Materials Express

2158-5849/2019/9/653/007
Copyright © 2019 by American Scientific Publishers
All rights reserved. doi:10.1166/mex.2019.1549
Printed in the United States of America www.aspbs.com/mex

Augmentation of ferromagnetism in CuO–Al2 O3

nanocomposite synthesized via solution
combustion method
Mir Waqas Alam1, ∗ , Farooq Ahmad Dar2 , Fida Mohmed3 , Abdullah Aljaafari1 , and Osama Saber1
1
Department of Physics, College of Science, King Faisal University, Al-Hassa 31982, Saudi Arabia
2
Special Center for Nanotechnology, Department of Physics, National Institute of Technology Srinagar, 190006,
Jammu and Kashmir, India
3
State Key Lab of New Ceramics and Fine Processing, School of Materials Science and Engineering,
Tsinghua University, Beijing, 100084, China

Article
ABSTRACT IP: 5.10.31.211 On: Sat, 29 Apr 2023 16:15:14
Copyright:
The finite size effect of CuO nanoparticles andAmerican Scientific
their effect Publishers
on the magnetic behavior of a CuO–Al2 O3 nanocom-
Delivered by Ingenta
posite synthesized via a solution combustion method are discussed here. It is observed that the introduction
of CuO nanoparticles of ∼20 nm in size on the surfaces of Al2 O3 nanosheets strongly influences the mag-
netic moment of the nanocomposite. The X-ray diffraction pattern reveals the presence of a CuO phase in the
CuO–Al2 O3 nanocomposite. Electron microscopy imaging shows the presence of CuO nanoparticles distributed
over the surfaces of Al2 O3 nanosheets. Magnetic measurements performed at 5 and 300 K revealed a strong
enhancement in the saturation magnetization of the CuO–Al2 O3 nanocomposite at both temperatures. This
increase is due to the formation of CuO nanoparticles on the surfaces of the Al2 O3 nanosheets. These CuO
nanoparticles show a ferromagnetic nature due to the uncompensated surface Cu2+ spins of the copper ions.
The presence of the Cu2+ state in the CuO nanoparticles in the CuO–Al2 O3 nanocomposite was confirmed by
X-ray photoelectron spectroscopy (XPS) measurements.
Keywords: Nanoparticles, CuO–Al2 O3 Nanocomposite, Magnetic Materials, Solution Process, Synthesis.

1. INTRODUCTION found in interfaces with deviant atoms displaying unsatis-

Significant research into magnetic nanoparticles is cur-
rently taking place worldwide, both from technological
and fundamental research perspectives. Nanocomposites
are considered as one of the most complex magnetic Nano
system with finite size and interfacial interactions play-
ing the dominant roles. A magnetic nanocomposite may
be considered as a mixture of well-defined phases with
at least one being nanosized and revealing a magnetic
ordering. With the nanocrystallites being of a very small
size, much of the volume fraction of the material can be
∗
Author to whom correspondence should be addressed.
Email: wmir@kfu.edu.sa
fied bonds. With these peculiarities in the structural and
morphological properties of nanocomposites, they display
significantly different physical and mechanical properties
from their large grain polycrystalline analogues.
The size of the particles plays an important role in
modifying the magnetic behavior of the system. Finite
size effects can reshape the spin density of states and the
net magnetic moment associated with the atoms placed at
the surface/interface. Nanosized systems can induce unex-
pected magnetic properties in the system by modifying
the relative number of surface/interface positions along
with suitably adopting the intrinsic magnetic properties of
the bulk components. The nanostructuring results in an

