Materials Today: Proceedings xxx (xxxx) xxx

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Materials Today: Proceedings

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Study on structural, electro-optical and optoelectronics properties of

CuO nanoparticles synthesis via sol gel method
D. Sivayogam a,⇑, I. Kartharinal Punithavathy a, S. Johnson Jayakumar a, N. Mahendran b
a
Department of Physics, T.B.M.L. College, Porayar, Affiliated to Bharathidasan University, Trichy, Tamilnadu 609307, India
b
Department of Physics, Idhaya College for Women, Kumbakonam Affiliated to Bharathidasan University, Trichy, Tamilnadu 612001, India

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

Article history: In this work, the popular metal oxide; Copper oxide (CuO) were prepared by well-known method; sol gel
Received 25 March 2021 technique. The structural and morphological examination was carried out on the fabricated metal oxide
Received in revised form 24 April 2021 and the XRD evaluation results validated the strong amalgamation of monoclinic bravais lattice system.
Accepted 28 April 2021
The nano level of the Cu particles was tested and the size determined to be 52–36 nm which was found to
Available online xxxx
be varied with respect to annealing temperatures. The structural modification of nanoparticle ensemble
crystal by the application of temperatures was studied. The Photocatalytic ability was tested and it was
Keywords:
evaluated by applying Tri-(chloroisopropyl) phosphate with CuO material. The optical property induce-
CuO
Monoclinic bravais
ment was recognized in the material by observing UV–Visible characteristics curves. The electric oper-
Electro-optical ated optical response between lower and higher wavelength zones in visible region was tested by
I-V characterization hyper polarization.
Ó 2021 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Confer-
ence On Impact Of Innovations In Science And Technology For Societal Development: Materials Science.

1. Introduction of photoconductive and electro-optical devices [8,9]. It also

behaved as field emission emitters and critical temperature oper-
In nanotechnology world, nano sized atomic-amalgamated ated high energy superconductors. It is a promising candidate
materials generally possessed specially customized and fanatically material to act as electrode materials for lithium ion battery and
tuned unique electro-optical, electro-mechanical, opto-electronic super-capacitors [10]. Because of its catalytic action, it is acted as
and opto-magnetic properties [1–3]. In recent days, transparent catalyst [11] in electro chemical hydrogen storage materials [9].
metal oxides and transparent conducting metal oxides have Due to its enhanced performance and new functionality character-
fascinated a great deal of notice since their easy synthesis and istics, it is directly used in solar cells [12] and gas sensors [13]. In
great tunable optoelectronic properties [4,5]. The copper metal is spite of its wide range of applications in opto-electronic industry,
transition metal hold many chemical and physical properties. It very few works have been traced in the literatures [14,15]. In this
is normally elastic and ductile, but only moderately acquiescent attempt, experimental results of the structural, morphological,
material and can be modulated by applying temperatures optical and magnetic properties studies are exposed in order to
(Table 1). reveal real application of nano CuO.
In general, copper oxide is a well-known semiconducting oxide
which normally existed in two phases; cupric oxide (CuO) and
cuprus (Cu2O) and they are amalgamated as monoclinic and cubic
structure [6,7] respectively. It is being a low production cost and 2. Experimental methods
excellent stability at room temperature, CuO is an important
transition-habituate material which is peculiarly enabled incredi- 2.1. Chemical handling
ble properties for wide range of applications such as fabrication
The Copper chloride (CuCl2), Sodium hydroxide (NaOH),
de-ionized water and ethyl acetate were purchased from Sigma
⇑ Corresponding author. Aldrich. All the chemicals were authenticated as an analytical
E-mail address: [email protected] (D. Sivayogam). grade and can be used without further purification.

https://doi.org/10.1016/j.matpr.2021.04.494
2214-7853/Ó 2021 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference On Impact Of Innovations In Science And Technology For Societal
Development: Materials Science.

