Proc. Natl. Acad. Sci., India, Sect. A Phys. Sci.

https://doi.org/10.1007/s40010-023-00855-7

SCIENTIFIC RESEARCH PAPER

Experimental Investigation on Structural, Optical, Electrical

and Magnetic Properties of Copper Oxide Nanoparticles
S. Atchaya1 · J. Meena Devi1

Received: 4 January 2022 / Revised: 11 August 2023 / Accepted: 29 September 2023

© The Author(s), under exclusive licence to The National Academy of Sciences, India 2023

Abstract In this paper, we present the structural, optical,

electrical and magnetic properties of the copper oxide nano-
particles prepared by co-precipitation method. The prepared
copper oxide nanoparticles have been characterized by scan-
ning electron microscopy, X-ray diffraction, X-ray electron
spectroscopy and Fourier transform infrared spectroscopy.
CuO nanoparticles exhibit spherical shape with the average
particle size of around 42 nm. The X-ray diffraction pattern
reaveals the crystalline monoclinic phase. The optical prop-
erties of the CuO nanoparticles studied by diffuse reflectance
spectroscopy show the blue-shifted band gap of 1.45 eV. The
electrical conductivity value of the sample has been meas-
ured using Keithley meter and it is 0.16 S/m. The magnetic
properties measured using vibrating sample magnetometer
at room temperature show a weak ferromagnetic behaviour
with the dominant paramagnetic contribution of the CuO
nanoparticles. The weak room temperature ferromagnetic Keywords Copper oxide nanoparticles · Band gap ·
behaviour may be associated with the oxygen vacancies and Electrical conductivity and ferromagnetism
spin ordering induced by thermal energy and reduction in
particle size.
Graphic Abstract 1 Introduction

Metal oxides are considered as prime candidates for scien-

tific and technological research due to their rich, unique,
ineresting, diverse, physical and chemical properties.
Among the metal oxides, copper oxide (CuO) commonly
known as tenorite is a simple, stable member of the family of
the copper compounds and transition metal oxides. Copper
oxide is an inexpensive, abundantly available, environmen-
tally benign, non-toxic, magnetic semiconductor. Copper
* J. Meena Devi
[email protected] oxide is a p-type, narrow band gap semiconductor, and the
band gap can be tuned roughly in the range of 1.2–2.1 eV
1
Centre for Nanotechnology and Advanced Biomaterials through quantum confinement effect. Copper oxide nano-
(CeNTAB), Department of Physics, School of Electrical structures exhibit excellent catalytic activity, thermal sta-
and Electronics Engineering (SEEE), SASTRA Deemed
University, Thanjavur 613401, Tamilnadu, India bility, mechanical strength, electrical conductivity, electron

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Vol.:(0123456789)
 S. Atchaya, J. Meena Devi

