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Sci.Int.(Lahore),27(4),3085-3088,2015 ISSN 1013-5316; CODEN: SINTE 8 3085
July-August
SYNTHESIS OF COPPER NANOPARTICLES BY CHEMICAL REDUCTION
METHOD
Hina Khalid, S. Shamaila*, N. Zafar
Department of Physics, University of Engineering and Technology, Lahore-54890, Pakistan.
*Corresponding author: Email: drshamaila.uet@gmail.com
Shamaila Shahzadi
Associate Professor.
Department of Physics,
University of Engineering and Technology, Lahore-54890, Pakistan.
Ph. (off) +92-42-99029204
ABSTRACT: Copper nanoparticles have been synthesized by using chemical reduction method using de-ionized water as
solvent. The surface morphology is observed by Atomic Force Microscope (AFM). The formation of copper nanoparticles was
confirmed by UV-Visible spectrophotometer (UV-Vis), X-ray diffraction (XRD) and fourier transform infrared spectroscopy
(FTIR). Copper nanoparticles fabricated by chemical reduction method have diameter in the range 14 nm to 55 nm. Structural
analysis revealed the face centered cubic (fcc) crystal structure of copper nanoparticles.
Keywords: Chemical Reduction, Copper, UV-Visible Spectrophotometer, AFM, FTIR.
INTRODUCTION
Nanoparticles are fascinating materials that find many
applications in fields of basic and applied research. Copper
(Cu) nanoparticles (NPs) with high fraction of surface atoms
and high specific surface area have been widely studied. The
Cu NPs have special physical and chemical characteristics
which include catalytic activity, optical properties, anti-
microbial activity and electronic properties [1]. Copper
nanoparticles can be fabricated by using different physical
and chemical techniques such as chemical reduction [2, 3],
laser ablation [4, 5], electrochemical [3], thermal
decomposition [6] and polyol method [7]. Among all these
methods chemical reduction is convenient method for the
fabrication of nanoparticles. High yield of metallic
nanoparticles has been attained by chemical reduction
method (CRM). This method is economical, simple, faster
and can have better size distribution of nanoparticles by
controlling the experimental parameters [8]. Currently, noble
metal nanoparticles have been extensively studied for many
applications. For nanoparticles synthesis the noble metals
such as silver and gold are being used, despite their cost [9-
11]. In this context, copper are good alternative material
because they are more economical than silver and gold. L. A.
Figueroa et al have reported that chemically synthesized
copper nanoparticles having diameter of 25 nm [12].
In the current research, the attention have been focused on the
fabrication of Cu NPs. Nanoparticles are synthesized by
chemical reduction method (CRM).The Cu NPs were
characterized by using different techniques such as UV-
Visible Spectrometry, Atomic force microscopy (AFM), X-
ray diffractometer (XRD) and Fourier transform infrared
spectra (FTIR).
Materials and method
Materials
All of chemicals used in experiment are of analytical grade
and used as purchased without any purification. Copper
sulfate pentahydrate (CuSO4·5H2O), of 98% purity is used.
De-ionized water used as a solvents. Sodium borohydride
(NaBH4) is used as reducing agent, while sodium hydroxide
(NaOH) is used to adjust the pH. Ascorbic acid is used as the
antioxidant for colloidal Cu NPs.
METHOD
The flowchart of experimental procedure is shown in figure
1. Ascorbic acid solution (0.02 M) was prepared in de-
ionized water. A 0.01 M solution of copper sulfate
pentahydrate (CuSO4·5H2O) separately prepared in de-
ionized water and this was added to ascorbic acid solution
under continuous magnetic stirring. To adjust the pH, 1 M
solution of NaOH in de-ionized water was added. After
stirring for 30 minutes at room temperature, 0.1 M solution of
NaBH4 in de-ionized water was added under continuous
stirring. The stirring was continued for 15 minutes in ambient
atmosphere to complete the reaction. The blue color of initial
reaction mixture turned red-brown color as shown in figure 2.
Cu2+ + 2BH4- Cu + H2 + B2H6
Figure 1: Flow chart of experimental process.
3086 ISSN 1013-5316; CODEN: SINTE 8 Sci.Int.(Lahore),27(4),3085-3088,2015
July-August
Figure 2: Colloidal solution of copper nanoparticles, initial blue
color turned red-brown.