Please cite this article as: D. Sivayogam, I. Kartharinal Punithavathy, S. Johnson Jayakumar et al., Study on structural, electro-optical and optoelectronics
properties of CuO nanoparticles synthesis via sol gel method, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2021.04.494
D. Sivayogam, I. Kartharinal Punithavathy, S. Johnson Jayakumar et al. Materials Today: Proceedings xxx (xxxx) xxx

Table 1
Structural Parametersof CuO nanoparticles different temperature.

Temperature Crystalline Size D(nm) Dislocatiuon Density(d)(x1015cm
2) Microstrain(e) (10-3) Stackingfault(SF) (x  10-2)
300 °C 17.66 5.4807 2.3455 1.1136
500 °C 39.19 0.9573 1.0023 0.4775
700 °C 41.82 0.8920 0.9520 0.4799

2.2. Synthesis set of (1 1 1) and (
1 1 1) inverted plane peaks were observed with
maximum intensity which represent the strong existence of planes
The most appropriate and easy to handle Sol-gel method was [11]. All other peaks were found with minimum intensity which
employed to prepare copper oxide nano particles. In this method- showed continuation of weak planes. The observed peaks with dif-
ological synthesis, Copper choloride (0.1 M) was taken to dissolve ferent intensities were confirmed the simple monoclinic lattice pat-
in DI water and then NaOH (0.2 M) was mixed in 100 ml of DI tern amalgamated in the nano CuO crystal. Apart from the major
water. The mixture was stirred separately for 30 min. The NaOH peaks, some other XRD signals were obtained along with the regular
solution was added drop by drop in to the copper Chloride solution pattern which showed the virtual or reciprocal lattice pattern of the
by using the burette. Afterward, the mixer was maintained under present existed CuO crystal. Here, the signals from inverted planes
constant stirring for two hours. Then, the precipitated gel was also appeared in the pattern which illustrated that, very appropriate
washed 4 to 5 times by using the mixer of ethanol and ethyl acet- monoclinic crystal system was formed in the synthesis.
ate and dried for 10 hrs at 80° C in fine hot air oven. Finally the In the case of annealing temperatures, particularly at 300° and
dried powder were calcined for three odd temperatures such as 500° C, so many peaks were not present with satisfactory intensity
300 °C, 500 °C, and 700 °C for one hour. which confirmed that, the crystal planes were not appeared to be
amalgamated perfectly. At the 700° XRD crest was appeared to
2.3. Characterization be acceptable and they found around agreeable angle of diffracted
pattern and these peaks emphasized that, the cubic lattice forma-
The X-ray diffraction studies of prepared nano particles are per- tion was obtained by the application of annealing temperatures
formed using EXPERT-PRO system with Goniometry PW 3050/60 above 600 °C. The present monoclinic crystal type was very strong
by CuKa radiation (k = 1.5406 Å). The Photoluminescence spectra when compared with other bravais lattice and concurrently, it
are recorded using the F-2500FL model photoluminescence spec- exposes very fanatic physical and chemical properties. According
trometer ROMVERSION (400001) with different excitation sources. to the assigned planes, the crystal parameters were calculated to
The absorption spectrum is taken from JASCO V-670 UV – VIS-IR be a = 4.689 Å, b = 3.426 Å and c = 5.132 Å. All the experiential
Spectrometer. The Vibrational spectra are recorded using FT-IR XRD signals predicted that, the present crystal made by nano
solid phase KBr pellet techniques. CuO was pure and free from contamination. According to the
Debye Scherrer’s formula [16], the particle size was measured to
be 36 nm and it was fine size which moderate and definitely the
3. Results and discussions
present nano Cu particles will expose its actual property.
3.1. XRD parametric analysis
3.2. UV–Visible spectral studies
The XRD spectral blueprint was recorded at different annealing
temperatures 300°, 500°, and 700° respectively, for the prepared The UV–Visible spectra were recorded for present nano sample;
sample of CuO and are shown in Fig. 1. According to the patter, the CuO at different annealing temperatures (300 °C to 700° C) in order
XRD peaks were obtained at 32°, 36°, 38°, 42°, 48°, 58°, 62° and 68° to study the temperature effect on nano sample and it is displayed in
which were assigned for the crystal interplanes; (1 1 0), (
1 1 1), the Fig. 2. The UV–Visible spectral pattern is usually measured for
(1 1 1), (
1 1 2), (
2 0 2), (0 2 0) and (
1 1 3). Of the all peaks, the first identifying the optical characteristics of the nano composite and it

