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Int. J. Bio-Inorg. Hybd. Nanomat., Vol. 1, No.

4 (2012), 253-256

International Journal of Bio-Inorganic Hybrid Nanomaterials

A Simple Method for Synthesis of γ-Aluminum Oxide


Nanostructure Using PEG as a Neutral Surfactant

Masoumeh Tabatabaee*, Naser Saberi

Department of Chemistry, Yazd Branch, Islamic Azad University, Yazd, Iran

Received: 14 October 2012; Accepted: 18 December 2012

ABSTRACT
Nano-sized γ-Al2O3 was synthesized successfully by a simple method using Al2(SO4)3·18H2O as
aluminium source and in the presence of polyethylene glycol (PEG 2000). FTIR spectroscopy,
X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron
microscope (TEM) were used to characterize the structure and morphology of synthesized
powder. The results showed that PEG played a significant role in the decomposition of aluminum
nitrate to γ-aluminum oxide nanoparticles with a size range of 10-15 nm. The experimental results
showed that polyethylene glycol can avoid hard agglomerate during precipitation and that
calcination temperature was the major factor to particles size of the final product and it played a
significant role in the decomposition of aluminum nitrate to γ-aluminum oxide nanoparticles.

Keyword: Nanoparticles; γ-Alumina; Hydrothermal synthesis; Polyethylene glycol; Particles size;


X-ray diffraction.

1. INTRODUCTION
In the past few years, much attention has been [7]. It is extensively used as catalyst, catalytic
focused on the research field of nano-crystalline supports [8, 9] and adsorbents [9-11]. Chemical
oxide materials, both because of their fundamental routes for production of Al2O3 include sol-gel,
importance and the wide range of potential techno- hydrothermal processing and control precipitation
logical applications [1-6]. Alumina exists in a of aluminum salts, alkoxides and metallic powders
variety of metastable structures including γ-, η-, δ-, [12-15]. Polyethylene glycol (PEG) in aqueous
θ-, κ-and χ-alumina, as well as its stable α-alumina solution is a highly mobile molecule with large
phase. Among these transitions, γ-alumina is one exclusion volume, and mainly free of charges
kind of extremely important nanosized materials which can avoid the strong interaction between the

(*) Corresponding Author - e-mail: tabatabaee45@gmail.com


Int. J. Bio-Inorg. Hybd. Nanomat., Vol. 1, No. 4 (2012), 253-256 Tabatabaee M et al

constituents [16, 17]. In continuation of our research 3. RESULTS AND DISCUSSION


on synthesis of metal-oxide in the presence of poly-
ethylene glycol [18, 19], we report a new method Figure 1 illustrates the XRD patterns of the
for the synthesis of nano-sized aluminum oxide prepared powders. It indicates the diffraction peaks
under hydrothermal condition and in the at 2θ values are attributed to the formation of
presence of polyethylene glycol in this work. XRD, γ-alumina and no characteristic peaks from other
SEM, TEM and FTIR were used to characterize the impurities were detected. The entire d-line patterns
product. The experimental results showed that match with reported values (JCPDS Card Pattern:
polyethylene glycol can avoid hard agglomerate 01-1307). It is very clear from Figure 1 that the
during precipitation and that calcination tempera- Al2O3 precursor particles show nano-size nature as
ture was the major factor for particle size of the it is seen from line broadening due to the presence
final product. When the calculation temperatures of small crystallite sizes.
were controlled between 400-600°C, the agglomer-
ate-free nano-sized γ-alumina particles were
obtained.

