Effect of GNP and MWCNT Addition on Lap Shear

Strength of Adhesively Bonded Joints

2022 19th International Bhurban Conference on Applied Sciences and Technology (IBCAST) | 978-1-6654-6051-4/22/$31.00 ©2022 IEEE | DOI: 10.1109/IBCAST54850.2022.9990107

Hassan Ejaz* Aamir Mubashar* Muhammad A.M Saad Waqar

Department of Mechanical
Engineering, SMME
National University of Sciences
and Technology
Islamabad, Pakistan.
hassan_ejaz@live.com
Department of Mechanical
Engineering, SMME
National University of Sciences
and Technology
Islamabad, Pakistan.
aamir@smme.nust.edu.pk
Department of Mechanical and
Aerospace Engineering
Air University
Islamabad, Pakistan.
muhammad.abbas.mehdi@gmail.
com
Department of Mechanical and
Aerospace Engineering
Air University
Islamabad, Pakistan.
saadwaqar29@hotmail.com

* Corresponding author

Abstract— This research explores the experimental effects of
Graphene Nanoplatelets (GNPs) and Multi-Walled Carbon
Nanotubes (MWCNTs) inclusion on the strength properties of
bonded single lap joints. GNPs and MWCNTs were added in the
amount of 1 wt% in high-strength epoxy adhesive Araldite 2011.
Mixing of the nano-particles in the adhesive was carefully carried
out for uniform dispersion GNPs and MWCNTs. The substrate
used in fabrication of the joints was Al 5083. Room temperature
testing of the joints was carried out to evaluate the load
displacement behavior. A comparison of strength between joints
was made after the testing. The results of the comparison showed
a substantial increase of the joint strength of reinforced joints. An
improvement of 59.69% and 28.84% in lap shear strength was
observed with the added MWCNTs and GNPs, respectively.
Scanning Electron Microscopy (SEM) was used for high
magnification analysis of fracture surfaces.
Keywords—Adhesively bonded Joints, Shear Strength,
Nanofillers, GNPs, MWCNTs.
I. INTRODUCTION
The need for low weight and high strength structures is of
critical importance, especially in the areas of automotive,
aeronautical, and aerospace sectors. In recent times, the use of
fiber reinforced composite materials has led manufacturers to
drastically minimize the weight of the structures without
compromising on rigidity and strength. Conventional
mechanical methods (bolting & reverting) of joining
components can damage the composite fibers by creating local
defects and stress concentrations points around reverts and bolt
holes [1, 2]. Adhesive bonding an alternate method to
mechanical methods overcome these issues by distributing the
load over a larger area, consequently reducing localized stress
regions. In addition to that adhesive bonding provides several
other advantages. These include weight savings resistance
towards corrosion, better fatigue performance, no thermal
defects, no local defects, good stability in geometric dimensions,
and most importantly joining dissimilar substrates and thin
sheets of metals without damaging [3-6].
However, these bonded joints require special treatments of
the surfaces to be joined, and even after that the joint strength is
not on par with its mechanical counterpart. Because of this
reason, several studies on this topic have been conducted in
recent decades to increase the strength of these joints [7-10].
These methods are mostly based on geometric optimization of
adherend geometry and the applied adhesive. These range from,
the generation of adhesive spew fillets, adherend notches,
external and internal tapering of adherends, and adherend
rounding [11]. The way these methods work is by reducing the
stress peaks within the adhesive layer and making it more
uniform, hence delaying the crack initiation.
Changing the intrinsic properties of the host epoxy adhesive
in recent times is a relative new technique that has shown results
that are more effectual in increasing the strength properties of
adhesively bonded joints [12]. Metallic and non-metallic nano-
particles are added in volume or weight fractions within the
adhesive and their effects on joint behavior were investigated by
several researchers. These ranges to aluminum oxide (Al2O3),
silica (SiO2), nano clay, rubber particles, carbon black, and
graphite. Non-organic carbon-related components like CNTs
and GNPs have gained an appreciable amount of recognition
among researchers because of their exceptional properties. It has
been estimated that CNTs have an elastic modulus in the range
of 270-950 GPa and ultimate tensile strength of 11-63 GPa in
the axial direction. For graphene, the ultimate tensile strength is
in order of 130 GPa [13-15]. Several researchers have studied
the effect of these nanofiller inclusion in enhancing the
mechanical properties of polymers, adhesives and bonded joints
[15-20]. The studies mostly utilized low viscous laminating
resins for the ease of mixing and dispersion of nano-particles in
the adhesive. Moreover, improvement in strength at lower
percentages (≤ 1 wt%) at various degrees was reported.
It the literature that there are many independent studies
related to the effects of GNPs and MWCNTs on the lap shear
strength of adhesive joints, in which scattered nature of results

