Research Journal of Chemistry and Environment____________________________________Vol.
24 (10) October (2020)
Studies on the effect of functional additives on the
performance of epoxy based structural adhesive
Arora Pinklesh*, Singh Rakesh Kumar and Kaicker Praveen Kumar
Material Science Division, Shriram Institute for Industrial Research, 19, University Road, New Delhi – 110007, INDIA
*pinklesh@shriraminstitute.org
Abstract
In the present investigation, two components based
structural epoxy adhesive system has been developed
for bonding of aluminum as well as other dissimilar
substrates. To develop the adhesive system, epoxy
resins have been modified by incorporation of
performance additives, alumina and aluminum. The
effect of these additives was studied on bonding
performance of adhesive by means of lap shear
strength, pull off strength and hardness etc. The
rheology of modified epoxy system was also studied to
understand its ease of applicability. Thermal stability
with any physical or chemical interaction was studied
by thermo-gravimetric analysis (TGA), differential
scanning Calorimetry (DSC), FT-IR and other relevant
instrumental techniques. The morphology of the
adhesives was also studied by Transmission electron
microscopy (TEM) and Scanning Electron Microscopy
(SEM). The present study correlates the effect of
varying concentrations of performance additives i.e.
alumina and aluminum on the thermal, mechanical and
bonding properties of adhesive formulations for
aluminum metal.
The studies showed remarkable improvement in
performance of epoxy based adhesives. The significant
enhancement in the glass transition and thermal
behavior temperature of modified epoxy formulations
was found vis-a-vis base epoxy polymer favoring high
temperature applications. Lap shear strength of
prepared adhesives exhibited an increase of ~20% by
increasing the concentration of filler content from 0 to
40%. The prepared adhesive compositions showed very
strong bonding with aluminum substrate.
Keywords: Epoxy adhesive, Performance additives,
Aluminum, Alumina, Lap shear strength, Pull off Strength.
Introduction
Adhesives play a significant role in bonding of metal,
plastic, rubber and other substrates in automobile, aircraft
and aerospace industries because they offer low weight,
fatigue resistant and aerodynamically sound method of
assembling the larger parts with less labor in cost effective
manner. The unique properties of adhesives requiring low
and high temperature resistance with good mechanical
strength for bonding of dissimilar substrates are the needs of
development1. The structural adhesives used often possess
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high mechanical and thermal properties based on epoxy
resins.
Epoxy resins are thermosetting resins cured using a wide
variety of curing agents/hardeners. The properties of epoxy
adhesives depend on the specific combination of the type of
epoxy resins and curing agents2. The outstanding properties
of epoxy resins include high strength, low shrinkage, no
volatile emission during curing, excellent adhesion to
various substrates, effective electrical insulation, chemical
and solvent resistance, low cost and low toxicity etc.
These are most commonly used in structural and specialty
composite applications such as aerospace, marine and other
high-performance applications.
Epoxy resins are polymeric molecules that are converted to
a solid hard material by crosslinking with hardener/ curing
agent to form a crosslinked network of molecules, thermoset.
These crosslinked polymers are irreversibly, rigid and
relatively unaffected by heat.
The epoxy adhesive systems are of two types: (i) one
component and (ii) two components. In one component
epoxy system, heat is required for curing, but two
component epoxy system is either cured at room temperature
or at elevated temperature depending upon the reactivity of
resin and hardener.
There are several types of epoxy systems of commercial
significance such as diglycidyl ethers of bisphenol-A
(DGEBA), epoxy novolacs, glycidyl ether of
tetraphenolethane, bisphenol F based and aliphatic and
cycloaliphatic resins3. The epoxy novolac resins have greater
functionality than DGEBA resins resulting into increased
crosslink density at elevated temperature with improved
chemical resistance. As these resins form very rigid structure
due to crosslinking, they are often used as modifiers in basic
epoxy adhesive systems.
Similar to epoxy novolac resins, glycidyl ether of
tetraphenolethane is used in combination with lower
molecular weight epoxy resins. Due to the presence of high
aromatic ring content combined with polyfunctionality, they
provide high thermal stability for high temperature
applications. Bisphenol F resins are lower viscosity epoxy
resins as compared to DGEBA and provide greater
flexibility at lower temperature. Cycloaliphatic epoxy resins
are a class of materials of choice for a wide variety of
electrical, electronic and structural applications.
Research Journal of Chemistry and Environment____________________________________Vol. 24 (10) October (2020)
The inherent low viscosity of these resins enables them to be
formulated with higher levels of inorganic fillers4. Glycidyl
ethers of aliphatic polyols have low viscosities and good
wetting properties. These resins provide flexibility when
cured with amine curing agents5. Amongst structural
adhesives, epoxy resin based diglycidyl ethers of bisphenol-
A (DGEBA) have received much attention due to its easy
crosslinking with amine groups.
Epoxies are most versatile family of adhesives because they
are bonded well to different substrates whereas these are
brittle in nature and can be modified by incorporation of
performance additives such as diluents, flexibilizers and
fillers. The improvement of properties of epoxy resins
depends on the types of fillers and their properties such as
size and shape, surface chemistry, dispersion and
compatibility with base resin.
Several approaches have been used to enhance the properties
of epoxy resins such as chemical modification of epoxy
backbone, incorporation of toughening agents and
flexibilizers6-10 and incorporation of inorganic fillers into the
