Ni Doped Sno2

Iranica Journal of Energy & Environment 4 (1) Special Issue on Nanotechnology: 49-52, 2013
ISSN 2079-2115
IJEE an Official Peer Reviewed Journal of Babol Noshirvani University of Technology
DOI: 10.5829/idosi.ijee.2013.04.01.08
BUT
Ni-Doped SnO2 Nanoparticles Synthesized by Chemical Co-Precipitation Method

1
Mousa Aliahmad and 2Mohsen Dehbashi
1
Department of Physics, Faculty of sciences, University of Sistan and Baluchestan, Zahedan, Iran
2
Department of Physics, Faculty of sciences, University of Zabol, Zabol, Iran
(Received: August 15, 2012; Accepted in Revised Form: February 4, 2013)

Abstract: Ni-doped SnO2 nanocrystalline powders have been synthesized by the co-precipitation method from
SnCl2.2H2O and NiCl2.6H2O. Nanoparticles crystallize in lower temperature (350°C) and shorter time (2hours)
respect to other methods. The samples have been characterized by various advanced techniques such as, X-ray
diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Transmission electron microscopy (TEM)
and Vibrating sample magnetometer (VSM). The X-ray diffraction reveals that all samples are pure rutile-type
tetragonal phase and the average particles size was observed to vary from 32 nm to 24 nm as the nickel content
was increased, The TEM images confirms the size of tin oxide particles in nanoscale and VSM measurements
indicate that Ni-doped samples have superparamagnetic properties and they are single-domain nanoparticles.
Key words: Nanoparticles Nickel Tin oxide Superparamagnetic
INTRODUCTION precise control over the stoichiometry, low temperature

synthesis, high purity and high chemical homogeneity.
In recent years, the interest in the physical properties
of semiconducting metal oxide, such as SnO2, TiO2 and MATERIALS AND METHODS
ZnO, has significantly increased due to their potential
applications, in special when they are intentionally doped Ni doped SnO2 nanoparticles have been synthesized
with magnetic elements. Tin oxide (SnO2) with a wide- by chemical co-precipitation method, SnCl 2.2H2O
band-gap n-type semiconductor (3.6eV at 300°K), known (98% Merck, Germany) and NiCl 2.6H2O (98% Merck)
as one of the most widely used semiconducting oxides have been used as starting materials for the synthesis of
due to its chemical and mechanical stabilities. It has been Ni doped SnO2 nanoparticles. The required amounts of
widely studied over decades because of its most SnCl2.2H2O and NiCl2.6H2O were added to double-distilled
applications in various optoelectronic devices, water and dissolved. Then, an aqueous ammonia (1M)
transparent electrodes and sensors [1-3].The properties of was dropped into the mixture solution with constant
SnO2 nanostructures can be enhanced by several ways stirring at 30°C until a pH of 5 reached. The resulting
like impurity doping [4], coating with surfactants [5] and precipitate were collected, washed with distilled water and
annealing [6]. The final properties of impurity doped then dried at 100°C for several hours. Heating treatments
SnO2 nanoparticles are related to both composition and of the synthesized nano-powders were conducted at
processing method. Nanoparticles of tin oxide have been 350°C for 2 hours. The preparation process of Ni-doped
synthesized through different chemical routes, such as SnO2 nanocrystalline powders is shown in Figure 1.
co-precipitation[7], hydrothermal [8] and sol gel [9] Crystallinity, structure and particle size of Ni-doped SnO 2
methods among others. In this work, we synthesized nanoparticles were determined by X-ray diffraction (XRD)
Ni-SnO2 nanoparticles by chemical coprecipitation method using Rigaku-Miniflex X-ray diffractometer with CuK
because this method has some advantages such as radiations ( =0.15406 nm) in 2 range from 10° to 70°.
Corresponding Author: M. Aliahmad, Department of Physics, Faculty of sciences, University of Sistan and Baluchestan,
Zahedan, Iran. Tel/Fax: +985412446565, E-mails: [email protected].
49
Iranica J. Energy & Environ., 4 (1) Special Issue on Nanotechnology: 49-52, 2013
Fig. 2: XRD patterns of (S1) SnO2, (S2) Sn0.99Ni0.01O2 and

