Journal of Molecular Structure 1227 (2021) 129543

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Journal of Molecular Structure

journal homepage: www.elsevier.com/locate/molstr

Novel NiO nanoparticles via phytosynthesis method: Structural,

morphological and optical properties
Harits A. Ariyanta, Tribidasari A. Ivandini, Yoki Yulizar∗
Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Indonesia, Depok, 16424, Indonesia

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

Article history: Nickel oxide nanoparticles (NiO NP) were successfully fabricated by phytosynthesis method using Agera-
Received 9 August 2020 tum conyzoides L leaf extracts (ACLE) in the various extract fractions such as water (NiO-W), methanol-
Revised 28 October 2020
water (NiO-MW) and n-hexane (NiO-Hx). Each extract fraction produced NiO NP with different structures,
Accepted 28 October 2020
bandgap energies and morphologies due to the effect of calcination temperature during the phytosyn-
Available online 29 October 2020
thesis and biomolecules dissolved in each fraction. NiO NP was characterized by EDS and FTIR. Specifi-
Keywords: cally, the structural, optical and morphological properties of NiO NP were confirmed by XRD, UV-Vis DRS
Nickel oxide nanoparticles and SEM, respectively. As a result, NiO-W, NiO-MW, NiO-Hx showed the morphologies of flakes-shaped,
Ageratum conyzoides L. a porous foam-like and spherical, respectively. Meanwhile, various calcination temperatures caused the
Extract fraction structural change of NiO NP. Additionally, the optical band gap of NiO-W, NiO-MW, and NiO-Hx were
Calcination temperature 3.77; 3.53 and 3.32 eV, respectively, by the increase of crystallite size to 20.47 nm; 23.09 nm and
Green synthesis
23.43 nm, respectively.
Phytosynthesis
© 2020 Elsevier B.V. All rights reserved.

1. Introduction nanoparticles, nickel oxide (NiO) is commonly used as photocata-

The green synthesis of nanomaterials, such as metal and metal
oxide nanoparticles, is still widely developed by considering the
reactivity, toxicity, and low-cost preparation compared to the con-
ventional chemical-physical methods [1–3]. The aforementioned
method offers an attractive, environmentally friendly, and inexpen-
sive alternative by involving biological systems such as plant, al-
gae, fungi, bacterium and biological molecules [4]. Plant is the best
candidate for nanomaterial synthesis, which is well-known as phy-
tosynthesis, compared to other biological systems due to its high
reaction speed, high availability, simple and safe preparation [5–
7]. The plant contains biomolecules (proteins, amino acids, organic
acid, vitamins) and secondary metabolites (flavonoids, alkaloids,
polyphenols, terpenoids, heterocyclic compounds, polysaccharides)
[4–6,8–11], which act as reducing and capping agent [7,8,12,13],
chelating agent [8] as well as a weak base source [10,11] in the
synthesis of both metal and metal oxide nanoparticles. Moreover,
each plant extract fraction contains different biomolecules and sec-
ondary metabolites [14].
On the other hand, the calcination temperature induces the
growth of nanoparticle crystals, resulting in the different struc-
ture and particle size [15]. Among the various types of metal oxide
∗
Corresponding author.
E-mail address: yokiy@sci.ui.ac.id (Y. Yulizar).
lyst, electrocatalyst, supercapacitor, and battery [16–20] due to its
good electron transfer capabilities. Also, NiO is a p-type semicon-
ductor with a wide bandgap range of 3.45 - 4.00 eV, depending
on its defects nature and density [21,22]. Therefore, NiO possesses
unique properties due to their crystal structure, morphology, and
particle size.
Many studies on nanoparticle phytosynthesis have been con-
ducted. However, the effect of extract fractions and calcination
temperature on the structural and morphological properties of
nanoparticles have yet to be reported. This work focuses on the
NiO NP fabrication via a phytosynthesis method using Ageratum
conyzoides L. leaf extract (ACLE) with various extract fractions
and calcination temperatures. Ageratum conyzoides L. contains sec-
ondary metabolites of alkaloids, tannins, phenols, saponins, and
flavonoids [10] with alkaloids content of 9.4 % [23] as a weak
base source. The previous researches of NiO phytosynthesis were
reported by using toxic chemical base sources such as ammo-
nium hydroxide [24], mono-ethanol amines [16] and sodium hy-
droxide [18]. In this study, ACLE was used in the various extract
fractions such as water (ACLE-W), methanol-water (ACLE-MW)
and n-hexane (ACLE-Hx) with a calcination temperature range of
50 0–80 0 °C. The structural and morphological properties of NiO
NP were analyzed by XRD and SEM. Furthermore, the charac-
terization was performed by using EDS, UV-Vis DRS and FT-IR
spectroscopy.

