Documente Academic
Documente Profesional
Documente Cultură
Received 20 August 2005; received in revised form 12 November 2005; accepted 18 November 2005
Abstract
Cubic nickel oxide (NiO) nanoparticles with uniform size around 4050 nm and well dispersion have been synthesized using a mixture of
nickel acetate and poly(vinyl acetate) (PVAc) as precursor followed by heat treatment at 723 K. The structure, morphology and crystalline phase
of the nickel oxide nanocrystals have been investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray
diffraction (XRD), Raman spectrum, UVvisible absorption spectrum and FT-IR. TEM images showed that the nickel oxide nanoparticles have
hexagonal structure with uniform size distribution around 4050 nm. Phase pure, cubic nickel oxide formation was identified from the XRD data.
2005 Elsevier B.V. All rights reserved.
1. Introduction gle phase, cubic NiO nanoparticles with nearly uniform par-
ticle size around 4050 nm and appreciable dispersion using
Nanoscale oxide particles of transition metals are gaining nickel acetate/poly(vinyl acetate) (PVAc) composite mixture
continuous importance for various applications such as cata- as precursor followed by heat treatment at 723 K. Properties
lysts, passive electronic components and ceramic materials [1]. of NiO nanoparticles were characterized by scanning electron
Due to their small size, nanoparticles exhibit novel material microscopy (SEM), transmission electron microscopy (TEM),
properties that are significantly different from those of their X-ray diffraction (XRD), Raman, UVvisible absorption and
bulk counterparts. Nickel oxide (NiO) nanoparticles with a FT-IR spectra.
uniform size and well dispersion are desirable for many appli-
cations in designing ceramic, magnetic, electrochromic and 2. Experimental
heterogeneous catalytic materials [2]. Several researchers have
prepared NiO nanoparticles by various methods like solgel Nickel(II) acetate tetrahydrate (Aldrich), N,N-dimethy for-
[3], surfactant-mediated synthesis [4], thermal decomposition mamide (Aldrich), 2-methoxy ethanol (Aldrich) and PVAc
[5], polymer-matrix assisted synthesis [6] and spray-pyrolysis (Celanase, Mn = 50,000) were used as received without further
[7]. Some of the above methods suffer from the difficulty in purification. Nickel oxide nanoparticles were prepared as fol-
size-homogeneity and well dispersion of NiO nanoparticles. lows. Ni(OAc)2 4H2 O (0.1 mol) was dissolved in 2-methoxy
In this article, we describe a simple method to prepare sin- ethanol (1 mol) by heating at 343 K for 2 h under stirring. PVAc
(14 wt.%) solution was prepared in DMF by stirring at room
temperature. Then a mixture of nickel acetate and PVAc in the
Corresponding authors. Tel.: +82 63 270 2351; fax: +82 63 270 2348.
1:4 ratio was stirred for 3 h at room temperature. The resulting
E-mail addresses: dharmaraj67@yahoo.com (N. Dharmaraj), composite mixture was heated at 423 K to remove the solvent
khy@moak.chonbuk.ac.kr (H.Y. Kim). and water. Finally, the solid mass obtained was ground well
0921-5107/$ see front matter 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.mseb.2005.11.021
112 N. Dharmaraj et al. / Materials Science and Engineering B 128 (2006) 111114
Fig. 2. Transmission electron microscopic (TEM) images of NiO nanoparticles; (a) lower magnification and (b) higher magnification (inset in (a) showed the selected
area electron diffraction pattern).
N. Dharmaraj et al. / Materials Science and Engineering B 128 (2006) 111114 113
Fig. 3. XRD pattern of NiO nanoparticles. Fig. 5. UVvisible absorption spectrum of NiO nanoparticles.
The formation of pure nickel oxide nanoparticles after heat some strong absorption in the region 12001800 cm1 that can
treatment at 723 K was also identified by FT-IR spectral studies be assigned to PVAc molecule (curve a). The samples obtained
(Fig. 6). The spectrum of nickel acetate/PVAc precursor showed after heating at 723 K did not exhibit any such bands thereby
confirming the complete removal of PVAc at this temperature,
but new peaks were found at 445 and 490 cm1 (curve b). These
peaks were undoubtedly assigned to Ni O stretching as was
reported earlier by other researchers [9,10].
4. Conclusion
Acknowledgements [3] K.C. Liu, M.A. Anderson, J. Electrochem. Soc. 143 (1996) 124.
[4] Y.D. Wang, C.L. Ma, X.D. Sun, H.D. Li, Inorg. Chem. Commun. 5
(2002) 751.
We gratefully acknowledge The Korean Research Foundation
[5] L. Xiang, X.Y. Deng, Y. Jin, Scripta Mater. 47 (2002) 219.
(KRF), Ministry of Science and Technology, Republic of Korea, [6] S. Deki, H. Yanagimito, S. Hiraoka, Chem. Mater. 15 (2003)
for awarding Brain Pool Fellowship (041S-4-12, 2004) to one of 4916.
the authors (N. Dharmaraj). We also thank Mr. Kang Jong-Gyun, [7] S.F. Liu, C.Y. Wu, X.Z. Han, Chin. J. Inorg. Chem. 19 (2003)
Electron microscope (EM) Laboratory, Center for University- 624.
[8] W. Xing, F. Li, Z.F. Yan, G.Q. Lu, J. Power Sources 134 (2004)
wide Research Facilities, Chonbuk National University, Chonju
1426.
561-756, Republic of Korea, for his help in recording the TEM [9] H. Guan, C. Shao, S. Wen, B. Chen, J. Gong, X. Yang, Inorg. Chem.
images of the nanoparticles. Commun. 6 (2003) 1302.
[10] P.S. Patil, L.D. Kadam, Appl. Surf. Sci. 199 (2002) 211.
References [11] M. Kanthimathi, A. Dhathathreyan, B.V. Nair, Mater. Lett. 58 (2004)
2914.
[1] C. Feldman, H.O. Jungk, Angew. Chem. Int. Ed. 40 (2001) 359. [12] S.I. Cordoba-Torresi, A. Hugot-Le Goff, S. Joiret, J. Electrochem. Soc.
[2] D. Tao, F. Wei, Mater. Lett. 58 (2004) 3226. 138 (1991) 1554.