Fig. 2. UV–visble absorption spectra of the CuO nanoparticles calcined at different

Fig. 1. XRD Plot of CuO nanoparticles calcined at different temperature. temperature.

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D. Sivayogam, I. Kartharinal Punithavathy, S. Johnson Jayakumar et al. Materials Today: Proceedings xxx (xxxx) xxx

was registered in the region of 200–700 nm. Here, the observed annealing temperatures such as 300 °C, 500 °C, 700 °C are shown
spectra illustrated that, at 300 °C, the optical response was found in Figs. 4 and 5 respectively. For CuO nano composite at normal
to be more than 60% and it was increased more than 75% for nano temperature, the PL peak was observed at 380 nm with maximum
samples at 500°and 700° C. the optical response was found to be ele- intensity. From this peak, it was found that, the excitation was tak-
vated for higher temperatures which was mainly due to the ing place in the material at 380 nm which was mainly due to the
improvement of the quality of the crystallinity for the present case. intrinsic characteristics of the CuO in which the interstitial vacancy
Here, up to 300 nm, the optical activity was linearly increased with produced inside the material [11,20].
wavelength and it was saturated from 400 nm up to 700 nm. In this The Fig. 4 showed the series of peaks of parallel graphs which
case, the linear optical property was interpreted since the metal was are recorded for the annealing temperatures from 300 °C to
paramagnetic. When the magnetic field is applied on the nano mate- 700 °C for CuO extrinsic composite. Here, at all temperatures, the
rial, the polarizability of Cu–O bonds is responded and hyper polar- similar peaks were appeared by which it was found that, there
ization is taking place [17–19]. Simultaneously, the linear optical was no characteristics shift observed with respect to the annealing
property is changed in to non linear optical property. From this temperatures. Instead of that, the intensity of the peaks was
observation, it was found that, the optical characteristics were found increased much due to the annealing temperatures. The PL signals
facilitated by electric field and it is tunable. were obtained at 360, 375, 386, 411, 494, 505, 525 and 545 nm
respectively for all temperatures. In this graph, the peak intensity
3.3. SEM analysis was observed maximum from UV region to visible region, particu-
larly, at high frequency of visible region, the PL intensity was found
The scanned image of micro surface of nano CuO is presented in to be maximum and it was clear that, the PL activity of the nano
the Fig. 3. As seen in figure, two pictorial diagrams were obtained composite was observed to be more in high frequency region.
at two different annealing temperatures such 500°Cand 700 °C. The Apart from that, at higher wavelength region, the peaks at 525
surface topography and particles compositions in the material and 545 were appeared with additive PL intensity which was due
were seen in the figure clearly. At 500 °C, the amalgamation of to the enriched PL activity of the present nano material. In this
CuO nano particles was formally obtained in which the particles case, the PL spectral impression was found on either side of lower
assimilation was virtually appeared and approximate grain size and higher wavelength region. From this observation, it was
can be measured. At 700 °C, the well defined formation of Cu nano inferred that, the PL activity can be tuned in the CuO material by
particles was observed. The Fig. 3 showed well distinguished nano doping nano impurity.
particles between two temperatures which confirmed the anneal-
ing temperature influencing the particle size and morphological
3.5. I-V characterization of junction diode
amalgamation of monoclinic crystallization. From this observation,
it was confirmed that, the method using in this work was found to
The formation of the P-N junction diode is carried out by the n-
be efficient to prepare nano particles and proportionately, the Cu
type Si wafer with p-type materials annealed at different temper-
nano particles are formed perfectly and efficiently. Such particles
ature such as as-prepared CuO (300 °C), CuO (500 °C) and CuO
will expose its fundamental physical and chemical property surely.
(700 °C) samples. The ideality factor (n) and barrier height (Ub)
were measured under darkness and illumination of light for pre-
3.4. PL examination pared junction diodes. The reverse to forward bias current mea-
surement is taken for the applied voltage of
3 to + 3 V. Fig. 5
The photoluminescence spectra for CuO nano composite was shows the I-V characteristics of prepared junction diode under
recorded at 250 nm and 300 nm as excitation wavelengths for dark and illumination. The samples junction diode exhibits a good
rectifying nature in dark and under illumination.
Fig. 6 illustrates the semi-log plot of the current density In(J)
versus applied voltage (V). The diode parameters of ideality factor