https://doi.org/10.1016/j.molstruc.2020.129543
0022-2860/© 2020 Elsevier B.V. All rights reserved.
H.A. Ariyanta, T.A. Ivandini and Y. Yulizar
2. Experimental section
2.1. Materials
Ageratum conyzoides L. leaf was obtained from Biofarmaka
IPB, Bogor, West Java, Indonesia. Nickel nitrate hexahydrate
(Ni(NO3 )2 .6H2 O) was purchased from Merck, Germany. Methanol
and n-hexane were used without further purification. Double dis-
tilled water used in this research was purified with Millipore
Direct-Q® 5 UV.
2.2. Preparation of ACLE
Ageratum conyzoides L. leaf was washed, dried, and mashed
into powders. ACLE-W and ACLE-Hx were prepared by macerating
50 g of powders in 250 mL distilled water and n-hexane (96%),
respectively, for 7 days by a continous stirring. Afterwards, the
filtrate was filtered by using Whatman no. 40 filter paper and
stored at 4 °C. The result was applied for NiO NP phytosynthesis.
For the ACLE-MW preparation, 50 g powders were macerated in
methanol. Subsequently, the filtrate was further fractionated in n-
hexane with a volume ratio of 1:1. The result was evaporated and
dissolved into 100 mL distilled water. Finally, the obtained ACLE-
MW was stored at 4 °C for NiO NP phytosynthesis.
2.3. Phytosynthesis of NiO NP
NiO NP was fabricated via phytosynthesis method through a
sol-gel process. Ni(NO3 )2 0.015 M was added in ACLE-W, ACLE-MW,
and ACLE-Hx, respectively, to produce 100 mL mixture with a vol-
ume ratio of 1:4. The ACLE-W and ACLE-MW sol were produced
by heating at 65 °C for 2 h. Meanwhile, ACLE-Hx sol was obtained
with high-speed stirring at 23,0 0 0 rpm. The sol was further heated
at 120 °C for 2 h and centrifuged to form gel. Finally, the gel was
dried, and calcined for 2 h at 50 0, 60 0, 70 0 and 800 °C to obtain
black powders of NiO NP, then labeled as NiO-(fraction) (calcina-
tion temperature), for example: NiO-W 500.
Fig. 1. FT-IR spectra of ACLE-W, ACLE-MW, and ACLE-Hx
2
Journal of Molecular Structure 1227 (2021) 129543
2.4. Materials characterization and analysis
FEI Quanta 650 scanning electron microscopy (SEM) and Ox-
ford instruments energy dispersive X-ray spectrometer (EDS) were
used to determine the morphology and elemental analysis. X-
Ray diffraction (XRD) technique using Miniflex 600-Rigaku X-
ray analytical instrument with a filtered Cu Kα radiation source
(λ = 1.54 Å) was used to analyze the structure phase. IR Prestige-
21 Shimadzu Fourier transform infra-red (FT-IR) spectroscopy was
used to investigate the functional groups. Shimadzu 2450 UV-
visible diffuse reflectance spectroscopy (UV-Vis DRS) was used to
determine the bandgap values.
3. Results and discussion
3.1. FT-IR Characterization
Functional groups in ACLE-W, ACLE-MW, and ACLE-Hx were an-
alyzed by using FT-IR to predict the content of secondary metabo-
lites which act as weak base sources and capping agents in NiO
NP phytosynthesis. Fig. 1 shows the FTIR spectra of ACLE-W, ACLE-
MW, and ACLE Hx.
The FT-IR spectrum of ACLE-W showed absorption bands at
3332, 1600, 1383, 1266, 1055, and 678 cm−1 , indicating the vibra-
tion of O-H stretching, N-H bending, C-C stretching, C-N stretching
and N-H wagging, respectively. For ACLE-MW, it possesses a simi-
lar spectrum to ACLE-W with new peaks at 2930 and 1148 cm−1 ,
indicating the vibration of C-H (sp3 ) stretching and C-N stretch-
ing. The O-H stretching vibrations in both ACLE-W and ACLE-MW
indicates the presence of flavonoids [9]. Meanwhile, the vibration
of N-H wagging and C-N stretching in ACLE-W and ACLE-MW indi-
cate the presence of alkaloid [25,26]. For ACLE-Hx, there was no vi-
bration of O-H stretching. However, a very strong vibration of C-H
(sp3 ) stretching was observed. Also, ACLE-Hx presented a vibration
of C-C stretching, indicating the presence of steroids [27]. More-
over, the appearance of N-H wagging and C-N stretching vibrations
are ascribed to the content of alkaloids in ACLE-Hx. Generally, FT-
IR result is presented in Table 1.
H.A. Ariyanta, T.A. Ivandini and Y. Yulizar Journal of Molecular Structure 1227 (2021) 129543

