Synthesis of large surface area LaFeO3 nanoparticles by SBA-16 ...

J Nanopart Res 

DOI 10.1007/s11051-009-9647-5 

RESEARCH PAPER 

Synthesis of large surface area LaFeO 3 nanoparticles 

by SBA-16 template method as high active visible 

photocatalysts 

Haijiao Su Æ Liqiang Jing Æ Keying Shi Æ 

Changhao Yao Æ Honggang Fu 

Received: 25 October 2008 / Accepted: 28 April 2009 

Ó Springer Science+Business Media B.V. 2009 

Abstract Nanosized LaFeO 3 with large specific 

surface area has been successfully synthesized by an 

impregnation process, with mesoporous silica SBA-16 

as hard template and corresponding metal nitrates as 

La and Fe resources, and the resulting LaFeO 3 is also 

characterized by thermogravimetry–differential thermal 

analysis (TG–DTA), X-ray diffraction (XRD), N 2 

adsorption–desorptions, Brunauer Emmett Teller 

(BET) technique, transmission electron microscopy 

(TEM), X-ray photoelectron spectroscopy (XPS), 

UV–visible diffuse reflection spectrum (UV–Vis 

DRS), and surface photovoltage spectroscopy (SPS). 

It is found that, compared with that prepared by the 

conventional citrate method, the as-prepared LaFeO 3 

with 20-50 nm particle size has remarkable large 

specific surface area, even still with the surface area as 

large as about 85 m 2 g -1 after calcination at 800 °C, 

which is attributed to its mesoporous structure as well 

as the small particle size. During the photocatalytic 

degradation of Rhodamine B solution under visible 

H. Su L. Jing (&) K. Shi C. Yao H. Fu (&) 

Key Laboratory of Functional Inorganic Materials 

Chemistry, Ministry of Education, Heilongjiang 

University, Harbin 150080, People’s Republic of China 

e-mail: Jinglq@hlju.edu.cn 

H. Fu 

e-mail: Fuhg@vip.sina.com 

irradiation, all the LaFeO 3 samples obtained are 

superior to P25 TiO 2 , and the activity becomes high 

with increasing calcination temperature. It is revealed 

that the excellent photocatalytic performance is 

mainly ascribed to the large surface area and high 

photogenerated charge separation rate. 

Keywords LaFeO 3 Nanoparticle 

SBA-16 template method Visible photocatalysis 

Introduction 

In recent years, nanoscale structures have attracted 

extensive attention as a result of their novel sizedependent 

properties (Wang and Herron 1991; Guldi 

et al. 2005; Gleiter et al. 2001). Most of the research 

efforts which were concentrated on the mixed metal 

oxides of the perovskite family, ABO 3 , where 

A = rare-earth and B = transition element, are important 

in advanced technologies such as fuel cells 

(Plonczak et al. 2008), catalysis (Arendt et al. 2008), 

electrode materials (Zhang et al. 2008), and sensors (Li 

et al. 2001). It has been observed that the perovskite 

oxides also function as good photocatalysts (Yang et al. 

2007). In the last two decades, the development of 

photocatalysts with visible-light response has been 

studied extensively from the viewpoint of the utilization 

of solar light energy. Intense research activity in 

this area has resulted in many novel mixed metal oxide 

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photocatalysts for water splitting such as SrTiO 3 , 

NaTaO 3 , etc. (Subramanian et al. 2006; Kato and Kudo 

2003; Maeda and Domen 2007; Penä and Fierro 2001), 

and the photocatalytic decompositions of organic 

compounds have been widely studied, but all the 

performance need to be advanced. 

The specific surface area and crystal structure are 

the most important two factors influencing catalytic 

activity. During several conventional synthetic processes 

of perovskites, such as citrate method and 

solid state reactions, the high-temperature thermal 

treatments needed usually lead to the sintering of the 

resulting particles, consequently decreasing greatly 

the specific surface area, which will largely influence 

the performance of the resulting perovskites and 

hinder their widespread use as catalysts. Thus, novel 

synthetic methods to obtain materials with large 

specific surface area are greatly desired. 

