J N CS

Journal of Nepal Chemical Society January 2021, Vol. 42, No. 1, 45-50
ISSN: 2091-0304 (print)
DOI: https://doi.org/10.3126/jncs.v42i1.35328
RESEARCH ARTICLE

Green Synthesis of Zirconia (ZrO2) Nanoparticles Using Curcuma

Longa Extract and Investigation of Compressive Strength of Epoxy
Resin (EP)/ZrO2 Nanocomposites
Manish Bishwokarma1, Arun Bhujel1, Manish Baskota1, Rajesh Pandit*1
1
Department of Chemistry, Tri-Chandra Multiple Campus, Tribhuvan University, Kathmandu, Nepal
*Corresponding E-mail: [email protected]
(Received: March 30, 2020; Revised: January 20, 2021; & Accepted: January 20, 2021)

Abstract
Zirconia (ZrO2) nanoparticles are polymorphic materials having a wide range of applications. It can be synthesized
via green as well as chemical synthesis methods. In this work, ZrO2 nanoparticles were synthesized by the
green method using Curcuma longa extract. Curcuma longa extract was prepared using the standard method.
The synthesized ZrO2 was characterized by the X-ray diffraction (XRD) analysis and Fourier transform infra-
red (FTIR) spectroscopy for their structural and size analysis. The analysis of the XRD pattern of ZrO2 showed
the tetragonal phase structure and the size was calculated using the Debye Scherrer equation which was about
35 nm. The FTIR spectra analysis showed a broad absorption peak particularly at about 774 cm-1 and about 499
cm-1 correspondings to Zr-O2-Zr asymmetric and Zr-O stretching modes, respectively. The characterized ZrO2
nanoparticles were used for the preparation of epoxy resin/ZrO2 nanocomposites. The compressive strength of
pure epoxy resin and epoxy resin/ZrO2 nanocomposites were measured by a compressive strength tester and
the result indicates the high amount of zirconia showed the less compressive strength in nanocomposites.
Keywords: Zirconia, green synthesis, epoxy resin, compressive strength, nanocomposite

Introduction at the elevated temperature and cooled to the area

Nanotechnology is employed for the assembly, temperature, the quantity expansion occurs from cubic
manipulation, and use of materials ranging in to tetragonal. This volume change causes large stress
nanometers [1,2]. Nanomaterials are one in the entire that results in cracking. Thus, bulk zirconia cannot be
foremost component of the nanotechnology and wide used at elevated temperatures [6].
class of materials that has particulate substances Zirconia nanoparticles will be synthesized employing
which have one dimension from 1 to100 nm in size various methods like sol-gel [7], combustion [8],
[3]. There are several kinds of nanoparticles such hydrothermal [9], co-precipitation [10], and green
as metal, semi-conductor, and bio, out of those [11]. The green method is greatly employed in
nanoparticles, zirconia (ZrO2) is polymorphic, and synthesizing the nanoparticles using plant extract
advanced ceramic material having useful optical, using from leaves, roots, barks, etc. [11]. The extract
electrical, thermal, hardness, and other characteristics. may contain the reducing agent and some compounds
Its molar mass is 231.891 g/mol, the freezing point is act as a capping agent such as flavonoids, terpenoids,
2715°C and the boiling point is 4300°C [4]. reducing sugars, etc. [12].
It is further employed in different industries as a Likewise, Zirconia nanoparticles are used as fillers in
refractory material, cutting tools, limit coating, polymeric nanocomposites to boost their strength and
catalyst support, sensors, fuel cells, optical devices, stiffness. However, because of the high aggregation
metallic glasses [5]. ZrO2 exists in three crystal tendency of nanoparticles, structural defects occur in
phases i.e. monoclinic phase is clinically stable at nanocomposites, leading to a decreased possibility
gas pressure, the tetragonal phase exists within the of mechanical property improvement [13]. Liquid
temperature range of 1100-2370℃ and therefore the epoxy resin is employed as structural adhesives
cubic phase is found above 2370℃. When it is used and coating material because of its low cost, good
workability, volatile compound free eco-friendliness,
©Nepal Chemical Society https://www.nepjol.info/index.php/JNCS
45
Journal of Nepal Chemical Society, January 2021, Vol. 42, No.1 M. Bishwokarma et al., 2021