correlation effects, spin dynamics, electrochemical, mag- are extensively explored [14]. CuO nanostructures of differ-
netic, super-hydrophobic, photovoltaic property, multifer- ent size and shapes have been reported as prepared by vari-
roicity and biocidal activity. The unique physicochemical ous methods such as solid-state reaction, chemical precipita-
properties of the nanoscale cupric oxide have been harnessed tion, electrochemical deposition, thermal annealing, vapour
for its diverse potential applications, such as optoelectronic phase synthesis, green synthesis and microwave irradiation
devices, sensors, catalysis, lithium-ion batteries, high criti- method [1, 2]. The co-precipitation method is a simple, safe,
cal temperature superconductors, super-capacitors, magnetic time and cost-effective method for larger yield of nanoscale
storage media, solar energy conversion, smart windows, CuO in powder form. The main objective of our present
optical limiters, thin film transistors, field emission emit- work is to investigate the structural, optical, electrical and
ters and biomedicine [1–4]. magnetic properties of copper oxide nanoparticles prepared
CuO crystallizes in the monoclinic crystal structure with by co-precipitation method.
a space group C2/c. The unit cell of cupric oxide has four
CuO molecules. The copper atoms have square-planar coor-
dination, whereas the oxygen atoms are almost tetrahedrally 2 Instrumentation Details
coordinated. Each copper atom is coordinated to four copla-
nar oxygen atoms located at the corners of a parallelogram The morphology of the copper oxide nanoparticles has been
and they form chains by sharing the edges. Each oxygen examined using a field emission scanning electron micro-
atom is coordinated to four copper atoms located at the cor- scope (FE-SEM) of model JSM 6701, JEOL, Japan. The
ners of a side sharing distorted tetrahedron. C ­ uO2 ribbon X-ray diffraction (XRD) pattern has been recorded on a dif-
chains made up of edge-sharing C ­ uO4 square planar units fractometer of model D8 Focus, Bruker, Germany, using
form the building blocks of atomic structure of cupric oxide CuKα radiation of wavelength 1.5406 Å. X-ray photoelec-
[3, 4]. The magnetic interaction between the C ­ u2+ ions is tron spectrum (XPS) measurement has been performed
2−
mainly mediated through the neighbouring ­O ions, and it using PHI Versa probe III X-ray photoelectron spectrom-
depends on the Cu–O–Cu bond angle [5]. eter. Fourier transform infrared (FTIR) spectrum has been
Cupric oxide is an antiferromagnetic material with the obtained using FTIR spectrometer of model Spectrum 100,
Neel temperature of around 230 K. The large magnetic Perkin Elmer, USA. The optical properties have been stud-
super-exchange interactions and the strongest magnetic ied by diffuse reflectance spectroscopy (DRS), employing
ordering in Cu–O–Cu chains favour antiferromagnetism. spectrometer of model DRS, Varian cray 5. The electri-
The local magnetic moment of CuO has been reported [16] cal resistivity has been measured using Keithley interac-
to be 0.86μB, as the magnetic moment per copper atom is tive digital sourcemeter of model 2450. The magnetization
0.68μB and the magnetic moment per oxygen atom is 0.18μB. measurements have been carried out in a vibrating sample
The existence of oxygen vacancies, uncompensated surface magnetometer of model VSM, 7410 Lakeshore at room
spins, reduction in particle size, and anisotropy of nanostruc- temperature.
ture have been attributed to the origin of ferromagnetism
[5–12]. The magnetic properties of CuO nanostructures are
diverse, and their origin and mechanism have not been fully 3 Preparation Method
understood. Hence, it is therefore needed to understand the
magnetism of CuO nanoparticles to develop them as a reli- Copper oxide nanoparticles have been prepared by chemi-
able robust magnetic material for the magnetoelectronics cal precipitation method using cupric acetate, glacial acetic
and spintronic applications. acid and sodium hydroxide as shown in Fig. 1. To one molar
Copper oxide nanoparticles exhibit remarkable biological aqueous solution of cupric acetate, 10 ml of diluted glacial
properties such as antimicrobial, anticancer and antioxidant acetic acid was added and stirred continuously at room tem-
efficacy, detection of biomolecules, photoimaging, photo- perature for 45 min. This mixture was then heated around
thermal therapy, and magnetically response drug delivery, 70° C, followed by the dropwise addition of 20 ml of one
which renders them a potential tool for biomedical applica- molar aqueous solution of sodium hydroxide under vigorous
tions [13]. The extraordinary benefits of semiconducting, stirring. This solution was then heated and stirred continu-
optical, magnetic and biological properties of CuO nanopar- ously at a constant temperature range of 70–80° C for about
ticles may be blended to design a multifunctional material 5 h. The colour of the solution gradually changed from blue
for biomedical as well as optical, electronic, optoelectronic to brownish black indicating the formation of copper oxide
and magnetic applications. Chemical, electrochemical and nanoparticles. The resulting brownish black precipitate was
biological methods have been used for the synthesis of cop- dried in hot air oven at 120° C for 3 h. The dried powder was
per oxide nanoparticles, and their biological properties and then subjected to calcination at 300° C for 3 h. Finally, black
biomedical, catalytic, sensing, optoelectronic applications powder of the copper oxide nanoparticles has been obtained.

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Experimental Investigation on Structural, Optical, Electrical and Magnetic Properties of…

Cu(OH)2 → CuO + H2 O (2)

4 Results and Discussions

4.1 Morphological Studies

The representative SEM image of the prepared copper

oxide nanoparticles and their size distribution is presented
in Fig. 2. The prepared copper oxide nanoparticles have a
spherical shape, and they are found to be aggregated. The
diameter of the copper oxide nanoparticles ranges from
around 20 to 150 nm. The average diameter of the copper
oxide nanoparticles is around 42 nm.