Among various preparation methods of nanosized 

materials, the template method, which provides a 

good choice for the synthesis of nanoparticles with 

controllable size and shape because of being in a 

confined three-dimensional (3D) space, has recently 

sparked great research interests (Lu and Schüth 2006; 

Schüth 2003). Unlike conventional surfactant templates, 

the hard template could effectively maintain 

the local strain caused by the crystallization of 

precursors. Zhao et al. synthesized highly dispersed 

TiO 2 nanoparticles using SBA-15 as hard template 

(Zhao and Yu 2006). Valdés-Solís et al. prepared 

nanosized perovskites and spinels through a silica 

xerogel template route (Valdés-Solís et al. 2005). 

However, so far the articles on the use of the SBA-16 

as hard template to synthesize nanosized solid 

materials are seldom reported. SBA-16 is a kind of 

3D, ‘‘cage-like’’ mesoporous silica, and its pores are 

connected by some mesoporous windows, so as to be 

beneficial for the substance transportation. Thus, it 

can be deduced that its negative replica is 3D 

connected structure (Shi et al. 2005a, b; Schüth and 

Schmid 2002; Kärger and Freude 2002), so that the 

SBA-16 as template to prepare porous solid materials 

with large surface area is feasible. It has been 

demonstrated that mesoporous structure is highly 

desirable for effective photocatalysis, since such 

structures enable more light to be harvested and also 

possess continuous pore channels that facilitate the 

transfer of reactant molecules. 

As a kind of important functional material, LaFeO 3 

with a typical ABO 3 -type perovskite structure has 

many applications, such as catalytic oxidation, electrode 

materials, and chemical sensors for the humidity 

and alcohols, and it also is an ideal potential semiconductor 

material for visible photocatalyst because of its 

small band gap energy (Wang et al. 2006; Li et al. 

2007). Herein, nanosized LaFeO 3 with large surface 

area was synthesized with mesoporous silica SBA-16 

as hard template for the first time. The as-prepared 

LaFeO 3 exhibits excellent visible-light photocatalytic 

activity, which is attributed to the large surface area, as 

well as to the high photoinduced charge separation rate 

mainly based on the SPS responses. This should be 

valuable for the practical application of LaFeO 3 and 

also provides a new strategy to prepare other highperformance 

nanostructured oxide composite materials 

with large surface area. 

Experimental 

Preparation of the template SBA-16 

The SBA-16 was synthesized by a sol–gel process as 

described elsewhere (Shi et al. 2005a, b). The F127 

(EO 106 PO 70 EO 106 , BASF) and Ethyl silicate 

(C 8 H 20 O 4 Si) were used as surfactant and silicon 

sources, respectively. After the resulting xerogel was 

calcined at 550 °C with a heating rate of 1 °C min -1 

and ground, the mesoporous silica SBA-16 was 

obtained eventually. 

Synthesis of the samples 

Nanosized LaFeO 3 was synthesized according to the 

flowchart shown in Fig. 1. First, 1 g of freshly 

as-synthesized SBA-16 was dispersed in 2 mL of 

ethanol solution, containing 0.0041 mol of La(NO 3 ) 3 

6H 2 O and 0.0041 mol of Fe(NO 3 ) 3 9H 2 O. After 

ultrasonication for 10 min, the mixture obtained was 

kept at 60 °C under stirring until the solvent was 

evaporated completely. Subsequently, the LaFeO 3 – 

SBA-16 composite was obtained after the above 

mixture was dried in a vacuum at 80 °C and calcined 

in air at needed temperature for 2 h. Finally, the 

template-free LaFeO 3 nanopowder was gained by 

washing, drying, grinding, and heat-treatment at 

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La(NO 3 ) 3·6H 2 O 

Fe(NO 3 ) 3·9H 2 O 

Ethanol 

Nitrate ethanol solution 

Adding 

Fresh SBA-16 

Mixed solution 

Drying and grinding 

precursor 

Calcining 

Template-containing LaFeO 3 

Washing, drying and calcining 

after treatment with NaOH 

Template-free LaFeO 3 

Fig. 1 Flowchart of the synthetic processes of nanosized 

LaFeO 3 

500 °C after the silica in the composite was dissolved 

in the 2 M NaOH solution. 

