M. GANAPATHY, E. RASU: INVESTIGATION OF Ni-P COATED BAMBOO FIBRE/NANO-TiO2 ...
525–531
INVESTIGATION OF Ni-P COATED BAMBOO FIBRE/NANO-TiO
2
POLYESTER MATRIX COMPOSITE PROPERTIES
RAZISKAVA LASTNOSTI Ni-P OPLA[^ENIMI BAMBUSOVIMI
VLAKNI IN NANO DELCI TiO
2
Magesh Ganapathy
*
, Elansezhian Rasu
Department of Mechanical Engineering, Pondicherry Engineering College, Puducherry, India
Prejem rokopisa – received: 2022-06-15; sprejem za objavo – accepted for publication: 2022-07-25
doi:10.17222/mit.2022.532
Natural-fibre-reinforced polymer composites are most commonly employed in the automotive, aerospace and structural indus-
tries. This research focuses on the synthesis and analysis of the dynamic properties of a bamboo fibre used with a polyester ma-
trix in a nanocomposite produced with titanium oxide nanoparticles. Bamboo-fibre samples were prepared using the electroless
plating method in both their uncoated and nickel-phosphorus-coated states. Bamboo-fibre contents of (4.5, 9, 13.5 and 18) w/%
and nanoparticles of (0.5, 1, 1.5 and 2) w/% with and without the coating were examined for these qualities. Coated bamboo
fibres were mixed with 13.5 w/% and 1.5 w/% of titanium oxide. It was concluded that dynamic and thermomechanical proper-
ties of the polyester matrix reinforced with bamboo fibres coated with nanoparticles allow excellent bonding as compared to the
nanocomposite of the polyester matrix reinforced with uncoated bamboo fibres.
Keywords: bamboo fibre, nano-TiO2, dynamic and thermomechanical properties, nickel-phosphorus
Polimerni kompoziti oja~ani z naravnimi vlakni so danes razvojni trend in zato se zelo pogosto uporabljajo v avtomobilski in
letalski industriji, kot tudi v strojni{tvu in gradbeni{tvu. V raziskavi predstavljeni v ~lanku, so se avtorji osredoto~ili na sintezo
in analizo dinami~nih in termo mehanskih lastnosti z bambusovimi vlakni in nano delci titanovega oksida (TiO2) oja~anega
polimernega kompozita s poliestersko matrico. Vzorce bambusovih vlaken so pripravili z uporabo metode elektrolitskega
platiranja in uporabo dodatnega opla{~enja kompozitnih vlaken s spojino oziroma zlitino niklja in fosforja (Ni-P). V izdelanih
vzorcih kompozitov je bila vsebnost bambusovih vlaken in nano delcev TiO2 razli~na (4,5, 9, 13,5 in 18) w/% vlaken ter 0,5, 1,
1,5 in 2) w/% nano delcev). Vse izdelane opla{~ene in neopla{~ene kompozite so kakovostno ovrednotili. Najbolj{e lastnosti je
imel kompozit s 13,5 w/% opla{~enih bambusovih vlaken in 1,5 w/% nano delcev TiO2. Na osnovi raziskave so avtorji zaklju~ili,
da imajo izdelani kompoziti s poliestersko matrico oja~ani z opla{~enimi bambusovimi vlakni bolj{e termo mehanske in
dinami~ne lastnosti z odli~no vezavno trdnostjo v primerjavi s kompoziti, ki vsebujejo neopla{~ena vlakna.
Klju~ne besede: bambusova vlakna, nano titanov oksid, dinami~ne in termo mehanske lastnosti, nikelj-fosfor
I INTRODUCTION
Composites are made by physically combining/mix-
ing two or more elements to create a new component
with properties that are superior to those of individual
components.
1–3
Natural fibre based polymer composites
are nowadays most common in the industrial field;
hence, they are used in a wide range of applications, ex-
hibiting better properties. They are bio-degradable, re-
newable, inexpensive, eco-friendly and recyclable.
