Chin , Hui Shun (2012) Synthesis And Characterization Of Sb2O3 Nanoparticles By Chemical Reduction Method. Masters thesis, Universiti Sains Malaysia.
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Abstract
Nanopartikel antimoni trioksida (Sb2O3) dengan saiz kurang daripada 100 nm, berbentuk sfera dan taburan yang sekata telah berjaya dihasilkan melalui kaedah penurunan kimia. Antimoni triklorida (SbCl3) telah diturunkan oleh hidrazin dalam kehadiran natrium hidroksida (NaOH) sebagai pemangkin dalam etilena glikol (EG) pada suhu 120 oC selama 60 minit. Bagi menghasilkan nanopartikel Sb2O3 dengan saiz partikel yang kecil (2 - 12 nm), berbentuk sfera dan taburan yang sekata, kesan kepekatan hidrazin ([N2H5OH]/[SbCl3] = 0.75, 5, 10, 20 dan 30), kepekatan NaOH ([NaOH]/[SbCl3] = 0, 1, 3 dan 5), kepekatan prapenanda ([SbCl3]/[N2H5OH] = 0.05, 0.1, 0.15 dan 0.2), suhu tindak balas (60, 90, 120 dan 150oC), masa tindak balas (30, 60, 90 dan 120 minit) dan suhu didih (25, 50, 80 dan 110oC) telah dikaji secara sistematik. Microskop penghantaran elektron (TEM), kawasan yang dipilih pola pembelauan elektron (SAED) dan mikroskop elektron resolusi tinggi (HRTEM) telah diaplikasikan untuk mengkaji morfologi dan penghabluran nanopartikel. Pemerhatian menunjukkan bahawa saiz partikel berkurang dan tidak berubah apabila kepekatan hidrazin ([N2H5OH]/[SbCl3]) ≥ 10. Partikel yang lebih besar telah dihasilkan apabila kepekatan NaOH dan prapenanda, serta suhu dan masa tindak balas dinaikkan. Selanjutnya kajian penghabluran dan fasa nanopartikel telah dibantu oleh pembelauan sinar-X (XRD). XRD menunjukkan bahawa nanopartikel Sb2O3 adalah dalam fasa kubik. (ICDD file no. 00-043-1071) dengan kekisi jarak 1.68 Å. Walaubagaimanapun, puncak pembelauan SbCl3 telah dikesan apabila hidrazin ditambahkan ke dalam campuran yang belum didih, campuran tersebut mengandungi kedua-dua SbCl3 dan NaOH dalam EG. Penambahan hidrazin ke dalam campuran yang belum mendidih mempengaruhi mekanisme penurunan SbCl3 dan seterusnya penghasilan nanopartikel Sb2O3. Analisis ultraungu-nampak (UV-vis) spektrofotometer menunjukkan bahawa penyerapan panjang gelombang maksimum nanopartikel Sb2O3 telah berlaku dalam linkungan 280 hingga 318 nm. Keputusan kajian menunjukkan partikel yang kecil menyerap pada panjang gelombang UV-vis yang rendah, manakala partikel yang besar menyerap pada panjang gelombang UV-vis yang tinggi. Oleh itu, hubungan antara penyerapan panjang gelombang UV-vis nanopartikel dan saiznya telah ditetapkan. _______________________________________________________________________________________________________ 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.
| Item Type: | Thesis (Masters) |
|---|---|
| Additional Information: | full text available at http://irplus.eng.usm.my:8080/ir_plus/institutionalPublicationPublicView.action?institutionalItemId=1906 |
| Subjects: | T Technology T Technology > TP Chemical Technology > TP1-1185 Chemical technology |
| Divisions: | Kampus Kejuruteraan (Engineering Campus) > Pusat Pengajian Kejuruteraan Bahan & Sumber Mineral (School of Material & Mineral Resource Engineering) > Thesis |
| Depositing User: | Mr Mohd Jasnizam Mohd Salleh |
| Date Deposited: | 04 Jun 2018 06:51 |
| Last Modified: | 04 Jun 2018 06:51 |
| URI: | http://eprints.usm.my/id/eprint/40680 |
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