Characterization of the samples 

The thermogravimetry–differential thermal analysis 

(TG–DTA) of the dry mixtured precursor was 

performed using a Rigaku TAS 100 thermal analyzer, 

with the temperature rate of 10 °C min -1 in air, 

referenced to a-Al 2 O 3 . The crystal structure of the 

samples was determined by X-ray diffraction (XRD) 

method (Rigaku D/MAX-rA powder diffractometer, 

Japan). N 2 adsorption–desorption isotherm of the 

sample was carried out at the temperature of liquid 

nitrogen by using a Micromeritics ASAP 2020 M 

system, outgassed for 10 h at 300 °C prior to the 

measurements. Transmission electron microscopy 

(TEM) observation of the sample was performed on 

a JEM-3010 electron microscope (JEOL, Japan), with 

an acceleration voltage of 300 kV. The BET surface 

area was evaluated by a ST-2000 constant volume 

adsorption apparatus. The surface composition and 

elemental chemical state of the samples were examined 

by X-ray photoelectron spectroscopy (XPS) 

using a Model VG ESCALAB apparatus with AlKa 

X-ray source. The binding energies were calibrated 

with respect to the signal for adventitious carbon 

(binding energy = 284.6 eV). The UV–visible diffuse 

reflection spectrum (UV–vis DRS) of the 

samples was recorded with Shimadzu UV-2550 

Spectrophotometer, using BaSO 4 as reference. The 

SPS measurement of the samples was carried out with 

a home-built apparatus that had been described 

elsewhere (Jing et al. 2003). 

Photocatalytic activity measurement 

Rhodamine B (C 28 H 31 ClN 2 O 3 ) is a common dye that is 

extensively used in a variety of industrial applications 

(Wang et al. 2008; Huang et al. 2003). Therefore, the 

photocatalytic activity of the as-synthesized samples 

was evaluated by photodegradation of Rhodamine B 

under irradiation of visible light (k [ 400 nm). The 

light source was a high-pressure Xe lamp (150 W). 

Light passed through a cutoff filter and then was 

focused onto a 100-mL beaker. The reaction was 

maintained at ambient temperature. In a typical 

experiment, aqueous suspensions of Rhodamine B 

and 0.10 g of the photocatalyst powder were placed in 

the beaker. Prior to irradiation, the suspension was 

magnetically stirred in the dark to ensure the establishment 

of an adsorption/desorption equilibrium. At 

given irradiation time, 10 mL of the suspension was 

collected and centrifuged to remove the particles; then, 

the dye concentration was determined by measuring 

the UV–Vis absorbance of the dye aqueous solution. 

Results and discussion 

Measurements of TG–DTA and XRD 

Figure 2 is the TG–DTA curves of the dry mixed 

powder obtained. There are three stages during the 

weight loss process, one is at the temperature range 

from the room temperature to 250 °C, with endothermic 

phenomenon, mainly attributed to desorption 

of water that is physically adsorbed. The next is from 

300 to 500 °C, with three maximum exothermic 

peaks, accompanied by drastic weight loss which was 

attributed to vaporization of inner water and autocombustion 

during the nitrate decomposition of the 

dried powder. There is a slight loss process at the 

temperature higher than 500 °C, which is mainly 

caused by desorption of residual hydroxyl (OH) 

group (Nosaka et al. 1998). In this case, the slight 

exothermic phenomenon can be seen, which is 

possibly attributed to the gradual crystallization of 

LaFeO 3 . 

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Mass loss (%) 

Fig. 2 

100 

90 

80 

70 

60 

50 

40 

TG 

DTA 

Exo 

0 

Endo 

-2 

200 400 600 800 1000 

Temperature (°C) 

The XRD patterns of the as-prepared LaFeO 3 

samples calcined at different temperature are shown 

in Fig. 3. For the sample calcined at 500 °C, no 

obvious XRD peaks can be seen, indicating that there 

is mainly amorphous. When the calcination temperature 

is higher than 500 °C, the marked XRD peaks, 

which can be indexed to the ABO 3 -type LaFeO 3 as 

shown in the standard JCPDS No. 15-0148, display, 

and the XRD intensity gradually increases with 

enhancing the calcination temperature, implying that 

the crystallinity becomes much high. 

