Synthesis And Characterization Of Sb2o3 Nanoparticles By Chemical Reduction Method
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Date
2012-03
Authors
Chin, Hui Shun
Journal Title
Journal ISSN
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Publisher
Universiti Sains Malaysia
Abstract
Antimony trioxide (Sb2O3) nanoparticles with particle size less than 100 nm, spherical in shape and well distributed were successfully synthesized by chemical reducing method. Antimony trichloride (SbCl3) was reduced by hydrazine in the presence of sodium hydroxide (NaOH) as catalyst in ethylene glycol (EG) at 120 oC for 60 minutes. In order to synthesis Sb2O3 nanoparticles with smaller particle size (2 - 12 nm), spherical in shape and well distribution, effects of hydrazine concentration ([N2H5OH]/[SbCl3] = 0.75, 5, 10, 20 and 30), NaOH concentration ([NaOH]/[SbCl3] = 0, 1, 3 and 5), precursor concentration ([SbCl3]/[N2H5OH] = 0.05, 0.1, 0.15 and 0.2), reaction temperature (60, 90, 120 and 150oC), reaction time (30, 60, 90 and 120 minutes) and boiling temperature (25, 50, 80 and 110oC) were investigated. Transmission electron microscope (TEM), selected area electron diffraction (SAED) pattern and high resolution electron microscope (HRTEM) were employed to study the morphology and crystallinity of the nanoparticles. It was observed that the particle size decreased and remained constant when concentration of hydrazine ([N2H5OH]/[SbCl3]) ≥ 10. Increasing the concentration of NaOH and precursor, as well as reaction temperature and reaction time, larger particles were formed. Further study on the crystallinity and phase of the nanoparticles was assisted by X-ray diffraction (XRD). XRD revealed a cubic phase of Sb2O3 (ICDD file no. 00-043-1071) with lattice spacing of 1.68 Å. However, diffraction peaks of SbCl3 were detected when hydrazine was added into an un-boiled mixture, which consists of both SbCl3 and NaOH in EG. It was found that adding hydrazine to the un-boiled
mixture influenced the mechanism of reduction of SbCl3 and eventually affected the production of Sb2O3 nanoparticles. From the ultraviolet-visible (UV-vis) spectrophotometer analysis, maximum absorption wavelengths of Sb2O3 nanoaparticles were occurred from 280 to 318 nm. The results showed that smaller particles were showed lower UV-vis absorption wavelength, while larger particles were showed higher UV-vis absorption wavelength. Therefore, correlation between UV-vis absorption wavelengths of the nanoparticles and their sizes has been established.
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Keywords
Synthesis and characterization of sb2o3 nanoparticles , by chemical reduction method