(S3) Sn0.98Ni0.02O2 nanoparticles
Fig. 3: The effect of the Ni-doping quantities on the

average particle size of Ni-SnO2 nanocrystalline
Fig. 1: The preparation process schema of Ni-SnO2 powders
nanoparticles
Morphologies and particle sizes of the samples were

observed with a Hitachi H-800 transmission electron
microscope (TEM), FTIR spectrum was recorded in the
range 400-4000 cm 1 on a FTIR 460-plus
spectrophotometer using KBr pellets. The magnetic
measurements were obtained using a Vibrating Sample
Magnetometer (VSM) in the room temperature.
RESULTS AND DISCUSION

Fig. 4: FT-IR spectra of (S1) SnO2, (S2) Sn0.99Ni0.01O2 and
XRD patterns of Sn1-xNixO2 (with x = 0, 0.01 and 0.02) (S3) Sn0.98Ni0.02O2 nanoparticles
annealed at 350°C for 2 h are shown in Figure 2, in which
S1, S2 and S3 correspond to x = 0, 0.01 and 0.02, peaks decreases with increasing Ni content and the
respectively. All diffraction peaks are well assigned to full-width at half-maximum (FWHM) of the peaks increases
tetragonal crystalline phase of tin oxide (with the with increasing Ni content, as well indicates that average
reference pattern JCPDS 880287) and the Ni doping does particle size of samples decreases gradually as the Ni
not change the tetragonal structure of SnO2. From content increases (Figure 3). The average particle size of
Figure 2, it is noted that the intensity of the Sn1-xNixO2 samples are calculated using Scherrer’s formula,
50
Fig. 5: TEM images of (S1) SnO2, (S2) Sn0.99 Ni0.01O2 and (S3) Sn0.98 Ni0.02O2 nanoparticles
Fig. 6: Room temperature hysteresis curves of (S2) Sn 0.99 Ni0.01O2 and (S3) Sn 0.98 Ni0.02O2 nanoparticles
0.9 3398 cm 1 is owing to the vibration of O-H and the band