good adhesion, heat resistance electrical insulation, it. Then the mixture was boiled for a half-hour with
chemical resistance, and weather resistance. However, continuous stirring by a magnetic stirrer. Then the
the most epoxy resin needs additional fillers to boiled mixture was filtered carefully and therefore the
improvise mechanical and thermal properties thanks resulting filtrate was the extract.
to their inherent brittleness and industrial requirement. Synthesis of Zirconia nanoparticles
Zirconia nanoparticles are used as fillers to enhance About 50 mL of 0.1 M zirconyl chloride octahydrate
their strength and stiffness. Organic modifiers are [ZrOCl2.8H2O] was taken in a 250 mL beaker and
accustomed to progress interfacial bonding between 10 mL of prepared turmeric extract was added to
fillers and resin [14]. it. The resulting solution was heated at 80°C with
Polymer nanocomposite (PNC) comprises polymer or continuously stirred by a magnetic stirrer for two
copolymer with nanoparticles or nanofillers dispersed hours. Then the final solution was kept undisturbed
in the polymer matrix. The PNC’s belong to the for two days and brownish crystals of zirconia
category of the multiple-phase system (MPS). These nanoparticles were obtained.
systems require controlled mixing, stabilization of
achieved dispersion, the orientation of phase, and Synthesis of epoxy resin/ZrO2 nanocomposites
compounding strategies for all MPS including PNC [Bulk adhesives]
[15]. Microhardness property was improved in First of all, 35 mL of pure epoxy and hardener were
epoxy resin/SBS/layered silicate (LS) and boehmite mixed in plastic propylene mold. For this, the mixed
nanocomposite due to dispersion of layered silicate content was pre-cured for 12 hours at 70°C and
and boehmite nanofillers [16]. Recently, it was found post-cured for 12 hours at 120°C. Then, epoxy/ZrO2
that the introduction of inorganic nanoparticles nanocomposites were prepared with different wt.-%
to polymeric adhesives at a low percentage may (i.e 1, 3, 5 and 10 wt.-%) of zirconia. The various
cause the advance of shear resistance of structural wt.-% of zirconia nanofiller was mixed with 35 mL
joints. Only some studies of epoxy-ZrO2 composites of epoxy resin and hardener 25 min with continuous
associated with their morphology and mechanical stirred with a magnetic stirrer. A similar curing process
properties are reported and that they show that the was followed to the epoxy/ZrO2 nanocomposite as
mechanical resistance and toughness of synthetic Then the solutions were pre-cured at 70°C for 12 hrs
resin are improved by increasing the content of ZrO2 and post-cured at 120°C for 12 hrs.
nanoparticles. This can be attributed to the fact that
ZrO2 nanoparticles have a way higher strength than c. Characterization
epoxy matrix alone and to the nice bonding between The synthesized ZrO2 nanoparticles and EP/ZrO2
filler and matrix [17]. In this paper, the herbaceous nanocomposites were then analyzed to understand
plant extract is employed for the synthesis of zirconia their properties and behavior. The characterizations of
nanoparticles, and therefore the compressive strength the prepared samples were applied by powder X-ray
of epoxy resin (EP)/ZrO2 nanocomposites is discussed diffraction (XRD) and Fourier transform infrared
for mechanical purposes. spectroscopy (FTIR). Average particle size was
determined from the XRD pattern by calculating the
Materials and Methods value of full width at half maxima (FWHM) of peak
a. Materials after removing instrumental broadening using Debye-
Curcuma longa was collected from the local market
Scherrer formula [18].
and grinded to a fine powder for the preparation of its
extract. Zirconyl chloride octahydrate (ZrOCl2.8H2O),
(98% purity) was manufactured by LOBA Chemie
Pvt. Ltd, Mumbai, India. Epoxy and hardener were
where λ is the wavelength of X-ray, is full width at
marketed from a local supplier in Kathmandu. All
half maximum (FWHM) of the most intense XRD peak
the reagents used were of analytical grades and used
expressed in radians and is Bragg’s diffraction angle.
without further purification.
The crystalline structure of ZrO2 nanoparticles was
b. Methods confirmed from XRD peaks [18]. The experiment
Preparation of Curcuma longa extract was carried out using Rigaku ultima IV model XRD
About 20 g of turmeric powder was weighed and kept diffractometer employing CuKα radiation (λ =
in a 500 mL beaker. 200 mL of water was added to 0.15406 nm).