4.2 X‑ray Diffraction Pattern

X-ray diffraction pattern of the prepared copper oxide nano-

Fig. 1  Scheme for the preparation of copper oxide nanoparticles particles is shown in Fig. 3, and the calculated values of the
major structural parameters obtained from the XRD data are
listed in Table 1. The well-defined XRD peaks confirm the
The chemical reaction [4] involved in the formation of cop- crystalline nature of the prepared CuO nanoparticles cor-
per oxide nanoparticles due to the reaction between cupric responding to the monoclinic C2/c space group. The crystal
acetate and sodium hydroxide is given below. planes corresponding to the XRD peaks located around 27°,
32°, 36°, 38°, 42°, 48°, 53°, 58°, 61°, 66°, 68°, 72° and 75°
CuCH3 (COO)2 . H2 O + NaOH → Cu(OH)2 + CH3 COONa
are indexed as (021), (110), (11–1), (111), (131), (20–2),
(1)
(020), (202), (11–3), (31–1), (220), (311) and (222), respec-
tively [15, 16].

Fig. 2  SEM analysis of copper oxide nanoparticles a SEM micrograph b particle size distribution

13
 S. Atchaya, J. Meena Devi

𝛽
𝜀= (3)
4tan(𝜃)

where β represents full width at half maxima. The lat-

tice strain of the sample is 0.0054. The crystal structure
of the prepared copper oxide nanoparticles obtained from
Rietveld analysis has been visualized using VESTA soft-
ware (Fig. 4). Cu–O bond length is found to be 1.96 Å.
The values of the lattice constants, determined from the
XRD data for the prepared copper oxide nanoparticles,
are a = 4.67 Å, b = 3.42 Å, c = 5.13 Å, α = 90°, β = 99°,
γ = 90°. These calculated values of the structural param-
eters are consistent with the values reported by Meyer
et al. [3].

Fig. 3  XRD pattern of copper oxide nanoparticles

4.3 X‑ray Electron Spectroscopy

Table 1  Structural properties of copper oxide nanoparticles The chemical composition and electronic state of the pre-
pared copper oxide nanoparticles are analysed using XPS
S. No Structural parameters Values
spectra shown in Fig. 5 a, b and c. The measured XPS survey
1 Chemical formula CuO spectrum confirms the presence of constituent Cu element
2 Crystal structure Monoclinic (Cu ­2p1/2, Cu ­2p3/2 Cu 3 s, Cu 3p and Cu LMM) and O ele-
3 Space group C2/c ment (O 1 s and O KLL) in the CuO nanoparticles. The pres-
4 Lattice constants a = 4.67 Å ence of carbon can be sourced to adsorbed organic species
b = 3.42 Å (acetate group) due to usage of precursor salt cupric acetate
c = 5.13 Å for preparation. The characteristic peaks with binding energy
α = 90°
β = 99° around 953 and 933 eV correspond to C ­ u2+ state, and they
γ = 90° could be assigned to Cu ­2p1/2 and Cu ­2p3/2 core levels of
5 Unit cell volume 80.99 Å3 CuO, respectively. The satellite peak around 943 eV indi-
6 Number of CuO molecules per 4 cates the existence of CuO. The peaks around 121 and 62 eV
unit cell are attributed to Cu 3 s and Cu 3p orbitals, respectively. The
7 Density 6.52 g/cm3 peak around 529 eV is indexed to O 1 s orbital. These results
8 Cu–O (bond length) 1.96 Å are consistent with the XPS data of CuO [15, 17, 18].
9 Cu-Cu (distance) 2.89 Å
10 O–O (distance) 2.62 Å

The crystallite size of the sample calculated using

Debye-Scherer formula is 20.74 nm. There is difference
in the particle size obtained from the SEM measurements
and crystallite size obtained from the XRD measurements.
Generally, the particle size is larger than the crystallite
size, because a single particle consists of number of crys-
tallites. A particle is an agglomeration of several crystal-
lites. When the particle is made up of just one crystallite,
crystallite size is same as the particle size. The smaller
particles in the size range 20 nm may me made up of just
one crystallite.
The lattice strain (ε) has been calculated using the fol-
lowing formula.

Fig. 4  Crystal structure of copper oxide nanoparticles

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Experimental Investigation on Structural, Optical, Electrical and Magnetic Properties of…

Fig. 5 a  XPS survey spectrum of copper oxide nanoparticles. b XPS core level spectrum of Cu 2p. c XPS core level spectrum of O 1 s

4.4 FTIR Studies

The chemical functional groups present in the prepared

copper oxide nanoparticles have been identified from FTIR
spectra displayed in Fig. 6. The characteristic IR peaks are
observed around 3220, 1670, 1410, 1040 and 600 ­cm−1. The
broad absorption peak around 3220 ­cm−1 corresponds to the
OH stretching vibration of the adsorbed water molecules.
The IR active vibrations around 1670, 1410 and 1040 ­cm−1
are assigned to the stretching of acetate functional group,
found in the sample due to the precursor cupric acetate. The
narrow band around 600 ­cm−1 reveals the formation of pure
CuO phase copper oxide nanoparticles [19, 20].