4,5
Natural fibres can replace synthetic fibres such as glass,
carbon nanotubes and graphite due to their low cost,
smaller energy consumption and better properties such as
mechanical and dynamic mechanical properties,
bio-degradability and damping capacity. Reinforcement
is used when natural fibres combined with different ma-
trix materials are studied. In the automobile field,
20–25 % of such polymer composites is used and 50 %
of them is widely used in the construction field.
6–9
Natu-
ral-fibre-reinforced polymer-matrix composites were in-
vestigated in several research works to improve the com-
posites in this way.
10–12
Nano-filler materials maximise
interfacial adherence and uniform distribution.
13,14
Tita-
nium oxide (TiO
2
) nanoparticle has been the most stud-
ied metal-oxide nanoparticle
15,16
because of its
one-of-a-kind mix of properties, including thermal sta-
bility, increased oxygen storage capacity and corrosion
resistance.
17–20
The mechanical properties of natural-fibre reinforce-
ment in bio-composites are not significantly improved
even after a chemical treatment process. As a result, de-
spite the fact that natural fibre/plastic composites have
been commercialised, their applicability in many indus-
tries is limited. This has motivated a lot of researchers to
improve the thermal and mechanical properties of com-
posites. The best way to increase the mechanical perfor-
mance of natural-fibre-based composites is to combine
nano-fillers like metal nanoparticles, nanoclay, and car-
bon nanotubes (CNT) with polymer resins such polyes-
ters, epoxy and vinyl ester resins.
21–23
The systematised
autocatalytic reduction of metallic salt
24
and electroless
deposition/coating of abrasive particles are becoming in-
creasingly common as a particle treatment method.
25
Several researchers have enhanced material properties
Materiali in tehnologije / Materials and technology 56 (2022) 5, 525–531 525
UDK 620.1:661.882 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 56(5)525(2022)
*Corresponding author's e-mail:
mrgmagesh025@gmail.com (Magesh Ganapathy)

using these coating techniques.
26
To improve the me-
chanical behaviour of polymer composites, an electroless
technique was performed to achieve a particle reinforce-
ment. The deposition of copper phosphorus on the sili-
con carbide particles was used in an electroless process.
27
The friction and wear behaviour of nickel-phosphorus
coating on silicon particles was tested using the
electroless deposition approach at an increased tempera-
ture, and it was established that the applied layer was ro-
bust.
28
In the present study, bamboo fibres with and without
a coat of nickel-phosphorous were added to a polyester
matrix material and a small amount of titanium oxide
nanoparticles were used. The crucial parameter in this in-
vestigation was the change in the nanoparticle and fibre
content. The distribution of nanoparticles and the frac-
ture surface of the nanocomposite were studied using
high-resolution scanning electron micrographs
(FESEM). The dynamic and viscoelastic properties of
the polymer-matrix composite reinforced with bamboo
fibres and nanoparticles were investigated.
2 EXPERIMENTAL PART
2.1 Materials
The polyester resin was purchased from a local poly-
mer vendor, Kamatchi Polymer Ltd., Puducherry, India,
while methyl-ethyl-ketone peroxide as the catalyst and
accelerator used for cobalt was obtained from another lo-
cal polymer vendor. Bamboo fibres were procured from
Go-Green India ltd., Chennai (India). Titanium oxide
nanoparticles were procured from Subra Scientific Ltd.,
Pondicherry (Sigma Aldrich) at a density of 6.4 g/mL at
28 °C with 99 % purity and a nanoparticles size of
<40nm.
2.2 Electroless plating process
Ni-P is applied on a bamboo-fibre substrate using an
electroless plating process. Bamboo fibres must be
cleansed and pre-treated before this operation to achieve
consistent coating. The bamboo fibre is an insulating
substrate; hence, it should be pre-treated with a tin II
chloride and palladium chloride solution as the catalyst,
activating the bamboo fibre in 20 min. Electroless coat-
ing consists of a chemical solution such as nickel sul-
phate as the source of nickel, sodium hypophosphite, tri
sodium citrate and ammonium chloride. The pH value is
maintained in the bath during this process, using ammo-
nium chloride. The temperature of chemical solution in
the bath is controlled by a PID set-up. Figure 1 shows
the experimental set-up of the electroless-bath hot plate.
