Caspian Journal of Applied Sciences Research, 1(12), pp.

1-7, 2012
Available online at http://www.cjasr.com
ISSN: 2251-9114, 2012 CJASR

Full Length Research Paper

Synthesis and Characterization of Al2O3:Fe Nanoparticles Prepared via
Aqueous Combustion
Saeid Kakooei1*, Jalal Rouhi2, Arash Dehzangi3, Ehsan Mohammadpour1, Mahmoud Alimanesh2
1

Department of Mechanic Engineering, UniversitiTeknologi PETRONAS, Tronoh 31750, Bandar Seri Iskandar,
Malaysia.
2
Nano-Optoelectronic Research (NOR) Lab, School of Physics, Universiti Sains Malaysia, Malaysia.
3
Institute of Microengineering and Nanoelectronics(IMEN) Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor,
Malaysia.
*Corresponding Author: skakooei59@hotmail.com
Received 3 September 2012; Accepted 6 October 2012

Iron-doped Al2O3 nanoparticles were prepared via an aqueous combustion synthesis technique using
stoichiometric amounts of aluminum nitrate [(Al9NO3)3.9H2O], ferric nitrate [Fe(NO3)3.9H2O], and sucrose
(C12H22O11). The heat treatment of the nanoparticles at two temperatures (900 C and 1100 C) formed porous
agglomerated iron-doped alumina nanoparticles. The heat-treated powders were characterized by X-ray
diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. Characterization results
showed existence of -Al2O3 calcined at 1100 C. In this study, iron-doped alumina particles with average
crystallite size (38.94 nm) were successfully synthesized by using sucrose as dispersion agent and carbon source.
Al2O3:Fe nanoparticles can be used in different fields as catalyst support and biocompatible material and for
electrical applications.
Key words: Nanomaterials; Iron Doped Alumina; Heat Treatment; Combustion Synthesis

structural and electrical applications (Pathak et al.,

2002; Toniolo et al., 2005; Meng et al., 2010). The
phase transition temperature can be decreased
by doping -Fe2O3 (hematite) with alumina. In
addition, smaller -Al2O3 particles can be
synthesized (Bye et al., 1974; Cordier et al., 2006).
Fe atoms in substitute solid solutions have been
known to change the diffusion properties of
alumina (Bataille et al., 2005). These effects are
related to the enhancement of the cation lattice
diffusion (via vacancies and interstitials) with rapid
oxygen diffusion in grain boundaries. The
diffusion changes are attributed to the presence of
Fe2+ cations which have relatively low solubility in
alumina. On the contrary, Fe3+ cations slightly
influence species diffusion properties and present
higher solubility in alumina (Bataille et al., 2005;
Cordier et al., 2006; Lucio-Ortiz et al., 2011).
Kobayashi et al. (2012) reported adding a small
quantity of Fe2O3 to the Al2O3 base catalyst
considerably enhanced catalyst stability and
catalytic activity (Kobayashi et al., 2012). The
doping agent modified catalytic behavior with an
influence on the morphology and textural porosity
in the alumina catalyst (Nomura et al., 2012).

1. INTRODUCTION
The combustion synthesis of Fe and Al2O3
composite method was reported by Holt and Kelly
for the first time in 1993 (Holt et al., 1993). This
method is a particularly safe, simple, and rapid
fabrication process, and its main advantages are its
time and energy efficiency (Mukasyan et al., 2007;
Deraz et al., 2009). The aqueous combustion
technique was recently used to synthesize alumina
nanopowders (Cordier et al., 2006; ZHAI et al.,
2006; Edrissi et al., 2007). However, the
combustion reaction mechanism is quite complex.
The main parameters influencing the reaction
include the main fuel type, ratio of fuels, fuel-tooxidizer ratio, pH level of the solution, amount of
excess oxidizer, and calcination rate. In general,
fuels should not react violently nor produce toxic
gases and must act as a complexing agent for metal
cations (Pathak et al., 2002; de Andrade et al.,
2006; Lima et al., 2006; Edrissi et al., 2008).
Alumina or -Al2O3 (corundum) has been
widely investigated because of its important
applications in advanced engineering as, for
example, catalyst support (Breen et al., 2002),
biocompatible material, and nanocomposite for

