Supercritical CO2 Extraction of Porogen Phase: An Alternative Route to Nanoporous Dielectrics
Abstract
We present a supercritical CO{sub 2} (SCCO{sub 2}) process for the preparation of nanoporous organosilicate thin films for ultra low dielectric constant materials. The porous structure was generated by SCCO{sub 2} extraction of a sacrificial poly(propylene glycol) (PPG) from a nanohybrid film, where the nanoscopic domains of PPG porogen are entrapped within the crosslinked poly(methylsilsesquioxane) (PMSSQ) matrix. As a comparison, porous structures generated by both the usual thermal decomposition (at ca. 450 C) and by a SCCO{sub 2} process for 25 wt% and 55 wt% porogen loadings were evaluated. It is found that the SCCO{sub 2} process is effective in removing the porogen phase at relatively low temperatures (< 200 C) through diffusion of the supercritical fluid into the phase-separated nanohybrids and selective extraction of the porogen phase. Pore morphologies generated from the two methods are compared from representative three-dimensional (3D) images built from small angle x-ray scattering (SAXS) data.
- Authors:
- Publication Date:
- Research Org.:
- Stanford Linear Accelerator Center (SLAC), Menlo Park, CA
- Sponsoring Org.:
- USDOE Office of Science (SC)
- OSTI Identifier:
- 839790
- Report Number(s):
- SLAC-PUB-10846
TRN: US200516%%462
- DOE Contract Number:
- AC02-76SF00515
- Resource Type:
- Technical Report
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE; DIELECTRIC MATERIALS; DIFFUSION; PERMITTIVITY; PYROLYSIS; SCATTERING; THIN FILMS
Citation Formats
Lubguban, J. Supercritical CO2 Extraction of Porogen Phase: An Alternative Route to Nanoporous Dielectrics. United States: N. p., 2004.
Web. doi:10.2172/839790.
Lubguban, J. Supercritical CO2 Extraction of Porogen Phase: An Alternative Route to Nanoporous Dielectrics. United States. doi:10.2172/839790.
Lubguban, J. Thu .
"Supercritical CO2 Extraction of Porogen Phase: An Alternative Route to Nanoporous Dielectrics". United States.
doi:10.2172/839790. https://www.osti.gov/servlets/purl/839790.
@article{osti_839790,
title = {Supercritical CO2 Extraction of Porogen Phase: An Alternative Route to Nanoporous Dielectrics},
author = {Lubguban, J.},
abstractNote = {We present a supercritical CO{sub 2} (SCCO{sub 2}) process for the preparation of nanoporous organosilicate thin films for ultra low dielectric constant materials. The porous structure was generated by SCCO{sub 2} extraction of a sacrificial poly(propylene glycol) (PPG) from a nanohybrid film, where the nanoscopic domains of PPG porogen are entrapped within the crosslinked poly(methylsilsesquioxane) (PMSSQ) matrix. As a comparison, porous structures generated by both the usual thermal decomposition (at ca. 450 C) and by a SCCO{sub 2} process for 25 wt% and 55 wt% porogen loadings were evaluated. It is found that the SCCO{sub 2} process is effective in removing the porogen phase at relatively low temperatures (< 200 C) through diffusion of the supercritical fluid into the phase-separated nanohybrids and selective extraction of the porogen phase. Pore morphologies generated from the two methods are compared from representative three-dimensional (3D) images built from small angle x-ray scattering (SAXS) data.},
doi = {10.2172/839790},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Thu Nov 04 00:00:00 EST 2004},
month = {Thu Nov 04 00:00:00 EST 2004}
}
-
We are examining the potential of water in CO2 microemulsions as a new medium for the extraction of metal ions from contaminated surfaces with the ultimate goal of extracting actinides from heterogeneous waste to aid in decontamination and waste reduction.
-
Micelle Formation and Surface Interactions in Supercritical CO2. Fundamental Studies for the Extraction of Actinides from Contaminated Surfaces.
The goals of this research program included: (1) Study solubility of extractants and formation of micelles--(a) Do surfactants form micelles in scCO{sub 2} and what is the mechanism of their formation? (b) Can the pressure/density of scCO{sub 2} be used to alter surfactant solubility or micelle structure? (c) Can surfactant micelles be used to transport water based microphases? (2) Examine the solubilization of metals--(a) What influence does metal binding have on the surfactant solubility or micelle structure? (b) What is the selectivity of metal binding in promising systems? (c) Are all solubilized metals bound to surfactant ligands or is anmore » -
SIMULTANEOUS MECHANICAL AND HEAT ACTIVATION: A NEW ROUTE TO ENHANCE SERPENTINE CARBONATION REACTIVITY AND LOWER CO2 MINERAL SEQUESTRATION PROCESS COST
Coal can support a large fraction of global energy demands for centuries to come, if the environmental problems associated with CO{sub 2} emissions can be overcome. Unlike other candidate technologies, which propose long-term storage (e.g., ocean and geological sequestration), mineral sequestration permanently disposes of CO{sub 2} as geologically stable mineral carbonates. Only benign, naturally occurring materials are formed, eliminating long-term storage and liability issues. Serpentine carbonation is a leading mineral sequestration process candidate, which offers large scale, permanent sequestration. Deposits exceed those needed to carbonate all the CO{sub 2} that could be generated from global coal reserves, and mining andmore » -
Coal liquefaction process streams characterization and evaluation. Characterization of coal-derived materials by field desorption mass spectrometry, two-dimensional nuclear magnetic resonance, supercritical fluid extraction, and supercritical fluid chromatography/mass spectrometry
Under contract from the DOE , and in association with CONSOL Inc., Battelle, Pacific Northwest Laboratory (PNL) evaluated four principal and several complementary techniques for the analysis of non-distillable direct coal liquefaction materials in support of process development. Field desorption mass spectrometry (FDMS) and nuclear magnetic resonance (NMR) spectroscopic methods were examined for potential usefulness as techniques to elucidate the chemical structure of residual (nondistillable) direct coal liquefaction derived materials. Supercritical fluid extraction (SFE) and supercritical fluid chromatography/mass spectrometry (SFC/MS) were evaluated for effectiveness in compound-class separation and identification of residual materials. Liquid chromatography (including microcolumn) separation techniques, gas chromatography/massmore »