Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli

Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli

A Supercritical fluid (SCF) is a processing technique which a fluid simultaneously heated and compressed above its critical temperature and pressure. A SCF is used to produce many types of materials since their properties can be varied with different reaction temperature (Treaction) and/or reaction...

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Main Author: Wan Zulkifli, Wan Zuliana
Format: Thesis
Language:English
Published: 2019
Online Access:https://ir.uitm.edu.my/id/eprint/90512/1/90512.pdf
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spelling my-uitm-ir.905122024-05-10T09:03:08Z Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli 2019 Wan Zulkifli, Wan Zuliana A Supercritical fluid (SCF) is a processing technique which a fluid simultaneously heated and compressed above its critical temperature and pressure. A SCF is used to produce many types of materials since their properties can be varied with different reaction temperature (Treaction) and/or reaction pressure (Preaction). In this study, cerate and/or zirconate based ceramic powders of BaCe0.9Y0.1O2.95 (BCY), BaZr0.9Y0.1O2.95 (BZY) and BaCe0.54Zr0.36Y0.1O2.95 (BCZY) were synthesized by a high pressure-high temperature (HP-HT) batch wise reactor system using a SCF method. Ethanol was used to synthesize BCY and BZY powders at a constant Preaction (4 MPa) but a different in the Treaction ranging from 150 – 300 °C. Conversely, BCZY powder was synthesized using six different reaction media, namely ethanol, methanol, hexane, pentane, acetone and dichloromethane. Later, a SCF assisted sol-gel (SCF-SG) method was proposed by employment of Polyoxyethyle (10) oleyl ether (Brij97) as a surfactant to improve the properties of BCZY powder. In the synthesis of BCZY sample using a SCF-SG method, a gel was dried at temperature (Tdrying) of 150 – 325 °C. Then, it was subjected to HP-HT batch wise reactor system using a SCF at a constant Treaction (150 °C) and different Preaction ranging from 2 – 4 MPa. The prepared samples were characterized using Fourier transform infrared (FTIR) spectroscopy, X-ray diffractometry (XRD) and scanning electron microscope/energy dispersive X-ray (SEM/EDX). The presence of carbonate compound at ~800 cm-1 and metal-oxide (M–O) bond at 700 – 400 cm-1 in the BCY, BZY and BCZY after calcined at 1100 °C was confirmed by FTIR analysis. XRD result revealed that a single perovskite of BCY and BZY was formed at minimum calcination temperature of 800 °C and 1100 °C, respectively. The BCZY prepared by a SCF using ethanol as reaction medium at calcination temperature of 1100 °C showed the less secondary phases of BaCO3, BaCeO3, BaZrO3, CeO2, ZrO3, BaO2 and Ba(OH)2 compared to others medium. The formation of single perovskite phase of BCZY was only obtained after prepared via a SCF-SG at Preaction 2 MPa. The SEM results depicted that the particles of the single perovskite phase of BCY and BZY samples prepared by a SCF are respectively, cubical and spherical in shape. The employment of Brij97 in a SCF-SG produced homogeneous and fewer agglomerated particles with size ranging from 60 to 90 nm. As a conclusion, the used of surfactant in a SCF-SG method able to produce a single perovskite phase of BCZY ceramic powder with homogeneous and fine particles. Therefore, a study on significant parameter involved in a SCF and SCF-SG methods may contribute to a significant new knowledge in the synthesis of cerate, zirconate and cerate-zirconate ceramic powders at a relatively lower processing temperature. 2019 Thesis https://ir.uitm.edu.my/id/eprint/90512/ https://ir.uitm.edu.my/id/eprint/90512/1/90512.pdf text en public masters Universiti Teknologi MARA (UiTM) Faculty of Applied Science Osman, Nafisah
institution Universiti Teknologi MARA
collection UiTM Institutional Repository
language English
advisor Osman, Nafisah
description A Supercritical fluid (SCF) is a processing technique which a fluid simultaneously heated and compressed above its critical temperature and pressure. A SCF is used to produce many types of materials since their properties can be varied with different reaction temperature (Treaction) and/or reaction pressure (Preaction). In this study, cerate and/or zirconate based ceramic powders of BaCe0.9Y0.1O2.95 (BCY), BaZr0.9Y0.1O2.95 (BZY) and BaCe0.54Zr0.36Y0.1O2.95 (BCZY) were synthesized by a high pressure-high temperature (HP-HT) batch wise reactor system using a SCF method. Ethanol was used to synthesize BCY and BZY powders at a constant Preaction (4 MPa) but a different in the Treaction ranging from 150 – 300 °C. Conversely, BCZY powder was synthesized using six different reaction media, namely ethanol, methanol, hexane, pentane, acetone and dichloromethane. Later, a SCF assisted sol-gel (SCF-SG) method was proposed by employment of Polyoxyethyle (10) oleyl ether (Brij97) as a surfactant to improve the properties of BCZY powder. In the synthesis of BCZY sample using a SCF-SG method, a gel was dried at temperature (Tdrying) of 150 – 325 °C. Then, it was subjected to HP-HT batch wise reactor system using a SCF at a constant Treaction (150 °C) and different Preaction ranging from 2 – 4 MPa. The prepared samples were characterized using Fourier transform infrared (FTIR) spectroscopy, X-ray diffractometry (XRD) and scanning electron microscope/energy dispersive X-ray (SEM/EDX). The presence of carbonate compound at ~800 cm-1 and metal-oxide (M–O) bond at 700 – 400 cm-1 in the BCY, BZY and BCZY after calcined at 1100 °C was confirmed by FTIR analysis. XRD result revealed that a single perovskite of BCY and BZY was formed at minimum calcination temperature of 800 °C and 1100 °C, respectively. The BCZY prepared by a SCF using ethanol as reaction medium at calcination temperature of 1100 °C showed the less secondary phases of BaCO3, BaCeO3, BaZrO3, CeO2, ZrO3, BaO2 and Ba(OH)2 compared to others medium. The formation of single perovskite phase of BCZY was only obtained after prepared via a SCF-SG at Preaction 2 MPa. The SEM results depicted that the particles of the single perovskite phase of BCY and BZY samples prepared by a SCF are respectively, cubical and spherical in shape. The employment of Brij97 in a SCF-SG produced homogeneous and fewer agglomerated particles with size ranging from 60 to 90 nm. As a conclusion, the used of surfactant in a SCF-SG method able to produce a single perovskite phase of BCZY ceramic powder with homogeneous and fine particles. Therefore, a study on significant parameter involved in a SCF and SCF-SG methods may contribute to a significant new knowledge in the synthesis of cerate, zirconate and cerate-zirconate ceramic powders at a relatively lower processing temperature.
format Thesis
qualification_level Master's degree
author Wan Zulkifli, Wan Zuliana
spellingShingle Wan Zulkifli, Wan Zuliana
Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli
author_facet Wan Zulkifli, Wan Zuliana
author_sort Wan Zulkifli, Wan Zuliana
title Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli
title_short Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli
title_full Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli
title_fullStr Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli
title_full_unstemmed Supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / Wan Zuliana Wan Zulkifli
title_sort supercritical fluid: a potential route in the synthesis of cerate, zirconate and cerate-zirconate ceramics powder / wan zuliana wan zulkifli
granting_institution Universiti Teknologi MARA (UiTM)
granting_department Faculty of Applied Science
publishDate 2019
url https://ir.uitm.edu.my/id/eprint/90512/1/90512.pdf
_version_ 1804889823413010432

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