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Photocatalytic activity under visible light of Fe-doped CeO 2 nanoparticles

synthesized by flame spray pyrolysis

Article in Ceramics International · October 2013

DOI: 10.1016/[Link].2012.09.093

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CERAMICS
INTERNATIONAL
Ceramics International 39 (2013) 3129–3134
[Link]/locate/ceramint

Photocatalytic activity under visible light of Fe-doped CeO2

nanoparticles synthesized by flame spray pyrolysis
D. Channeia,d, B. Inceesungvorna, N. Wetchakunb, S. Phanichphantc,n, A. Nakarukd,n,
P. Koshyd, C.C. Sorrelld
a
Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200, Thailand
b
Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200, Thailand
c
Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai 50200, Thailand
d
School of Materials Science and Engineering, University of New South Wales, Sydney, NSW 2052, Australia
Received 8 August 2012; received in revised form 26 September 2012; accepted 27 September 2012
Available online 3 October 2012

Abstract

CeO2 nanoparticles (undoped and Fe-doped) were synthesised using flame spray pyrolysis with varying Fe-dopant concentrations.
X-ray diffraction analysis revealed the absence of any impurity phases in all samples. BET (Brunauer, Emmett and Teller) tests showed
that the average sizes of undoped and Fe-doped CeO2 particles were 6.39 and 5.94 nm, respectively. Specific surface area of the particles
increased with increasing Fe-dopant concentration. High resolution transmission electron microscopy (HRTEM) revealed that the
nanoparticles were either spherical or equiaxed in shape. UV–vis spectroscopy showed a shift of the adsorption edge towards longer
wavelengths along with a decrease in the optical indirect band gap from 3.18 to 2.90 eV for undoped particles and 2 mol% Fe-doped
particles. In terms of photocatalytic performance, Fe-doped CeO2 nanoparticles were responsible for an increased degradation of the
carbon from formic and oxalic acids. Furthermore, the photocatalytic efficiency was 100% when 2 mol% Fe-doped CeO2 particles
were used for testing.
& 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Keywords: D. CeO2; Nanoparticles; Flame Spray Pyrolysis; Photocatalytic Activity

1. Introduction humans. On the other hand, ceria is slightly more expensive,

and it is also hygroscopic in nature.
There have been an increasing experimental focus on CeO2 is a large band gap semiconductor with an optical
characterising cerium dioxide (ceria, CeO2) which has been indirect band gap of 3.20 eV [7], which limits its applica-
identified to possess a unique photocatalytic activity, in tion to within the ultraviolet (UV) radiation range. In
addition to high chemical stability, and low biological order to reduce the band gap and to enhance the photo-
toxicity. CeO2 has been used for a wide range of applications, activity of CeO2, transition metals ions of variable valency
including solar cells, for water purification [1], gas sensors have been introduced into the CeO2 lattice viz., iron (Fe)
[2,3], and as polishing agents [4]. Furthermore, compared to [8], copper (Cu) [9], nickel (Ni) [10], manganese (Mn) [11],
other metal oxides such as TiO2, ZnO, and Al2O3, CeO2 has cobalt (Co) [12] and silver (Ag) [13]. Of these ions, iron is
no deleterious effect on human cells [5,6], and therefore use considered to be one of the most promising candidate,
of ceria for photocatalytic applications such as water since Fe3 þ can easily substitute for Ce-ions or enter the
purification and food packaging will pose minimal risk for interstices of the crystal lattice of CeO2 [14], leading to the
creation of donor or accepter levels between the valence
and conduction bands [15].
n
Corresponding authors.
Several techniques have been used to prepare CeO2
E-mail addresses: sphanichphant@[Link] (S. Phanichphant), nanoparticles, including hydrothermal synthesis [16],
[Link]@[Link] (A. Nakaruk). homogeneous precipitation [17], sonochemical synthesis

0272-8842/$ - see front matter & 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
[Link]
3130 D. Channei et al. / Ceramics International 39 (2013) 3129–3134