Fig. 2. The FTIR spectra of NiO-W, NiO-MW, NiO-Hx at calcination temperatures of 500 and 700 °C

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H.A. Ariyanta, T.A. Ivandini and Y. Yulizar Journal of Molecular Structure 1227 (2021) 129543

Table 1
The FTIR result of ACLE-W, ACLE-MW, and ACLE-Hx

Types of Wave-number
Vibration (cm−1 ) ACLE-W ACLE-MW ACLE-Hx
√ √
O-H stretching 3332 -
√ √
C-H (sp3 ) 2930 -
stretching
√ √
C=O stretching 1717 -
√ √ √
N-H 1600
bending
√ √ √
C-C stretching 1383
√ √ √
C-O stretching 1266
√ √
C-N stretching 1148 -
√ √ √
C-N stretching 1055
√ √ √
N-H 678
wagging

Fig. 3. FT-IR spectra of NiO-W, NiO-MW, and NiO-Hx

Fig. 2 shows FT-IR spectra of NiO with different extract frac-
tions at calcination temperatures of 500 and 700 °C. The typi-
cal absorption band of Ni-O stretching appeared at 430–490 cm−1
[11,15,28]. Also, the vibration of Ni-O stretching was shown at
around 450 cm−1 in NiO-W, NiO-MW and NiO-Hx. It can be seen
that NiO was successfully synthesized using ACLE in the various
extract fractions.
Moreover, the absorption band at 3332, 1600, 1055, and
678 cm−1 were ascribed to the vibration of O-H stretching, N-H
bending, C-N stretching and N-H wagging vibrations, respectively.
The O-H stretching vibration could indicate the remains of sec-
ondary metabolites of flavonoids, saponins, polyphenols [11] and
physical adsorption of H2 O from the atmosphere [15,28–30]. Mean-
while, the vibrations of N-H bending, C-N stretching and N-H wag-
ging could indicate the remains of alkaloids. Alkaloids play an im-
portant role as a weak base source [31–33] for NiO NP phytosyn-
thesis.
Fig. 3 shows the comparison FT-IR spectra of NiO-W, NiO-MW,
and NiO-Hx. FT-IR spectrum of NiO-W displays a strong absorption
band of alkaloid compared to NiO-MW and NiO-Hx. This allowed
the formation of NiO which was still mixed with the remains
of secondary metabolites. In addition, FT-IR spectrum of NiO-Hx
shows an incisive absorption band of Ni-O. It indicates that the
two-phase reaction system between ACLE-Hx and Ni2+ efficiently
acts in NiO-Hx phytosynthesis.
3.2. XRD characterization
XRD characterization was performed to determine the crystal
structure, purity, and phase of NiO-W, NiO-MW, and NiO-Hx. Fig. 4
presents the NiO diffraction patterns with various extract fractions
at calcination temperatures of 50 0, 60 0, 70 0 and 800 °C. XRD pat-
tern of NiO-W 500 showed a weak NiO crystalline phase as shown
in Fig. 4 (a). For NiO-W 600, the cubic crystalline phase was iden-
tified at 2θ of 37.2; 43.2; 62.8; 75.3; and 79.2o which indexed to
(111), (200), (220), (311) and (222) (JCPDS No. 00-047-1049). How-
ever, another peak was observed. It can be seen that the formed
NiO has lower purity. This result indicates that a high calcina-
tion temperature of NiO-W resulted the NiO with strong crystalline
phase
XRD pattern of NiO-MW 500 presented a weak crystalline
phase of NiO as shown in Fig. 4 (b). For NiO-MW 600, the cubic
crystalline phase was identified at 2θ of 37.2; 43.4; 62.8; 75.3 and
79.2o which indexed to (111), (200), (220), (311) and (222) (JCPDS
No. 00-047-1049). However, two other peaks were detected. Mean-
while, for NiO-MW 700, the diffraction pattern resulted in a single-
crystalline cubic phase of NiO. Table 2 displays the full width at
half maximum (FWHM) value decreases while the calcination tem-
perature is increased. This result indicates that the high calcination
temperature can form a single-crystalline phase of NiO-MW by the
increase of crystallite size due to the thermally promoted crystal-