Fig. 3. SEM image of CuO nanoparticles calcined at different temperature. Fig. 4. Photoluminescence spectra of the prepared samples of CuO nanoparticles.

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D. Sivayogam, I. Kartharinal Punithavathy, S. Johnson Jayakumar et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 5. I-V characteristics for prepared, PN Junction diodes in dark and under illumination.

!
(n) and barrier height (Ub) are calculated from the forward bias J-V KT AA T2
plot. These parameters provide an information about the charge Ub ¼ ln ð3Þ
q J0
transport mechanism of the p-n junction interface and the elec-
trode contact with the oxide layer. Using the thermionic emission
(TE) equations, the current density (J) of the samples junction
diode was calculated as following Eq. (1) [21],


qV
J ¼ J0 exp
1 ð1Þ
nKT where A is the active area of prepared diode and A* is the Richard-
where Jo is reverse saturation current density, q is charge of son constant. The n and Ub values under darkness and under light
electron, V is applied potential, n is ideality factor, K is Boltzmann illumination values are shown in Table 2.
constant and T is absolute temperature. Using Eq. (1) for V  3kT/q, The n value is unity (i.e., n = 1) for an ideal P-N diode but in the
n and Jo values were obtained from the slope and interception of present work, the n values are obtained as more than unity. The
semi-log forward bias J-V plot. Thus, n and Ub were calculated results suggest that the non-ideal behavior of prepared junction
by the following Eqs. (2) and (3), diode samples may be owing to the presence of an interfacial thin
native oxide layer (SiO2) and barrier in-homogeneities.It may also
q dV be owing to series resistance and nonlinear metal–semiconductor
n¼ ð2Þ
KT dðln JÞ contact. Another reasons may be the abnormalities of the inorganic
film thickness and non-uniformity of the interfacial charges.
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D. Sivayogam, I. Kartharinal Punithavathy, S. Johnson Jayakumar et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 6. Plots ln J vs. V for prepared,PN Junction diode in dark and under illumination.

Table 2
The parameters of Ub and n calculated from J-V method.

Diode J-V method

Barrier width (Ub) Ideality factor (n)
Dark Light Dark Light
300 °C 0.721425117 0.751743354 11.53065617 4.597503229
500 °C 0.727219917 0.700699071 16.87776516 6.166840901
700 °C 0.684575461 0.66091448 5.290324069 8.857295495

4. Conclusion analysis. The optimized results were obtained and the observation
was made on the examination was validated with the literatures.
In this attempt, the CuO nano particles were synthesized and The obtained results of XRD peaks showed the present nano com-
the metal oxide formation was successfully made. The morpholog- posite was to be monoclinic. The crystal size was measured to be
ical and structural studies were carried out by performing the XRD ranged from 52 to 36 nm by the application of annealing

5
D. Sivayogam, I. Kartharinal Punithavathy, S. Johnson Jayakumar et al. Materials Today: Proceedings xxx (xxxx) xxx

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