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-

* J. Meena Devi
jmeenadevi@sastra.ac.in
1
Centre for Nanotechnology and Advanced Biomaterials
(CeNTAB), Department of Physics, School of Electrical
and Electronics Engineering (SEEE), SASTRA Deemed
University, Thanjavur 613401, Tamilnadu, India
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
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
through quantum confinement effect. Copper oxide nano-
structures exhibit excellent catalytic activity, thermal sta-
bility, mechanical strength, electrical conductivity, electron

13
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correlation effects, spin dynamics, electrochemical, mag-
netic, super-hydrophobic, photovoltaic property, multifer-
roicity and biocidal activity. The unique physicochemical
properties of the nanoscale cupric oxide have been harnessed
for its diverse potential applications, such as optoelectronic
devices, sensors, catalysis, lithium-ion batteries, high criti-
cal temperature superconductors, super-capacitors, magnetic
storage media, solar energy conversion, smart windows,
optical limiters, thin film transistors, field emission emit-
ters and biomedicine [1–4].
CuO crystallizes in the monoclinic crystal structure with
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
coordinated. Each copper atom is coordinated to four copla-
nar oxygen atoms located at the corners of a parallelogram
and they form chains by sharing the edges. Each oxygen
atom is coordinated to four copper atoms located at the cor-
ners of a side sharing distorted tetrahedron. C ­ uO2 ribbon
chains made up of edge-sharing C ­ uO4 square planar units
form the building blocks of atomic structure of cupric oxide
[3, 4]. The magnetic interaction between the C ­ u2+ ions is
2−
mainly mediated through the neighbouring ­O ions, and it
depends on the Cu–O–Cu bond angle [5].
Cupric oxide is an antiferromagnetic material with the
Neel temperature of around 230 K. The large magnetic
super-exchange interactions and the strongest magnetic
ordering in Cu–O–Cu chains favour antiferromagnetism.
The local magnetic moment of CuO has been reported [16]
to be 0.86μB, as the magnetic moment per copper atom is
0.68μB and the magnetic moment per oxygen atom is 0.18μB.
The existence of oxygen vacancies, uncompensated surface
spins, reduction in particle size, and anisotropy of nanostruc-
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
understood. Hence, it is therefore needed to understand the
magnetism of CuO nanoparticles to develop them as a reli-
able robust magnetic material for the magnetoelectronics
and spintronic applications.
Copper oxide nanoparticles exhibit remarkable biological
properties such as antimicrobial, anticancer and antioxidant
efficacy, detection of biomolecules, photoimaging, photo-
thermal therapy, and magnetically response drug delivery,
which renders them a potential tool for biomedical applica-
tions [13]. The extraordinary benefits of semiconducting,
optical, magnetic and biological properties of CuO nanopar-
ticles may be blended to design a multifunctional material
for biomedical as well as optical, electronic, optoelectronic
and magnetic applications. Chemical, electrochemical and
biological methods have been used for the synthesis of cop-
per oxide nanoparticles, and their biological properties and
biomedical, catalytic, sensing, optoelectronic applications
13
S. Atchaya, J. Meena Devi
are extensively explored [14]. CuO nanostructures of differ-
ent size and shapes have been reported as prepared by vari-
ous methods such as solid-state reaction, chemical precipita-
tion, electrochemical deposition, thermal annealing, vapour
phase synthesis, green synthesis and microwave irradiation
method [1, 2]. The co-precipitation method is a simple, safe,
time and cost-effective method for larger yield of nanoscale
CuO in powder form. The main objective of our present
work is to investigate the structural, optical, electrical and
magnetic properties of copper oxide nanoparticles prepared