Measurements of N 2 adsorption–desorption, 

TEM, and BET 

In order to reveal the structure of the as-prepared 

LaFeO 3 , we took the measurements of N 2 adsorption–desorption 

and TEM observation of the sample 

10 

TG–DTA curves of the dry mixed powder obtained 

8 

6 

4 

2 

Heat flow (mV) 

calcined at 700 °C. Figure 4 shows the N 2 adsorption–desorption 

isotherm of the LaFeO 3 and pore size 

distributions (inset) calculated from desorption 

branch by the BJH method. The isotherm exhibits a 

long and narrow hysteresis loop, which is due to the 

nonstandard porous structure (Jin et al. 2006; Zapilko 

et al. 2007), and it can be seen that the template-free 

LaFeO 3 has disordered porous structure from the low 

values of dV/dR at BJH pore size distributions. The 

isotherm which starts a sharp capillary condensation 

step at low relative pressures must be caused by the 

pore size centered between 2 and 5 nm and has the 

hysteresis loop taken at high relative pressures 

attributed to its having large slit-like pores, size of 

which extended to above 10 nm, between the particles 

rather than a mesostructure. The TEM image 

reported in Fig. 5 confirms the monodisperse nanoparticles 

of LaFeO 3 with the particle sizes ranging 

from 20 to 50 nm. 

Table 1 reflects the specific surface areas of the 

LaFeO 3 prepared by the template method and the 

citrate method in our group (Li et al. 2007), 

respectively. By comparison, two main points can 

be found. One is that, at the same calcination 

temperature, the LaFeO 3 prepared by the template 

method has much larger surface area than that 

prepared via the citrate method and the other is that 

the surface area of the LaFeO 3 gradually decreases 

with increasing calcination temperature, which is 

mainly attributed to the increase in the particle size. 

However, compared with the LaFeO 3 prepared via 

the citrate method at the low temperature, the LaFeO 3 

Intensity (a.u.) 

900°C 

800°C 

700°C 

600°C 

500°C 

Absorbed volume (cm 3 / g) 

80 

60 

40 

20 

dV/dR (cm 3 g -1 nm -1 ) 

0.002 

0.001 

0.000 

0 5 10 15 20 25 30 

Pore diameter (nm) 

20 30 40 50 60 

2θ (degree) 

Fig. 3 XRD patterns of LaFeO 3 samples calcined at different 

temperature 

0.0 0.2 0.4 0.6 0.8 1.0 

Relative pressure (p / p o 

) 

Fig. 4 N 2 adsorption–desorption isotherm for the templatefree 

LaFeO 3 calcined at 700 °C and pore size distributions 

calculated from desorption branch by the BJH method 

123


Fig. 5 TEM image of LaFeO 3 calcined at 700 °C 

Table 1 BET surface area of the LaFeO 3 samples prepared 

by different methods 

Calcination 

temperature (°C) 

prepared by the template method still can have a high 

surface area, even after calcination at 900 °C. Based 

on the above analyses of the N 2 adsorption–desorption, 

BET, and TEM observation, it can be deduced 

that the disordered porous structure in the particles 

and the relative small particle size are responsible for 

the high surface area of the resulting LaFeO 3 . 