The pH value and bath temperature are maintained at
(80 ± 2) °C and 7–8 pH so that a uniform coating of the
fibres is obtained. Sodium hypophosphate acts as the re-
ducing agent, releasing free electrons during the
electroless process. The free electrons react with the
nickel source, nickel sulphate in the electrolyte bath,
converting them into nickel particles. The excess elec-
trons liberated from the electrolyte solution in the bath
deoxidize the phosphorus ions in the reducing agent, re-
sulting in phosphorus particles that are deposited over
the entire surface of the fibres along with nickel. The
nickel and phosphorus particles are placed over the fibre
substrate after the palladium chloride solution is acti-
vated in the electroless bath.
Table 1: Prepared polyester nanocomposite specimens with various
compositions
Sp.
No.
Specimen
ID
Composition of the material
Polyester
resin
(w/%)
Without
Ni-P
coated
bamboo fi-
ber (w/%)
With Ni-P
coated
bamboo fi-
ber (w/%)
TiO
2 nano-
particle
(w/%)
1 PUC-1 95 4.5 – 0.5
2 PUC-2 90 9 – 1
3 PUC-3 85 13.5 – 1.5
4 PUC-4 80 18 – 2
5 PC-1 95 – 4.5 0.5
6 PC-2 90 – 9 1
7 PC-3 85 – 13.5 1.5
8 PC-4 80 – 18 2
PUC – polyester uncoated composite, PC – polyester coated compos-
ite
2.3 Preparation of the composite material
The polyester nanocomposite is reinforced with bam-
boo fibres using the compression moulding method. The
polyester composite samples are prepared without coated
bamboo fibres and with nickel-phosphorous coated bam-
boo fibres with standard sizes of (250 × 250 × 3) mm in
length, width and thickness of the specimen. The polyes-
ter resin matrix is weighed in a weighing machine; 250 g
of it is placed in a 500 mL glass beaker; it is cleaned;
then 4.5–18 w/% of bamboo fibre is added in intervals,
each time in the amount of 4.5 w/% . Then (0.5, 1, 1.5
and 2) w/% of titanium oxide nanopowder is placed in
M. GANAPATHY, E. RASU: INVESTIGATION OF Ni-P COATED BAMBOO FIBRE/NANO-TiO2 ...
526 Materiali in tehnologije / Materials and technology 56 (2022) 5, 525–531
Figure 1: Experimental electroless plating set-up

the 100 mL beaker. The bamboo fibres with and without
the coating are placed over the cleaned mould surface
and then the nano titanium oxide powder is poured into
the polyester resin. A mechanical stirrer is used to stir
thoroughly both the resin and powder for 20 min. There-
after, 0.2 mL of MEKP, as the catalyst, is added with a
syringe into the polyester resin and also 0.1 mL of co-
balt, as the accelerator, is added to the polyester resin
with a disposal syringe. Both the catalyst and accelerator
are stirred well for 2 min. The mould surface is cleaned
and white wax, as the releasing agent, is applied. The
prepared composite mixture is poured into the fabricated
steel mould, coated with white wax as the releasing
agent for different samples and left to be cured for 12 h
at an applied pressure of 2.5 MPa at room temperature.
After that the sample is removed from the steel mould.
Eight different samples are prepared, having weight frac-
tions of bamboo fibre of (4.5, 9, 13.5 and 18) w/% and
additions of nano-TiO
2
of (0.5, 1, 1.5 and 2) w/%; sam-
ples can be without the coated fibre or with the nickel
phosphorous coating. The fibre/polyester matrix nano-
composite is thus developed. The prepared eight speci-
mens with different compositions are shown in Table 1.
2.4 Synthesis of TiO
2
nanoparticles
TiO
2
nanoparticles are synthesized using a slightly
modified sol–gel process that was developed earlier for
the synthesis of molecularly imprinted titania. Briefly, a
solution comprised of absolute ethanol (40 mL) and
deionized water (5 mL) is placed in a 100 mL two-neck
round-bottom flask equipped with a septum, condenser
and magnetic bar. The solution is warmed gently, and
TiCl
4
(0.6 mL, 0.05 M) is injected into the solution
through the septum. The mixture is stirred continuously
for1hat60°C.Afterwards, a dilute solution of NH
4
OH
(0.05 M) is slowly dropped through the septum to main-
tain a pH of 9. The mixture is subsequently aged over-
night at 60 °C with consistent magnetic stirring. The
product is heated under vacuum at 100 °C to yield white
TiO
2
powder. Later, this powder is subjected to different
thermal and chemical treatments for the synthesis of
crystalline or functional TiO
2
nanoparticles. Figure 2
demonstrates the sol–gel process for the synthesis of
TiO
2
nanoparticles.