by co-precipitation method.
2 Instrumentation Details
The morphology of the copper oxide nanoparticles has been
examined using a field emission scanning electron micro-
scope (FE-SEM) of model JSM 6701, JEOL, Japan. The
X-ray diffraction (XRD) pattern has been recorded on a dif-
fractometer of model D8 Focus, Bruker, Germany, using
CuKα radiation of wavelength 1.5406 Å. X-ray photoelec-
tron spectrum (XPS) measurement has been performed
using PHI Versa probe III X-ray photoelectron spectrom-
eter. Fourier transform infrared (FTIR) spectrum has been
obtained using FTIR spectrometer of model Spectrum 100,
Perkin Elmer, USA. The optical properties have been stud-
ied by diffuse reflectance spectroscopy (DRS), employing
spectrometer of model DRS, Varian cray 5. The electri-
cal resistivity has been measured using Keithley interac-
tive digital sourcemeter of model 2450. The magnetization
measurements have been carried out in a vibrating sample
magnetometer of model VSM, 7410 Lakeshore at room
temperature.
3 Preparation Method
Copper oxide nanoparticles have been prepared by chemi-
cal precipitation method using cupric acetate, glacial acetic
acid and sodium hydroxide as shown in Fig. 1. To one molar
aqueous solution of cupric acetate, 10 ml of diluted glacial
acetic acid was added and stirred continuously at room tem-
perature for 45 min. This mixture was then heated around
70° C, followed by the dropwise addition of 20 ml of one
molar aqueous solution of sodium hydroxide under vigorous
stirring. This solution was then heated and stirred continu-
ously at a constant temperature range of 70–80° C for about
5 h. The colour of the solution gradually changed from blue
to brownish black indicating the formation of copper oxide
nanoparticles. The resulting brownish black precipitate was
dried in hot air oven at 120° C for 3 h. The dried powder was
then subjected to calcination at 300° C for 3 h. Finally, black
powder of the copper oxide nanoparticles has been obtained.
Experimental Investigation on Structural, Optical, Electrical and Magnetic Properties of…
Fig. 1  Scheme for the preparation of copper oxide nanoparticles
The chemical reaction [4] involved in the formation of cop-
per oxide nanoparticles due to the reaction between cupric
acetate and sodium hydroxide is given below.
CuCH3 (COO)2 . H2 O + NaOH → Cu(OH)2 + CH3 COONa
(1)
Fig. 2  SEM analysis of copper oxide nanoparticles a SEM micrograph b particle size distribution
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-
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
crystalline nature of the prepared CuO nanoparticles cor-
responding to the monoclinic C2/c space group. The crystal
planes corresponding to the XRD peaks located around 27°,
32°, 36°, 38°, 42°, 48°, 53°, 58°, 61°, 66°, 68°, 72° and 75°
are indexed as (021), (110), (11–1), (111), (131), (20–2),
(020), (202), (11–3), (31–1), (220), (311) and (222), respec-
tively [15, 16].
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
S. No Structural parameters
1 Chemical formula
2 Crystal structure
3 Space group
4 Lattice constants
5 Unit cell volume
6 Number of CuO molecules per
unit cell
7 Density
8 Cu–O (bond length)
9 Cu-Cu (distance)
10 O–O (distance)
The chemical composition and electronic state of the pre-
pared copper oxide nanoparticles are analysed using XPS
Values
spectra shown in Fig. 5 a, b and c. The measured XPS survey
CuO spectrum confirms the presence of constituent Cu element
Monoclinic (Cu ­2p1/2, Cu ­2p3/2 Cu 3 s, Cu 3p and Cu LMM) and O ele-
C2/c ment (O 1 s and O KLL) in the CuO nanoparticles. The pres-
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
80.99 Å3 CuO, respectively. The satellite peak around 943 eV indi-
4 cates the existence of CuO. The peaks around 121 and 62 eV
are attributed to Cu 3 s and Cu 3p orbitals, respectively. The
6.52 g/cm3 peak around 529 eV is indexed to O 1 s orbital. These results
1.96 Å are consistent with the XPS data of CuO [15, 17, 18].
2.89 Å
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