Kakooei et al.
Synthesis and Characterization of Al2O3:Fe Nanoparticles Prepared via Aqueous Combustion

The -Al2O3 is the primary intermediate phase

created from -Al2O3 containing Fe3+ in solid
solution, although crystallinity significantly
decreased with addition of Fe. The conversion rate
of intermediate phase to -Al2O3 was increased by
the additions of Fe (Bye et al., 1974).
In this research, sucrose (C12H22O11) was used
as fuel and dispersion agent. Then, the effects of
different heat treatment temperatures on the
crystallite size of the combustion-synthesized alumina powders were investigated. The powders
obtained via combustion synthesis were
characterized by X-ray diffraction (XRD),
scanning electron microscopy (SEM), differential

thermal analysis (DTA), and energy-dispersive Xray spectroscopy (EDX).

2. MATERIALS and METHODS
The iron-doped alumina nanoparticles were
prepared by using the solution combustion method.
Al(NO3)3.9H2O was used as an Al source, whereas
sucrose (C12H22O11) was used as a water-soluble
organic carbon source. As shown in Figure 1, 14.7
g aluminum nitrate and 12.86 g sugar were mixed
with deionized water respectively. Then, the
mixtures were combined to obtain a stable
suspension. Subsequently, 0.1 g of Fe(NO3)39H2O
was dissolved into the mixture.

Fig. 1: Schematic diagram of stages of Fe-doped Al2O3 nanoparticles synthesis by aqueous combustion method; (1)
Aqueous combustion reaction of mixtures leading to sponge-shape

The excess water from the mixtures was

evaporated on a hot plate until a gelatinous mixture
was formed. The chemical reaction of the
mentioned process is as follows:

ground by using an agate pestle and mortar to

break the agglomerates. The schematic diagram of
these stages is shown in Figure 1.
All powders (as-prepared, calcined at 900 C,
and calcined at 1100 C) were examined via XRD
using Cu K radiation (Bruker D4 Endeavor). The
XRD data were analyzed to study the phase
formation and to identify unit cell parameters,
which were calculated using the Eva software. In
flowing air, differential thermal analyses (DTA,
Netzsch 404S) were performed on the powders
calcined at 900 C and 1100 C (from 25 C to
1100 C) at heating rates of 10 C/min. Both
calcined powders were observed by using SEM.

2Al(NO3)3 + C12H22O11 + Fe(NO3)3 Al2O3 +

11H2O + 9NO2 + 6CO + 6C+Fe3++3e- (1)
The as-prepared powders were then submitted
to two thermal treatments in flowing air to obtain
the corundum () phase. The first heat treatment
was at 900 C for 5 h, whereas the second heat
treatment was at 1100 C for 5 h. Both heat
treatments utilized natural furnaces to cool the
heated powders to room temperature. The same
heating rate of 5 C/min was applied to both
samples. The iron-doped alumina powders were

Caspian Journal of Applied Sciences Research, 1(12), pp. 1-7, 2012

finding is significantly consistent with earlier

results (Pathak et al., 2002; Peng et al., 2006; Jamil
et al., 2011). The peak broadening method was
used to calculate the average crystallite size.
The full width at half maximum (FWHM) of
the peak was measured and the average crystallite
sizes were estimated using the Scherrer equation:

3. RESULTS and DISCUSION

The XRD patterns of the powders calcined at 900
C and 1100 C for 5 h are shown in Figure 2. The
-Al2O3 and -Al2O3 phases are evident in the
sample calcined at 900 C. Pure phase diffraction
peaks of -Al2O3 were predominant in the XRD
patterns of the sample calcined at 1100 C. This

0.9

cos

(2)