3 RESULTS AND DISCUSSION
3.1 Characterization
The surface characteristics of the uncoated bamboo
fibre and Ni-P coated bamboo fibre are shown in Fig-
ure 3. The surface of the bamboo fibre has a satiny ap-
pearance and clean texture, as shown in Figure 3a.How -
ever, there are many impurities on the surface, making
the plating process more time-consuming. Hence, metha-
nol, acetone and NaOH solutions are utilised to remove
the impurities from the bamboo-fibre substrate. The
bamboo-fibre surface is activated with palladium chlo-
ride, ensuring a better coating on the entire surface. Ini-
tially, the bamboo fibre is coated with Ni-P using the
bath composition for plating mild steel, described by
Elansezhian et al.
29
and presented in Table 2. This con-
centration is used to test the electroless Ni-P coating on
the bamboo fibre. As an electroless bath decomposes in a
very short period without a proper uniform coating over
the surface, the coating of bamboo fibre (BF) using this
bath composition is extremely challenging. As a result of
the chemical concentrations, operating temperature and
the potential of hydrogen (pH) values for the electroless
bath are adjusted with a proper coating on the surface
based on trial and error.
Finally, the suitable bath composition for proper BF
plating is determined, as shown in Table 3. A field emis-
sion scanning electron microscope (FESEM) image of
the bamboo fibre plated with Ni-P is seen in Figure 3b
M. GANAPATHY, E. RASU: INVESTIGATION OF Ni-P COATED BAMBOO FIBRE/NANO-TiO2 ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 525–531 527
Figure 2: Schematic representation of the synthesis and functionalization of TiO
2
nanoparticles

at a 200× magnification and another image at a 500×
magnifications is shown in Figure 3c. The Ni-P deposi-
tion over the BF is achieved with a uniform, thick and
unbroken structure, as illustrated in Figure 3b. The Ni-P
particles on the substrate are silvery grey. In addition, a
considerable number of Ni-P particles are evenly distrib-
uted across the entire surface of the BF and are securely
bonded to it, as seen in Figure 3b.The structure of the
Ni-P particles is clearly shown to be oblate, as seen in
Figure 3c.
Table 2: Electrolyte-bath solution components
Chemical elements in the EN bath
Bath components
in EN (g/L)
Nickel sulphate as the nickel source 32
Sodium hypophosphite as the reducing
agent
45
Tri-sodium citrate as the stabilizer 20
Ammonium chloride as the complex
agent
40
Table 3: Electrolyte bath solution for proper coating determined on
the basis of Table 2
Chemical elements in the EN bath
Bath components
in EN (g/L)
Nickel sulphate as the nickel source 45
Sodium hypophosphite as the reducing
agent
50
Tri-sodium citrate as the stabilizer 40
Ammonium chloride as the complex
agent
55
3.2 Morphological properties of the composite
The TiO
2
nanoparticles distributed into the bamboo
fibre-reinforced matrix material are shown in Figure 4a.
This figure shows a FESEM image with a varied
nanoparticle content that correlates well with the me-
chanical tests. When compared to the uncoated compos-
ite sample, Figure 4a clearly shows that the reduction in
the rough lines suggests that the nanoparticles are spread
equally within the fibre-reinforced matrix. The
pulled-out fibre and the surrounding matrix are separated
by a large void in Figure 4b. This shows that the neat
uncoated composite has poor interfacial adhesion. Fig-
ure 4c shows the components that are adhered effec-
tively, where the nanoparticles stimulate an increase in
the specific surface area to improve interfacial bonding.