13
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

13

Table 2  Optical properties of copper oxide nanoparticles
S. No Optical parameters
1 Band gag (Eg)
2 Refractive index (n)
3 High-frequency dielectric constant (ε∞)
4 Static dielectric constant (ε0)
Fig. 7  Kubelka–Munk transformed reflectance spectrum of copper
oxide nanoparticles
constant (Table 2) have been calculated and studied using
diffuse reflectance spectroscopy. The fundamental proper-
ties such as energy gap and refractive index determine the
optical and electronic behaviour of semiconductors. The
relation between diffuse reflectance of the sample (R) and
Kubelka–Munk function F(R) has been used to determine
the band gap.
F(R) = (1 − R)2 ∕2R
(F(R) × hυ) 2 has been plotted against energy (hυ) in
Fig. 7. The linear increase of this curve is extrapolated
to meet at x axis to find the value of band gap. The pre-
pared copper oxide nanoparticles have a band gap (E g)
of 1.45 eV. The band gap value of bulk copper oxide
is 1.20 eV. The blue shift in the band gap energy by an
amount 0.25 eV is due to the quantum confinement effect
of the nano size copper oxide particles.
The refractive index of the semiconductor represents
the measure of its transparency to incident spectral radia-
tion. The relation between energy gap and refractive index
of semiconductors is proposed by Herve–Vandamme.
Herve-Vandamme relation is based on classical oscilla-
tory theory where the difference between UV resonance
energy and band gap energy is assumed as constant [21].
13
S. Atchaya, J. Meena Devi
The refractive index is obtained from the band gap value
Values using Herve–Vandamme relation given below:
)2
1.45 eV
(
A
n2 = 1 + (5)
2.98 Eg + B
8.86
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)
The estimated values of high-frequency dielectric con-
stant and static dielectric constant fairly agrees with the val-
ues of Sarker et al. [23].
4.6 Electrical properties
The prepared copper oxide nanoparticles in the powder form
is converted into a pellet form and its electrical resistance is
measured using Keithley meter at room temperature. From
the measured electrical resistance (R), electrical resistivity
(ρ) and electrical conductivity (σ) have been determined
(4) using the following relations.
𝜌 = RA∕𝜄 (8)
𝜎 = 1∕𝜌 (9)
where A is the cross-sectional area and Ɩ is the length of the
material. The electrical conductivity of the prepared cop-
per oxide nanoparticles calculated from the above relation
is 0.16 S/m. This value lies in the same range of electrical
conductivity as reported for CuO in the literature [24, 25].
CuO is a p-type semiconductor, and so the majority charge
carriers are holes in the valence band. The holes originate
from the copper vacancies and oxygen interstitials. The con-
ductivity of copper oxide nanoparticles occurs due to the
motion of holes in the valence band and due to the motion
of electrons in the conduction band.
Experimental Investigation on Structural, Optical, Electrical and Magnetic Properties of…
Fig. 8  Hysteresis loop of copper oxide nanoparticles
4.7 Magnetic Properties
The plot of magnetic moment versus applied field of the
CuO nanoparticles recorded using vibrating sample mag-
netometer at room temperature is shown in Fig. 8. The
coercivity and retentivity values are found to be 85.202 G
and 3.48 X ­10–2 emu/g, respectively. The magnetization has
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-
iour observed in the sample may be attributed to reduction in
particle size, oxygen vacancies and uncompensated surface
spins. At nanoscale, copper oxide exihibits different mag-
netic properties, due to the electronic and atomic structural
complexities and due to the reduction in particle size, grain
dimension, increase in surface area, anisotropy of nanostruc-
ture, oxygen vacancies, structural disorder, defects, surface
spins and magnetic exchange coupling. The room tempera-
ture ferromagnetism in nanoscale CuO has been reported by
Gao et al. [5]. They have observed room-temperature fer-
romagnetism in CuO flower-like nanostructures and have
suggested oxygen vacancies to be the origin of ferromag-
netism. Zhao et al. [8] observed room-temperature ferro-
magnetism in CuO nanosheets and nanostructures, and they
suggested uncompensated surface spins to be the origin of
ferromagnetism.
Cu2+ ion, which has electron spin S = 1/2, plays a major
role in the magnetic properties of CuO systems. CuO
behaves like a spin only system as the orbital moment of
3d hole of the C ­ u2+ ion is completely quenched in crystal-
line environments [26]. The copper and oxygen in CuO
exist as ­C u 2+ and ­O 2− ions, which has been confirmed
through XPS analysis. The electronic configuration of cop-
per in ­Cu2+ valence state is ­1s2 ­2s2 ­2p6 ­3s2 ­3p6 ­3d9 and of
oxygen in O ­ 2− valence state is 1­ s2 ­2s2 ­2p6. The spin of the
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
oxygen vacancies and uncompensated surface spins. The
oxygen vacancies may contribute to the spin that arise
from unpaired electron of ­C u 2+. The generated oxygen
vacancies liberate bound electrons to create free carriers
and this may induce the interactions between the uncom-
pensated surface spins, resulting in ferromagnetism. The
oxygen voids and quantum confinement effect may be
responsible for the observed ferromagnetism in cupric
oxide nanoparticles.
5 Conclusions
In this experimental study, pure, spherical, crystalline,
monoclinic phase, copper oxide nanoparticles have been
prepared using co-precipitation method and their struc-
tural, optical, electrical, and magnetic properties have been
investigated. The values of electrical conductivity, band gap,
refractive index, high frequency and static dielectric constant
have been determined as 0.16 S/m, 1.45 eV, 2.98, 8.86 and
14.05, respectively. The prepared copper oxide nanoparticle
exihibits weak room temperature ferromagnetic behaviour
with the dominant paramagnetic contribution. The reduction
in particle size and the oxygen vacancies might have caused
the room temperature ferromagnetism. The findings of this
work may be harnessed for the development of magnetic
semiconducting cupric oxide nanoparticles for optoelec-
tronic, magnetic and biomedical applications.
Acknowledgements J. Meena Devi expresses her sincere thanks to
the TRR Research Scheme, SASTRA Deemed University, Thanja-
vur, for the financial support. We acknowledge the DST-FIST Project
[SR/FST/PS-1/2020/135] for the facilities. J. Meena Devi acknowl-
edges the Abdus Salam International Centre for Theoretical Physics
(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.
Jeyaprakash, School of Electrical and Electronics Engineering (SEEE),
SASTRA Deemed University, Thanjavur, for his valuable suggestions.
13
 S. Atchaya, J. Meena Devi

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