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H.A. Ariyanta, T.A. Ivandini and Y. Yulizar Journal of Molecular Structure 1227 (2021) 129543

Fig. 4. (a) Diffraction patterns of NiO-W, (b) NiO-MW and (c) NiO-Hx at calcination temperatures of 50 0, 60 0, 70 0, 80 0 °C (d) the optimum calcination temperature for the
formation of NiO-W, NiO-MW and NiO-Hx

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H.A. Ariyanta, T.A. Ivandini and Y. Yulizar Journal of Molecular Structure 1227 (2021) 129543

Fig. 5. The indirect Eg determination of NiO-W (800 °C), NiO-MW (800 °C), and NiO-Hx (700 °C)

Fig. 6. SEM images of a) NiO-W, b) NiO-MW at calcination temperatures of 500 and 800 °C, c) NiO-Hx at calcination temperatures of 500 and 600 °C

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H.A. Ariyanta, T.A. Ivandini and Y. Yulizar Journal of Molecular Structure 1227 (2021) 129543

Fig. 7. EDS result of (a) NiO-W, (b) NiO-MW at calcination temperatures of 500 and 800 °C, (c) NiO-Hx at calcination temperatures of 500 and 600 °C

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H.A. Ariyanta, T.A. Ivandini and Y. Yulizar Journal of Molecular Structure 1227 (2021) 129543

