Polymer Testing 109 (2022) 107528

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Polymer Testing
journal homepage: www.elsevier.com/locate/polytest

Effects of loading rate, temperature, and thickness on the tensile strength of

precision adhesive joints
Lei Guo a, Jianhua Liu a, d, Huanxiong Xia a, d, *, Xiayu Li c, Xiumin Zhang a, Hongfan Yang a,
Ye Yang b
a
School of Mechanical Engineering, Beijing Institute of Technology, Beijing, 100081, China
b
School of Mechanical and Material Engineering, North China University of Technology, Beijing, 100144, China
c
Beijing Spacecraft, Beijing, 100094, China
d
Yangtze Delta Region Academy of Beijing Institute of Technology, Jiaxing, 314000, China

A R T I C L E I N F O A B S T R A C T

Keywords: The influences of the micron bondline thickness, temperature, and loading rate on the tensile strength of ad­
Precision bonding hesive joints were studied for the precision adhesive structures, and the fractured surfaces were analyzed by the
Bondline thickness infrared imaging and SEM methods. The testing results show that the tensile strength increases and then linearly
Temperature
decreases with the increase of bondline thickness; the peak tensile strength is always acquired at the bondline
Loading rate
thickness of around 30 μm; the maximum tensile strength increases up to 28.6% as the thickness increases from
10 to 30 μm at the loading rate of 1 mm/min; the strength decreases by more than 33% and finally reaches a
closed value at different bondline thicknesses as the temperature rises from − 30 to 110 ◦ C. The results indicate
that reducing the bondline thickness, less than about 10 μm, could result in a weak bonding interface; the tensile
strength increases with the increase of the loading rate, exhibiting the strain-rate hardening effect below the Tg;
the plastic-damage characteristic appears and becomes clearer on the fractured surface as the temperature in­
creases. Under the tested conditions, the temperature shows the most significant effect on the tensile strength,
then the bondline thickness followed by the loading rate.

1. Introduction thickness could cause more uniform stress and strain distributions along
the bondline of single-lap-joints (SLJs) [8]. Some studies showed that
Epoxy resins are widely used in automotive and aerospace industry increasing the bondline thickness resulted in a higher peel strength for
products, especially in precision optical, mechanical and electrical in­ peel joints, while it harmed the fracture toughness of the DCBs [9–13].
struments, owing to their low volatility and low shrinkage upon curing However, the effect of bondline thickness on the bonding strength is still
[1–4]. For some of these precision instruments that often serve in severe an open issue. It has been reported that the dependences of the shear
environments, such as high temperature or high-frequency vibration, strength on the bondline thickness are much different for the ductile and
the mechanical properties of the bonded structures greatly affect the brittle adhesives [14–17]. The shear strength of SLJs decreases as the
stability of product performance [5]. Additionally, to maintain good bondline gets thicker, and this change is more pronounced for brittle
dimensional accuracy and stability of adhesive assemblies, the bondline adhesive joints. Gleich et al. [18] using a linear finite-element analysis
thickness in precision instruments is usually extremely thin, which can method showed that the peak shear and peel stresses increase with the
reach several microns [6]. bondline thickness increasing, but the averaged adhesive stresses
Due to the inherent characteristics of polymer materials, the per­ decrease. Kahraman et al. [19] investigated the influence of adhesive
formance characteristics of epoxy resins are not only related to the thickness on the bonding strength of an aluminum-powder filled epoxy
bonded size, but also sensitive to the environment, such as loading rate by both FEM analysis and experimental method, the results showed that
and temperature [7]. The bondline thickness is a critical parameter that the strength decreases as the thickness increases. Xu et al. [20] examined
affects the mechanical properties of adhesive joints, such as strength and the impact of the adhesive thickness on the cohesive properties and the
toughness. The published work claimed that increasing the adhesive overall strength using the cohesive zone model. They found that the

* Corresponding author. School of Mechanical Engineering, Beijing Institute of Technology, Beijing, 100081, China.
E-mail address: [email protected] (H. Xia).

https://doi.org/10.1016/j.polymertesting.2022.107528
Received 13 August 2021; Received in revised form 6 January 2022; Accepted 28 February 2022
Available online 1 March 2022
0142-9418/© 2022 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
L. Guo et al. Polymer Testing 109 (2022) 107528

Fig. 1. The preparation tooling and SLJ specimens.

