In-Situ FTIR Kinetic Study in the Silylation of Low-k Films with Hexamethyldisilazane Dissolved in Supercritical CO2

Eduardo Vyhmeister; Héctor Valdés-González; Lorenzo Reyes-Bozo; Roman Rodríguez-Maecker; Anthony Muscat; L. Antonio Estévez; David Suleiman

doi:10.1080/00986445.2015.1124098

In-Situ FTIR Kinetic Study in the Silylation of Low-k Films with Hexamethyldisilazane Dissolved in Supercritical CO₂

Eduardo Vyhmeister, Héctor Valdés-González, Lorenzo Reyes-Bozo, Roman Rodríguez-Maecker, Anthony Muscat, L. Antonio Estévez, David Suleiman

Chemical and Environmental Engineering

Research output: Contribution to journal › Article › peer-review

1 Scopus citations

Abstract

In-situ Fourier transform infrared spectroscopy measurements were obtained by using an innovative equipment to study the heterogeneous reaction between a hydrolyzed porous methylsilsesquioxane film and hexamethyldisilazane (HMDS) dissolved in CO₂ at supercritical conditions. Gas and solid infrared signatures were separated to obtain kinetic information of the heterogeneous reaction. A two-step reaction mechanism was observed: a fast first step controlled by kinetics and a second step controlled by the diffusion of the HMDS inside the porous material. Infrared information was used to derive a rate law expression of the silylation reaction between HMDS and Si-OH. A first order of reaction relative to the concentration of hydrophilic sites was observed with activation energy of 51.85 ± 1.25 kJ/mol.

Original language	English (US)
Pages (from-to)	908-916
Number of pages	9
Journal	Chemical Engineering Communications
Volume	203
Issue number	7
DOIs	https://doi.org/10.1080/00986445.2015.1124098
State	Published - Jul 2 2016

Keywords

HMDS
Kinetics
Reaction engineering
Semiconductors
Silylation
Supercritical fluids

ASJC Scopus subject areas

General Chemistry
General Chemical Engineering

Access to Document

10.1080/00986445.2015.1124098

Cite this

@article{14894c79d26347459ea21c1dc79dc9fb,

title = "In-Situ FTIR Kinetic Study in the Silylation of Low-k Films with Hexamethyldisilazane Dissolved in Supercritical CO2 ",

abstract = "In-situ Fourier transform infrared spectroscopy measurements were obtained by using an innovative equipment to study the heterogeneous reaction between a hydrolyzed porous methylsilsesquioxane film and hexamethyldisilazane (HMDS) dissolved in CO2 at supercritical conditions. Gas and solid infrared signatures were separated to obtain kinetic information of the heterogeneous reaction. A two-step reaction mechanism was observed: a fast first step controlled by kinetics and a second step controlled by the diffusion of the HMDS inside the porous material. Infrared information was used to derive a rate law expression of the silylation reaction between HMDS and Si-OH. A first order of reaction relative to the concentration of hydrophilic sites was observed with activation energy of 51.85 ± 1.25 kJ/mol.",

keywords = "HMDS, Kinetics, Reaction engineering, Semiconductors, Silylation, Supercritical fluids",

author = "Eduardo Vyhmeister and H{\'e}ctor Vald{\'e}s-Gonz{\'a}lez and Lorenzo Reyes-Bozo and Roman Rodr{\'i}guez-Maecker and Anthony Muscat and Est{\'e}vez, {L. Antonio} and David Suleiman",

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T1 - In-Situ FTIR Kinetic Study in the Silylation of Low-k Films with Hexamethyldisilazane Dissolved in Supercritical CO2

AU - Vyhmeister, Eduardo

AU - Valdés-González, Héctor

AU - Reyes-Bozo, Lorenzo

AU - Rodríguez-Maecker, Roman

AU - Muscat, Anthony

AU - Estévez, L. Antonio

AU - Suleiman, David

PY - 2016/7/2

Y1 - 2016/7/2

N2 - In-situ Fourier transform infrared spectroscopy measurements were obtained by using an innovative equipment to study the heterogeneous reaction between a hydrolyzed porous methylsilsesquioxane film and hexamethyldisilazane (HMDS) dissolved in CO2 at supercritical conditions. Gas and solid infrared signatures were separated to obtain kinetic information of the heterogeneous reaction. A two-step reaction mechanism was observed: a fast first step controlled by kinetics and a second step controlled by the diffusion of the HMDS inside the porous material. Infrared information was used to derive a rate law expression of the silylation reaction between HMDS and Si-OH. A first order of reaction relative to the concentration of hydrophilic sites was observed with activation energy of 51.85 ± 1.25 kJ/mol.

AB - In-situ Fourier transform infrared spectroscopy measurements were obtained by using an innovative equipment to study the heterogeneous reaction between a hydrolyzed porous methylsilsesquioxane film and hexamethyldisilazane (HMDS) dissolved in CO2 at supercritical conditions. Gas and solid infrared signatures were separated to obtain kinetic information of the heterogeneous reaction. A two-step reaction mechanism was observed: a fast first step controlled by kinetics and a second step controlled by the diffusion of the HMDS inside the porous material. Infrared information was used to derive a rate law expression of the silylation reaction between HMDS and Si-OH. A first order of reaction relative to the concentration of hydrophilic sites was observed with activation energy of 51.85 ± 1.25 kJ/mol.

KW - HMDS

KW - Kinetics

KW - Reaction engineering

KW - Semiconductors

KW - Silylation

KW - Supercritical fluids

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