Characterization study of platinum-doped stannic oxide ceramics for methane sensing in air

Pure SnO2 and Pt-SnO2 ceramics were prepared by the dry-pressing method using a pressure of 40 MPa and sintered at various temperatures between 100-000oC from a mixture of powders of (100-x)SnO2.xPt (0 = x wt % = 5). The electrical properties of the ceramics were studied using a home-made Sensor Ele...

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Main Author: Ibrahim, Zuhairi
Format: Thesis
Language:English
Published: 2005
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Online Access:http://eprints.utm.my/id/eprint/4290/1/ZuhairiIbrahimPFS2005.pdf
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spelling my-utm-ep.42902018-01-16T07:47:02Z Characterization study of platinum-doped stannic oxide ceramics for methane sensing in air 2005-06 Ibrahim, Zuhairi QD Chemistry Pure SnO2 and Pt-SnO2 ceramics were prepared by the dry-pressing method using a pressure of 40 MPa and sintered at various temperatures between 100-000oC from a mixture of powders of (100-x)SnO2.xPt (0 = x wt % = 5). The electrical properties of the ceramics were studied using a home-made Sensor Element Characterization System (SECS) and an Impedance Analyzer. The sensing probe of the SECS was modified so it was much slimmer with most of the electrical connections concealed and could measure either the bulk or surface resistance of the ceramic. The optimum composition for detecting methane in air was 0.5 wt.% Pt-SnO2 sintered at 1000oC and the optimum operating temperature was at 400oC. The resistance of the 0.5 wt.% Pt-SnO2 in 25000 ppm methane decreases from ~ 54.0 kO to ~ 4.6 kO at temperatures of 200oC up to 440oC respectively. The activation energies were between 0.30 eV and 0.45 eV for temperatures between 200oC and 400oC. The corresponding conductance (G) decreased with Pt loading and the gas partial pressure (p) or methane flow rate (?). As such, it indicates that the doped SnO2 is an n-type semiconductor. The conductance power law takes the form G ~ p-0.5 and this indicates that the chemisorbed ions on the doped ceramics depended only on temperature. The conductance (G)- methane concentration (c) takes the form G = kc0.35. A linear relationship ln G = 0.35 ln c – 11.9 was obtained when plotting ln G against ln c. The relative conductance change (?G/G) and the square root of methane concentrations (c½) obey the relationship ?G/G = 0.08c ½ which indicates the doping with 0.5 wt.% Pt increased the sensitivity of the base material (SnO2) to methane by a factor of 133. The response and recovery times were affected by the methane flow rate, operational temperature, level of doping with values between 30 s up to 154 s and between 600 s up to 1317 s respectively. The doping of Pt at 0.1 wt.% up to 5 wt.% in SnO2 produced ceramics with densities of 7.01g/cm3 up to 7.03 g/cm3 which exceeds the full density of pure SnO2 (6.90 g/cm3). The strength and stability were indicated from the doped SnO2 measurements of Vickers hardness (10 GPa and up to 19 GPa), Young modulus (20 GPa and up to 55 GPa) and Bulk modulus (20 GPa and up to 80 GPa) for Pt loadings between 0.1wt.% and 2.5 wt.%. High resolution X-ray diffraction showed that the mean crystallite size ranges between 25 nm and 55 nm for Pt loadings from 1 wt% up to 5 wt.% in SnO2. The strain in doped samples could not be eradicated by either sintering at high temperature (1000oC) or high Pt loading (5 wt.%). X-ray photoemissions spectroscopy (XPS), Mössbauer and nuclear magnetic resonance (NMR) analysis showed that the doped SnO2 has additional chemical environment (compared to pure SnO2) can be attributed to the ease of detecting methane in air via electrical measurements. 2005-06 Thesis http://eprints.utm.my/id/eprint/4290/ http://eprints.utm.my/id/eprint/4290/1/ZuhairiIbrahimPFS2005.pdf application/pdf en public phd doctoral Universiti Teknologi Malaysia, Faculty of Science Faculty of Science
institution Universiti Teknologi Malaysia
collection UTM Institutional Repository