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Journal of Nepal Chemical Society, January 2021, Vol. 42, No.1 M. Bishwokarma et al., 2021

FTIR is an analytical technique used to identify 3000

organic, polymeric, and in some cases inorganic Z r O 2 n a n o p a r tic le s
materials. The FTIR analysis uses infrared light to 2500

scan test samples and observe chemical properties

[19]. The characterization of synthesized nanoparticle 2000

(101)
and nanocomposites were done using FTIR analysis

Intensity
1500
and the instrument used for characterization was IR-

(110)
Prestige-21 (Shimadzu) within the range of 500 cm-1 1000
to 5000 cm-1.

(202)

(313)

(222)
500
d. Compressive strength test
Compressive strength is the resistance of a material 0
to breaking under compression which is the capacity 0 10 20 30 40 50 60 70 80 90
2 (degree)
of a material to withstand loads tending to reduce
size. Compressive strength is an important aspect
in the design of materials or structures and is a vital 2000

aspect in determining the load-carrying capacity of

the structures [20]. A compressive strength test is a
mechanical test measuring the amount of compressive
Intensity
1000

load, a material can bear before fracturing. Normally

it is determined by the casting and testing of material
specimens in the laboratory. The compressive 0
strengths of various nanocomposites were measured
using a universal compression testing machine in the
laboratory [21].
30 40 50
Results and Discussion 2 (d e g re e s )

Size and phase analysis using XRD pattern Figure 1: (a) XRD pattern of ZrO2 nanoparticle synthesized from
The phase purity and crystalline nature of the 0.1M ZrOCl2.8H2O and (b) corresponding Lorentzian fitting
synthesized zirconia nanoparticle samples were synthetic method using 0.1 M ZrOCl2.8H2O and
analyzed using XRD diffraction. The diffraction Curcuma longa extract within the range of 500 cm-1 to
pattern of synthesized zirconia nanoparticles is shown 5000 cm-1 is shown in Figure 2. Thus prepared zirconia
in Figure 1(a). The peaks were obtained at a 2θ value nanoparticle using 0.1M ZrOCl2.8H2O and Curcuma
of 28.2 (101), 40.55(110), 50.66 (202), 59.36 (313), longa extract had broad absorption peak particularly
66.65 (222) which are indexed to tetragonal ZrO2 at about 774 cm-1 and about 499 cm-1, corresponding
phase compared to JCPDS card number 081-1544 to Zr-O2-Zr asymmetric and Zr-O stretching modes
[10]. The size of the nanoparticles was calculated via respectively, which confirms the formation of ZrO2
the data obtained from Lorentzian fitting spectra of phases based on the works of literature, according to
the corresponding samples given in Figure 1(b). which the respective absorption band are 740 cm-1 and
With the help of Lorentzian fitting and FWHM 500 cm-1, respectively [22].
calculation using the Debye-Scherer equation, the The significant peaks representing the functional
particle size was calculated to be 35 nm. groups present in ZrO2 are further shown in Table 1.
Therefore, the synthesized zirconia nanoparticle was Thus the FTIR spectra confirm that the zirconia was
successfully characterized using XRD diffraction successfully synthesized which indicates from the
which indicated that the prepared ZrO2 nanoparticles peaks at 499 cm-1 and 774 cm-1 and other functional
were tetragonal phase structures having an average groups from the Curcuma longa extract.
size of 35 nm.
Functional group analysis of epoxy resin (EP)/
Structural analysis of zirconia nanoparticles using ZrO2nanocomposites
FTIR spectra The FTIR spectra of epoxy resin (EP)/ZrO2
The FTIR spectra of the synthesized zirconia nanocomposites prepared by mixing the various filler
nanoparticles which were prepared using the green