variation of overall strength is much dependent on the adhesive thick­

ness due to the toughness and strain hardening capacity of the adhesive.
Hence, it is generally known that a thin bondline of brittle epoxy resin
could result in high static strength of joints. In many industrial appli­
cations, such as aerospace products, around 0.1–0.2 mm is a typically
used bondline thickness, considering the adhesive stiffness, joint ge­
ometry, and applied loading [18]. However, in precision devices, such as
electromechanical and optical instruments, the bondline thicknesses are
usually much thinner than 0.1 mm and even several microns. Many
engineering practices have shown that the adhesive layers have a sig­
nificant effect on the performance of such precision devices, while few
related studies have been reported.
Precision devices used in the aerospace or optical fields often suffer Fig. 2. Tensile testing device.
from environments with violent vibration and impulse and a wide range
of temperatures. For such devices, the adhesive structures are expected 2. Materials and methods
of sufficient strength or toughness to ensure the stability of the assem­
bled structures [21]. da Silva and Adams [22,23] designed a mixed joint 2.1. Materials
suitable for low and high temperatures by the combination of two ad­
hesives, which gives a better performance of load capacity over the The applied epoxy resin adhesive is developed for precision in­
considered temperature range. Banea and da Silva [24] studied the SLJs struments, which is a three-component system. This adhesive is sug­
from − 40 ◦ C to 80 ◦ C, finding that the bonding strength reduces as the gested 4 h for curing at 80 ◦ C, and its glass transition temperature (Tg) is
temperature increases. Marques et al. [25] claimed that the mechanical tested approximately 115 ◦ C by DSC method.
properties are significantly changed and it is difficult to predict the The adherend metal is 2A12-T4 aluminum alloy, the aerospace
non-linear viscoelastic behavior due to high-level molecular mobility in industry-grade, with a high tensile strength of over 400 MPa and elas­
adhesive materials as the temperature is approaching the glass transition ticity modulus of 70 GPa. The Al substrates are manufactured to a
temperature. Sharon et al. [26] studied four structural adhesives and thickness of 5 mm and then treated by the phosphoric acid anodizing
found that the yield stress and modulus decrease with the increase of (PAA) method.
temperature, and the loading rate had a pronounced effect on the yield
stress while a negligible influence on the modulus. Banea et al. [27] 2.2. Specimen preparation
performed tensile tests at different loading rates and temperatures, the
results showed that the tensile stress decreases almost linearly with the To prepare the single-lap adhesive joints (SLJs) with different micron
increase of the temperature while increases nearly logarithmically with thicknesses of bondline, a special tooling was designed, as shown in
the loading rate. Carlberger et al. [28] studied the effects of strain rate Fig. 1. The basic principle and the geometrical parameters of the tooling
on the fracture energy and peak stress of two bonding modes. They and the specimen were described in detail in our previous work [32].
found that the fracture energy increases slightly with the increase of The thickness of the Al substrate is 5 mm, the overlap width is 25 mm,
strain rate in the peel mode while decreases in the shear mode and the and the overlap length is 12 mm. Standard gaskets (FEIN TOOL, China)
peak stresses in the peel and shear modes both increased as the strain with different thicknesses were used to prepare the specimens with 5,
rate increases. Park et al. [29] presented a nonlinear viscoelastic model, 30, 50, 100, and 150 μm.
which could account for the rate dependence at large strains, showing a
good agreement with the tensile data below 20% strain.
2.3. Testing methods and devices
The effects of loading rate, temperature, or bondline thickness on the
bonding performances of adhesive structures are a conventional issue
The tensile testing method referred from ASTM D1002 was con­
for the commonly appeared adhesive structures, however, very few re­
ducted to obtain the mechanical properties of the SLJs. To examine the
ported studies have examined this issue for precision adhesive structures
comprehensive influences of loading rate and temperature on the SLJs
with a very thin adhesive layer [30,31]. This work will focus on the
with different micron bondline thicknesses, a hydraulic tensile testing
aforementioned effects of precision adhesive joints that have a
machine with an environmental chamber was used for the tensile tests,
micron-level bondline thickness, in which a specially designed prepa­
as shown in Fig. 2. The experiments were performed at three different
ration tooling, infrared imager, and SEM, are used to analyze the
loading rates (1, 10, and 50 mm/min) and four temperatures (− 30, RT,
connection, fracture, and damage characteristics of the precision adhe­
80, and 110 ◦ C) for various levels of bondline thickness. Where RT
sive joints. This work and its experimental data would be helpful and
represents the room temperature and also the typical storage tempera­
useful for understanding and improving the bonding process in the
ture, about 23 ◦ C. The allowed lowest storage temperature is − 30 ◦ C,
manufacturing of precision devices.
and the typical service temperature is mostly about 80 ◦ C. The 110 ◦ C is
the extreme temperature, which is close to Tg.
The infrared imaging and SEM methods were used to analyze the
residual adhesive and failure mode after the tensile tests. An infrared

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L. Guo et al. Polymer Testing 109 (2022) 107528

Table 1 again by using a high-precision coating thickness gauge.

