In situ FTIR experimental results in the silylation of low-k films with hexamethyldisilazane dissolved in supercritical carbon dioxide

Eduardo Vyhmeister; Lorenzo Reyes-Bozo; Héctor Valdés-González; José Luis Salazar; Anthony Muscat; L. Antonio Estévez; David Suleiman

doi:10.1016/j.supflu.2014.01.019

In situ FTIR experimental results in the silylation of low-k films with hexamethyldisilazane dissolved in supercritical carbon dioxide

Eduardo Vyhmeister, Lorenzo Reyes-Bozo, Héctor Valdés-González, José Luis Salazar, Anthony Muscat, L. Antonio Estévez, David Suleiman

Chemical and Environmental Engineering

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

19 Scopus citations

Abstract

In situ Fourier Transform Infrared Spectroscopy measurements were performed using an innovative equipment to study the surface modification reaction between a functionalized porous MSQ-film and hexamethyldisilazane (HMDS) dissolved in CO₂ at supercritical conditions (scCO₂). scCO₂ was used in the heterogeneous reaction due to enhancing properties, ideal for porous materials. Different infrared signatures, from the gas and solid phases, were observed and identified, implying gas-gas and solid-gas phase reactions. Among the different component signatures observed in the gas phase, carbonic acid was observed as a possible silylating gas phase nucleophilic component, while in the solid phase the predominant reaction mechanism proceeded by forming SiOSi bonds and Trimethylaminosilane (as gas phase product).

Original language	English (US)
Pages (from-to)	134-143
Number of pages	10
Journal	Journal of Supercritical Fluids
Volume	90
DOIs	https://doi.org/10.1016/j.supflu.2014.01.019
State	Published - Jun 2014

Keywords

HMDS
Heterogeneous reaction
In situ FTIR
Low-k
Silylation

ASJC Scopus subject areas

General Chemical Engineering
Condensed Matter Physics
Physical and Theoretical Chemistry

Access to Document

10.1016/j.supflu.2014.01.019

Cite this

@article{8b8f85f4263e4128a6b8e8db40f65004,

title = "In situ FTIR experimental results in the silylation of low-k films with hexamethyldisilazane dissolved in supercritical carbon dioxide",

abstract = "In situ Fourier Transform Infrared Spectroscopy measurements were performed using an innovative equipment to study the surface modification reaction between a functionalized porous MSQ-film and hexamethyldisilazane (HMDS) dissolved in CO2 at supercritical conditions (scCO2). scCO2 was used in the heterogeneous reaction due to enhancing properties, ideal for porous materials. Different infrared signatures, from the gas and solid phases, were observed and identified, implying gas-gas and solid-gas phase reactions. Among the different component signatures observed in the gas phase, carbonic acid was observed as a possible silylating gas phase nucleophilic component, while in the solid phase the predominant reaction mechanism proceeded by forming SiOSi bonds and Trimethylaminosilane (as gas phase product).",

keywords = "HMDS, Heterogeneous reaction, In situ FTIR, Low-k, Silylation",

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

year = "2014",

month = jun,

doi = "10.1016/j.supflu.2014.01.019",

language = "English (US)",

volume = "90",

pages = "134--143",

journal = "Journal of Supercritical Fluids",

issn = "0896-8446",

publisher = "Elsevier B.V.",

}

TY - JOUR

T1 - In situ FTIR experimental results in the silylation of low-k films with hexamethyldisilazane dissolved in supercritical carbon dioxide

AU - Vyhmeister, Eduardo

AU - Reyes-Bozo, Lorenzo

AU - Valdés-González, Héctor

AU - Salazar, José Luis

AU - Muscat, Anthony

AU - Estévez, L. Antonio

AU - Suleiman, David

PY - 2014/6

Y1 - 2014/6

N2 - In situ Fourier Transform Infrared Spectroscopy measurements were performed using an innovative equipment to study the surface modification reaction between a functionalized porous MSQ-film and hexamethyldisilazane (HMDS) dissolved in CO2 at supercritical conditions (scCO2). scCO2 was used in the heterogeneous reaction due to enhancing properties, ideal for porous materials. Different infrared signatures, from the gas and solid phases, were observed and identified, implying gas-gas and solid-gas phase reactions. Among the different component signatures observed in the gas phase, carbonic acid was observed as a possible silylating gas phase nucleophilic component, while in the solid phase the predominant reaction mechanism proceeded by forming SiOSi bonds and Trimethylaminosilane (as gas phase product).

AB - In situ Fourier Transform Infrared Spectroscopy measurements were performed using an innovative equipment to study the surface modification reaction between a functionalized porous MSQ-film and hexamethyldisilazane (HMDS) dissolved in CO2 at supercritical conditions (scCO2). scCO2 was used in the heterogeneous reaction due to enhancing properties, ideal for porous materials. Different infrared signatures, from the gas and solid phases, were observed and identified, implying gas-gas and solid-gas phase reactions. Among the different component signatures observed in the gas phase, carbonic acid was observed as a possible silylating gas phase nucleophilic component, while in the solid phase the predominant reaction mechanism proceeded by forming SiOSi bonds and Trimethylaminosilane (as gas phase product).

KW - HMDS

KW - Heterogeneous reaction

KW - In situ FTIR

KW - Low-k

KW - Silylation

UR - http://www.scopus.com/inward/record.url?scp=84901006055&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=84901006055&partnerID=8YFLogxK

U2 - 10.1016/j.supflu.2014.01.019

DO - 10.1016/j.supflu.2014.01.019

M3 - Article

AN - SCOPUS:84901006055

SN - 0896-8446

VL - 90

SP - 134

EP - 143

JO - Journal of Supercritical Fluids

JF - Journal of Supercritical Fluids

ER -

In situ FTIR experimental results in the silylation of low-k films with hexamethyldisilazane dissolved in supercritical carbon dioxide

Abstract

Keywords

ASJC Scopus subject areas

Access to Document

Other files and links

Fingerprint

Cite this