Preparation and characterization of NiO nanofibres via an electrospinning technique

Article abstract of DOI:10.1016/j.inoche.2003.08.003

Thin PVA/nickel acetate composite fibres were prepared by using sol-gel processing and electrospinning technique. After calcinations of the above precursor fibres, NiO nanofibres with a diameter of 50-150 nm could be successfully obtained. The fibres were characterized by SEM, FT-IR, WAXD, respectively. The results showed that the crystalline phase and morphology of NiO fibres were largely influenced by the calcination temperature.

Full text of DOI:10.1016/j.inoche.2003.08.003

Inorganic Chemistry Communications 6 (2003) 1302–1303
www.elsevier.com/locate/inoche
Preparation and characterization of NiO nanofibres
via an electrospinning technique
*
Hongyu Guan, Changlu Shao , Shangbin Wen, Bin Chen, Jian Gong, Xinghua Yang
Department of Chemistry, Northeast Normal University, 130024 Changchun, China
Received 18 June 2003; accepted 12 August 2003
Published online: 3 September 2003
Abstract
Thin PVA/nickel acetate composite fibres were prepared by using sol–gel processing and electrospinning technique. After cal-
cinations of the above precursor fibres, NiO nanofibres with a diameter of 50–150 nm could be successfully obtained. The fibres were
characterized by SEM, FT-IR, WAXD, respectively. The results showed that the crystalline phase and morphology of NiO fibres
were largely influenced by the calcination temperature.
Ó 2003 Elsevier B.V. All rights reserved.
Keywords: NiO nanofibres; PVA/nickel acetate composite; Electrospinning; PVA
In recent years, nanostructured materials have been
actively studied due to both scientific interests and po-
tential applications [1,2]. Among them, much attention
has been focused on the research field of one-dimen-
sional nanostructured materials, such as nanorods,
nanowires, or nanofibres, because of their potential
applications in nanodevices [3–5]. Nickel oxide (NiO) is
a very important material extensively used in catalysis
PVA/nickel acetate composite was obtained. Then, it
was contained in a plastic capillary. A copper pin con-
nected to a high-voltage generator was placed in the
solution, and the solution was kept in the capillary by
adjusting the angle between capillary and the fixing bar.
A grounded iron drum, covered with an aluminium foil,
served as counter electrode. A voltage of 20 kV was
applied to the solution and a dense web of fibres was
[
6], battery cathodes [7,8], gas sensors [9], electrochromic
films [10,11], and magnetic materials [12,13]. A few
methods on the preparation of NiO nanocrystalline
powder and films were reported [14–16]. However, to
our knowledge, there have been no reports on the
preparation of NiO nanofibres.
[200]
[111]
[220]
In this paper, we obtained the electrospun fibres of
PVA/nickel acetate composite by using sol–gel process-
ing and electrospinning technique. And, then got the
NiO nanofibres by calcinations of the precursor fibres.
The procedure was as follows. Fifteen grams aqueous
PVA (Mn 80,000) solution of 10 wt% was dropped
slowly into the solution of nickel acetate (1 g Ni(CH3
COO)2 ꢀ 4H2O and 4.0 g H2O), and the reaction pro-
ceeded in a water bath at 50 °C for 5 h. A viscous gel of
d
c
b
a
10
20
30
40
50
60
70
2
θ(degrees)
Fig. 1. WAXD results for various fibre samples: (a) PVA/nickel acetate
composite fibres; (b) calcinations at 400 °C; (c) calcinations at 550 °C;
(d) calcinations at 700 °C.
*
Corresponding author. Tel.: +864315269551; fax: +864315269941.
E-mail address: changlushao@yahoo.com.cn (C. Shao).
1
387-7003/$ - see front matter Ó 2003 Elsevier B.V. All rights reserved.
doi:10.1016/j.inoche.2003.08.003