[18], and flame spray pyrolysis (FSP) [19]. The latter is an 400 nm/min, step size 1 nm). The absorbance spectra were
attractive, versatile, and practical method to prepare CeO2 used to calculate the optical indirect band gap using the
nanoparticles due to several advantages such as low cost, Schuster–Kubelka–Munk equation [20,21].
simplicity of operation and experimental setup, capacity
for mass production, ease of doping, reproducibility, and
rapid particle growth.
2.3. Photocatalytic activity
Thus, it is clear that the preparation and use of CeO2
nanopaticles doped with Fe by flame spray pyrolysis would
The photocatalytic performances of nanoparticles were
be advantageous; moreover, there is a potential for
assessed in terms of the decomposition of both formic acid
improving the photocatalytic performance of the material.
(HCOOH) and oxalic acid (COOH)2 in a spiral reactor
Therefore, the present work aims: (1) to synthesise CeO2
under UV irradiation from a fluorescent lamp (Sylvania
nanoparticles doped with Fe using flame spray pyrolysis,
fluorescent lamp, 18 W) filtered with a Roscos E-colour
and (2) to analyse these particles in terms of their
UV filter, as shown in Fig. 1. The radiation was filtered
mineralogical and morphological characteristics, and
using a double layer of UV cut-off filter (Rosco E-Colour,
photocatalytic performance.
360–400 nm).
The spiral reactor conduit included a borosilicate glass
2. Experimental procedure
tube of dimensions 5 mm OD and 3 mm ID, which was
formed into a coil of 50 mm OD and 700 mm length. The
2.1. Synthesis of CeO2 nanoparticles
light source (30 mm diameter, 700 mm length) was centred
within the coil. This assembly was wrapped with an outer
Cerium nitrate-hexahydrate (Ce(NO3)3  6H2O, Sigma-
layer of aluminium foil as a light shield. The solution was
Aldrich, 99.99%) and iron acetyl-acetonate (Fe(C5H7O2)3,
circulated continuously through the conduit using a peri-
Sigma-Aldrich, 97%) were used as the sources of cerium and
staltic pump (Masterflex Model 7553-79; 7.0 mL/min) with
iron, respectively. The precursors were prepared by dissolving
silicone tubing. These conditions resulted in an operating
cerium nitrate-hexahydrate in ethanol solution (Scharlau,
temperature of the recirculating solution of  28 1C.
99.9%) at 0.5 M Ce concentration. The Fe-dopant concen-
Nanoparticles were suspended in a solution of 50 mL
trations used were 0.25, 0.50, 0.75, 1.00, 1.50, and
ethanol, and then dispersed into a vibra-cell sonicator
2.00 mol%. During the synthesis process, the precursor was
(Sonics VCX 750) for 20 min. The suspension then was
fed into a FSP reactor using a syringe pump at a feed rate of
loaded into a spiral photoreactor. Oxalic acid or formic
5 mL/min and the dispersion rate of O2 was fixed at 5 L/min.
acid equivalent to 500 mg carbon was injected into the
The flow rates of combustion gases were fixed at 1.19 and
photocatalytic suspension through the inlet port. The
2.46 L/min for methane and O2, respectively. The pressure at
photocatalytic efficiency was determined based on the
the nozzle tip was set at 1.5 bars. Finally, the synthesised
carbon dioxide (CO2) generation rate using a conductivity
nanoparticles were collected on a glass microfiber with the
metre (Eutech Instrument Cyberscan PC 5500/5000). The
aid of a vacuum pump.
overall organic compound degradation process can be
summarised in terms following equations [22]:
2.2. Characterisation
Oxalic acid : ðCOOHÞ2 þ 2OH  !2CO2 þ 2H2 O ð1Þ
The mineralogy of the nanoparticles was analysed using
X-ray diffraction (XRD; Philips X’pert MPD; CuKa
Formic acid : HCOOH þ 2OH  !CO2 þ 2H2 O ð2Þ
radiation; 45 kV; 40 mA; step size 0.021 2y; scanning speed
5.51 2y/min; aluminium sample holder). The mean particle
size and specific surface area (SSA) were evaluated using
the Brunauer, Emmett, and Teller (BET) nitrogen adsorp-
tion method (Quantachrome Autosorp 1 MP; 0.25 g sam-
ple; 1 h at 150 1C degassing). High resolution transmission
electron microscopy (HRTEM, JEOL JEM-2010; 200 kV
accelerating voltage) was used to determine the particle
size distribution and particle morphology of the synthe-
sised particles. The amount of dopant present in the
synthesised particles was confirmed using energy-
dispersive X-ray spectroscopy (EDS; JEOL JSM-6335F;
15 kV accelerating voltage). The reflectance of nanoparti-
cles (mounted in the recess of a standard aluminium
sample support) was obtained using a UV–vis spectro-
photometer equipped with an integrating sphere detector
(Perkin Elmer Lambda 950, 300–800 nm, monochromatic, Fig. 1. Schematic of the photocatalytic activity test system.
 D. Channei et al. / Ceramics International 39 (2013) 3129–3134 3131