Measurement of XPS 

BET surface area (m 2 g -1 ) 

By the template 

method 

500 – 15.0 

600 129.6 9.2 

700 101.1 6.3 

800 85.4 4.3 

900 34.5 3.2 

By the citrate 

method 

The XPS spectra of La3d, Fe2p, and O1s of the 

resulting LaFeO 3 after calcination at 700 and 800 °C 

were performed, as shown in Fig. 6. The binding 

energies obtained in the XPS analysis are standardized 

for specimen charging using C1s as the reference 

at 284.6 eV. The XPS peak positions of La3d 5/2 

(Fig. 6a) and Fe2p 3/2 (Fig. 6b) are at about 834.8 and 

710.5 eV, respectively, demonstrating that the main 

chemical valences of La and Fe in the two samples 

both are ?3 according to the method principle and 

handbook of the XPS instrument and the literature 

(Yang et al. 2006). The two O1s XPS spectra 

(Fig. 6c) are wide and asymmetric, demonstrating 

that there are at least two kinds of O chemical states 

according to the binding energy range from about 

526.0 to 534.0 eV, including crystal lattice oxygen 

(O L ) and hydroxyl oxygen (O H ) with increasing 

binding energy (Zhang et al. 2006; Jing et al. 2006). 

Thus, the O1s XPS spectrum is fitted to two kinds of 

chemical states with the Origin software by Gaussian 

rule. The O L XPS signal is attributed to the contribution 

of La–O and Fe–O in LaFeO 3 crystal lattice, 

and its peak position is at about 529.5 eV. The O H 

XPS is close related to the hydroxyl groups resulting 

mainly from the chemisorbed water, and its peak 

position is at about 531.5 eV. As seen from Fig. 6c, 

the amount of hydroxyl oxygen (O H ) decreases as the 

thermal treatment is enhanced. 

Measurements of UV–Vis DRS and SPS 

Figure 7 shows the UV–Vis DRS spectra of LaFeO 3 

samples calcined at different temperature; it can be seen 

that the DRS spectra of all LaFeO 3 samples are similar, 

and upon the calcination temperature increasing, the 

absorption of the spectra above 550 nm is decreased 

gradually, which is the cause that the LaFeO 3 crystallinity 

increases with the calcination temperature 

increasing on the basis of XRD measurement. According 

to the energy band structure of LaFeO 3 similar to 

that of a-Fe 2 O 3 (Lu et al. 2005), it can be concluded that 

the DRS spectra of LaFeO 3 nanoparticles are ascribed 

to the electronic transitions from the valence band to 

conduction band (O 2p ? Fe 3d ) (Li et al. 2000). In 

addition, it can be ascertained that the as-prepared 

LaFeO 3 samples can be excited by the light with the 

wavelength of equal to or smaller than 550 nm. 

The SPS technique can provide a rapid, nondestructive 

test of semiconductor solid surface property, 

and is also a very effective way to study the separation 

and transfer behavior of photoinduced charge carriers at 

a surface or interface (Jing et al. 2006). Figure 8 shows 

the SPS response of LaFeO 3 nanoparticles calcined at 

different temperature. It can be found that all of these 

samples display obvious SPS response in the 

123


a 

La3d 

50 


800°C 

3d 5/2 

3d 3/2 

DRS (%) 

40 

30 

20 

10 

900°C 

800°C 

700°C 

600°C 

b 



820 830 840 850 860 

Binding energy (eV) 

c 

700°C 

800°C 

700°C 

2p 3/2 

2p 1/2 

700 710 720 730 


800°C 

700°C 

524 528 532 536 


Fe2p 

wavelength range from 300 to 550 nm, with a SPS peak 

at about 390 nm, which can be attributed to the 

photoinduced electronic transitions from the valence 

band to conduction band (O 2p ? Fe 3d ) (Li et al. 2000). 

O L 

O L 

O H 

O H 

O1s 

Fig. 6 XPS spectra of La3d (a), Fe2p (b), and O1s (c) of 

LaFeO 3 samples calcined at 700 and 800 °C 

0 

300 350 400 450 500 550 600 650 700 

Wavelength (nm) 

Fig. 7 UV–Vis DRS spectra of LaFeO 3 samples calcined at 

different temperature 

Moreover, the SPS response becomes much stronger 

with increasing calcination temperature, which is close 

related to the increase in the crystallinity of the LaFeO 3 . 