2. EXPERIMENTAL PROCEDURE

All chemicals are analytical-grade reagents without


further purification. Aluminum sulfate pentahy-
drate, Al2(SO4)3·18H2O, (4 g) and polyethylene
glycol (5 g) (abbreviated as PEG2000) were
dissolved in 100 mL distilled water. An amount of
ammonia (25%) was added into the above solution,
giving rise to milky precipitates at pH= 9. The Figure 1: The XRD patterns of synthesized Al2O3 nano-
reaction mixture was stirred for 1 h at room sized.
temperature. Then the reaction mixture was placed
in a Parr-Teflon lined stainless steel vessel. It was
sealed and heated at 130°C for 48 h. The reaction
mixture was gradually cooled to room temperature.
The resulting precipitate was filtered and washed
three to four times using double distilled water and
ethanol to remove polyethylene glycol and other
impurities. The synthesized Al2O3 powder was
dried at 100°C for 1 h and was calculated at 400°C
for 2 h. The sample was characterized by powder
X-ray diffraction (Bruker, Advance D8) with
Cu Kα (λ=1.5406 Å) incident radiation. The size
distribution and morphology of the sample was
analyzed by scanning electron microscopy (SEM,
Philips XL30) and Transmission electron Figure 2: TEM image of the synthesized Al2O3 nano-
microscopy (TEM, Philips CM10). Energy sized.
dispersive spectrometry (EDS) attached to SEM
was employed to perform the elemental analyses of The crystalline size was estimated from the
the nanostructure powder. broadening of Al2O3 diffraction peak using

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Tabatabaee M et al Int. J. Bio-Inorg. Hybd. Nanomat., Vol. 1, No. 4 (2012), 253-256

Scherrer's formula: width at half maximum (FWHM) and θ is the angle


kλ of diffraction. The crystalline size of nano-sized
t= Al2O3 is found to be ~10 nm. The TEM micrograph
B cos θ
of nano-sized powder along with the electron
Where t is the average size of the crystallite, diffraction pattern is shown in Figure 2. The
assuming that the grains are spherical, k is 0.9, λ is morphology of the Al2O3 nano-crystalline was
the wavelength of X-ray radiation, B is the peak full shown in Figure 3.

Figure 3: Scanning electron micrographs of synthesized.

Figure 4: FTIR spectra of γ-Al2O3.

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Int. J. Bio-Inorg. Hybd. Nanomat., Vol. 1, No. 4 (2012), 253-256 Tabatabaee M et al

FTIR spectra (Figure 4) of calcined product H., & Tabatabaee M., Microchim Acta,
shows that a broad band around 3470 cm-1 and 175(2001), 69.
1650 cm-1, which are assigned to stretching and 10. Baltrusaitis J., Schuttlefield J., Jensen J.H., &
bending modes of adsorbed water. The bonds in the Grassian V.H., Phys. Chem. Chem. Phys.,
region of 500-750 cm-1 and 800 cm-1 are assigned 9(2007), 4970.
to ν-AlO6 and ν-AlO4 [13]. 11. Sharma Y.C., Srivastava V., Upadhyay S.N., &
Weng C.H., Ind. Eng. Chem. Res., 47(2008),
8095.
4. CONCLUTIONS 12. Li J., Li W., Nai X., Bian S., Liu X., & Wei M.,
J. Mater. Sci., 45(2010), 177.
Nanoparticles of γ-Al2O3 were obtained by 13. Parida K.M., Amaresh C., Pradhan J.D. & Sahu
hydrothermally synthesis in the presence of poly N., Mater. Chem. Phys., 113(2009), 244.
ethylene glycol as a neutral surfactant. FTIR 14. Gun'ko V.M., Zarko V.I., Turov V.V., Oranska
spectra and XRD patern show the formation of O.I., Goncharuk E.V., Nychiporuk Y.M., Pakh-
γ-alumina. The broad XRD line indicates that the lov E.M., Yurchenko G.R., Leboda R.,
γ-Al2O3 particles are of nano size. Skubiszewska-Zieba J., Osovskii V.D., Ptushi-
nskii Y.G., Derzhypolskyi A.G., Melenevsky
D.A., & Blitz J.P., Powder Technology, 195
ACKNOWLEDGMENT (2009), 245.
15. Gleiter H., Acta Mater, 48(2000), 1.
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financial support. 60(2006), 1918.
17. Qiu C., Xiao X., Liu R., Ceramics Interna-
tional, 34(2008), 1747.
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