H. Guan et al. / Inorganic Chemistry Communications 6 (2003) 1302–1303
1303
Fig. 2. Scanning electron microscopy photographs of various fibre samples: (a) PVA/nickel acetate composite fibres; (b) calcinations at 400 °C; (c)
calcinations at 550 °C; (d) calcinations at 700 °C.
collected on the aluminium foil. The fibres thus formed
were dried initially 12 h at 70 °C under vacuum, and
then calcined at 400–700 °C at a rate of 240 °C h and
remained 10 h at the required temperature.
fibres of PVA/nickel acetate composites as precursor
and through calcinations treatment. This route might
open a new door to making nanofibres of inorganic
materials. By modifying the parameters of sol–gel or
electrospinning processing, one could also expect to be
able to make nanofibres of inorganic materials with
smaller diameter.
ꢁ
1
IR results showed that all the organic molecules could
be removed completely from PVA/nickel acetate com-
posite fibres after calcination at 700 °C, and a new peak
ꢁ
1
around 442 cm assigned to mNi–O of nickel oxide (NiO)
appeared [17,18], indicating that the fibres obtained at
this temperature were pure inorganic NiO species. Fig. 1
gave the WAXD curve for various fibres samples. As
showed in Fig. 1(a), there existed a broad peak around
Acknowledgements
The present work is supported financially by Na-
tional Natural Science Foundation of Jilin Technology
Government (No. 20020613).
2
h ¼ 20°, corresponding to the (1 0 1) plane of semi-
crystalline PVA [19] in PVA/nickel acetate composite
fibres.
However, after the PVA/nickel acetate composite fi-
bres were calcined at 400 °C (Fig. 1(b)), crystalline peak
of PVA disappeared, and three broad reflection peaks
corresponding to pure cubic NiO [16] appeared at
References
[
[
[
1] R.E. Cavicchi, R.H. Silsbe, Phys. Rev. Lett. 52 (16) (1984) 1435.
2] P. Ball, G. Li, Nature 355 (1992) 761.
3] J. Hu, M.Y. Ouyang, C.M. Lieber, Nature 399 (1999) 48.
2
h ¼ 37:2° (1 1 1), 43.2° (2 0 0), 62.8° (2 2 0). Notably,
when increasing calcination temperature to 550 and 700
C (Fig. 1(c) and (d)), all the peaks belong to NiO cubic
°
[4] D.S. Xu, G.L. Guo, L.L. Gui, Y.Q. Tang, E.J. Shi, E.X. Jin, Appl.
Phys. Lett. 75 (1999) 481.
phase were markedly sharpening with high intensity,
which suggested that the crystallinity of NiO phase was
higher at high calcination temperature than which ob-
tained at low calcination temperature. As compared
with the IR results, the products obtained at 700 °C were
pure NiO fibres. The SEM photographs of PVA/nickel
acetate composite fibres and the fibres calcined at 400–
[
5] J.R. Heath, P.J. Kuekes, Snyderg, R.S. Williams, Science 280
(
1998) 717.
[
[
6] D. Levin, J.Y. Ying, Stud. Surf. Sci. Catal. 110 (1997) 367.
7] M. Yoshio, Ag. Okada, M. Takash, J. Power Sources 74 (1) (1998)
46.
[
[
8] H.X. Yang, D.F. Dong, X.H. Hu, J. Power Sources 79 (2) (1999)
2
9] T. Hidehiro, Patent J P 09263444 7 10 (1997) 5.
56.
7
00 °C were showed in Fig. 2. It can been seen that the
[
10] E.L. Miller, R.E. Rocheleau, J. Electrochem. Soc. 144 (1997)
072.
[11] Y. Wu, G. Wu, X. Ni, J. Vac. Sci. Technol. 19 (3) (1999) 228.
surface of PVA/nickel acetate composite fibres (Fig. 2(a))
was smooth due to the amorphous nature of PVA and
nickel acetate composites. On calcinations at 400 and
3
[
[
12] Y. Wang, J. Ke, High Technol. Lett. 3 (1) (1997) 92.
13] A.C. Felic, Ag. Lama, M.J. Piacentini, Appl. Phys. 80 (12) (1997)
5
50 °C (Fig. 2(b) and (c)), due to the decomposition of
3
14] J. Estelle, P. Salagre, Y. Cesteros, M. Serra, Ag. Medina, J.E.
678.
PVA and the development of NiO crystalline, the di-
ameters of fibres became smaller, and the surface be-
came rougher than samples that were not calcined. After
increasing the calcination temperature to 700 °C
[
Sueiras, Solid State Ionics 156 (2003) 233–243.
[15] S.Y. Wang, W. Wang, W.Z. Wang, Y.W. Du, Mater. Sci. Eng. 39
2002) 133.
(
[
[
[
16] L. Xiang, X.Y. Deng, Y. Jin, Scr. Mater. 47 (2002) 219.
17] P.S. Patil, L.D. Kadam, Appl. Surf. Sci. 199 (2002) 211.
18] R.C. Korosec, P. Bukovec, J. Therm. Anal. Calorimetry 56 (1999)
(
Fig. 2(d)), nanofibres of NiO, with smooth surface and
diameters of 50–150 nm, were prepared.
For the first time, NiO nanofibres, with diameters of
587.
[19] Y. Nishio, R.S. Manley, Macromolecules 21 (1998) 1270.
5
0–150 nm, were prepared by using the electrospun thin