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 exist (increase and decrease in lap shear strength have been B. Surface Treatment
reported) The findings about the comparison of GNPs and Aluminum surfaces are prone to natural oxidation in the
MWCNTs addition on strength properties of lap joints haven’t ambient environment. These oxide layers are weak in nature
been discussed in detail and correlated clearly. The aim of the and therefore compromise the joint strength when bonded. The
current work is to experimentally study and compare the effects main objective of doing pre-treatment is to remove these oxide
of GNPs and MWCNTs on joint strength behavior. The GNPs layers and bring out a fresh surface suitable for bonding. In this
and MWCNTs were added in the weight fractions of 1 wt% in a work, aluminum adherends were both chemically and
structural epoxy adhesive Araldite 2011. For comparison of electrochemically treated. The graphic illustration of the
strength results lap shear testing of joints was carried out on process performed is shown in detail in Fig. 1 [21]. The
UTM. Digital microscopy was used for examining of untreated chemicals were obtained from BDH Analar and Sigma Aldrich
and treated surfaces. SEM was used for fracture surface analysis UK.
at high magnification.
II. MATERIALS AND METHODOLOGY
A. Materials
Aluminum 5083 alloy is well-known for its highest strength
in the category of non-heat-treated alloys and has exceptional
corrosion resistance even in extreme environments. Used in
commercial, marine, and defense applications. For
manufacturing of the lap joints, the Al 5083 sheet of 3mm was
utilized. Huntsman Araldite 2011 was used as adhesive. The
high strength structural adhesive system is in the form of two
components and generally used to join non-metals, rubbers,
ceramics, and other materials in common use due to its superior
strength and toughness properties. The combined viscosity of
the resin hardener mixture is 40-45000 mPa.s. The properties
of Al 5083 and Adhesive 2011 were evaluated in house after
cutting dog bone specimens and testing them on UTM. The
average values of the results along with SD. is given in Table
1. The GNPs and MWCNTs nano-particles were acquired from
Cheap Tubes, United States of America. The dimensions of
nano fillers are shown in Table 2.
Fig. 1. Anodization process of adherends.

Table 1. Mechanical properties of Al 5083 and Araldite 2011.

Property Al 5083 Araldite 2011

E (GPa) 76 ± 2 1.43 ± 0.1
σut (MPa) 330 ± 2.5 29.21 ± 1.13
ν 0.33 0.36
εf (%) 18 ± 1 7.61 ± 0.8

Table 2. Dimensional properties of GNPs and MWCNTs.

Property GNPs MWCNTs

Length 1-2 μm 3-30 μm
Thickness/Dia. 3-10 nm 13-18 nm Fig. 2. Magnetic stirring of the mixture at elevated
temperature.
Surface Area 600-750 m2/g -
Purity 97% 99%
The process starts with thorough cleaning of coupons with
mild detergent and toluene solution. The coupons were then