base epoxy resin.11
Parimalam et al12 studied the effect of nanosilica, zinc oxide,
titanium oxide on the performance parameters such as
chemical and heat resistance of epoxy based coatings. The
results showed that the chemical and heat resistance of
epoxy based coatings was improved in presence of TiO2 and
SiO2 nanoparticles.
The incorporation of surface modified kaolin with sodium
polyacrylate into diglycidyl ether of bisphenol A (DGEBA)
epoxy resin with polyamidoamine as hardener was carried
out. The results showed good clay particle distribution in
polymer matrix and improved microhardness of synthesized
adhesive system by incorporation of 33% filler.13
Epoxy-based adhesive reinforced with nano and micro-
particles of silica and ceramic were developed for bonding
of wood. Thermal properties of epoxy adhesives were
studied by using dynamic mechanical thermal analysis
(DMTA) and differential scanning calorimetry (DSC). The
glass transition temperature (Tg) of developed adhesive
system was increased about 22°C in presence of ceramic
particles.14
The effect of metal powders, copper and aluminum was
studied on the mechanical properties of epoxy based
adhesives. Enhancement in lap shear strength was observed
with 5% aluminum powder and decreased lap shear strength
was measured with copper.15
The most common fillers used in epoxy based adhesive
formulations are aluminum, alumina, aluminum salts,
calcium salts, silica, clay, glass fibre and titanium dioxide
etc. The selection of fillers for epoxy adhesive formulations
depends on the substrate to be bonded and desired properties
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Res. J. Chem. Environ.
of adhesives. In this research work the adhesive formulations
were developed to bond aluminum and on the basis of
previous research, aluminum and alumina were selected as
performance fillers to study their effects on the performance
of epoxy based adhesive formulations.
Not much literature was found on the effect of aluminum and
alumina functional fillers on thermal and mechanical
properties of epoxy based adhesive with respect to aluminum
bonding. In the present study, two component epoxy based
structural adhesive system has been developed for bonding
of aluminum by modification of diglycidyl ethers of
bisphenol-A (DGEBA) epoxy resin with alumina and
aluminum.
The effects of functional additives on bonding performance
of adhesives, thermal properties, viscosity, dispersion
ability, lap shear strength and hardness etc. were studied.
Material and Methods
Materials: During studies, epoxy resin, diluent, hardener
and functional additives were used (summarized in table 1).
All the materials were used as such without further
purification for preparation of adhesive formulations. The
aluminum alloy substrate of thickness 2 mm from Hindalco
Industries Ltd., India was used to perform the adhesive
properties.
Methods
Preparation of epoxy resin compositions: Compositions
of epoxy resins (Lapox A-16) were prepared with diluent
BGE (5%) and varying concentrations of alumina and
aluminum powder i.e. 0%, 10%, 20%, 30% and 40%.
Functional additives were gradually added to epoxy resin
under stirring to prevent lump formation. The mixture was
mechanically stirred at 50°C for two hours to achieve
uniform dispersion in formulation.
Characterization
Fourier Transform Infrared Spectroscopy (FT-IR): The
FTIR analysis of prepared epoxy resin formulation was
carried out to identify the change in functionality of the
modified one with unmodified epoxy resin and to establish
interactions between functional additives with epoxy resin.
Fourier Transform Infrared Spectroscopy (FT-IR) analysis
of prepared epoxy resin formulations was performed using
FTIR instrument (Model Schimadzu –IR Affinity 1S) by
applying epoxy resin compositions on salt plate made of
KBr.
Viscosity Measurements: The viscosity of prepared epoxy
formulations was measured by the Rheometer (MARS,
Thermo Fisher) at 25°C temperature. The samples were
loaded between aluminum plates of 50 mm diameter with
0.05 mm gap. The samples were kept at 25°C for 5 minutes
to reach a thermal equilibrium and the apparent viscosity
was measured by 30s scan.
Research Journal of Chemistry and Environment____________________________________Vol. 24 (10) October (2020)
Scanning Electron Microscopy (SEM): SEM studies of
cured adhesive samples were carried out by using EVO 18
Special Edition (Zeiss, Germany) for imaging. The samples
were mounted on aluminum stub with the help of double-
sided adhesive carbon tapes (Agar Scientific, UK). The
mounted samples were then exposed to ~20nm gold coating
at 20mA for 165 second by Sputter coater SC7620 (Quorum
Technologies Ltd., UK) to make them electrically
conductive. The magnification of the microscope was
selected as required for the detailed morphological study of
the samples.
Differential Scanning Calorimetry (DSC): Differential
Scanning Calorimetry (DSC) of cured adhesives was carried
out using TA Instruments differential scanning calorimeter,
model Q200 with a controlled cooling accessory from room
temperature to 250°C in nitrogen atmosphere at a heating
rate of 5°C/min. Adhesive samples were weighed between
10 to 20 mg and taken in a closed aluminum pan to run the
experiments.
Res. J. Chem. Environ.
analyses were carried out using TA Instruments, Universal
V4.5A, from room temperature to 1000°C in air atmosphere
at a heating rate of 10°C/min.
Lap Shear Strength: Lap shear test of epoxy based
adhesive composites was performed according to standard
ASTM C-961. To carry out this analysis, the adhesive
compositions were applied between two aluminum sheets
(25 mm x 75 mm dimension) in the area of 25 mm x 25 mm.
The joint samples were cured at room temperature for 7 days
and the lap shear strength of the samples was measured on a
Universal Testing Machine (UTM) Model Instron-
5982U3176 with load cell capacity of 100 kN and accuracy
of ±1 N at loading rate of 12.7 mm/min. Each test result is
the average of four test recordings.
Shore D Hardness: The hardness of adhesive samples was
tested by Shore D hardness Durometer according to standard
ASTM D-2240. The given results of hardness are the
average of five test observations.