4.5 Optical Properties

The optical properties of the copper oxide nanoparticles

such as energy band gap, refractive index and dielectric Fig. 6  FTIR spectrum of copper oxide nanoparticles

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 S. Atchaya, J. Meena Devi

Table 2  Optical properties of copper oxide nanoparticles The refractive index is obtained from the band gap value
S. No Optical parameters Values using Herve–Vandamme relation given below:
)2
1 Band gag (Eg) 1.45 eV
(
A
n2 = 1 + (5)
2 Refractive index (n) 2.98 Eg + B
3 High-frequency dielectric constant (ε∞) 8.86
4 Static dielectric constant (ε0) 14.05 where A and B are numerical constants with values of
13.6 and 3.4 eV, respectively. The refractive index n of the
prepared copper oxide nanoparticles is found to be 2.98.
Babu et al. [22] have reported the refractive index value
of CuO thin film to be 2.35 from Herve–Vandamme rela-
tion. The refractive index value estimated for copper oxide
nanoparticles in our present work is comparable to the value
reported in the literature. The refractive index value of bulk
copper oxide is 2.6. The refractive index value of the pre-
pared copper oxide nanoparticles estimated from Herve-
Vandamme relation is slightly larger than the bulk value.
The values of high-frequency dielectric constant (ε∞) and
static dielectric constant (ε0) have been estimated as 8.86
and 14.05 and, respectively, using the following relations.

𝜀∞ = n 2 (6)

𝜀0 = 18.52 − 3.08 Eg (7)

Fig. 7  Kubelka–Munk transformed reflectance spectrum of copper
oxide nanoparticles The estimated values of high-frequency dielectric con-
stant and static dielectric constant fairly agrees with the val-
ues of Sarker et al. [23].

constant (Table 2) have been calculated and studied using

diffuse reflectance spectroscopy. The fundamental proper- 4.6 Electrical properties
ties such as energy gap and refractive index determine the
optical and electronic behaviour of semiconductors. The The prepared copper oxide nanoparticles in the powder form
relation between diffuse reflectance of the sample (R) and is converted into a pellet form and its electrical resistance is
Kubelka–Munk function F(R) has been used to determine measured using Keithley meter at room temperature. From
the band gap. the measured electrical resistance (R), electrical resistivity
(ρ) and electrical conductivity (σ) have been determined
F(R) = (1 − R)2 ∕2R (4) using the following relations.
(F(R) × hυ) 2 has been plotted against energy (hυ) in 𝜌 = RA∕𝜄 (8)
Fig. 7. The linear increase of this curve is extrapolated
to meet at x axis to find the value of band gap. The pre- 𝜎 = 1∕𝜌 (9)
pared copper oxide nanoparticles have a band gap (E g)
of 1.45 eV. The band gap value of bulk copper oxide where A is the cross-sectional area and Ɩ is the length of the
is 1.20 eV. The blue shift in the band gap energy by an material. The electrical conductivity of the prepared cop-
amount 0.25 eV is due to the quantum confinement effect per oxide nanoparticles calculated from the above relation
of the nano size copper oxide particles. is 0.16 S/m. This value lies in the same range of electrical
The refractive index of the semiconductor represents conductivity as reported for CuO in the literature [24, 25].
the measure of its transparency to incident spectral radia- CuO is a p-type semiconductor, and so the majority charge
tion. The relation between energy gap and refractive index carriers are holes in the valence band. The holes originate
of semiconductors is proposed by Herve–Vandamme. from the copper vacancies and oxygen interstitials. The con-
Herve-Vandamme relation is based on classical oscilla- ductivity of copper oxide nanoparticles occurs due to the
tory theory where the difference between UV resonance motion of holes in the valence band and due to the motion
energy and band gap energy is assumed as constant [21]. of electrons in the conduction band.