Mater. Express, Vol. 9, No. 6, 2019 653

 Materials Express
increase in the number of magnetic neighbors, as well
as impacts on the exchange integrals, considering their
reduced coordination and symmetry in comparison to the
bulk atoms. Transition metals are far more sensitive to
such effects, significantly influencing their site specific
occupancy and local coordination [1].
Studies on the preparation and characterization of alu-
minum oxide (Al2 O3 ) nanocomposites to form metal
matrix composites have been attracting scientific interest
because of the nanocomposites possessing special physi-
cal, chemical, mechanical and magnetic properties [2–6].
The techniques used in the synthesis of nanoparticles
also play a remarkable role on the properties of the
nanocomposites, which in turn have a significant impact
on their applications [5, 7–9]. In addition to spintronic
and semiconductor applications, nanoparticles show poten-
tial medical applications, such as improving the quality
of medical resonance imaging, the treatment of malignant
cells, manipulating cell membranes and site specific drug
delivery [10–12]. The magnetic behavior of nanoparticles
has additional promising biomedical applications, espe-
cially in the field of cancer research [7, 13–15]. In the cop-
per oxide-alumina (CuO–Al2 O3 ) nanocomposite system,
the CuO nanoparticle distribution can provide distinctive
Article
characteristics, such as high electrical/thermal conduc-
tivities and magnetic proprieties, as well as excellent
IP: 5.10.31.211
resistance and high strength at high temperature anneal-On: Sat, 29 Aprby2023
Copyright: American Scientific
ing [16, 17]. In addition to this, CuO nanoparticles are byshown
Delivered
showing immense medical application [18], besides being
used in semiconductor applications, like in supercapac-
itors, magnetic storage media, sensors, catalysis and so
on [19–22]. Furthermore, the magnetic behavior possessed
by the CuO nanoparticles especially enhances their appli-
cations in the field of cancer treatment [23–27]. Here,
we discuss the structural, morphological and magnetic
properties of a CuO–Al2 O3 nanocomposite synthesized
via a solution combustion technique. The enhanced mag-
netic behavior of the nanocomposite will find its biomed-
ical application, like site specific drug delivery, cancer
diagnosis, as well as magnetic nanocomposite facilitated
targeted and image guided drug delivery of cancerous
cells [28–31].
2. EXPERIMENTAL DETAILS
Aluminum (III) nitrate in its hydrated form (Al(NO3 )3 ·
9H2 O), copper nitrate Cu(NO3 )2 (3, 6 and 9 wt.%), urea
as a fuel (CO(NH2 )2 ) and ethanol as a solvent were used
to prepare the CuO–Al2 O3 nanocomposite. All chemicals
were used in their pure form. Aluminum nitrate in its
hydrated form was added to a stoichiometric amount of
copper nitrate (5 wt.%). This mixture was then added in
200 ml of ethanol solvent to acquire 0.1 M solution. Fur-
ther, for fuel urea was used and dissolved in 200 ml of
ethanol solvent. Using magnetic stirrer, both the achieved
solutions continuously and distinctly stirred until a clear
654
Augmentation of ferromagnetism in CuO–Al2 O3 nanocomposite
Alam et al.
solution was achieved. Then both of these solutions (urea
to aluminum nitrate and copper nitrate) were added to a
molar ratio of 2.5:1, which were kept for 3 h under con-
stant stirring on a hot plate until a gel-like material were
obtained. After the solution turned into a gel, it was placed
on a hot plate and the mixture changed into a black vis-
cous resin. The resin was then heated at 200  C for 1 h
and then kept for cooling to room temperature were the
resin was changed into a black mass. The black mass was
then ground to a fine powder in an agate mortar and was
calcinated for 1 h 200  C in a wraped furnace to obtain
the final specimens.
The surface morphology and structural properties were
analyzed by using field emission scanning electron
microscopy (FESEM, FESEM-EDX Oxford INCA 400)
and X-ray diffraction (XRD, D8-XRD, Bruker) respec-
tively. The elemental states were verified using X-ray
photoelectron spectroscopy (XPS, Model ESCALAB™
+
XI , Thermo Fisher). The magnetic properties were
obtained from a superconducting quantum interference
device (SQUID, MPMS® 3, Quantum Design).
3. RESULTS AND DISCUSSION
3.1. Structural Characterization
The phase purity and crystallinity of the samples were ana-
lyzed 16:15:14
performing XRD in the 2 range of 20 to 80, as
inPublishers
Ingenta
Figure 1. XRD was performed using an Advance
X-ray diffractometer with Ni-filtered Cu-K radiation of
wavelength ( = 1540 Å (40 kV and 40 mA) at a scan
rate of 2 /min and a step size of 0.002. The crystal struc-
ture of the pure Al2 O3 was identified as a hexagonal lat-
tice structure belonging to the space group R-3c (167).
The peaks were indexed using the JCPDS diffraction file
(card No: 82-1399). Only the pure phase was observed
for the Al2 O3 sample, without the presence of any sec-
ondary phase. However, for the CuO–Al2 O3 nanocom-
posite sample, the XRD clearly showed the presence of