Thermogravimetric Analysis (TGA): Thermal stability The methodology of the studies is given as form of flow
and decomposition behavior of the cured adhesive samples chart (Figure 1).
were studied by Thermogravimetric analysis (TGA). These

Epoxy Resin Diluent

Stirring

Addition of varying concentrations of performance fillers

Stirring

Modified Epoxy Resin Hardener

Characterization
Ratio 1:1
FT-IR Viscosity Curing

Adhesive Formulation

Characterization

Scanning Electron Differential Scanning Thermogravimetric Lap Shear Shore D

Microscopy (SEM) Calorimetry (DSC) Analysis (TGA) Strength Hardness

Figure 1: Flow chart of methodology

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Results and Discussion
Fourier Transform Infrared Spectroscopy (FT-IR):
FTIR analysis of prepared epoxy resin formulation was
carried out to identify the change in functionality of the
modified and unmodified epoxy resin and to study
interactions happening between alumina and aluminum with
epoxy resin [Figure 2a and b]. The broad peak at 3495 cm-1
relates to O-H stretching of hydroxyl groups. The peak at
Res. J. Chem. Environ.
3057 cm-1 indicates the C-H band stretching of oxirane ring.
The peaks at 1247 cm-1, 1036 cm-1, 771 cm-1 and 831 cm-1
indicate the ring stretching band for epoxides, C-O-C
stretching for ethers and C-O-C stretching of oxirane group
respectively. As reported in literature, the surface of alumina
and aluminum particles has hydroxyl groups16. The
stretching vibration peak at 778 cm-1 and 504 cm-1 indicates
physical interaction between OH groups of functional
additives and OH groups of epoxy resin3.

