Pyrolysis of self-assembled organic monolayers on oxide substrates

Hyunjung Shin; Yuhu Wang; Uma Sampathkumaran; Mark R. De Guire; Arthur H. Heuer; Chaim N. Sukenik

doi:10.1557/jmr.1999.0286

Pyrolysis of self-assembled organic monolayers on oxide substrates

Hyunjung Shin, Yuhu Wang, Uma Sampathkumaran, Mark R. De Guire, Arthur H. Heuer, Chaim N. Sukenik

Department of Chemistry

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23 Scopus citations

Abstract

The pyrolysis of siloxy-anchored, organic self-assembled monolayers (SAMs) on oxide substrates [titanium dioxide powder; hydrolyzed silicon dioxide on (100) silicon] was studied using x-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and mass spectroscopy (MS). Pyrolysis in air began on heating at 200°C and was complete by 400°C for both octadecyltrichlorosilane (OTS) and C₁₆-thioacetate (TA) SAMs, as observed in TGA of SAM-coated TiO₂ powders, and in XPS studies of TA-SAM-coated TiO₂ powders and Si wafers after various heat treatments. In low-oxygen environments, pyrolysis of SAMs began at higher temperatures: between 250 and 400°C for heating in ultrahigh vacuum (10^-8 Torr) as observed in XPS studies of TA-SAMs on Si, and between 300 and 400°C in nitrogen, as observed in TEM analysis of sulfonate SAMs under a TiO₂ thin film on Si substrates.

Original language	English
Pages (from-to)	2116-2123
Number of pages	8
Journal	Journal of Materials Research
Volume	14
Issue number	5
DOIs	https://doi.org/10.1557/jmr.1999.0286
State	Published - May 1999

Bibliographical note

Funding Information:
The authors thank Dr. R. J. Collins for her helpful discussions and for assistance with synthesis of the organic silanes. We also thank Professor P. K. Gallagher at The Ohio State University Dept. of Chemistry for carrying out the thermogravimetric analysis and Dr. H. Kahn of CWRU for assistance with the heat treatments in vacuum. Professor M. Rühle of the Max-Plank Insti-tut für Metallforschung in Stuttgart, Germany provided valuable insight regarding contrast in TEM images. During part of this research, H. Shin was an Alexander von Humboldt Junior Fellow and M. R. De Guire was a visiting scientist at the Max-Plank Institut für Metallforschung in Stuttgart, Germany, which support is gratefully acknowledged. Financial support was provided by AFOSR under Contract No. F49620-92J-0282 and by the Basic Missile Defense Office through an STTR Award to Solid State Scientific Corporation. C. N. Sukenik acknowledges the support of the Israel Ministry of Science.

Funding

The authors thank Dr. R. J. Collins for her helpful discussions and for assistance with synthesis of the organic silanes. We also thank Professor P. K. Gallagher at The Ohio State University Dept. of Chemistry for carrying out the thermogravimetric analysis and Dr. H. Kahn of CWRU for assistance with the heat treatments in vacuum. Professor M. Rühle of the Max-Plank Insti-tut für Metallforschung in Stuttgart, Germany provided valuable insight regarding contrast in TEM images. During part of this research, H. Shin was an Alexander von Humboldt Junior Fellow and M. R. De Guire was a visiting scientist at the Max-Plank Institut für Metallforschung in Stuttgart, Germany, which support is gratefully acknowledged. Financial support was provided by AFOSR under Contract No. F49620-92J-0282 and by the Basic Missile Defense Office through an STTR Award to Solid State Scientific Corporation. C. N. Sukenik acknowledges the support of the Israel Ministry of Science.

Funders	Funder number
Basic Missile Defense Office
Air Force Office of Scientific Research	F49620-92J-0282
Ministry of science and technology, Israel

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10.1557/jmr.1999.0286

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title = "Pyrolysis of self-assembled organic monolayers on oxide substrates",

abstract = "The pyrolysis of siloxy-anchored, organic self-assembled monolayers (SAMs) on oxide substrates [titanium dioxide powder; hydrolyzed silicon dioxide on (100) silicon] was studied using x-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and mass spectroscopy (MS). Pyrolysis in air began on heating at 200°C and was complete by 400°C for both octadecyltrichlorosilane (OTS) and C16-thioacetate (TA) SAMs, as observed in TGA of SAM-coated TiO2 powders, and in XPS studies of TA-SAM-coated TiO2 powders and Si wafers after various heat treatments. In low-oxygen environments, pyrolysis of SAMs began at higher temperatures: between 250 and 400°C for heating in ultrahigh vacuum (10-8 Torr) as observed in XPS studies of TA-SAMs on Si, and between 300 and 400°C in nitrogen, as observed in TEM analysis of sulfonate SAMs under a TiO2 thin film on Si substrates.",

author = "Hyunjung Shin and Yuhu Wang and Uma Sampathkumaran and {De Guire}, {Mark R.} and Heuer, {Arthur H.} and Sukenik, {Chaim N.}",

note = "Funding Information: The authors thank Dr. R. J. Collins for her helpful discussions and for assistance with synthesis of the organic silanes. We also thank Professor P. K. Gallagher at The Ohio State University Dept. of Chemistry for carrying out the thermogravimetric analysis and Dr. H. Kahn of CWRU for assistance with the heat treatments in vacuum. Professor M. R{\"u}hle of the Max-Plank Insti-tut f{\"u}r Metallforschung in Stuttgart, Germany provided valuable insight regarding contrast in TEM images. During part of this research, H. Shin was an Alexander von Humboldt Junior Fellow and M. R. De Guire was a visiting scientist at the Max-Plank Institut f{\"u}r Metallforschung in Stuttgart, Germany, which support is gratefully acknowledged. Financial support was provided by AFOSR under Contract No. F49620-92J-0282 and by the Basic Missile Defense Office through an STTR Award to Solid State Scientific Corporation. C. N. Sukenik acknowledges the support of the Israel Ministry of Science.",

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AU - Heuer, Arthur H.

AU - Sukenik, Chaim N.

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Pyrolysis of self-assembled organic monolayers on oxide substrates

Abstract

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