secondary phases, as marked by stars in Figure 1. These
secondary phase peaks were identified to be the single
phase CuO having a monoclinic structure with lattice con-
stants of a = 46837 Å, b = 34226 Å and c = 51288 Å,
as obtained from the standard JCPDS card no. 72-0629.
The XRD pattern clearly revealed the presence of CuO in
the nanocomposite. The crystallite sizes of CuO nanoparti-
cles were calculated from the most prominent peak (1̄11),
using the well-known Debye-Scherrer equation:
k
D=
 cos 
where k = 09 and is the shape factor,  = 0154 nm and
is the wavelength of the X-rays,  is the angle of diffrac-
tion and  is the full width at half maximum (FWHM).
The FWHM was obtained by Gaussian fitting of the (1̄11)
peak of CuO, as shown in Figure 1(b). The crystalline
sizes of the CuO nanoparticles, as calculated from the
Mater. Express, Vol. 9, 2019
Augmentation of ferromagnetism in CuO–Al2 O3 nanocomposite
Alam et al.
(a)
Fig. 1. (a) X-ray diffraction (XRD) pattern for the Al2 O3 and CuO–Al2 O3 nanocomposites (b) shows the FWHM for CuO peak obtained after
performing the Gaussian fitting of the raw data.
XRD analysis, were found to 24, 13 and 11 nm for 3,
6 and 9 wt.% concentrations of CuO, respectively. We
observed a decrease in particle size as the concentra-
tion of CuO was increased. However, this smaller size
of CuO in the CuO–Al2 O3 nanocomposite contributed to
the higher values of magnetism in IP:the5.10.31.211
composite, asOn:
dis-Sat, 29 Apr 2023 16:15:14
cussed in the next section. XRD analysis clearly indicates
Copyright: American Scientific
that material are nanocomposite as shown in [JCPDS Delivered
card byTo Ingenta
no. 72-0629 and card No: 82-1399]. In addition to that
previous research [7, 13, 15–17] is in good agreement with
the present results.
3.2. Morphological Properties
A morphological study was carried out using FESEM fit-
ted with energy dispersive X-ray spectrometry. The SEM
micrographs, as presented in Figure 2, revealed the size
of the particles within the nano range. The SEM micro-
graphs shown in Figure 2(a) reveal the pure Al2 O3 of the
nanosheets with a slightly rough surface with no demarca-
tion of prominent grain boundaries or particles. After the
addition of CuO nanoparticles to the host matrix, the par-
ticles become clearly visible with prominent grain bound-
aries on the surfaces of the Al2 O3 nanosheets, as shown
in Figure 2(b) for the 9% CuO–Al2 O3 nanocomposite.
The particle sizes of the CuO nanoparticles observed from
microscopy were calculated for all three samples using
Lorentz curve fitting, as shown in Figures 2(c)–(e) for 3, 6
and 9 wt.% concentrations of CuO nanoparticles, respec-
tively. The particle sizes obtained from the analysis of
FESEM micrographs were 24, 12 and 9 nm for 3, 6 and
9 wt.% of CuO nanoparticles, respectively. The observed
particle sizes from microscopy are in good agreement with
the particle size calculated from XRD analysis using the
Scherrer equation. The ionic radius ratio of Cu and Al
(73:53 pm), during the formation of nanocomposite Al ion
Mater. Express, Vol. 9, 2019
Materials Express
(b)
may be replaced by Cu ion with the result there is com-
pressive stress and chemical pressure in the composite and
results the decrease in particle size [32, 33]. This smaller
particle size (nanosized) results in the enhancement of
Article
magnetism in the nanocomposite.
Publishers
3.3. Magnetic Properties
analyze the influence of CuO nanoparticle substitution
in the Al2 O3 matrix, the magnetic properties of nanocom-
posite and the magnetic hysteresis of the garnets were
obtained from SQUID measurements. The SQUID mea-
surements were performed in a magnetic field of 1 kOe
at 5 and 300 K, as shown in Figures 3(a) and (b),
respectively. The saturation magnetization Ms and coerciv-
ity Cr obtained from the SQUID measurements are pre-
sented in Table I. From the magnetic measurements, it
is clear that the Al2 O3 nanoparticles show a character-
istic hysteresis behavior, indicating ferromagnetic behav-
ior even at room temperature. We obtained Ms values of
∼0.0019 and 0.0013 emu/gm at 5 and 300 K, respec-
tively. Bulk Al2 O3 is known to show diamagnetic behavior
and does not reveal any room temperature ferromagnetism.
However, the observed ferromagnetism behavior of Al2 O3
nanoparticles, even at room temperature, is a surface
effect attributed to the oxygen vacancies at the surface of
nanoparticles, i.e., F+ centers [34–36].
In the case of the CuO–Al2 O3 nanocomposite, it is
clearly visible from the hysteresis measurement that the
introduction of CuO nanoparticles resulted in an increase
in both saturation magnetization and coercivity, both at
low and room temperature. For instance, the 9% CuO–
Al2 O3 nanocomposite showed Ms values of ∼0.0051 and
∼0.0022 emu/gm at 5 and 300 K, respectively, which are
around double the values obtained for pure Al2 O3 , reveal-
ing a strong enhancement of magnetism in the CuO–Al2 O3
655
 Materials Express Augmentation of ferromagnetism in CuO–Al2 O3 nanocomposite
Alam et al.