language English
topic QD Chemistry
spellingShingle QD Chemistry
Ibrahim, Zuhairi
Characterization study of platinum-doped stannic oxide ceramics for methane sensing in air
description Pure SnO2 and Pt-SnO2 ceramics were prepared by the dry-pressing method using a pressure of 40 MPa and sintered at various temperatures between 100-000oC from a mixture of powders of (100-x)SnO2.xPt (0 = x wt % = 5). The electrical properties of the ceramics were studied using a home-made Sensor Element Characterization System (SECS) and an Impedance Analyzer. The sensing probe of the SECS was modified so it was much slimmer with most of the electrical connections concealed and could measure either the bulk or surface resistance of the ceramic. The optimum composition for detecting methane in air was 0.5 wt.% Pt-SnO2 sintered at 1000oC and the optimum operating temperature was at 400oC. The resistance of the 0.5 wt.% Pt-SnO2 in 25000 ppm methane decreases from ~ 54.0 kO to ~ 4.6 kO at temperatures of 200oC up to 440oC respectively. The activation energies were between 0.30 eV and 0.45 eV for temperatures between 200oC and 400oC. The corresponding conductance (G) decreased with Pt loading and the gas partial pressure (p) or methane flow rate (?). As such, it indicates that the doped SnO2 is an n-type semiconductor. The conductance power law takes the form G ~ p-0.5 and this indicates that the chemisorbed ions on the doped ceramics depended only on temperature. The conductance (G)- methane concentration (c) takes the form G = kc0.35. A linear relationship ln G = 0.35 ln c – 11.9 was obtained when plotting ln G against ln c. The relative conductance change (?G/G) and the square root of methane concentrations (c½) obey the relationship ?G/G = 0.08c ½ which indicates the doping with 0.5 wt.% Pt increased the sensitivity of the base material (SnO2) to methane by a factor of 133. The response and recovery times were affected by the methane flow rate, operational temperature, level of doping with values between 30 s up to 154 s and between 600 s up to 1317 s respectively. The doping of Pt at 0.1 wt.% up to 5 wt.% in SnO2 produced ceramics with densities of 7.01g/cm3 up to 7.03 g/cm3 which exceeds the full density of pure SnO2 (6.90 g/cm3). The strength and stability were indicated from the doped SnO2 measurements of Vickers hardness (10 GPa and up to 19 GPa), Young modulus (20 GPa and up to 55 GPa) and Bulk modulus (20 GPa and up to 80 GPa) for Pt loadings between 0.1wt.% and 2.5 wt.%. High resolution X-ray diffraction showed that the mean crystallite size ranges between 25 nm and 55 nm for Pt loadings from 1 wt% up to 5 wt.% in SnO2. The strain in doped samples could not be eradicated by either sintering at high temperature (1000oC) or high Pt loading (5 wt.%). X-ray photoemissions spectroscopy (XPS), Mössbauer and nuclear magnetic resonance (NMR) analysis showed that the doped SnO2 has additional chemical environment (compared to pure SnO2) can be attributed to the ease of detecting methane in air via electrical measurements.
format Thesis
qualification_name Doctor of Philosophy (PhD.)
qualification_level Doctorate
author Ibrahim, Zuhairi
author_facet Ibrahim, Zuhairi
author_sort Ibrahim, Zuhairi
title Characterization study of platinum-doped stannic oxide ceramics for methane sensing in air
title_short Characterization study of platinum-doped stannic oxide ceramics for methane sensing in air
title_full Characterization study of platinum-doped stannic oxide ceramics for methane sensing in air
title_fullStr Characterization study of platinum-doped stannic oxide ceramics for methane sensing in air
title_full_unstemmed Characterization study of platinum-doped stannic oxide ceramics for methane sensing in air
title_sort characterization study of platinum-doped stannic oxide ceramics for methane sensing in air
granting_institution Universiti Teknologi Malaysia, Faculty of Science
granting_department Faculty of Science
publishDate 2005
url http://eprints.utm.my/id/eprint/4290/1/ZuhairiIbrahimPFS2005.pdf
_version_ 1747814508162711552