Clumps arise when the amount of nanoparticles added
exceeds a particular threshold. This is due to the agglom-
erates that become weak areas when loaded. Figure 3d
clearly shows the agglomeration of the nanoparticles.
These findings are consistent with those obtained with
tensile testing.
3.3 EDAX analysis on the bamboo fibre
EDAX spectroscopy of the Ni-P plating of the BF is
shown in Figure 4 where we can clearly see a set of
strong peaks on the curve indicating the deposition of
Ni-P particles on the substrate. According to the EDAX
analysis of Ni-P/BF, the concentration of the Ni-P parti-
cles over the bamboo-fibre substrate includes about
91.36 w/% of nickel and 8.53 w/% of phosphorus. The
FESEM image and EDAX spectrum indicate the pres-
ence of the Ni-P particles, effectively coating the entire
surface of the bamboo-fibre substrate after the electroless
coating technique has been successfully used. Daramola
et al.
30
obtained a similar outcome for long-bamboo-fibre
bundle/PLA composites.
M. GANAPATHY, E. RASU: INVESTIGATION OF Ni-P COATED BAMBOO FIBRE/NANO-TiO2 ...
528 Materiali in tehnologije / Materials and technology 56 (2022) 5, 525–531
Figure 4: FESEM images of the polymer composite with the Ni-P
coating and nanoparticles: a) 0.5 w/%, b) 1 w/%, c) 1.5 w/%, d) 2 w/%
of nano-TiO
2
Figure 3: FESEM images: a) neat bamboo fibre without the coating, b) and c) Ni-P coated fibre at 200×, c) Ni-P coated fibre at 500×

3.4 Thermogravimetric analysis (TGA)
The thermograms of various hybrid bamboo-fibre
composites are clearly shown in Figure 6. A thermo-
gravimetric analysis was carried out to evaluate the ther-
mal stability of the PMBF composites at high tempera-
tures. The results show that when the Ni-P coated BF is
utilised as reinforcement, the thermal stability of the
polyester composite is increased. It also indicates that a
higher concentration of TiO
2
nanoparticles, as the rein-
forcement in the polyester composite, improves the ther-
mal stability, which is confirmed by the experiment re-
sult.
30
During the thermal investigation of the polyester
composite material, three different phases of degradation
are identified, as shown in Figure 6. The beginning of
decomposition is very slow due to the presence of a
small amount of moisture that evaporates, and it lasts up
to 300 °C. In the thermogravimetric testing, this is re-
ferred to as the initial stage of decomposition. During the
second stage, the hybrid composite degrades rapidly,
with over 85 % of the composite material degraded in the
case of the coated BF-reinforced composite. In this stage
of the coated bamboo fibre composite, the starting and
finishing temperatures are 300 °C and 425 °C,
respectively. If the Ni-P coated BF is utilised as the rein-
forcement, the starting temperature tends to rise, and this
trend continues as the concentrations of the TiO
2
nano-
particles and Ni-P/BF reinforcement increase. The end
temperature of this stage also increases significantly,
from 425 °C to around 485 °C for 1.5 w/% of TiO
2
nanoparticle and 13.5 w/% of Ni-P/BF. This happens due
to increased adhesion force and better interfacial bond-
ing between the added nanoparticles with the matrix ma-
terial and the nickel phosphorus-coated BF. As a result,
the temperature at which the degradation occurs
rises.
31–33
In this stage, the temperature is high because
the composite material is hardened.
34,35
The residual
stage is the last step. For the polyester hybrid composite
containing 1.5 w/% of nanoparticles, a maximum residue
of 60 % is left over when the nanoparticles are added to
the composite and the temperature resistance increases.
3.5 Dynamic mechanical analysis
For polymer composites, the dynamic mechanical
analysis (DMA) is increasingly being utilised to analyse
the mechanical properties of a composite material sub-
jected to dynamic loading conditions. It is also utilised to
investigate the polymer chain mobility and interfacial
bonding between the polyester matrix, TiO
2
nano-
particles and coated or uncoated bamboo fibres in com-
posites. The dynamic mechanical behaviour of a polyes-
ter hybrid nanocomposite depends on different factors
such as filler concentration, fibre loading, resin
wettability, reinforcing material orientation and ma-
trix/reinforcement interfacial area.