The experimental parameters and testing results. In Table 1, the tensile strength is significantly affected by the loading
Temperature/ Loading Bondline Results rate, temperature, and bondline thickness. The maximum tensile
◦
C rate/mm/ thickness/μm strength is 39.39 MPa obtained at the combined condition of − 30 ◦ C, 1
Actual Tensile
min
thickness/μm strength/ mm/min, and 50 μm and the minimum tensile strength is 22.07 MPa
MPa obtained at 110 ◦ C, 1 mm/min, and 100 μm. The tensile strength greatly
− 30 1 5 7.30 37.82
reduces by 43.9%, indicating that the temperature performed a very
− 30 1 50 47.77 39.39 important role in these tests. The measured bondline thicknesses are
− 30 1 100 100.37 33.03 well-matched with the corresponding designed values except showing
20 1 5 10.10 25.57 moderate large relative errors at the thinnest thickness, while they still
20 1 30 30.53 32.89
make sense.
20 1 50 47.23 31.55
20 1 100 97.60 28.44
20 1 150 152.45 26.44
3.1. Effect of bondline thickness
20 10 5 11.70 30.36
20 10 30 30.23 33.19
20 10 50 56.34 32.31 The plots of tensile strength versus bondline thickness at different
20 10 100 101.33 31.80 temperatures and loading rates, as shown in Fig. 3, increase firstly and
20 10 150 155.00 30.90 then decrease with the increase of bondline thickness except the one at
20 50 5 9.13 32.17
20 50 30 30.57 35.28
110 ◦ C drops slightly, the peak tensile strengths always appear at around
20 50 50 45.63 34.41 30 μm bondline thickness whether the loading rate increases from 1 to
20 50 100 98.07 33.20 50 mm/min or the temperature increases from − 30 to 80 ◦ C. Taking the
20 50 150 151.08 32.20 combination of RT and 1 mm/min as an example in Fig. 3(a), the tensile
80 1 5 5.33 23.18
strength increases by 28.6% as the bondline thickness increases from
80 1 50 53.43 27.01
80 1 100 99.00 26.29 10.10 μm to 30.53 μm and then linearly decreases by 19.6% when the
80 10 50 59.73 27.13 thickness increases from 30.53 μm to 152.45 μm, which the increasing
80 50 50 47.37 27.51 rate is much larger than the decreasing rate, showing that the bonding
110 1 5 5.10 22.65 strength is much more sensitive to the change of the bondline at a
110 1 50 60.70 22.42
110 1 100 99.90 22.04
thinner thickness. A similar response can be seen in Fig. 3(b), especially
110 10 50 49.87 26.13 for the trend of tensile strength changing with the increase of bondline
110 50 50 48.70 27.36 thickness at RT. Therefore, a small deviation of the adhesive layer can
result in a significant change of the bonding strength for such SLJs with a
micron-level bondline thickness. Additionally, it can be seen that when
thermal imaging camera uses the infrared detector and optical objective
the bondline thickness is thicker than 50 μm, the tensile strength almost
lens to receive the infrared radiation energy of measured targets to
linearly decreases with the increase of bondline thickness, which
obtain the infrared thermal images, which reflect the temperature dis­
essentially agrees with the reported studies for the bondline thickness
tribution on the surface of the measured object. To observe clear thermal
more than 100 μm [33–35]. However, the conclusion is opposite for the
images, the fractured substrates were heated to an appropriate tem­
bondline thickness less than 50 μm or even 30 μm. This is a critical
perature of 80 ◦ C firstly, and then the distribution of the residual ad­
characteristic for assembling a precision device using a micron-level
hesive on the surface of the substrates can be distinguished from the
bonding process.
infrared thermal images since the adhesive and the Al substrate have
different temperatures due to their different heat dissipation rates.
3.2. Effect of temperature
3. Results and discussion
The glass transition temperature Tg of the used adhesive is about
The SLJs tensile testing results, including actual bondline thickness 115 ◦ C, which is measured by DSC method. To invest the mechanical
and tensile strength, are listed in Table 1, which were acquired at properties of the adhesive at the storage and service conditions, the
different loading rates, temperatures, and bondline thicknesses. The tensile tests were carried out at the temperature from − 30 ◦ C to 110 ◦ C
tensile strength was calculated according to ASTM D1002. After the below the Tg. Fig. 4 shows the tensile strengths tested from low to high
tensile tests, the actual values of bondline thickness were measured temperatures at three different bondline thicknesses. The results show
that the tensile strength always appears the largest value at the lowest