lite growth [15,32]. The Debye-Scherer’s equation was applied to Table 2

The crystallite size of NiO NP from XRD pattern using
calculate the crystallite size of NiO NP [12,21]:
Debye-Scherer’s equation.
0.9 λ
D= Sample FWHM(°) Crystallite size(nm)
β cosθ
NiO-W 500 0.8673 10.4576
Where, Dis the crystallite size average, λis the wavelength of NiO-W 600 0.5656 15.5806
the X-rays (0.15406 Å), β is the FWHM and θ is the diffraction angle. NiO-W 700 0.4977 18.2786
NiO-W 800 0.4526 20.4689
In contrast to NiO-W and NiO-MW, XRD pattern of NiO-Hx
NiO-MW 500 0.7721 11.7005
500 °C exhibited single-crystalline NiO with cubic phase at 2θ of NiO-MW 600 0.4910 18.5000
37.2; 43.2; 62.8; 75.3 and 79.4o (JCPDS No. 00-047-1049) as shown NiO-MW 700 0.4907 19.0456
in Fig. 4(c). Therefore, calcination is not carried out at even higher NiO-MW 800 0.4032 23.0932
temperatures (800 °C). Furthermore, it can be seen that the higher NiO-Hx 500 0.5871 16.4164
NiO-Hx 600 0.4470 18.9404
the calcination temperature, the higher the intensity of diffraction NiO-Hx 700 0.3614 23.4293
peak which was marked by an increase of crystallite size. Fig. 4(d)
displays the diffraction pattern comparison of NiO-W, NiO-MW and
NiO-Hx with the optimum calcination temperature. NiO-W exhibits
a diffraction pattern of the typical peak of NiO at 800 °C. However, coordination complexes as ligands to result in different morpholo-
other peaks were detected. For NiO-MW, a single-crystalline NiO gies [37].
was systemically formed at 700 & 800 °C. Meanwhile, for NiO-Hx, EDS characterization was performed to determine the elemen-
a single-crystalline NiO was properly formed at 500 °C. This result tal composition in both NiO NP and ACLE [8]. Fig. 7 shows EDS
conforms with the FT-IR spectra, indicating that there were still the spectra of NiO-W, NiO-MW and NiO-Hx with distinct calcination
remains of secondary metabolites in NiO-W. temperatures.
Pure NiO cannot be formed in both NiO-W 500 and NiO-W 800
3.3. UV-Vis DRS characterization due to the presence of C, Mg, Si, K, Cl and Ca, which were naturally
derived from ACLE as presented in Fig. 7 (a). These results were in
UV-Vis DRS characterization was performed to estimate the good agreement with the results of both FTIR and XRD. However,
bandgap energy (Eg ) of NiO. The indirect Eg is converted from the the atomic compositions ratio of Ni and O on NiO-W 500 and NiO-
UV-Vis absorbance value through the following equation: W 800 increased from 16.9:34.7 to 25.5:36.1 (% At), which close to
the stoichiometric ratio of NiO. For NiO-MW 500, the EDS spec-
[α hv] = A(hv − Eg )
2
trum still presents the impurities, similar to the NiO-W 500. How-
where A is the proportionality constant, v is the frequency, h is ever, pure NiO contains Ni and O with atomic compositions ratio of
the Planck constant, α is the absorption coefficient and Eg is the 48.9:51.1 (% At) at a calcination temperature of 800 °C as presented
bandgap energy [7]. The indirect Eg can be obtained by extrapolat- in Fig. 7 (b). Moreover, EDS spectrum of both NiO-Hx 500 and NiO-
ing the linear region of the [α hv]2 vs hvcurve. Hx 600 exhibited the formation of pure NiO with atomic compo-
Fig. 5 shows that the estimated Eg of NiO-W, NiO-MW, and NiO- sitions ratio of Ni and O compositions of 55.7: 44.3 and 44.9: 55.1
Hx are 3.77; 3.53 and 3.32 eV, respectively. The bandgap energy (% At), respectively as presented in Fig. 7(c).
of NiO-W and NiO-MW conforms with the previous research, stat-
ing that NiO has a range of Eg values, which was 3.45 - 4.00 eV 4. Conclusions
[21,22]. However, the bandgap energy of NiO-Hx was a bit lower
than the previous work. This result could be affected by the for- NiO NP with different structures, bandgap energies and mor-
mation of new energy levels due to chemical defects or vacancies phologies were formed through phytosynthesis method using ACLE
in the intergranular regions [7,15]. The difference in Eg values in with various extract fractions and calcination temperatures. Ac-
the three samples is probably caused by the type of extract frac- cording to the various extract fractions, different morphologies
tion and the components dissolved therein. The various types of of NiO such as flakes-shaped, a porous foam-like and spherical
extract fractions allow different nucleation and crystals orientation were synthesized from NiO-W, NiO-MW, and NiO-Hx, respectively.
of the nanoparticle so that it affects the morphology and parti- For the optimum calcination temperature, a puresinglecrystalline
cle size. The large crystallite size (Table 2) causes an increase in phase with a porous foam-like morfology of NiO-MW was suc-
the number of molecular orbitals (both bonding and antibonding) cessfully formed at calcination temperatures of 700 and 800 °C
due to the overlapping number of atomic orbitals, hence the Eg de- with a pore diameter range of 10 0–20 0 nm. Meanwhile, a single-
creases. Therefore, Eg values become varied according to the mor- crystalline phase of NiO-Hx was successfully formed at a calcina-
phology and particle size [34–36]. tion temperature of 500 °C with a particle size range of 30–60 nm.
Additionally, the various bandgap energy of NiO-W, NiO-MW, and
3.4. Morphology and elemental analysis NiO-Hx were obtained. The different structures, bandgap energies
and morphologies in NiO-W, NiO-MW, and NiO-Hx could be at-
The surface morphology of NiO-W, NiO-MW, and NiO-Hx was tributed to the calcination temperature during the phytosynthesis
characterized by SEM, as shown in Fig. 6. NiO-W 500 and NiO-W and biomolecules dissolved in each fraction, respectively.
800 are displayed as nanoflakes structure in 40–60 nm thickness.
For NiO-MW, the morphology was a porous foam-like with a pore
diameter range of 10 0–20 0 nm. However, NiO-MW 80 0 shows a Author contribution
rougher morphology in the foam pore framework than NiO-MW
500. Meanwhile, the morphology of both NiO-Hx 500 and NiO-Hx Author names: Harits Atika Ariyanta, M. Si: Acquisition of data
600 are homogeneous nanosphere in aggregation with a particle (laboratory or clinical), Data analysis and/or interpretation, Draft-
size range of 30–60 nm. The various morphologies could be as- ing of manuscript and/or critical revision.
cribed to the difference of secondary metabolites dissolved in the Prof. Dr. Ivandini Tribidasari Anggraningrum, M.Si: Drafting of
various extract fractions. The functional group of hydroxyl can form manuscript and/or critical revision, Approval of final version of
hydrogen bonds in the solvent, which further react with metal ions manuscript.

8
H.A. Ariyanta, T.A. Ivandini and Y. Yulizar
Prof. Dr. Yoki Yulizar, M.Sc: Conception and design of study,
Data analysis and/or interpretation, Drafting of manuscript and/or
critical revision, Approval of final version of manuscript.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared to
influence the work reported in this paper.
Acknowledgement
This work was funded by HIBAH PUTI TADOK No. NKB-
619/UN2.RST/HKP.05.00/2020 through Directorate of Research and
Development, Universitas Indonesia.
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