Material Science and Environmental Engineering – Chen (Ed.

)
© 2016 Taylor & Francis Group, London, ISBN 978-1-138-02938-5

Preparation of porous bismuth oxide by sol-gel method using

citric acid

Z.S. Jiang & Y.J. Wang

State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing, China

ABSTRACT: In this paper, uniform porous bismuth oxides were prepared using the sol-gel method.
These porous granules were prepared with and without the surfactant PEG200. X-ray diffraction and scan-
ning electron microscope were applied to characterize these porous bismuth oxides with and without the
surfactant. The results show that the adding of surfactant increased the degree of crystallinity, purity and
uniformity, and that many irregular pores were formed and distributed in bismuth oxides granules. Porous
bismuth oxides prepared with 0.8 mL PEG200 contains high intensity monoclinic phase bismuth oxides.

Keywords: sol-gel; porous; bismuth oxide; citric acid

1 INTRODUCTION paper, porous bismuth oxides were prepared by

the sol-gel method using citric acid and charac-
Bismuth oxide Bi2O3 has a lot of peculiar physi- terize these porous bismuth oxides using different
cal and chemical properties, such as a wide energy measurements.
gap change (from 2 to 3.96 eV), high oxide-ion
conductivity properties, high refractive index, die-
lectric permittivity, and marked photoconductiv- 2 EXPERIMENTAL
ity and photoluminescence (Leontie et al., 2002).
A characteristic feature of bismuth oxide consists 2.1 Materials
of its polymorphism: six modifications labeled as
All reagents used in this study were of ana-
α, β, γ, δ, ε and ω-phase have been reported (Gual-
lytical grade and were purchased without fur-
tieri et al., 1997: Cornei et al., 2006; Drache et al.,
ther purification. Bismuth nitrate pentahydrate
2007). Among them, the low-temperature α and
(Bi(NO3)3 ⋅ 5H2O) was used as received from
the high-temperature δ phases are stable and the
Sinopharm Chemical Reagent Co., Ltd., Citric
others are metastable under certain conditions
acid monohydrate (C6H8O7 ⋅ H2O) and poly-
(Deng et al., 2011). Due to the excellent properties
ethylene glycol (PEG200) was purchased from
and characteristics of bismuth, bismuth oxides can
Guangdong Xilong Chemical Co., Ltd. Ethylene
be used in a variety of areas such as solid oxide fuel
glycol was used as received from Tianjin Fu Chen
cells (Sammes et al., 1999), gas sensors (Gou et al.,
Chemical Reagents Factory. Nitric acid (HNO3)
2009), fine structure glasses (Leontie et al., 2005),
(67% in purity) was purchased from Beijing Chem-
and catalysts (Schlesinger et al., 2013). Bismuth
ical Factory.
oxides have attracted much attention and have
been studied widely.
2.2 Preparation of porous bismuth oxide
Recently, bismuth oxide particles have been pre-
pared through many kinds of methods, for exam- Porous Bi2O3 was prepared by a sol-gel method
ple, co-precipitation, solvothermal method (Wang using citric acid as complexing agent. In this syn-
et al., 2014), chemical vapor deposition (Shen thesis procedure, 4.85 g of Bi (NO3)3 ⋅ 5H2O was dis-
et al., 2007), and so on. But the above prepara- solved in a 24 mL nitric acid solution [V (HNO3):
tion methods are often expensive and complicated. V (H2O) = 1:8] under magnetic stirring. And then
Sol-gel methods have been proved to be good a 1.922 g of citric acid and 0.371 mL of ethylene gly-
way to prepare metal oxide particles, for exam- col was added in the above solution, and 0.8 mL
ple, TiO2 nanoparticles can be prepared through of PEG200 was added as surfactant. The above
sol-gel method (Myilsamy et al., 2015). There are solution was constantly stirred for 1 h, and then
not so many reports about preparing the porous the solution was heated to 80 °C and maintained
bismuth oxide through sol-gel methods. In the at 80 °C for 3 h to form a transparent yellow gel.

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 Figure 1. TG curve of the precursor prepared with (a) Porous bismuth oxide prepared with 0.8 mL PEG200;
0.8 mL of PEG200 adding. (b) Porous bismuth oxide prepared without PEG200.
Downloaded by [Cornell University] at 09:38 20 September 2016

Figure 2. XRD spectra of the produced porous bis-

muth oxide annealed at 600 °C.
This gel was dried in an oven at 110 °C for 12 h.
Subsequently, the above faint yellow fluffy precur-
sor (foam-like) was grounded finely and subjected
to thermogravimetric analysis (TG/DTA6300, SII
Nano Technology Inc., Japan) in order to estab-
lish a thermal treatment schedule for the precursor.
The precursor was decomposed completely when it
was heated to a high temperature.

2.3 Characterization
The composition and crystal structure of the bis-
muth oxide nanoparticles was determined by X-Ray
Diffraction (XRD, Bruker D8 advance) using a Cu
Kα (λ = 1.54056 Å). The scans were taken at room
temperatures over a wide range of 2θ = (20º−70º) at
0.05 degrees intervals. The morphologies of the as-
made samples were observed on Scanning Electron
Microscope (SEM, Hitachi S4800).

3 RESULTS AND DISCUSSION

3.1 Analysis of XRD results

Figure 2 displays the XRD spectra of the prepared
porous bismuth oxide. It can be seen from the spec-
tra that the porous bismuth oxide prepared with and
without PEG200 are mainly composed of mono-
clinic phase of bismuth oxide (α-Bi2O3) (JCPDS NO. (a) Porous bismuth oxide prepared without PEG200;
14–0699). The small peaks 2θ = 29.3° correspond- (b) Porous bismuth oxide prepared with 0.8 mL PEG200.
ing to the diffraction plane of Bi2O2.3 (JCPDS NO.
76–2477). It can be also noticed that the α phase of Figure 3. SEM photographs of porous bismuth oxide.
porous bismuth oxide accounts for most of the pro-
portion of the sample and only a small percentage of
3.2 Analysis of SEM results
the sample is Bi2O2.3. The high intensity indicates that
the α phase of bismuth oxides become more domi- The SEM micrographs of the porous bismuth
nant with the adding of PEG200 while the trend is oxides prepared with surfactant adding and with-
adverse for the Bi2O2.3, and the higher crystallinity out surfactant are shown in Figure 3. As shown in
products were acquired with the surfactant adding. Figure 3a, it can be noticed that the morphology

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 ACKNOWLEDGMENTS

This paper is supported by the project of State

Key Laboratory of Explosion Science and Tech-
nology (Beijing Institute of Technology, China)
(No. YBKT16-06).

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