Advanced Materials Research Vols.

299-300 (2011) pp 118-121 Online: 2011-07-27

© (2011) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/AMR.299-300.118

Synthesis and properties of cerium oxide nanoparticles

Li Yong 1,a He Jin Gui1,b Huang Xiao Wei2,c

1
School of Material and Metallurgy, Northeastern University, Shenyang, Liaoning 110004, China
2
National Engingeering Research Center for Rare Earth Materials, General Research Institute for
Nonferrous Metals, and Grire Advamced Materials Co., Ltd.,Beijing 100088,China
a
l_yong@126.com, b395254227@qq.com,chxw0129@126.com

Keywords: nanoparticles; cerium oxide; precipitation method; dispersing agent

Abstract. Cerium oxide(CeO2) nanoparticles were synthesized via a precipitation method using
cerous sulfate, ammonia water and cetyl three methyl brominated ammoniu(CTAB) as raw
materials. The effect of thermal treatment temperature and dispersing agent on the crystal structure
and morphology were discussed. The structural evolutions and morphological characteristics of the
nanoparticles were investigated using X-ray diffractometery, scanning electron microscopy, Fourier
transform infrared spectroscopy. The results showed that the broadening of CeO 2 peaks decreases
by the increasing in heat-treatment temperature and the dispersing agent playes key roles in
microstructure of the CeO2.

Introduction
Currently, there have been great interests on the research of nanomaterials materials, Particularly,
many efforts had been devoted to rare earth materials and high-end application products due to that
they always exhibit the unique physical and chemical properties significantly different from their
bulk counterparts. Nanosized ceria is one of the most reactive rare earth oxides with many attractive
properties that make it highly promising for diverse applications such as polishing powders,
catalysts, gas sensors, electrode materials for solid oxide fuel cells and so on [1,2].
Various chemical methods are adopted for the preparation of nanometer materials, including the
sol-gel methods, gas-phase methods, evaporative decomposition of solution, precipitation method
and wet chemical synthesis. Among these methods, precipitation method was the standing one due
to its simplicity and economy, and some different-shaped nanostructures of cerium oxide have been
successfully synthesized via the process[3-5].
In this paper, The cerium oxide nanoparticles were successfully synthesed by a facile
precipitation method in the presence of the difference surfactant. The properties of the materials
were characterized by X-ray diffraction (XRD) analysis, Fourier transformed infrared (FT-IR)
spectra, scanning electron microscopy (SEM).

Experimental
Materials. All chemicals provided by Xinxi Chemical Co.(china) were reagent grade and used
without further purification .
Preparation of cerium oxide nanoparticles. Cerium oxide nanopowder was prepared by a
precipitation method using cerous sulfate, ammonia water and dispersing agent :sodium dodecyl
benzene sulfonate (SDBS), cetyl three methyl brominated ammoniu (CTAB), OP-10. In a typical
synthesis procedure,1 g of cerous sulfate and a given amount of dispersing agent (such as CTAB)
were put into 100 mL distilled water to form a clear solution, which was stirred strongly at room
temperature for about 0.5 h. The obtained clear solution was added drop-wise to 10 mL precipitating
agent (1.4 M ammonia water) under constant stiring condition for 2 h. The resultant
synthesis precipitate was washed with deionized water and dried at 80 ℃ for 24 h.The dried
precipitate was calcined for 2 h in a tube furnace at different temperatures.

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 Advanced Materials Research Vols. 299-300 119

Characterization. FT-IR spectra of the composites were recorded on a microscope FT-IR US

Nicolet 380 apparatus in transmittance mode. The crystalline structure of the powders was
determined by a Rigaku D/max-RB X-ray diffraction (Japan) with Cu K_radiation.The morphology
of the composites was studied by a PhilipXL-20 scanning electron microscope, the fracture surfaces
of the specimens after tensile test were sputter-coated with gold before analysis.