Neat Epoxy resin

(a)

503
Epoxy resin with alumina

453
3495

771
2872

573
2927
2966

1608

1036

831
1508

1247

Neat Epoxy resin

(b)
503
453
3495

Epoxy resin with aluminum

3057

771
2927 2872

573
2966

1608

1036

831
1247
1508

Figure 2: FTIR spectra of (a) base epoxy resin with 40% alumina and (b) epoxy resin with 40% of aluminum

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Scanning Electron Microscopy (SEM): In order to observe
the morphology of epoxy based compositions and the
dispersion of functional additives in epoxy matrix, SEM
analysis was carried out. Figure 3a represents the
micrograph of aluminum powder indicating the particle
distribution ranging from 5µm to 15µm. These results were
also favored by Rikhtegar et al16 and Haghighi et al.17 The
SEM micrograph of alumina of free flowing consistency has
been shown in figure 3b indicating the tiny particles
agglomeration with uniformity15 of dimension in ranging
Res. J. Chem. Environ.
from 20 to 50 µm. figure 3c represents photomicrograph of
base epoxy resin without incorporating functional additives
showing smooth structure without any voids and cracks.
Figures 3d and 3e are the DGEBA composites with 20 and
40% aluminum powder concentration showing
homogeneous and uniform dispersion of aluminum filler
throughout the surface. The micrographs of DGEBA
compositions with 20 and 40% alumina concentration are
represented in figures 3f to 3g indicating the uniform
dispersion of alumina particles in epoxy matrix.19

a b

c d

e f

g h

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Res. J. Chem. Environ.

i j

Figure 3: Scanning Electron Microscope (SEM) of a) DGEBA (0% filler), b) Aluminum powder, c) surface view
and d) side view of DGEBA (20% aluminum), e) surface view and f) side view of DGEBA (40% aluminum),
g) Alumina powder, h) surface view and i) side view of DGEBA (20% alumina), j) surface view and
k) side view of DGEBA (40% alumina)

Viscosity Measurements: In order to study the effect of
alumina and aluminum on flow characteristics of
formulations, the epoxy formulations were characterized for
viscosity change. As can be seen in figure 4a, the addition of
alumina and aluminum powder results into increase in
viscosity of formulations as the additives content increases
mainly due to particle interactions suspended in the resin
matrix20 as the viscosity describes the resistance of matrix to
flow under external stress21.
Further viscosity increases with the thickening of the system
as the particles enter into polymer matrix interspaces
preventing free movement of polymeric chains22. It was
observed that the viscosity of epoxy formulations was
workable up to the addition of 40% aluminum powder and
alumina in epoxy resin.
Differential Scanning Calorimetry (DSC): To study the
effect of presence of additives, alumina and aluminum on the
thermal properties i.e. glass transition temperature of epoxy
adhesive system, compositions of varying amount of
alumina and aluminum were subjected to Differential
Scanning Calorimetry (DSC) study. From the figure 4b, it
was inferred that by introduction of inorganic functional
additives from 0-40% in both the systems, the glass
transition temperature increased from 126 to 131°C with
aluminum and 126 to 137°C with alumina. As the content
increases, the blocking effect at molecular level is likely to
increase, thus glass transition increases.23-25
Thermogravimetric Analysis (TGA): TGA analysis of
epoxy systems with and without alumina and aluminum
additives was performed to investigate any change in
thermal stability behavior while comparing with reference
base epoxy polymer (Figure 5). The TGA results are
summarized in table 2. TGA analysis of cured adhesive
samples showed that the initial decomposition temperature
(IDT) is marginally shifted from 295 to 313°C on
incorporation of aluminum and alumina additives. The
change in decomposition temperature indicates the
improved thermal stability of adhesive systems having
alumina and aluminum as functional additives vis-à-vis base
epoxy system.
Lap Shear Strength: Lap shear strength of adhesive is a key
property to evaluate the bonding performance of adhesives
towards substrates. To carry out the lap shear strength,
aluminum sheets of 2 mm thickness were used as substrate.
Figure 4c showed that the introduction of alumina and
aluminum into epoxy resins led to an increase in lap shear
strength from 68 Kg/cm2 to 76 Kg/cm2 in case of 40%
aluminum loading and 81 Kg/cm2 in case of 40% alumina.
From the results, it has been inferred that the lap shear
strength of adhesives can be improved with the addition of
alumina and aluminum26, however depending upon their
processability, the loading can be optimized.
Shore D Hardness: The incorporation of alumina and
aluminum showed an increase in their Shore D hardness

