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Analysis of wear behavior and shear properties of nano – ZnO2/jute

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DOI: 10.1016/[Link].2022.08.326

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Analysis of wear behavior and shear properties of nano – ZnO2/jute fiber/

epoxy composites by Hand layup technique
K.G. Sagar a,⇑, K. Ramachandran b, Koushik Kosanam c, B. Marxim Rahula Bharathi d, M. Rama e,
Sumanta Bhattacharya f
a
Department of Mechanical Engineering, Cambridge Institute of Technology, Bangalore 560036, Karnataka, India
b
Department of Mechanical Engineering, N.S.N College of Engineering & Technology, Karur 639003, Tamil Nadu, India
c
Master’s Student & Graduate Researcher, Department of Manufacturing Systems Engineering & Management, California State University, Northridge, 18111, Nordhoff St, CA 9133,
USA
d
Department of Mechanical Engineering, Aditya College of Engineering, Surampalem 533437, Andhra Pradesh, India
e
Department of Chemistry, [Link] Theresa’s College for Women (A), Eluru 530003, Andhra Pradesh, India
f
Department of Textile Technology, Maulana Abul Kalam Azad University of Technology, Kolkata 700064, West Bengal, India

a r t i c l e i n f o a b s t r a c t

Article history: Nano-ZnO2 was added to a jute fiber/epoxy composite whether it affected wear metrics and compressive
Available online xxxx strength. A silane-coupling agent with an amin-terminated end was used to functionalize the surface of
ZnO2 nanoparticles. The modified ZnO2 was characterized employing FTIR spectroscopy and TGA. Using
Keywords: the hand layup method, the multiscale composites were created by distributing different amounts of
Nano-ZnO2 nanoparticles (0.5, 1, 3, also 5 wt%) in matrix. The 3weight%ZnO2-filled compound has the finest charac-
Epoxy composites teristics out of all of these specimens. Adding ZnO2 to the composites caused in a 43 % increase in
Thermogravimetric analysis
Compressive property in the short-beam shear test. Adding 3 wt. %ZnO lowered wear rate by 80 % and
Interlaminar shear strength
Wear rate
COF by 48 %. Wear and fracture mechanisms were studied. According to the discoveries of this study,
M - ZnO2 is a promising alternative to be employed as a nanofiller in fiber-strengthened polymeric
matrix. An epoxy/jute composite was supplemented with nano-ZnO2 to examine the effects on wear met-
rics and interlaminar shearing strength during dry sliding, according to the study’s findings. A silane-
coupling agent with an amin-terminated end was used to functionalize the surface of ZnO2 nanoparticles.
The modified ZnO2 was characterized using Fourier-transform infrared spectroscopy and thermogravi-
metric studies. Hand layup was used to disperse different quantities of nanoparticles (0.5, 1, 3, also
5 wt%) in the matrix to create the multiscale composites. The 3 wt%ZnO2-filled composite has the finest
characteristics out of all of these specimens.
Copyright Ó 2023 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Confer-
ence on Newer Engineering Concepts and Technology.

1. Introduction qualities of glass and neat epoxy compounds were superior to

those of epoxy compounds reinforced with jute fibres, according
FRPs are popular engineering materials used in a range of to [8]. Nanofillers have recently aroused a lot of interest as a way
industries, including automotive, aerospace, and defence [1–2]. to enhance mechanical resistance of FRPs [9]. As is generally
Natural fibres are increasingly being used in a variety of applica- known, the mechanical resistance of nanofiller-filled FRP are typi-
tions as people become more concerned about environmental cally superior to those of plain FRP. For example, [10–11] found
issues [3]. Composites fabricated with both organic and inorganic that specimens strengthened with 5 % jute fibre and 5 % nanoclay
have variety of applications in numerous sectors [4]. Jute fibres had the maximum tensile and flexural strengths. Mechanical and
have been widely examined for their impact on mechanical charac- thermomechanical resistance of textile-reinforced composite
teristics of polymeric substances [5–7].It was found that the materials are enhanced by MWCNTs according to [12] (multi-
walled carbon nanotubes). According to [13–14], silanized CaCO-
⇑ Corresponding author. 3 nanoparticles improved the tensile and flexural characteristics
E-mail address: [Link]@[Link] (K.G. Sagar). of a basalt fiber/epoxy composites. They studied the mechanical

[Link]
2214-7853/Copyright Ó 2023 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference on Newer Engineering Concepts and Technology.