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Journal of Nepal Chemical Society, January 2021, Vol. 42, No.1 M. Bishwokarma et al., 2021

110 absence of a broad absorption band at around 764

Z ir c o n ia N a n o p a r tic le
100 cm-1 and about 499 cm-1 referring to the absence of
Zr-O2-Zr asymmetric and Zr-O stretching modes and
90
absence of ZrO2 phases in the pure epoxy composite.
T r a n s m itta n c e (% )

80 Whereas in the study of epoxy resin (EP)/ZrO2

1 9 9 0 .5 4
2 0 6 7 .6 9
(1wt.-%) nanocomposite and epoxy resin (EP)/ZrO2

1 3 4 2 .4 6
70
(5wt.-%) nanocomposite, the broad absorption band

1 4 3 5 .0 4
60 is seen at 763 cm-1-455 cm-1 and 771 cm-1-455 cm-1

1 6 2 0 .2 1

7 7 4 .0 5
50
respectively. Thus the presence of the ZrO2 phase is
3 1 9 4 .1 2

confirmed [22]. The various functional groups present

40
4 9 9 .1 3
within the nanocomposites prepared using various
30
amount in wt.-% of ZrO2 nanoparticles and epoxy
5000 4000 3000 2000 1000 resin is shown in Table 2.
W a v e n u m b e r (c m -1 ) The FTIR spectra show that the epoxy resin and
Figure 2: FTIR Spectra of zirconia nanoparticle prepared
zirconia nanoparticles were almost mixed up with
using 0.1 M ZrOCl2.8H2O and Curcuma longa
each other which were indicated by the peak presence
in the corresponding wavelength.
Table 1: Functional groups present in zirconia nanoparticles Measurement of compressive strength
Wavelength (cm-1) Group Compounds class
Compressive strength test or mechanical test measures
the maximum amount of compressive load a material
3194.12 O-H stretching alcohol can bear before fracturing. The prepared zirconia
2067.69 N=C=S stretching isothiocyanate nanoparticles of different amounts were mixed
1620.21 C=C stretching conjugated alkene
with epoxy resins and hardeners. Thus prepared
1435.04 C-H bending alkane
composite was compressed between the platens of the
contents of zirconia nanoparticles and epoxy resin/ compression testing machine having a factor of 3.7 by
hardener were analyzed by FTIR Spectroscopy. The a gradually applied load. The obtained data measured
FTIR spectra of various nanocomposites were then by universal compression testing machine (UCT) is
comparatively studied. The comparative analysis of represented in Table 3. The dimensions of the various
EP/ZrO2 nanocomposites is shown in Figure 3. nanocomposites' bulk were more or less similar.
The comparative study of nanoparticles shows the The compressive strength of the nanoparticles
Table 2: Significant peak representing functional groups present in the Epoxy resin and its nanocomposites
Wavelength (cm-1)
Pure EP EP/ZrO2Nanocomposite EP/ZrO2Nanocomposite
Group Compound class
(1% ZrO2) (5% ZrO2)
3371.57 3379.29 3356.14 N-N stretching Primary amine
2970.38 2962.66 2962.66 N-H stretching Amine salt
2870.08 2870.08 2870.08 C-H stretching Alkane
- 1782.13 - C=O stretching Conjugate acid
anhydride
1604.77 1604.77 1604.77 C=C stretching Conjugated alkene
1512.19 1504.48 1504.48 N-O stretching Nitro compound
1458.18 1411.89 - O-H bending Carboxylic acid
1373.32 1357.89 1381.03 O-H bending Phenol
1242.16 1234.44 1234.44 C-N stretching Amine
1050.29 1033.85 1026.33 S=O stretching Sulfoxide
825.53 825.53 825.53 C=C bending Alkene
662.00 555.50 555.50 C-Cl stretching Halo compound