B b
2

Where D is the average crystallite size, the

wavelength of the radiation, Braggs angle and B
and b are the FWHMs observed for the sample and
standard, respectively. Terms B and 2 were
obtained from XRD pattern. The average
crystallite size for each sample was calculated
using the above formula. The results demonstrated
that the average particle size of Al2O3:Fe
nanoparticles was about 38.94 nm.
The iron-doped alumina nanoparticles were also
subjected to DTA analyses to investigate the phase
transformations. Figure 3 shows that the DTA
curve has two significant steps. The curve for the
powder calcined at 900 C first progressed upward
until 500 C and then peaked at 1000 C. However,
no peaks were observed at this temperature for the
powders calcined at 1100 C because of the
phase transition during calcination. Edrissi et
al.(2007) have also observed this phase
transition at 1100 C (Edrissi et al., 2007). The
DTA results confirmed the possibility of phase
transformation into a thermodynamically stable
crystallographic alpha alumina at about 1100 C.
This finding is consistent with previous XRD data.
The SEM micrographs of the powders calcined
at 900 C and 1100 C for 5 h are shown in Figures
4 and 5. The synthesized powders are generally
foamy in nature and agglomerated. As shown in
Figure 5, the void formations on the powder
structures are created by the evolution of large
amounts of gases during combustion and heat
treatment. The sizes of the voids on the Al2O3:Fe
nanopowders significantly increased as the heat
treatment temperature increased. This development
can be a result of increasing gas moles, that is, the
agglomerates tend to break up and become more

porous. Toniolo et al. (Toniolo et al., 2005) and

Kishan et al. (Kishan et al., 2010) have also
observed the growth of void sizes due to increasing
gas moles.
The mixture compounds can be estimated via
EDX. Figure 6 shows the even distribution of Al,
O, and Fe elements. In addition, the figure clearly
shows that carbon already emerged. Table 1
summarizes the results of the energy-dispersive
analysis of the alumina samples sintered at 900 C.
The values are given in weight and atomic percent.
4. CONCLUSION
Iron-doped alumina particles with average
crystallite sizes (38.94 nm) were successfully
synthesized by using sucrose (C12H22O11) as fuel
and dispersion agent. The results show that
combustion synthesis has more outstanding
potential in producing nanocrystalline iron-doped
alumina
powders
compared
with
other
conventional methods. As a water-soluble organic
carbon source, sucrose had a significant influence
on the synthesis of Al2O3:Fe nanopowders via the
carbothermal reduction during the combustion
synthesis. The characteristics of the produced
nanopowders significantly depend on the total
effects of releasing gas and heat. More specifically,
higher calcination temperatures resulted in
crystallite growth and agglomeration. Fe doped
alumina nanoparticles are widly used in different
fields such as catalyst support, biocompatible
material, and electrical applications.

Kakooei et al.
Synthesis and Characterization of Al2O3:Fe Nanoparticles Prepared via Aqueous Combustion

Fig. 2: The XRD patterns of Al2O3:Fe powders calcined at a) 900 C and b) 1100 C for 5h

Caspian Journal of Applied Sciences Research, 1(12), pp. 1-7, 2012

Fig. 3: The DTA curve of Al2O3:Fe powders calcined at 900 C and 1100 C

Fig. 4: SEM images of the Al2O3:Fe powders heated at 900 C

Kakooei et al.
Synthesis and Characterization of Al2O3:Fe Nanoparticles Prepared via Aqueous Combustion

Fig. 5: SEM images of the Al2O3:Fe powders heated at 1100 C

Fig. 6: EDX spectra of iron doped alumina nanoparticles calcined at 900 C

Journal of the American Ceramic Society,

57(8): 367-371.
Cordier A, Peigney A, De Grave E, Flahaut E,
Laurent C (2006). Synthesis of the
metastable -Al1.8/ Fe 0.2/O 3 solid solution
from precursors prepared by combustion.
Journal of the European Ceramic Society,
26(15): 3099-3111.
De Andrade M, Lima M, Bonadiman R, Bergmann
C (2006). Nanocrystalline pirochromite
spinel
through
solution
combustion
synthesis. Materials research bulletin,
41(11): 2070-2079.