Please cite this article as: K.G. Sagar, K. Ramachandran, K. Kosanam et al., Analysis of wear behavior and shear properties of nano – ZnO2/jute fiber/epoxy
composites by Hand layup technique, Materials Today: Proceedings, [Link]
K.G. Sagar, K. Ramachandran, K. Kosanam et al. Materials Today: Proceedings xxx (xxxx) xxx

characteristics of CNFs, carbon fibres (CF), and epoxy composites 2.3. Dry-sliding and shear testing on short beams
[15–17]. When 2 % CNF was introduced to carbon fabric/epoxy,
the tensile and flexural strength amplified by 11 and 22.3 %, corre- Short-beam shear tests were donerendering to ASTMD 2344.
spondingly [18–19]. Nanofillers have been shown in studies to sug- Testing was performed three times using a universal testing device
gestively expand the wear characteristics of Fibre Reinforced with crosshead velocity of 1 mm/min. A 6:1 was chosen as the
Polymers. According to [20] and [21] research, the dry-sliding wear span-to-depth ratio. The ILSS values were computed and reported.
rate of the E-glass chopped strand mat/epoxy combination was A pin-on-disc machine was employed to done dry-sliding wear
reduced by half when nanoclay was introduced [22–24]. Research- testing at room temperature. A 5 mm diameter 52,100 steel pin
ers found that the Nomex fabric/phenolic composite with a 2 % gra- served as the counterpart. The tests were carried out on a
phene fill was the most durable, according to Ren and colleagues 23.4 mm diameter track with a sliding velocity of 408rev/min
[25]. According to [26–27], coir fiber-strengthened epoxy with and a speed of 0.5 m/s. The utilized stress was maintained at
Al2O3 additions has superior wear resistance than standard epoxy. 20 N, while the total sliding distance was maintained at 1000 m.
According to [28–29], the addition of CNF to basalt fiber/epoxy By dividing the volumetric loss by the applied force, the wear rate
composites significantly boosted wear resistance. Polyphenylene was obtained (sliding distance). The findings of the wear tests are
sulphide compounds with sub-micron ZnO2 resistances and short an average of at least three different investigations.
carbon fibres were explored by [30–31] for wear resistance. Those
with the best outcomes used a composite containing 15 % short
3. Results and discussions
carbon fibres and 5 % zinc oxide. Surface modification has been
proven to improve mechanical and wear resistance by enhancing
3.1. FTIR spectroscopic analysis
the interfacial adhesion among nanofillers and the polymeric
matrix [32–35]. Surface modification of nanofillers via silanization
The Fourier transform infrared spectrum of ZnO2 also M- ZnO2
appears to be a viable option. Organic and inorganic nanofillers can
as received are shown in Fig. 1. The detected band at 3200–
be linked together using silane-coupling agents [36]. The beneficial
3400 cm 1 in as-received ZnO2 is caused by the vibratory stretch-
effects of silanization on nanocomposites varied characteristics
ing of the hydroxyl group (OH) of the ZnO2Np. The vibrations of
have been thoroughly documented in the literature [37–38]. Com-
zirconia’s ZnAO and ZnAOAZn bonds create the bands observed
mercially available nano-ZnO2 has been used in a variety of appli-
at wavenumbers smaller than 1100 cm 1. In addition, the
cations. There have been few studies into micro ZnO2-reinforced
1628 cm 1 band equivalent to the ZnAOH method of flexion. A
FRP systems, according to the literature. As far as mechanical qual-
band at 940 cm 1 in M- ZnO2 FTIR spectra is comparable to the
ities, [39–40]tested a nano-ZnO2/flax fiber/epoxy combination.
ZnAOASi stretch vibration band, which is shown by the bands at
[41–42]investigated nano-ZnO2/flax fiber/epoxy composites in
3012 cm 1 and 2896 cm 1 for CH (methylene) group’s symmetric
Mode I and Mode II. ZnO2lading was studied to investigate how
and asymmetric stretching vibrations.
it affected wear behaviour and interlaminar shear characteristics
Absorptions in the range of 1000–1300 cm-1characterise the SiO
in composites produced from multiscale nano-ZnO2/jute fiber/
group. There are new lines at 1504 and 3360 cm 1 in the FTIR band
epoxy [43–44].
of M- ZnO2 that are attributable to the elongating of the NH2
groups. These findings show that ZnO2 surface was successfully
grafted with APTMS. Fig. 2 shows a diagram representation of
2. Experimental the response among M- ZnO2 and the epoxy matrix. When the
APTMS-grafted ZnO2 is disseminated throughout the epoxy resin,
2.1. Modification of zirconium oxide it forms a strong covalent bond by the amino terminus of the silane
mediator because the epoxide cluster of the composites responds
Using an amino-terminated crosslinking reagent was the key to it.
reason for reacting the amino groups with the epoxide groups in
the matrix and creating a covalent bond. The nanoparticles were
functionalized to rise interfacial adhesion amongZnO2 nanoparti- 3.2. Thermodynamic investigation
cles and the epoxy matrix. Salinization is most prevalent process
for surface modification. In this experiment, 3 mL of APTMS was Fig. 3 indicates the TGA curvatures for both as-received ZnO2as
mixed with 95 % ethanol and 5 % deionized water in a solvent. well as M-ZnO2. For ZnO2, weight loss happens at temperatures
The solution was then sonicated for 15 min after which ZnO2 between 25 and 2000 °C when water is physically removed from
was added. The combination was moved and refluxed at 800 °C the surface of the particles.
for 8 h after the pH was set to 4 using 37 % concentrated HCl. Furthermore, the water created by OH condensation on the sur-
The modified powders were then rinsed with ethanol before being face of ZnO2 is linked to the weight loss observed following 200 °C.
dried out at 100 °C for 24 h. The thermal degradation of APTMS chains results in a rapid weight
loss between 300 °C and 700 °C as shown in the TGA graph of M-
ZnO2. The loading of APTMS was determined to be roughly 7–8 % of
2.2. Sample creation the overall powder weight.