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Journal of Nepal Chemical Society, January 2021, Vol. 42, No.1 M. Bishwokarma et al., 2021

Table 3: Compressibility strength of Pure EP and EP/ZrO2 nanocomposite

Cubes Pure EP 1% ZrO2 3% ZrO2 5% ZrO2 10% ZrO2
Length 21.78 20.57 20.58 20.78 20.74
Dimension (cm) Breadth 21.44 20.18 21.50 22.12 21.10
Height 16.93 21.13 21.44 22.56 20.00
Weight (g) 8.88 9.66 9.89 10.76 9.84
Breaking load (g) 408 510 530 540 515
Compressibility strength (g/cm2) 1509.6 1887 1961 1998 1905.5

increases on increasing the EP and ZrO2 nanoparticles nanocomposite with resorcinol formaldehyde resin
ratio as shown in Figure 4. This shows that epoxy resin/ [23]. The reasons for such deviation can be known
zirconia nanocomposites have higher compressive by the detailed study of nanocomposites. The internal
strength than pure epoxy. It means that a significant morphology must be studied via TEM. Hence for
improvement has been achieved after the addition of further information TEM must be done. Overall, the
Zirconia nanoparticles to epoxy resin. Such results compressive strength of EP/ZrO2 nanocomposites
are due to the aggregation of zirconia nanoparticles. improved after adding zirconia nanoparticles at any
weight fraction.
Conclusion
3 3 5 6 .1 4

The implementation of a novel greener approach for the

2 8 7 0 .0 8

5 % Z rO 2+ e p
1 5 0 4 .4 8

biogenic synthesis of zirconium dioxide nanoparticles

7 7 1 .5 3

4 5 5 .2 0
T r a n s m itta n c e (a .u .)

using Curcuma longa has been successfully carried

1 7 8 2 .2 3

out. The synthesis method is faster, economical,

2 9 6 2 .6 6

1 6 0 4 .7 7

2 1 % Z rO + ep
7 6 3 .8 1

greener, non-toxic since this method avoids multiple

4 5 5 .2 0

reaction steps, conventional energy sources, and

harmful chemicals. FTIR spectra indicated that
3 3 7 1 .5 7

2 8 7 0 .0 8

zirconia nanoparticles and their nanocomposites

1 3 7 3 .3 2

pure ep
8 2 5 .5 3

with epoxy resin were successfully synthesized. The

5000 4500 4000 3500 3000 2500 2000 1500 1000 500
W a v e n u m b e r (cm-1) XRD pattern clearly showed that synthesized zirconia
Figure 3: FTIR spectra of pure EP and EP/ZrO2 nanoparticles were tetragonal structure and the size
nanocomposites (1% and 5% by wt. of zirconia nanoparticles) of the nanoparticle was found to average 35 nm. The
FTIR spectra of nanocomposites showed the presence
The compressive strength of nanoparticles increased of various compounds. Compression tests on the
up to Zirconia nanoparticles in epoxy nanocomposite
nanocomposites bulk adhesives indicated that the
and then decreased beyond that. This may be because
addition of zirconia nanoparticles to epoxy resin bulk
of the effect of agglomeration of a higher percentage
of nanoparticles on the crosslinking of the epoxy resin. increased the compressive strength. However, the
A similar result was also recorded in the extraction higher amount (about 10%) of zirconia nanoparticles
and characterization of chitosan and preparation of could not favor increasing the compressive strength in
epoxy resin/ZrO2nanocomposite.
Acknowledgments
2000

Authors acknowledge the Department of Mechanical

and Engineering Testing Laboratory, Pulchowk
C o m p r e s s iv e s tr e n g th

Campus, Lalitpur for their help to characterize the

1500 compressive strength test.
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