(a) (b)

Al2O3 (9%) CuO-Al2O3

Article

(c) (d) (6% CuO) (e) (3% CuO)

(9% CuO) IP: 5.10.31.211 On: Sat, 29 Apr 2023 16:15:14
Copyright: American Scientific Publishers
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4 6 8 10 12 14 16 18 20 22 24 5 10 15 20 25 30 35 40 0 10 20 30 40
Particle size (nm) Particle size (nm) Particle size (nm)

Fig. 2. Field emission scanning microscopy (FESEM) images of (a) Al2 O3 nano-sheets, (b) CuO-Al2 O3 nanocomposite (9% CuO) and EDX
histograms for (c) 9% CuO (d) 6% CuO and (e) 3% CuO nanoparticles.

(a) (b)

Fig. 3. Magnetic field versus magnetization hysteresis for the Al2 O3 and CuO–Al2 O3 .

656 Mater. Express, Vol. 9, 2019

Augmentation of ferromagnetism in CuO–Al2 O3 nanocomposite
Alam et al.
Materials Express
Table I. Lattice parameters, particles sizes and magnetization parameters of Al2 O3 and CuO–Al2 O3 nanocomposites.

Particle size nm Saturation magnetization (Ms  emu/g Coercivity (Cr ) Oe

Sample XRD SEM Ms at 5 K Ms at 300 K Cr at 5 K Cr at 300 K

Al2 O3 – – 0.0021 0.0013 35 ± 2 8±2

(3%) CuO–Al2 O3 24 ± 2 24 ± 2 0.0029 0.0015 73 ± 2 16 ± 2
(6%) CuO–Al2 O3 13 ± 2 12 ± 2 0.0037 0.0018 101 ± 2 16 ± 2
(9%) CuO–Al2 O3 11 ± 2 9±2 0.0054 0.0022 127 ± 2 17 ± 2

nanocomposite on the introduction of CuO nanoparticles
in the Al2 O3 matrix. This increase is directly attributed to
the introduction of CuO nanoparticles in the Al2 O3 matrix,
as discussed below.
The CuO nanoparticles are known to behave funda-
mentally different than their bulk analogue [37, 38]. The
CuO nanoparticles can show a ferromagnetic/paramagnetic
behavior, even at room temperature. This magnetic behav-
ior of CuO is the result of either the disordering of spins
on the nanoparticle surfaces or the spin-glass behavior of
the nanoparticles [38–40]. This magnetism in the CuO
nanoparticles is the direct consequence of the uncom-
pensated surface Cu2+ spins resulting in weak ferromag-
netism [37]. The confirmation of the Cu2+ state in the
CuO–Al2 O3 nanocomposite was provided by XPS analy-
sis, as shown in Figure 4. The chemical and electronic
states of copper and oxygen were determined directly
in the nanocomposite along the lines of Cu2p and O1s.