M- ZnO2 and epoxy resin are mechanically mixed for 20 min at 3.3. Results of Short-beam shear test
a speed of 2000 rpm. A Ti-6Al-4 V probe was used to sonicate the
mixture for 30 min at 150 W. The mixed container was placed in an Fig. 4 shows Composites with varied M-ZnO2 loadings and ILSS
ice-water bath to keep temperature increases through sonication. values. It was used to determine the ILSS of both the neat and mul-
The hardener is used after degassing was manually blended for tiscale specimens. The multiscale ILSS’s ILSS value increased when
5 min in a 10:100 epoxy resin weight ratio. Hand layup was used the M-ZnO2 loading was increased to 3 wt%. Frictional slippage is
to create the multiscale composites, which were then cold- minimized when the matrix is sandwiched among the jute fibres
pressed. The polymeric matrix was impregnated with five plies of and the polymeric matrix. When the matrix is sandwiched
jute cloth and cured at room temperature. A tidy jute fiber/epoxy between a jute fibre and a polymeric matrix, the ILSS increases
compound was constructed as a comparison sample. the most at a 3 wt% interfacial bonding and mechanical qualities
2
K.G. Sagar, K. Ramachandran, K. Kosanam et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 1. FTIR spectrum (a) ZnO2 and (b) M ZnO2 powders.

of the matrix. It has been generally reported that a strong bond 3 wt% M- ZnO2 loaded material, showing improved interfacial
amongthe fibres and the matrix is necessary to obtain a consider- bonding. These M- ZnO2 agglomerations in the interface area gen-
able improvement in ILSS. An increase in M- ZnO2 loading reduces erate an unwanted fiber–matrix adhesion on the fracture surface,
the ILSS because of the formation of M- ZnO2 agglomerates. The which is why this is happening. ZnO2 is filled to a weight propor-
epoxy matrix and jute fibre disintegrate at the fracture surface tion of 3 wt% on the tidy’s matrix fracture surface. Instead of a
because of a weak connection. According to this data set, the most clean matrix, the fracture occurs because ZnO2 is present in the
common failure mode for this specimen is fiber–matrix debonding. matrix. Using ZnO2 nanoparticles, the crack was unable to spread.
Jute fibres are entirely encased in matrix on fracture surfaces of a As for virgin epoxy matrixes, they are more likely to break when

3
K.G. Sagar, K. Ramachandran, K. Kosanam et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 2. The reaction between the epoxy matrix and M-ZnO2.

Fig. 3. Analysis of the ZnO2 and M-ZnO2powders by TGA.

Fig. 4. Composites with varied M-ZnO2 loadings and ILSS values.

they are subjected to mechanical stress. On the surface of samples

filled with 5 % M-ZnO2, ZnO2 agglomerations are plainly visible. As 3.4. Wear test results
a result, it’s important to recall that the evaluated approach for M-
ZnO2dispersion was less efficient at greater loadings, and a new As the M- ZnO2 loading increases, the rate of wear on M- ZnO2/
method should be used to attain homogenous dispersion. The pre- jute fiber/epoxy compounds changes. The presence of M- ZnO2 has
sent of these agglomerations at the interfacial region allows jute a substantial effect on composite wear rates, with the 3 wt% M-
fibre debonding from the matrix, acting as crack initiating zones. ZnO2 filled samples having the lower wear rate. Fig. 5 shows the

4
K.G. Sagar, K. Ramachandran, K. Kosanam et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 5. The M-ZnO2/jute fiber/epoxy wear rate changes with the M-ZnO2 loading. Fig. 6. Hybridized composites mean COF at various M-ZnO2 loadings.