3. Results and discussion that seen that small particle sizes have greater surface
areas.
The XRD patterns shown in Fig. 2 indicate that cerium The BET equivalent particle size was determined using
dioxide with cubic fluorite structure is the only crystalline the following equation [26]:
phase present in both undoped and Fe-doped CeO2
6
nanoparticle samples. Potential impurity phases such as dBET ¼ ð3Þ
Fe2O3, FeCeO3, and FeCe2O4 were not observed. More- rCeO2  SSA
over, the peak intensity of (111) plane was seen to decrease where dBET is the mean BET diameter, rCeO2 is the bulk
with increasing Fe-dopant concentration. This implies that density of CeO2 (E7.215 g/cm3) [27] and SSA is the Specific
the increasing incorporation of Fe ions into the CeO2 surface area
lattice tends to lower the crystallinity of the latter due to The particle size of CeO2 is shown in Table 1. In general,
introduction of anharmonicities in the lattice by the the crystallite size is not equal to the actual particle size
foreign cation. The crystallite sizes of the nanoparticles due to agglomeration effects in the latter [28]. However,
were determined using Scherrer’s equation [23] and the these results show that particle sizes are very close in value
values are presented in Table 1. From the table, it is seen to the crystallite sizes; and this clearly indicates that the
that the crystallite sizes decreased with increasing Fe- particles synthesised are single crystals [29].
dopant concentrations. Fig. 4 shows the high resolution transmission electron
The increase in the dopant concentration was observed microscopy (HRTEM) images of Fe-doped CeO2. The
to lower the crystallite size in addition to decreasing the images clearly demonstrate that undoped and Fe-doped
crystallinity of the nanoparticles (as seen from the decreas- CeO2 nanoparticles are spherical or equiaxed in shape. The
ing crystallite sizes in Table 1). Moreover, it can be noted distribution of particle diameters calculated from HRTEM
that doping CeO2 with Fe3 þ can hinder the grain growth micrographs has been found to be in the range of 6.25–
as well, and this supports the observance of decreasing 10 nm for undoped CeO2 and 5.00–6.25 nm for 2 mol%
crystallite sizes [24,25]. Fe-doped CeO2. These results support the crystallite size
The specific surface area (SSA) of CeO2 nanoparticles measurements and BET results which showed that increas-
was found to increase with increasing Fe-dopant concen- ing Fe-dopant concentrations result in a lowering of the
trations as shown in both Fig. 3 and Table 1. This supports particle sizes of CeO2.
the data on the crystallite sizes of the nanoparticles such Semi-quantitative elemental analysis of the Ce, O, and
Fe concentrations were carried out using energy dispersive

Fig. 2. X-ray diffraction (XRD) patterns of CeO2 nanoparticles as a Fig. 3. Variation in the specific surface area (SSA) and BET particle size
function of dopant concentration. of CeO2 nanoparticles as a function of the dopant concentration.

Table 1
Summary of analytical data.