D=
cos( ) located at 1636 cm 1 is due to the H-O-H vibrating mode
where is the wavelength of CuK radiation (= 0.154056 of the absorbed water, while the bands at around 528 and
nm), is the full width at half maximum (FWHM) of the 643 cm 1 can be attributed to the Sn-O stretching
(hkl) peak at the diffracting angle 2 [10], all the peaks are vibration and the O-Sn-O blending vibration in SnO2.
used to calculate the average particle size of samples. TEM images of (S1) SnO2, (S2) Sn 0.99Ni0.01O2 and (S 3)
The average particles size of samples are found to be Sn0.98Ni0.02O2 nanoparticles calcined at 350°C for 2 hours
32nm for sample S1, 29 nm for sample S 2 and 24nm for are shown in Figure 5. It is shown that the powders are
sample S3 by using scherrer’s formula. uniform in size and the particle size of samples decreases
The FT-IR transmittance spectra of different samples with increasing doping quantities of Ni. The particle
are given in Figure 4, in which the band located at shape of the samples is spherical with an average diameter
51
of 28 nm for pure SnO2, 25 nm for 1% Ni-doped SnO2 and 2. Lalauze, R., J.C. Le Thiesse, C. Pijolat and
21 nm for 2% Ni-doped SnO2. The results of average M. Soustelle, 1987. SnO2Gas Sensor. Effect of
particle size measurement from TEM observations are SO2Treatment on TheElectrical Properties of SnO2.
having good agreement with the XRD line broadening Solid State Ionics, 12: 453-457.
method. 3. Hidalgo, P., R.H.R. Castro, A.C.V. Coelho and
To probe the magnetic properties of Sn 0.99Ni0.01O2 and D. Gouvêa, 2005. Surface Segregation and
Sn0.98Ni0.02O2 nanoparticles, room temperature Consequent SO2 Sensor Response in SnO2 - NiO.
magnetization is performed on the samples and is shown Chemistry of Materials Journal, 17: 4149-4153.
in Figure 6. It shows no hysteresis loops and the 4. Cabrera, A.F., A.M. Mudarra Navarro, C.E. Rodríguez
magnetization curve exhibits zero remanence and Torres and F.H. Sánchez, 2007. Mechanosynthesis
coercivity (the coercive field is the applied magnetic field of Fe-doped SnO2 Nanoparticles. Physica B.,
that needs to be applied in the direction opposite the 398: 215-218.
initial magnetic field, to bring the magnetization back to 5. Khun Kamalpreet, K., A. Mahajan and R.K. Bedi,
zero), which proves that nanoparticles have 2011. Effect of Cationic/Anionic Organic Surfactants
superparamagnetic properties and they are single-domain on Evaporation Induced Self-Assembled Tin Oxide
nanoparticles [11, 12]. The superparamagnetism enables Nanostructured Films. Applied Surface Science,
the nanoparticles to respond to an applied magnetic field 257: 2929-2934.
without any permanent magnetization and redisperse 6. Cukrov, M.L., T. Tsuzuki and P.G. McCormick, 2000.
rapidly when the magnetic field is removed. In the SnO2 Nanoparticles Prepared by Mechanochemical
Figure 6, it can be also observed that magnetization of Processing. Scripta Materialia, 44: 1787-1790.
samples increases with increasing doping quantities of Ni. 7. Ricardo, H.R. Castro, P. Hidalgo, R. Muccillo and
D. Gouvea, 2003. Microstructure and Structure of
CONCLUSIONS NiO-SnO2and Fe2O3-SnO2systems.Applied Surface
Science, 214: 172-177.
Ni-doped SnO2 nanocrystalline powders were 8. Baik, N.S., G. Sakai, N. Miura and N. Jamazoe, 2000.
synthesized by the co-precipitation method from Preparation of Stabilized NanosizedTin Oxide
SnCl2.2H2O and NiCl2.6H2O. XRD results show that the Particles by Hydrothermal Treatment.Journal of the
average particles size is in the range from 24 to 32 nm, it is American Ceramic Society, 83: 2983-2987.
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nanoparticles have pure rutile structure, TEM images of Prepared by Cheap Chemical Method. Sensors and
SnO2 and Ni-SnO2 powders shows that the particle shape Actuators B., 70: 153-164.
of the samples is spherical with an average diameter of 10. Patterson, A.L., 1939. The Scherrer Formula for X-ray
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nm for 2% Ni-doped SnO2, confirming the reduction in Archives (PROLA), 56: 978-982.
particles size as a result of Ni doping in SnO2. Particles 11. Zhiya, M.A., G. Yueping and H. Liu, 2005. Synthesis
size obtained from TEM analysis is comparable with and Characterization of Micron-Sized Monodisperse
average particles size calculated from XRD spectra and Superparamagnetic Polymer Particles with Amino
VSM measurements of nickel doped SnO2 nanoparticles Groups. Journal of Polymer Science Part A: Polymer
indicates that both samples Sn0.99Ni0.01O2 and Sn 0.98Ni0.02O2 Chemistry, 43: 3433-3439.
have superparamagnetic properties and they are 12. Ashby, M.F., P.J. Ferreira and D. L.Schodek, 2009.
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52

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Iranica Journal of Energy & Environment 4 (1) Special Issue on Nanotechnology: 49-52, 2013

Ni-Doped SnO2 Nanoparticles Synthesized by Chemical Co-Precipitation Method

(Received: August 15, 2012; Accepted in Revised Form: February 4, 2013)

Key words: Nanoparticles Nickel Tin oxide Superparamagnetic

INTRODUCTION precise control over the stoichiometry, low temperature

Fig. 2: XRD patterns of (S1) SnO2, (S2) Sn0.99Ni0.01O2 and

Fig. 3: The effect of the Ni-doping quantities on the

Morphologies and particle sizes of the samples were

RESULTS AND DISCUSION

0.9 3398 cm 1 is owing to the vibration of O-H and the band

1. Vishwakarma, S.R., Rahmatullah and H.C. Prasad,

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