Fig. 3. The tensile strength against bondline thickness at different (a) temperatures and (b) loading rates.

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L. Guo et al. Polymer Testing 109 (2022) 107528

rate increases from 1 to 10 mm/min, while by 6.5%, 1.4%, and 4.7%

from 10 to 50 mm/min. Therefore, the used adhesive material is sensi­
tive to the loading rate factor, exhibiting the strain-rate hardening effect
below the Tg value [36].

3.4. Fractured surface analysis

The failure mode of the SLJs can be recognized from the fractured
surface of the substrates. For the specimens with a thin bondline, the
fracture always occurs at the interface between the adhesive and the
substrate, and it is difficult to determine the failure mode by visual
observation. The infrared imaging and SEM methods are used to analyze
the residual adhesive on the substrates.
Owing to the large difference in heat dissipation rate between Al
alloy and the adhesive materials, infrared imaging analyzers can acquire
a clear image of the residual adhesive on the substrate. Before imaging,
all the fractured samples were heated to 80 ◦ C, which could increase the
heat radiation intensity. Fig. 6 shows the thermal images on the frac­
Fig. 4. The tensile strength against the temperature for the specimens with tured surfaces for the specimens with different bondline thicknesses. The
different bondline thicknesses. ‘pink’ color, representing the high-temperature area, shows the residual
adhesive. The ‘blue’ color represents the low-temperature area, indi­
cating the Al substrates. The ‘green’ color, representing the medium-
temperature area, mainly results from the reflection of the surround­
ing heat on the rough surface, which is due to surface damage, impu­
rities, and adhesive spots on the substrate.
The thermal images show that the residual adhesive reduces and its
integrity and continuity both become worse as the bondline thickness
becomes thinner. Two fracture phenomena can be recognized from the
distributions of the residual adhesive, that is, the peeling fracture of the
bondline from the substrate (called Phenomenon I, Fig. 7(a)) and the
internal fracture of the bondline itself along the thickness direction
(called Phenomenon II, Fig. 7(b)). For the thicker bondline, the fracture
mainly starts with the Phenomenon I and then presents the Phenomenon
II finally at the middle line of the bonding area, as shown in Fig.6(c)–(e).
For the thinner bondlines, such as those below 30 μm shown in Fig. 6(a)
and (b), the Phenomenon II occurs earlier, accompanied by slight Phe­
nomenon I, yielding many fragments inside the adhesive. These phe­
nomena might result from two reasons: on the one hand, the adhesive
layer is very thin and brittle, as a consequence, the local internal damage
easily occurs, resulting in low average bonding strength during peeling
off the substrate surface; on the other hand, adhesive defects, such as
Fig. 5. The response of tensile strength to the loading rate at different adhesive lacking and micron-bubbles during the assembly processing,
temperatures. more easily appear in a thinner adhesive layer, which is more likely to
rupture prematurely, however, if the bondline thickness is greater than
temperature and decreases with the increase of temperature. When the 30 μm or 50 μm, the influence of those defects could be weakened, and
temperature rises from − 30 ◦ C to 110 ◦ C, the tensile strength of the the cohesive strength along the thickness direction of the adhesive is
specimens with three different bondline thicknesses decreases by 40.1%, sufficient to maintain its integrity, resulting in higher tensile strength.
43.1%, and 33.3%, respectively. Thus, it can be claimed that the in­ These indicate that reducing the bondline thickness, less than about 10
crease in temperature significantly decreases the bonding strength of μm, could result in a serious stress concentration and a weak bonding
SLJs. Moreover, when the temperature is close to the glass transition interface to reduce the bonding strength.
temperature, the specimens with different bondline thicknesses show The SEM method was further used to observe the micro-nano
similar tensile strength, indicating that the increase of the temperature morphology of the residual adhesive on the substrate surface. Fig. 8(a)
could weaken the effect of thickness on the bonding strength. and (b) show the original feature of the substrate surface with different
magnifications, where a clear PAA film with nano-scale porous structure
can be seen. Fig. 8(c), (d), (e), and (f) show the microscopic images of
3.3. Effect of loading rate the residual adhesive at four different conditions of temperature and
loading rate, respectively, which all covered the original feature of the
Loading rate plays an important role in the mechanical properties of substrate surface. These images represent the characteristics of the
adhesive joints due to the viscoelastic behavior of polymer materials. fractured surface and indicate that all the failure modes of SLJs are
Here, the tests were conducted under the loading rate in the range of 1 mainly subject to the cohesive failure of adhesive at the bonding inter­
mm/min to 50 mm/min and the bondline thickness of 50 μm. Fig. 5 face. Therefore, the PAA pretreated Al substrate is of benefit to the ad­
shows the tensile strength of 50 μm bondline thickness versus the hesive bonding under different bondline thicknesses, temperatures, and
loading rate at different temperatures. The tensile strength always in­ loading rates. Additionally, some different characteristics also can be
creases with the increase of loading rate even the temperature increases observed in the micro-morphologies of the fractured adhesive shown in
from RT to 110 ◦ C. Specifically, the tensile strength increases by 2.4%, Fig. 8(c)–(f). The fractured adhesive exhibits more plastic damage
0.4%, and 16.5% at RT, 80, and 110 ◦ C, respectively, when the loading characteristics as the testing temperature increases. At the temperature