4. Conclusions

M-ZnO2/jute fiber/epoxy wear rate changes with the M-ZnO2 Multiscale nano-ZnO2/jute fiber/epoxy compounds were tested
loading. for wear resistance and interlaminar shear resistance in this study.
More than eighty % of the jute fiber/epoxy specimen is worn out It was proven using FTIR and TGA that ZnO2 reacts with the APTMS
by the multiscale combination with 3 wt% M- ZnO2. M- ZnO2 ben- silane molecule. A maximum ILSS increase of 43 % in short-beam
eficial influence on the polymeric matrix’s mechanical characteris- shear testing was observed when the M-ZnO2 loaded jute fiber/
tics and the interfacial interaction between fibres and matrix could epoxy combination (3 wt%) was compared to the clean specimen.
be one possible explanation. Large fragmentation of the polymeric According to dry-sliding tests comparing the appealing sample to
matrix is prevented by the hard M- ZnO2 particles. When M- ZnO2 the M-ZnO2filled jute fiber/epoxy compound at 3 wt%, the wear
particles are added to the matrix of a fibre composite, the matrix rate and COF decreased by as much as 80 % and 48 %, respectively.
can withstand a higher percentage of the applied load, minimising The addition of 3wt %ZnO2 boosted the composite’s interlaminar
the stress attention on the fibre surface. The needed stress for a shear strength by 43 %, according to the findings of the short-
fibre fracture increases as a result of this. Similar outcomes have beam shear test. The wear rate and COF were lowered by 80 and
also been recorded. The compound wears more quickly in the spec- 48 %, respectively, when 3 wt. %ZnO2 was added to the jute fiber/
imen with 5 % M- ZnO2 filler. At larger nanofiller loadings, the epoxy composite. The wear and fracture mechanisms were studied
waste interfacial interaction between jute fibres and polymeric using scanning electron microscopy. M - ZnO2 was shown to be a
matrix will dramatically increase the rate of wear compound due good choice for usage as a nanofiller in fiber-strengthened polymer
to the information contained in nanofiller agglomerates. COF- compounds, according to the findings of this study.
sliding distance curves revealed that adding M- ZnO2 to jute
fiber/epoxy compounds reduces COF by up to 3 wt% of M- ZnO2.
Funding Statement
The COF of the compounds with 3 wt% M- ZnO2is clearly the lowest
(48 % lower than the neat specimen). The fiber/matrix adhesion
No funds or grants available for this work from any
properties are mostly to blame for this behaviour. M-ZnO2 can help
organization.
improve the interfacial bonding among the jute fibres and the
matrix, as described in the preceding paragraph. The neat epoxy
CRediT authorship contribution statement
had a COF of 0.52 and was used as a benchmark. The reduced
fiber/matrix interfacial contact caused by the addition of 5 wt%
K.G. Sagar: Writing – original draft. K. Ramachandran:
of M-ZnO2 increased the Coefficient of friction of the multiscale
Methodology. Koushik Kosanam: Conceptualization. B. Marxim
M-ZnO2/jute fiber/epoxy. Due to the fact that when a particle’s
Rahula Bharathi: Validation. M. Rama: Supervision. Sumanta
content crosses a certain threshold, it tends to clump together.
Bhattacharya: Formal analysis.
When agglomerated nanoparticles in composites are worn, the
agglomerations can simply fracture, offering no effective barrier.
Fig. 6 shows Hybridized composites mean COF at various M- Data availability
ZnO2 loadings.
The sample’s wearable surfaces are evaluated following the No data was used for the research described in the article.
wear test. Wearable and non-toxic surfaces were found in the
hybrid composite boosted with 3 and 5 wt% of M-ZnO2. 3 wt% Declaration of Competing Interest
M- ZnO2 laden specimen has a wearable surface that is much less
damaged than the pure specimen. There are no fibres coming out The authors declare that they have no known competing finan-
of the specimen’s worn surface, demonstrating that the 3 wt% M- cial interests or personal relationships that could have appeared
ZnO2filled specimen has better wear resistance. This sample shows to influence the work reported in this paper.
enhanced interfacial adhesion among the jute fibre and the matrix.
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