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 placed in a pure acetone bath to remove any leftover alignment, after applying the adhesive on the marked area the
containments adhered to the surface. The coupons were then joints were placed on their thickness side on a flat horizontal
etched using NaOH solution for 5 minutes at 50°C, followed by surface. After 10 minutes clips were placed on both sides of
a de-smutting step in an HNO3 bath for 3 minutes. To avoid the overlap region. For consistency of parameters across all
cross-contamination of the chemical baths, the coupons were joints, first, the excess adhesive squeezed out at the overlap area
thoroughly rinsed with distilled water after every step. With was removed. Secondly, the manufactured lap joints were
steel as a cathode, Phosphoric Acid Anodization (PAA) of the placed in an oven to be cured at 70°C for 2.5 hours. For
aluminum coupons was performed at 15V for 35 minutes. The repeatability of results a sample size of 4 and variation in the
temperature of the bath was kept in the range of 28 to 30°C. In data is shown in standard deviation terms.
the final step, rinsing of the coupons was thoroughly performed
with distilled water until the PH was neutralized to 7. The final
drying step was performed by drying the aluminum coupons at
a temperature of 25°C in desiccator cabinet. The treated
coupons were then immediately bonded to make lap joints.
C. Mixing Procedure Fig. 3. Geometric dimensions of manufactured SLJs.
The mechanical properties of adhesive reinforced with
nanofillers (organic or non-organic) are directly linked with the Testing of lap joints was carried out at a speed of 1.3
quality of its suspension and dispersion in the adhesive. Thus, mm/min on a UTM. (Fig. 4). The tests were performed at room
a comprehensive mixing method as per ref. [22] was adopted temperature. End tabs were placed on joints for alignment
for mixing GNPs and MWCNTs in the adhesive. The process purposes during testing. To ensure repeatability of results, a
starts with bath sonicating the solvent (acetone)/nanofiller minimum of four tests was conducted and the variation is
mixture for exfoliation of the stacked particles. During the reported in standard deviation terms. For the analysis of fracture
sonication process, the beaker was sealed with the use double- surfaces, a high-resolution SEM was utilized at an electron
sided tape and cling film to prevent the mixture from being beam voltage of 20 kV.
contaminated from foreign elements. In the next step, the
required amount of resin component of the adhesive was added
to the beaker and the mixture was stirred at around 500 RPM at
60°C using a magnetic stirrer, as shown in Fig. 2. The
temperature was set in a way to accelerate acetone removal. As
the acetone gradually evaporates, the mass of the mixture was
continuously checked through a precision balance during the
mixing step until there was no indication of the presence of
acetone. However, for the purpose of removing any traces of
solvent left, the beaker was then placed in a degassing chamber
at a pressure of 0.05 bar for 20 minutes. This was followed by
a second stage sonication step at an elevated temperature of
50°C. The hardener component of the epoxy adhesive was the
added in ratio 100:80 (Resin: Hardener) by weight. The mixture
was then hand-stirred for 10 minutes, followed by degassing
step. The prepared adhesive with 1 wt% GNPs and MWCNTs
was then used to make respective lap joint configurations. The
viscosity of the adhesive was increased with the added
nanofillers, however it did not provide any hinderance in
fabrication of lap joints, as the adhesive was applied and evenly
distributed on bond area with the help of plastic spatula.

D. Lap Joint Configuration and Evaluation

Single lap joints (SLJ) were prepared according to the
ASTM D1002 standard. The joints were manufactured using
aluminum coupons of 101.6×25.4 mm dimension according to
ASTM D1002-10 standard. The thickness of the coupons was
3 mm. The dimensional parameters of the manufactured lap
joints are shown in detail in Fig. 3. In preparation of the joints
careful attention was given in alignment of adherends as any
degree variation of overlap region will result in an additional
twisting moment, which will comprise the results. To ensure Fig. 4. UTM machine utilized for testing of lap joints.

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 III. RESULTS AND DISCUSSION
A. Surface Topography
The surface texture of the aluminum adherend before and
after the surface treatment is shown in Fig. 5 and Fig. 6,
respectively. Smooth micro rolling patterns generated during the
manufacturing of the sheet are visible in Fig. 5. The direction of
the patterns indicates rolling direction of sheet when it was
manufactured. The NaOH treatment of the aluminum adherend
results in plateau-like bulges of different sizes. The anodized
surface in Fig. 6 shows a significant increase in micro and
nanocavities that are spread across the entire area of the
adherend. These created micro features increase the surface
roughness of the adherend, which plays a vital role in increasing
the adhesion forces between the adherend and the adhesive.
Fig. 7. Comparison of lap shear strength of neat and GNPs &
MWCNTs reinforced SLJs.

The enhancement in the mechanical strength is attributed to

Fig. 5. Digital microscope image of the untreated surface.
the exceptional properties of GNPs and MWCNTs.
Furthermore, these nanoparticles may also act as crack barriers
towards crack initiation and crack path. These crack arresters
also act as diversions and forced the crack to follow longer path,
hence increasing strength. Furthermore, The glass transition
temperature (Tg) of the non-reinforced epoxy is around 60-
63°C. Based on the literature, it has been reported that the Tg
of adhesive system increases with the addition of GNPs and
MWCNTs [23, 24]. The Tg of the neat epoxy is around 60-
63°C. This increase in value of Tg also proves the strong
binding phenomenon between the adhesive and the nanofillers
which results in an overall increase of strength.
The most representative stress-displacement plot for neat
and GNPs and MWCNTs modified adhesive is shown in Fig. 8.
The added nanoparticles have increased the stiffens response
for both lap joint configurations as visible. The increase in
stiffness response can be an effect of the exceptional
mechanical properties of nanofillers as explained previously.