Parameters Dopant concentration (mol% Fe)

0.00 0.25 0.50 0.75 1.00 1.50 2.00

Crystallite size (nm) 7.15 6.70 6.65 6.60 6.41 6.31 6.22
Particle size (BET diameter, nm) 6.39 6.23 6.16 6.08 6.02 5.99 5.94
Particle size (TEM, nm) 6.25–10.00 7.50–9.50 6.50–9.00 6.50–9.00 5.00–6.25 5.00–6.25 5.00–6.25
Specific surface area (SSA, m2/g) 130.00 133.38 135.00 136.73 137.97 138.80 140.00
Fe concentration(at%) 0.00 0.19 0.36 0.63 0.96 1.38 1.73
Energy band gap (eV) 3.18 3.13 3.10 3.06 3.00 2.98 2.90
3132 D. Channei et al. / Ceramics International 39 (2013) 3129–3134

Fig. 4. High resolution transmission electron microscopy (HRTEM) images of CeO2 nanoparticles synthesised at varying dopant concentrations.

Fig. 5. Schuster–Kubelka–Munk absorbance plot of CeO2 nanoparticles Fig. 6. Optical indirect band gaps of CeO2 nanoparticles as a function of
as a function of dopant concentration. dopant concentrations.

spectrometry (EDS). As seen in Table 1, the composition The plot of F(RN) vs. wavelength of CeO2 nanoparticles
of the dopant in the sample was close to the dopant is shown in Fig. 5. The spectra show that the adsorption
concentration of the starting material. This clearly shows edge shifted towards longer wavelengths (red-shift) with
that Fe ions have entered the CeO2 lattice either intersti- increasing Fe-dopant concentration. Fig. 6 shows the
tially or substitutionally. optical indirect band gaps of CeO2 nanoparticles, and this
The Schuster–Kubelka–Munk absorbance data were figure suggests that an increase in the dopant concentra-
calculated from UV–vis reflection data using the following tion results in a lowering of the optical indirect band gap.
equation [20,21] The lowest band gap value is seen in the case of the
2.00 mol% Fe-doped CeO2 nanoparticles.
F ðR1 Þ ¼ ð1R1 Þ2 The reason for the enhanced performance in the case of
ð4Þ
2R1 doped CeO2 is due to the fact that the addition of Fe ions
results in the formation of interstitial sites which in turn
where F(RN) is proportional to the absorption constant of create new energy levels (impurity energy levels) between
the material at a particular wavelength RN is the reflec- the valence and conduction bands [30]. The impurity
tance of the sample (%) energy levels allow for intrinsic band gap excitation under
 D. Channei et al. / Ceramics International 39 (2013) 3129–3134 3133

The shifting of the absorption edge in visible region

towards longer wavelengths was found in the case of Fe-
doped CeO2 nanoparticles, and this lowered the optical
indirect band gap of CeO2 nanoparticles from 3.18 eV
(undoped) to 2.90 eV (2.00 mol% Fe-dopant). Under
visible light irradiation, the efficiency of formic and oxalic
acid degradations by Fe-doped CeO2 nanoparticles was
superior to that of undoped nanoparticles. Furthermore,
the photocatalytic performance of 2 mol% Fe-doped CeO2
nanoparticles resulted in almost complete degradation of
both formic and oxalic acids.

Acknowledgements
Fig. 7. Variation in the efficiency of formic and oxalic acid degradation
by CeO2 nanoparticles at varying dopant concentrations. The authors are grateful for the financial support
provided through the Royal Golden Jubilee Scholarship
Project of Thailand, which has allowed this work to be
undertaken. The authors also wish to thank Dr. Pat
visible light region, and this implies that the higher energy Photongkum (School of Materials Science and Engineer-
state of 3d-electrons from Fe-cation dopants can be excited ing, UNSW) for assistance in obtaining data for optical
to the conduction band of CeO2 [31], thereby enhancing its band gap and UV–vis spectrophotometry and Dr. Chawarat
photocatalytic performance. Siriwong (Silpakorn University, Thailand) for assistance in
The photocatalytic efficiency of CeO2 nanoparticles was nanoparticle preparation.
calculated by measuring the CO2 gas formed as a by-
product of formic or oxalic acid degradation. Fig. 7 shows References
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