REFERENCES
Bataille A, Addad A, Crampon J, Duclos R (2005).
Deformation behaviour of iron-doped
alumina. Journal of the European Ceramic
Society, 25(6): 857-862.
Breen J, Burch R, Coleman H(2002). Metalcatalysed steam reforming of ethanol in the
production of hydrogen for fuel cell
applications.
Applied
Catalysis
B:
Environmental, 39(1): 65-74.
Bye G, Simpkin G (1974). Influence of Cr and Fe
on Formation of Al2O3 from Al2O3.

Caspian Journal of Applied Sciences Research, 1(12), pp. 1-7, 2012

Deraz N, Shaban S (2009). Optimization of

catalytic, surface and magnetic properties of
nanocrystalline manganese ferrite. Journal of
Analytical and Applied Pyrolysis, 86(1):
173-179.
Edrissi M, Norouzbeigi R (2007). Synthesis and
characterization of alumina nanopowders by
combustion of nitrate-amino acid gels.
Materials Science-Poland, 25(4): 1029-1040.
Edrissi M, Norouzbeigi R (2008). Taguchi
Optimization for Combustion Synthesis of
Aluminum Oxide Nanoparticles. Chinese
Journal of Chemistry, 26(8): 1401-1406.
Holt JB, Kelly M (1993). Combustion synthesis
method and products, Google Patents.
Jamil RS, Abdul Razak K, Ahmad NF, Mohamad
H (2011). The Effect of Fuel Types on
Porous Alumina Produced via Soft
Combustion
Reaction
for
Implant
Applications.
Journal
of
Materials
Engineering and Performance: 1-6.
Kishan J, Mangam V, Reddy B, Das S, Das K
(2010). Aqueous combustion synthesis and
characterization
of
zirconia-alumina
nanocomposites. Journal of Alloys and
Compounds, 490(1-2): 631-636.
Kobayashi S, Kaneko S, Ohshima M, Kurokawa
H, Miura H (2012). Effect of iron oxide on
isobutane dehydrogenation over Pt/Fe 2 O3 Al2O3 catalyst. Applied Catalysis A:
General, Volumes 417418: 306312.
Lima M, Bonadimann R, de Andrade M, Toniolo J,
Bergmann C (2006). Nanocrystalline Cr 2 O
3 and amorphous CrO3 produced by solution
combustion synthesis. Journal of the
European Ceramic Society, 26(7): 12131220.
Lucio-Ortiz CJ, De la Rosa JR, Ramirez AH, De
los Reyes Heredia JA, del Angel P, MunozAguirre S, De Len-Covin LM (2011).

Synthesis and characterization of Fe doped

mesoporous Al2O3 by solgel method and its
use in trichloroethylene combustion. Journal
of sol-gel science and technology, 58(2):
374-384.
Meng FC, Tian ZQ, Zhang F, Tian CC, Huang WJ
(2010).
Combustion
Synthesis
of
Nanocrystalline Al2O3 Powders Using Urea
as Fuel: Influence of Different Combustion
Aids. Key Engineering Materials, 434: 868871.
Mukasyan A, Dinka P (2007). Novel approaches to
solution-combustion
synthesis
of
nanomaterials. International Journal of SelfPropagating High-Temperature Synthesis,
16(1): 23-35.
Nomura K, Kinoshita R, Sakamoto I, Okabayashi
J, Yamada Y (2012). Dilute magnetic
properties of Fe doped Al2O3 powders
prepared by sol-gel method. Hyperfine
Interactions: 1-5.
Pathak L, Singh T, Das S, Verma A,
Ramachandrarao P (2002). Effect of pH on
the combustion synthesis of nano-crystalline
alumina powder. Materials Letters, 57(2):
380-385.
Peng T, Liu X, Dai K, Xiao J, Song H (2006).
Effect of acidity on the glycine-nitrate
combustion synthesis of nanocrystalline
alumina powder. Materials research bulletin,
41(9): 1638-1645.
Toniolo J, Lima M, Takimi A, Bergmann C
(2005). Synthesis of alumina powders by the
glycine-nitrate
combustion
process.
Materials research bulletin, 40(3): 561-571.
Zhai X, Fu Y, Chu G (2006). New Technology
Reports Combustion synthesis of the
nano/structured
alumina
powder.
Nanoscience, 11(4): 286-292.