The high crystallinity makes electronic band perfect so 

as to enhance the built-in field strength, which can 

promote charge separation, meanwhile leading to the 

decrease of the defect amounts, which is also favorable 

for charge separation (Jing et al. 2006). According to the 

SPS method principles, it can be expected that the 

stronger is the SPS signal, the higher is the photoinduced 

charge separation rate. Thus, it can be supposed 

that the high crystallinity is favorable for the photoinduced 

charge separation and then improve the photocatalytic 

activity further. 

Photocatalytic activity evaluation 

The activity of the as-prepared LaFeO 3 was evaluated 

by photocatalytic degradation of Rhodamine B solution 

under visible light. Figure 9 shows the RhB 

degradation rate of photocatalytic reaction under 

visible irradiation and adsorption in the dark on the 

different LaFeO 3 samples and internationally commercial 

P-25 TiO 2 . As the calcination temperature is 

enhanced, it can be noticed that the photocatalytic 

activity of the as-prepared LaFeO 3 gradually increases, 

and the LaFeO 3 calcined at 900 °C exhibits excellent 

photocatalytic activity. Interestingly, all the LaFeO 3 

samples display higher visible activity than P25 TiO 2 

and those LaFeO 3 samples prepared via the citrate 

method (Li et al. 2007). Based on the above discussion, 

the high photocatalytic activity is mainly explained 

from the following two aspects. One is the large surface 

123


Photovoltage (a.u.) 

0.00008 

0.00006 

0.00004 

0.00002 

0.00000 

area of the as-prepared LaFeO 3 , which is favorable for 

the adsorption of RhB. This can be proved by the 

adsorption rate in Fig. 9, even still with a large RhB 

adsorption rate after calcination at 900 °C. The other is 

the high crystallinity of the as-prepared LaFeO 3 caused 

by calcined at the high temperature. The high crystallinity 

can promote the photoinduced charge separation 

(Jing et al. 2006). In addition, a certain amount of 

surface hydroxyl group is also beneficial for photocatalytic 

reactions. 

Conclusions 

900°C 

800°C 

700°C 

600°C 

300 350 400 450 500 550 600 

Wavelength (nm) 

Fig. 8 SPS responses of LaFeO 3 samples calcined at different 

temperature 

On the basis of the above systematical investigations, 

the following conclusions can be drawn: (1) nanosized 

LaFeO 3 with large surface area has been 

successfully fabricated by using mesoporous silica 

SBA-16 as hard template, still with 85 m 2 g -1 

surface area after calcination at 800 °C. At the same 

thermal treatment temperature, the surface area of the 

LaFeO 3 prepared by the template method is much 

larger than that prepared via the citrate method; (2) 

the as-prepared LaFeO 3 , especially for those calcined 

at high temperature, exhibits high visible activity; (3) 

the high activity of the as-prepared LaFeO 3 is 

attributed to the large surface area and high charge 

separation rate resulting from the high crystallinity, 

as well as to a certain amount of surface hydroxyl 

group. It can be suggested that the SPS method is an 

effective tool to reveal the processes of separation 

and transfer of photoinduced charges. This study 

provides a new route to design and synthesize other 

metal composite oxides with large surface area, and 

RhB degradation rate (%) 

50 

40 

30 

20 

10 

0 

would broaden the scope of the application of 

perovskite-type materials. 

Actually, compared with porous TiO 2 and other 

oxide nano-materials routinely with hundreds of 

meters squared per gram, the as-prepared nanosized 

LaFeO 3 has still low specific surface area. However, 

the superior visible photocatalytic performance of 

this LaFeO 3 over international P25 TiO 2 is confirmed, 

implying that the porous perovskite-based 

nanomaterials, as non-TiO 2 -based visible-driven 

photocatalysts, are feasible and promising. 

Acknowledgments We gratefully acknowledge the fundings 

received from the National Nature Science Foundation of 

China (No. 20501007, 20676027), the program for New 

Century Excellent Talents in universities (NCET-07-259), the 

Key project of Science & Technology Research of Ministry of 

Education of China (No. 207027), the Science Foundation of 

Excellent Youth of Heilongjiang Province of China 

(JC200701), and the Science Foundation of Harbin City of 

China (No. 2005AFQXJ060), for the completion of this study. 

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