3.6 Storage modulus
The storage modulus is the most crucial parameter
for determining the load-carrying capacity of polymer
composites. Figure 7 displays the storage modulus of the
M. GANAPATHY, E. RASU: INVESTIGATION OF Ni-P COATED BAMBOO FIBRE/NANO-TiO2 ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 525–531 529
Figure 6: Temperature vs. mass loss (w/%) plot of the polyester/Ni-P
BF nanocomposites
Figure 5: EDAX spectrum for the Ni-P coated bamboo fibre
Figure 7: Storage modulus vs. temperature plot for the polyester
nanocomposites

composites with different compositions at room tempera-
ture. The value of storage modulus E1 increases when
TiO
2
nanoparticles are added. For the polyester compos-
ite with 1.5 w/% of nanoparticles the maximum storage
modulus is determined to be 80 % of the matrix material.
This is due to an increase in the stiffness of the polyester
composite and a wide area of interfacial interactions cre-
ated by adding TiO
2
nanoparticles. The nanoparticles re-
duce the mobility of the polyester matrix, leading to an
increased storage modulus.
36,37
This is also most likely
due to the increased matrix stiffness provided by the sup-
port of Ni-P/BF, allowing a better stress transfer at the
matrix/bamboo fibre interface. The tensile strength of the
sample of the coated composite with 1.5 w/% of
nanoparticles has a higher storage modulus. The storage
modulus is increased mostly due to the excellent disper-
sion of the nanoparticles and Ni-P/BF.
3.7 Damping factor (tan  )
The damping factor is evaluated from the ratio of
storage modulus and loss of modulus. The damping fac-
tor of a material determines the viscoelasticity of a poly-
ester matrix composite. The peak value of tan! is used
to calculate the glass transition temperatures, T
g
,ofthe
uncoated polyester composite and other samples. Fig-
ure 8 shows that the reinforcement with coated BF and
TiO
2
nanoparticles raises the value of T
g
. The T
g
value for
the uncoated polyester composite is 85 °C, while the T
g
value of the composite including 13.5 w/% of the coated
fibre and 1.5 w/% of the TiO
2
nanoparticles reaches
91.3 °C. Figure 8 shows the tan! values for all the com-
posites. The viscoelastic properties of the polyester-ma-
trix composite is increased due to the addition of
nanoparticles and coated bamboo fibre so that the poly-
mer composite can withstand higher temperatures. The
maximum value of T
g
is raised at the optimum loading of
the coated fibre and nanoparticles.
4 CONCLUSIONS
Bamboo fibres are coated with nickel-phosphorous
using the electroless plating method and trial and error
method. The presence of nickel-phosphorus particles
over the entire surface of the bamboo fibre indicated by
spherically shaped bubbles is shown on FESEM images.
Polyester composites with the reinforcing bamboo fi-
bre that can be coated or uncoated, and titanium oxide
nanoparticles were developed using a compression
moulding process and various concentrations. An exfoli-
ated structure of the polyester-matrix nanocomposites
was revealed using an XRD analysis. The polyester
nanocomposite material with an addition of 1.5 w/% of
titanium oxide nanoparticles had stable thermal proper-
ties and a high residual content.
The storage modulus (E1) of the polymer matrix rein-
forced with coated bamboo fibres and 1.5 w/%. of nano-
particles was also high. Values of the storage modulus
and thermal temperature of 3.96 × 10
4
MPa and 91.3 °C
were obtained with 1.5 w/% of titanium oxide nano-
particles. The FESEM result determined the surface
properties of the composite.
The coated bamboo fibre and polyester matrix exhib-
ited effective interfacial bonding with the nanoparticles.
Finally, the experimental result showed that the mome-
chanical and dynamic mechanical properties of the poly-
ester matrix reinforced with the coated bamboo fibre and
nanoparticles allow excellent bonding as compared to the
composite including the polyester matrix reinforced with
the uncoated bamboo fibre.
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M. GANAPATHY, E. RASU: INVESTIGATION OF Ni-P COATED BAMBOO FIBRE/NANO-TiO2 ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 525–531 531