RESULTS AND DISCUSSIONS
To study the stability of Cu colloidal solution in air, the
absorption of Cu NPs was measured by UV-visible
spectroscopy. The absorption band of copper nanoparticles
has been reported in the range of 500-600nm [10, 13]. UV-
visible absorption spectra of Cu NPs by chemical reduction
method (CRM) is shown in figure 3. This spectrum is
recorded immediately after the synthesis of particles. The
figure show the absorption peaks at 588 nm respectively,
which proves the formation of the copper nanoparticles in the
solution [14]. The initial blue green color turned red-brown,
the shifting in color is due to the surface plasmon resonance
(SPR). Metals possess SPR in visible region due to free
electrons, which give such intense colors. These properties
observed in Cu, Ag and Au due to presence of free electrons
[12].
Figure 3: UV-visible spectra of copper nanoparticles fabricated
by chemical reduction.
AFM is an important technique for study the morphology of
nanoparticles. Tapping mode AFM imaging is applied to
study copper nanoparticles. Figure 4 shows an AFM image (2
μm ×2 μm) of copper nanoparticles (3D) having particle size
range 14 nm to 55 nm.
Figure 4: 3D topographical view of copper nanoparticles, having
particle size 14 nm to 55 nm.
Figure 5: XRD pattern of the copper nanoparticles.
The crystal structure and phase composition of synthesized
copper nanoparticles is analyzed by XRD, as shown in figure
5. The diffraction data exhibits that the copper nanoparticles
have face centered cubic structure (FCC) with characteristic
diffraction peaks (111), (200) and (220) at 2-theta value of
43.4º, 51.1º and 74.9º respectively. On the other hand, two
diffraction peaks were indexed to cuprous oxide (Cu2O)
having corresponding peaks to (110) and (220) at 2-theta
value of 29.1o and 60.5o respectively. The presence of Cu2O
indicates the partial oxidation of copper nanoparticles with
dissolved oxygen in the solution [14, 15].
For copper nanoparticles, the oxygen present in ambient
atmosphere rapidly forms an oxide layer on the particle
surface when exposed to air. This means that copper
nanoparticles could be synthesized in atmospheric
environment, at atmospheric pressure and at room
temperature by using de-ionized water as solvent in the case
of present work. It is not necessary to perform the chemical
Sci.Int.(Lahore),27(4),3085-3088,2015 ISSN 1013-5316; CODEN: SINTE 8 3087
July-August
reaction in an inert atmosphere. All the parameters or
variables reduce the cost of the process [15, 16].
Figure 6: FTIR spectra (a) de-ionized water (b) copper
nanoparticles.
FTIR spectra of de-ionized water and copper nanoparticles
are shown in Figure 6. In the 3500–3000 cm-1 region, a broad
absorption of hydroxyl group (O-H) of de-ionized water
appear at 3234 cm-1 and 3214 cm-1 before and after
nanoparticles formation, respectively, showing 20 units red
shift of this polar group. Intermolecular and intramolecular
hydrogen bonds are considered to be responsible for the
broadening of the –OH band in the FTIR spectra. This
decrease in wave number may occur due to interaction of
copper nanoparticles with–OH group [17]. The bands are in
the region 2000-1500 cm-1 are due to C=C bond. This bond
appears at 1629 cm-1 before nanoparticles formation and
shifted at 1619 cm-1 after nanoparticles formation. The
shifting in wave numbers was due to the C=C stretching and
shows the co-ordination with copper nanoparticles [18, 19].
CONCLUSION
In this work, synthesis of copper nanoparticles (Cu NPs) has
been investigated by chemical reduction method (CRM). The
average size of copper nanoparticles prepared by CRM is 14
to 55 nm. The absorption peak appeared at 591 nm which
confirms the formation of copper nanoparticles. The observed
fcc XRD peaks for copper nanoparticles are ascribed the
growth along different crystallographic planes. Another phase
coprous oxide (Cu2O), also observed which shows the partial
oxidation of copper nanoparticles with dissolved oxygen in
the solution.
ACKNOWLEDGEMENTS
The authors gratefully acknowledge the Physics and polymer
department of University of Engineering and Technology,
Lahore, Physics department of COMSATS, Lahore and
Chemistry department of Forman Christian College, A
Charted University, Lahore for accomplishing the AFM,
FTIR and XRD and UV- visible spectrophotometer analysis
of the synthesized nanoparticles respectively.
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