Compositional Analysis of SiOC(H) Powders: A Comparison of X-ray Photoelectron Spectroscopy (XPS) and Combustion Analysis

Accurate chemical analysis of small samples of fine powders in the Si–O–C–H system is challenging. We present a comparison of analysis by X-ray photoelectron spectroscopy (XPS) and combustion analysis, validating XPS as an accurate and simple methodology for Si, C, and O analysis to give bulk and no...

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Main Authors: Gerson J. Leonel, Xin Guo, Gurpreet Singh, Alexandra Navrotsky
Format: Article
Language:English
Published: MDPI AG 2023-01-01
Series:Ceramics
Subjects:
Online Access:https://www.mdpi.com/2571-6131/6/1/6
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author Gerson J. Leonel
Xin Guo
Gurpreet Singh
Alexandra Navrotsky
author_facet Gerson J. Leonel
Xin Guo
Gurpreet Singh
Alexandra Navrotsky
author_sort Gerson J. Leonel
collection DOAJ
description Accurate chemical analysis of small samples of fine powders in the Si–O–C–H system is challenging. We present a comparison of analysis by X-ray photoelectron spectroscopy (XPS) and combustion analysis, validating XPS as an accurate and simple methodology for Si, C, and O analysis to give bulk and not just surface compositions. The XPS analyses are supported by showing consistency in thermochemical calculations of heats of formation based on high temperature oxide melt solution calorimetry. However, because XPS is not suitable for quantitation of hydrogen, it must be combined with other techniques for samples with substantial H content.
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spelling doaj.art-1edcb3a50d7c493082c94e060e17449f2023-11-17T10:14:33ZengMDPI AGCeramics2571-61312023-01-0161748510.3390/ceramics6010006Compositional Analysis of SiOC(H) Powders: A Comparison of X-ray Photoelectron Spectroscopy (XPS) and Combustion AnalysisGerson J. Leonel0Xin Guo1Gurpreet Singh2Alexandra Navrotsky3School of Molecular Sciences, Arizona State University, Tempe, AZ 85287, USAEyring Materials Center, Arizona State University, Tempe, AZ 85287, USAMechanical and Nuclear Engineering Department, Kansas State University, 3002 Rathbone Hall, Manhattan, KS 66506, USASchool of Molecular Sciences, Arizona State University, Tempe, AZ 85287, USAAccurate chemical analysis of small samples of fine powders in the Si–O–C–H system is challenging. We present a comparison of analysis by X-ray photoelectron spectroscopy (XPS) and combustion analysis, validating XPS as an accurate and simple methodology for Si, C, and O analysis to give bulk and not just surface compositions. The XPS analyses are supported by showing consistency in thermochemical calculations of heats of formation based on high temperature oxide melt solution calorimetry. However, because XPS is not suitable for quantitation of hydrogen, it must be combined with other techniques for samples with substantial H content.https://www.mdpi.com/2571-6131/6/1/6industrial precusorspolymer-derived ceramicsnanodomain structurepolysiloxanesenergeticssilicon oxycarbide
spellingShingle Gerson J. Leonel
Xin Guo
Gurpreet Singh
Alexandra Navrotsky
Compositional Analysis of SiOC(H) Powders: A Comparison of X-ray Photoelectron Spectroscopy (XPS) and Combustion Analysis
Ceramics
industrial precusors
polymer-derived ceramics
nanodomain structure
polysiloxanes
energetics
silicon oxycarbide
title Compositional Analysis of SiOC(H) Powders: A Comparison of X-ray Photoelectron Spectroscopy (XPS) and Combustion Analysis
title_full Compositional Analysis of SiOC(H) Powders: A Comparison of X-ray Photoelectron Spectroscopy (XPS) and Combustion Analysis
title_fullStr Compositional Analysis of SiOC(H) Powders: A Comparison of X-ray Photoelectron Spectroscopy (XPS) and Combustion Analysis
title_full_unstemmed Compositional Analysis of SiOC(H) Powders: A Comparison of X-ray Photoelectron Spectroscopy (XPS) and Combustion Analysis
title_short Compositional Analysis of SiOC(H) Powders: A Comparison of X-ray Photoelectron Spectroscopy (XPS) and Combustion Analysis
title_sort compositional analysis of sioc h powders a comparison of x ray photoelectron spectroscopy xps and combustion analysis
topic industrial precusors
polymer-derived ceramics
nanodomain structure
polysiloxanes
energetics
silicon oxycarbide
url https://www.mdpi.com/2571-6131/6/1/6
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AT gurpreetsingh compositionalanalysisofsiochpowdersacomparisonofxrayphotoelectronspectroscopyxpsandcombustionanalysis
AT alexandranavrotsky compositionalanalysisofsiochpowdersacomparisonofxrayphotoelectronspectroscopyxpsandcombustionanalysis