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Res. J. Chem. Environ.
properties. The shore D hardness of base epoxy resin was Amaro et al27 also observed similar pattern of improvement
found as 65 and with the addition of alumina and aluminum in hardness of epoxy based composites on addition of nano
content to 40%, this can be increased to 90 (Figure 4d). alumina.

a b

c
d

Figure 4: a) Viscosity b) Glass transition temperature (Tg) c) lap shear strength and d) Shore D hardness of epoxy
resin formulations as a function of varying concentrations of alumina and aluminum

Table 1
List of Raw Materials
Name Source Function Properties
Lapox A-16, Bisphenol A Glycidyl Atul polymers, Base epoxy Epoxy equiv. weight 185-192 g/eq,
ether (DGEBA) Gujarat, India resin Viscosity 10000 – 16000 cps
Epothin 1014, Butyl glycedyl ether NVN Polymers, Diluent Epoxy equiv. weight 290-325 g/eq,
(BGE) Delhi, India Viscosity 5-10 cps
Lord-322, polyaminoamide and Lord Corporation, Hardener Viscosity 450,000-2,000,000 cps
[(Dimethylamino) methyl] phenol India
Aluminum fine powder S.D. fine Chemicals, Filler Density 2.7 g/cc3, Particle size 5-15 µm
Aluminum Oxide or Alumina powder India Filler Density 3.5 g/cc3, Size 20-50 µm

Table 2
Thermo-gravimetric Analysis of Modified Epoxy Resins
Adhesive Formulation Initial Decomposition Residual Mass at
Temperature (IDT) 1000°C
Temp. (°C) Weight Loss (%) (%)
DGEBA (0% filler) + Hardener (Control) 295 4.0 16
DGEBA with 20% Aluminum + Hardener 300 3.4 25
DGEBA with 40% Aluminum + Hardener 305 4.5 30
DGEBA with 20% Alumina + Hardener 310 5.2 24
DGEBA with 40% Alumina + Hardener 313 5.0 29

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Figure 5: Thermal Gravimetric Analysis (TGA) of epoxy resin and different concentrations of
fillers alumina and aluminum
Conclusion
Epoxy based adhesives with different levels of loading of
alumina and aluminum from 10 to 40% have shown
improved bonding performance with dissimilar surfaces.
SEM analysis of epoxy based adhesive composites showed
uniform dispersion of aluminum and alumina. The FT-IR
results showed the molecular interaction of alumina and
aluminum with epoxy resin.
The significant improvement in thermal stability
temperature of modified epoxy formulations was found vis-
a-vis base epoxy polymer favoring wide range of
temperature applicability. Lap shear strength of prepared
adhesives exhibited about 20% increase loading of 40%
functional additives, alumina and aluminum. The results of
these studies confirmed that the fillers alumina and
aluminum can be used as functional additives to improve the
performance of epoxy systems.
Acknowledgement
Authors wish to thank Defence Research and Development
Organization (DRDO) and Defence Laboratory, Jodhpur,
India to provide financial support and acknowledge the
encouragement provided by the Management of Shriram
Institute for Industrial Research, Delhi, India.
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(Received 22nd December 2019, accepted 04th March 2020)