Results and Discussion

The synthesis mechanisms may be described by the following reactions. A precipitate is obtained
by adding solution to NH4OH. The formation of cerium hydroxide occurred after oxidation of Ce 3+
to Ce4+ in solution at a high pH, leading to Ce3+ + H2O→Ce(OH)3+ + H+ + e−, with subsequent
hydrolysis to Ce(OH)4 and precipitation. However, oxidation of Ce(OH) 3 also occurs in air at room
temperature. Then Ce(OH)4 converts to CeO2 with removing the hydroxyl groups as reaction
Ce(OH)4→ CeO2 + 2H2O.
Fig.1 shows XRD patterns of as-synthesized nanopowers (CTAB as dispersing agent) at 300
℃,400 ℃, 500 , 800 ℃, respectively. The sample synthesized at 800 ℃exhibits XRD peaks that
℃
correspond to the (111), (200), (220),(311), (222), (400), (331), (420), and (422) planes of a cubic
fluorite structure (space group: Fm3m) of CeO2 as identified using the standard data JCPDS 34-
0394. It is clear that, by increasing the heat-treatment temperature, the broadening of CeO 2 peaks
decreases which shows growing the CeO2 nanocrystallites. This decrease results most probably
from broadening of diffraction peaks due to destabilization of the low-temperature cubic phases,
rather than from actual shrinking of crystallites [6].
111

220 311

200
Intensity(a.u.)

331 422
222 400 420

800 ℃

500 ℃

400 ℃
300 ℃

60 80
20 40
2θ(。)
Fig.1.XRD patterns of the as-prepared CeO2 nanostructures at at various temperatures.

Fig.2 shows the FT-Irspectra fort he as-prepared and calcined products structures.The band
centered at 3440cm -1 corresponds to the -OH stretching vibration which is originated from physical
absorbed H2O or surface -OH groups. There are peaks at 1630,1460, 1070cm -1 in the dried
precipitate. These peaks are associated with the characteristic vibration of water (OH), carbohydrate
(CH) and C-O, respectively. The broad band below 700 cm −1 is due to the envelope of the phonon
band of the metal oxide network. Iincreasing the temperature hydroxyl groups are decomposed in
the precipitate and only CeO2bands are remained.
120 Materials and Manufacturing

4000 3600 3200 280 0 2 40 0 2 0 00 1 600 1200800

-1
W ave n u mbe r ( cm )
400

Fig.2.FT-IR spectra of as-systhesized dried precipitate,calcined at 500

℃ and 800 ℃

SEM images of different dispersing agent appear in Fig. 3. The morphology of the particle
detected indicates a significant modification of the size and shape of the CeO 2 particle, as deduced
from the SEM images.Different from the structure of the CeO2 precipitate dispersed by CTAB
(Fig.3a), the precipitate obtained using SDBS, presented as bulk material (Fig. 3b); the precipitate ,
prepared by OP-10, exhibited as slice powders(Fig. 3c). This indicates that dispersing agent played
key roles in structure of the CeO2.

(a)

(b)
 Advanced Materials Research Vols. 299-300 121

(c)

Fig.3. SEM image of the precipitate as-systhesized using cetyl three methyl brominated ammoniu (a), sodium
dodecyl benzene sulfonate (b), OP-10(c)

Conclusions
In conclusion, ceria nanoparticles were successfully synthesed by a facile precipitation method in
the presence of the difference dispersing agent. The structure of the synthesized CeO2 nanoparticles
was determined by means of XRD. The structure of the nanoparticles is hcp in all the samples. It is
found that the shape and size of the obtained CeO 2 nanocrystals are strongly dependent on the
dispersing agent.

Acknowledgements
This work was financially supported by the National Science Foundation of China(No.
50934004 ).

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Materials and Manufacturing
10.4028/www.scientific.net/AMR.299-300

Synthesis and Properties of Cerium Oxide Nanoparticles

10.4028/www.scientific.net/AMR.299-300.118

DOI References
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