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L. Guo et al. Polymer Testing 109 (2022) 107528

Fig. 6. The infrared thermal images of residual adhesive on the fractured surface at different bondline thicknesses.

Fig. 7. The schematic diagram of the two fracture phenomena of SLJs.

of − 30 and 20 ◦ C, the fractured surface is relatively flat and smooth, (5) The tensile strength increases as the loading rate increases,
likely a brittle fracture. But at the higher testing temperature, the plastic exhibiting the strain-rate hardening effect below the Tg value.
deformation of adhesive appears on the micro fractured surface. (6) Under the tested conditions, the temperature presents the most
significant influence on the tensile strength and then the bondline
4. Conclusions thickness followed by the loading rate.
(7) The cohesive failure mode of adhesive on the bonding interface
This work performed a series of tensile testing experiments for the indicates that the porous structure of PAA film can always pro­
single-lap joints to examine the comprehensive influences of bondline vide a good surface for the adhesive bonding under the tested
thickness, temperature, and loading rate on the bonding properties of bondline thicknesses, temperatures, and loading rates.
the epoxy resin adhesive. The findings are listed as follows:
CRediT authorship contribution statement
(1) The maximum tensile strength was acquired at around 30 μm
bondline thickness, whether the loading rate increased from 1 Lei Guo: Conceptualization, Experiments operating, Data curation,
mm/min to 50 mm/min, or the temperature increased from Formal analysis, Investigation, Methodology, Roles/Writing - original
− 30 ◦ C to 80 ◦ C. draft. Jianhua Liu: Writing - review & editing, Funding acquisition,
(2) The micron deviation of bondline thickness can result in a change Project administration, Resources, Supervision. Huanxiong Xia:
of up to 28.6% of the tensile strength. The dimensional accuracy Conceptualization, Formal analysis, Methodology, Writing - review &
of bondline thickness has an important impact on the bonding editing, Funding acquisition, Project administration, Resources, Super­
performance of precision adhesive joints. vision. Xiayu Li: Writing - review & editing, Experiments operating,
(3) The tensile strengths of the SLJs with different bondline thick­ Formal analysis, Visualization. Xiumin Zhang: Writing - review & edit­
nesses decrease more than 33% as the temperature rises from ing, Formal analysis, Visualization. Hongfan Yang: Writing - review &
− 30 ◦ C to 110 ◦ C and eventually approach a similar value. editing, Formal analysis, Visualization. Ye Yang: Writing - review &
(4) Reducing the bondline thickness, less than about 10 μm, could editing, Funding acquisition, Project administration, Resources,
weaken the bonding strength. Supervision.

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L. Guo et al. Polymer Testing 109 (2022) 107528

Fig. 8. The SEM images of the fractured surfaces at different temperatures and loading rates (bondline thickness is 5 μm).

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