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Experimental Investigation on Structural, Optical, Electrical and Magnetic Properties of…

one unpaired electron in d shell of copper contributes to

the magnetic moment of CuO. The magnetic interactions
between ­C u2+ ions are enhanced due to the intervening
oxygen anions.
The magnetic properties of nanoparticles are predomi-
nantly determined by the surface spins, since the surface
area of the nanomaterials is larger than that of their bulk
counterpart. The surface spins dominate the magnetization
due to lower coordination and uncompensated exchange
couplings. The exchange coupling between the surface
and the core spins and the increase of imbalanced spins
from the increase of Fermi holes from the image charges
of surface electrons may lead to magnetic orderings in
nanoparticles [5]. The observed room temperature ferro-
magnetism in CuO nanoparticles may be associated with
Fig. 8  Hysteresis loop of copper oxide nanoparticles
oxygen vacancies and uncompensated surface spins. The
oxygen vacancies may contribute to the spin that arise
4.7 Magnetic Properties from unpaired electron of ­C u 2+. The generated oxygen
vacancies liberate bound electrons to create free carriers
The plot of magnetic moment versus applied field of the and this may induce the interactions between the uncom-
CuO nanoparticles recorded using vibrating sample mag- pensated surface spins, resulting in ferromagnetism. The
netometer at room temperature is shown in Fig. 8. The oxygen voids and quantum confinement effect may be
coercivity and retentivity values are found to be 85.202 G responsible for the observed ferromagnetism in cupric
and 3.48 X ­10–2 emu/g, respectively. The magnetization has oxide nanoparticles.
not attained saturation even for the maximum value of the
applied field (Fig. 8). The hysteresis curve shows a weak
ferromagnetic behaviour with the dominant paramagnetic
contribution. The room temperature ferromagnetic behav- 5 Conclusions
iour observed in the sample may be attributed to reduction in
particle size, oxygen vacancies and uncompensated surface In this experimental study, pure, spherical, crystalline,
spins. At nanoscale, copper oxide exihibits different mag- monoclinic phase, copper oxide nanoparticles have been
netic properties, due to the electronic and atomic structural prepared using co-precipitation method and their struc-
complexities and due to the reduction in particle size, grain tural, optical, electrical, and magnetic properties have been
dimension, increase in surface area, anisotropy of nanostruc- investigated. The values of electrical conductivity, band gap,
ture, oxygen vacancies, structural disorder, defects, surface refractive index, high frequency and static dielectric constant
spins and magnetic exchange coupling. The room tempera- have been determined as 0.16 S/m, 1.45 eV, 2.98, 8.86 and
ture ferromagnetism in nanoscale CuO has been reported by 14.05, respectively. The prepared copper oxide nanoparticle
Gao et al. [5]. They have observed room-temperature fer- exihibits weak room temperature ferromagnetic behaviour
romagnetism in CuO flower-like nanostructures and have with the dominant paramagnetic contribution. The reduction
suggested oxygen vacancies to be the origin of ferromag- in particle size and the oxygen vacancies might have caused
netism. Zhao et al. [8] observed room-temperature ferro- the room temperature ferromagnetism. The findings of this
magnetism in CuO nanosheets and nanostructures, and they work may be harnessed for the development of magnetic
suggested uncompensated surface spins to be the origin of semiconducting cupric oxide nanoparticles for optoelec-
ferromagnetism. tronic, magnetic and biomedical applications.
Cu2+ ion, which has electron spin S = 1/2, plays a major
role in the magnetic properties of CuO systems. CuO Acknowledgements J. Meena Devi expresses her sincere thanks to
the TRR Research Scheme, SASTRA Deemed University, Thanja-
behaves like a spin only system as the orbital moment of vur, for the financial support. We acknowledge the DST-FIST Project
3d hole of the C ­ u2+ ion is completely quenched in crystal- [SR/FST/PS-1/2020/135] for the facilities. J. Meena Devi acknowl-
line environments [26]. The copper and oxygen in CuO edges the Abdus Salam International Centre for Theoretical Physics
exist as ­C u 2+ and ­O 2− ions, which has been confirmed (ICTP), Trieste, Italy, for providing her Regular Associate award for the
period of 01 January 2019 to 31 December 2024. We thank Dr. B. G.
through XPS analysis. The electronic configuration of cop- Jeyaprakash, School of Electrical and Electronics Engineering (SEEE),
per in ­Cu2+ valence state is ­1s2 ­2s2 ­2p6 ­3s2 ­3p6 ­3d9 and of SASTRA Deemed University, Thanjavur, for his valuable suggestions.
oxygen in O ­ 2− valence state is 1­ s2 ­2s2 ­2p6. The spin of the

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 S. Atchaya, J. Meena Devi

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