Fig. 6. Digital microscope image of the surface after

anodization.

B. Tensile testing of Lap Joints

Tensile testing of single lap joints was performed to
compare the strength properties of neat, and nanofiller modified
adhesive. The results of which are presented in Fig. 7. The neat
lap joints showed an average lap shear strength of 16.29 MPa. Fig. 8. Stress-displacement plot for neat and GNPs &
The GNPs modified adhesive showed an increased response by MWCNTs reinforced SLJs.
reaching a value of 21 MPa. A percentage increase of around
28.84%. Adhesive with MWCNTs showed the highest lap shear The images of the fracture surfaces were analyzed to
strength by reaching a value of 26 MPa, which in percentage examine the mode of failure for GNPs and MWCNTs modified
terms comes out to be 59.64%. adhesive, as shown in Fig. 9. In both cases an adhesive failure

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 of the fracture surface was observed. For examination of the
surface at higher magnification, scanning electron microscopy
was used. Fig. 10 and Fig. 11 shows the results of the analysis.
It can be observed that fracture surface with MWCNTs is
significantly rough in nature as compared to GNPs. Shear
plastic deformation patterns cover the entire surface of the
fracture surface. These deformation marks are a clear indication
of strong interlaminar cohesion between the layers of adhesive,
arriving from the enforcing of the adhesive with MWCNTs.
The phenomenon can be explained by an analogy of steel-
reinforced concrete, which can take a tremendous amount of
axial load without failure relative to one without steel
reinforcement. Because of this, the strength behavior exhibited
by SLJ with MWCNTs nano-particles was superior to GNPs.
(a) (b)
Fig. 9. Fracture surface of (a) SLJ-GNP & (b) SLJ-MWCNT.
Fig. 10. SEM image of the fracture surface for SLJ-GNP.
Shearing Marks
Fig. 11. SEM image of the fracture surface for SLJ-MWCNT.
The adhesive failure shown in both the cases of lap joints
is a consequence of strong reinforcement phenomenon offered
by nanofillers. The surface treatment performed was best in the
class of electrochemical treatments, but failed to provide the
strong interlocking action for the adhesive. This is due the
reason that the reinforcement provided by the nanofillers in the
adhesive exceed the interlacing resistance between the
adherend and the adhesive, thus leading to an adhesive failure.
Regarding the rheological properties, the viscosity of the
adhesive was increased after the inclusion of nanofillers, but
this increase in viscosity did not affect the processing of
adhesive as solution mixing technique was utilized, which was
coupled with high temperature sonication. Also, the increase in
viscosity did not provide any hinderance in fabrication of lap
joints, as the adhesive was applied and evenly distributed on
bond area with the help of plastic spatula. Exact figures of the
increase in viscosity can’t be quoted as no test was performed,
however, based on the physical state it is estimated that the
viscosity got doubled with the addition of nanofillers.
IV. CONCLUSIONS
In this research, the effect of adding GNPs and MWCNTs
on the strength behavior of single lap bonded joints was
experimentally investigated. The nano-particles were added in
the fraction of 1 wt % in the epoxy adhesive. The 1 wt% filler
percentage was selected based on the literature findings of
strength improvement at lower percentages. A significant
increase in lap shear strength was observed with the added GNPs
and MWCNTs. However, added MWCNTs showed superior
strength properties relative to GNPs. On examining the fracture
surfaces at higher magnification, it was revealed that the fracture
surface of SLJ-MWCNT has shear deformation marks which is
an indication of strong interlaminar cohesion between the layers
of adhesive, arriving from the enforcing of adhesive with
MWCNTs fibers. This phenomenon was not present for GNPs,
which might be the cause of the lower strength improvement
depicted by SLJ-GNP. In terms of failure mode, adhesive failure
was observed in both the cases of lap joints which is
consequence of strong reinforcement phenomenon offered by
nanofillers. The surface treatment performed was best in the
class of electrochemical treatments, but failed to provide the
strong interlocking action for the adhesive. This led to the
adhesive failure of joints.
V. ACKNOWLEDGMENTS
The authors would like to acknowledge Nihal Polymers Inc.
Pakistan for their support in providing the epoxy adhesive at
discounted rates for research purposes.
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