus caused by the viscoelastic dissipation. According to the time-temperature
superposition principle for polymeric materials, higher loading rates are equivalent to lower
testing temperature because the motion of molecular chains is limited within short time and
is suppressed at a low temperature. The modulus of the adhesive is almost constant and not
changed in a temperature range lower than the Tg. Therefore, even if the loading rate
increases at room temperature, this condition is equivalent to temperature decreasing that
cannot affect the modulus of the adhesive.
Otherwise, the elongation increase in the impact condition, which is equivalent to the
increases of stress and strain, can be explained by the Kalthoff-and-Shockey's theory
(31)
.
Kalthoff and Shockey have presented their hypothesis that there is a particular minimum
duration necessary for the fracture of a material. In some impact conditions, stress can
increase rapidly within the duration.

Fig. 8 Stress-strain curves of specimens

(a) Static (b) Dynamic
Fig. 9 Specimens of brittle adhesive A after tests

(a) Static (b) Dynamic
Fig. 10 Specimens of ductile adhesive B after tests



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4.2 Ductile adhesive
The stress-strain curves of adhesive B are shown in Fig. 8. The ductile adhesive had
great plastic deformation in static conditions, and the maximum strain is 14% when the
stress is 37 MPa. The specimen of the adhesive after the static test is shown in Fig. 10 (a), in
which an area of whitening can be seen around the fractured sections at the center of the
specimen. This is due to crazing by shear band creation occurring often in rubber modified
plastics. The shear bands created in the matrix resin of an adhesive enable it to deform
largely and easily.
In contrast, the adhesive became brittle under impact loading of 4 m/s, where the
average strain rate is 70 s
-1
. The maximum strain became smaller and the maximum stress
became greater than those of the static test. No color change can be seen on the specimen
after the impact tests, as shown in Fig. 10 (b). This implies that shear band generation in the
matrix resin was suppressed probably by the viscoelastic characteristics of resin. Since the
ductility of rubber modified plastics is derived from the generation of shear bands, the
plastic deformation of the materials tends to decrease under high strain rate conditions. In
this case, the modulus and the maximum stress, however, increase. The increase of modulus
and maximum stress can be explained by brittle transition due to the time-temperature
superposition principle. Namely, according to the principle, an increase of strain rate has the
equivalent decrease of temperature, by which polymeric materials become more brittle and
stronger than those under lower strain rates.

5. Conclusion
Static and impact tensile tests of cured adhesives were carried out, using a brittle epoxy
adhesive and a ductile epoxy adhesive. For the tests, a novel specimen configuration:
concave specimen was utilized to localize the unstable deformation and fracture at the
center of the specimen, at which a plastic strain gage for large deformation was adhered.
The experimental results of the tests showed interesting phenomena concerning the rate
dependencies of the stress-stain relations as follows:

(1) For the brittle adhesive, the modulus is constant and not dependent to loading rate
although the maximum stress and strain increase with respect to loading rate.

(2) For the ductile adhesive, large plastic deformation occurs by static loading, where the
maximum strain is very large although the maximum stress is not high. In contrast, the
adhesive becomes brittle in impact conditions, i.e. the maximum stress increases and the
elongation decreases.

(3) These rate dependencies can be explained by the combination of the time temperature
superposition principle and the Kalthoff-and-Shockey's theory.

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