(a)

Article
IP: 5.10.31.211 On: Sat, 29 Apr 2023 16:15:14
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(b) (c)

Fig. 4. X-ray absorption spectrum for the copper and oxygen atoms in the CuO–Al2 O3 nanocomposite along the lines of (a) Cu (2p) (b) O (1s)
and (c) Al (2p3/2 ) (the spectrum shows both the raw data and the peak fitted data).

Mater. Express, Vol. 9, 2019 657

 Materials Express
Figure 4(a) shows the peak fitted XPS spectrum of the
Cu corresponding to Cu2p. The spectrum clearly reveals
the presence of Cu in the 2+ state with two strong peaks
at a distance of ∼19.8 eV from each other correspond-
ing to 2p3/2 and 2p1/2 at the peak positions at 934.34 and
954.14 eV, respectively. Each strong peak shows a satellite
peak (shake up) at a distance of ∼8.5 eV from the main
peak. This observation of the satellite peak is a character-
istic feature for the presence of the Cu2+ state in CuO nan-
particles [41]. Figure 4(b) shows the peak fitted spectrum
for oxygen for the 1s state. The spectrum shows a single
1s peak characterized by the binding energy of 529.3 eV.
It is important to note here that the presence of only a
single 1s peak for oxygen and the absence of the Ob com-
ponent are important for the enhancement of magnetism in
the nanocomposite. The presence of the Ob component is
associated with oxygen vacancies. The appearance of oxy-
gen vacancies will result in excess charge, leading to the
phase separation of the system and resulting in the appear-
ance of a diamagnetic state [39]. In addition to this, XPS
also verified the presence of Al2 O3 with a clear peak posi-
tion at a binding energy of 74.1 eV, corresponding to the
Al2 O3 phase, as shown in Figure 4(c). Furthermore, from
the magnetic measurements, we observed an increase in
the Ms as the content of CuO has from 3 to 9 wt.% at both
Article
temperatures. This behavior was observed for two reasons.
IP: 5.10.31.211 On: Sat, 29 Apr
Firstly, as the CuO nanoparticles showCopyright:
magnetic behavior,
American Scientific
an increase in their content will increase the total Delivered
magnetic by11.
moment in the sample. The second reason is the differ-
ence in particle sizes of the CuO in the three compositions,
as revealed from the XRD and microscopy analysis, since
the particle size of the CuO nanoparticles decreases the
magnetic moment increase both at low and high tempera-
tures [37, 38]. Both of these reasons collectively contribute
to the increase in the magnetic moment for 9% CuO–
Al2 O3 compared to the 3% CuO–Al2 O3 nanocomposite.
4. CONCLUSION
In summary, we have successfully synthesized a CuO–
Al2 O3 nanocomposite via a solution composition method.
Microscopy revealed the formation of CuO nanoparticles
on the surfaces of Al2 O3 nanosheets. The magnetic mea-
surement revealed an increase in its saturation magnetiza-
tion behavior, both at room and low temperature, with the
inclusion of CuO nanoparticles in the Al2 O3 matrix. This
observed magnetic behavior of the CuO–Al2 O3 nanocom-
posite, even at room temperature, is attributed to the
ferromagnetic nature of the CuO nanoparticles due to
uncompensated surface Cu2+ spins of copper ions.
Acknowledgment: The authors thank the Deanship of
Scientific Research in King Faisal University (Saudi
Arabia) for funding and providing the facilities required
for this research as a part of the Research Grants Program
(No. 17122002).
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Augmentation of ferromagnetism in CuO–Al2 O3 nanocomposite
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Received: 30 April 2019. Accepted: 30 August 2019.
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