Supercritical CO2 extraction of porogen phase: An alternative route to nanoporous dielectrics

J. A. Lubguban; S. Gangopadhyay; B. Lahlouh; T. Rajagopalan; N. Biswas; J. Sun; D. H. Huang; S. L. Simon; A. Mallikarjunan; H. C. Kim; J. Hedstrom; W. Volksen; R. D. Miller; M. F. Toney

doi:10.1557/JMR.2004.0413

Supercritical CO₂ extraction of porogen phase: An alternative route to nanoporous dielectrics

J. A. Lubguban, S. Gangopadhyay, B. Lahlouh, T. Rajagopalan, N. Biswas, J. Sun, D. H. Huang, S. L. Simon, A. Mallikarjunan, H. C. Kim, J. Hedstrom, W. Volksen, R. D. Miller, M. F. Toney

Chemical Engineering

Research output: Contribution to journal › Article

14 Scopus citations

Abstract

We present a supercritical CO₂ (SCCO₂) process for the preparation of nanoporous organosilicate thin films for ultralow dielectric constant materials. The porous structure was generated by SCCO₂ 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 approximately 450 °C) and by a SCCO ₂ process for 25 and 55 wt% porogen loadings were evaluated. It is found that the SCCO₂ 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.

Original language	English
Pages (from-to)	3224-3233
Number of pages	10
Journal	Journal of Materials Research
Volume	19
Issue number	11
DOIs	https://doi.org/10.1557/JMR.2004.0413
State	Published - Nov 2004

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Lubguban, J. A., Gangopadhyay, S., Lahlouh, B., Rajagopalan, T., Biswas, N., Sun, J., Huang, D. H., Simon, S. L., Mallikarjunan, A., Kim, H. C., Hedstrom, J., Volksen, W., Miller, R. D., & Toney, M. F. (2004). Supercritical CO₂ extraction of porogen phase: An alternative route to nanoporous dielectrics. Journal of Materials Research, 19(11), 3224-3233. https://doi.org/10.1557/JMR.2004.0413

Lubguban, J. A. ; Gangopadhyay, S. ; Lahlouh, B. ; Rajagopalan, T. ; Biswas, N. ; Sun, J. ; Huang, D. H. ; Simon, S. L. ; Mallikarjunan, A. ; Kim, H. C. ; Hedstrom, J. ; Volksen, W. ; Miller, R. D. ; Toney, M. F. / Supercritical CO₂ extraction of porogen phase : An alternative route to nanoporous dielectrics. In: Journal of Materials Research. 2004 ; Vol. 19, No. 11. pp. 3224-3233.

@article{3e302a926e3246ac8f51eeea86bc2466,

title = "Supercritical CO2 extraction of porogen phase: An alternative route to nanoporous dielectrics",

abstract = "We present a supercritical CO2 (SCCO2) process for the preparation of nanoporous organosilicate thin films for ultralow dielectric constant materials. The porous structure was generated by SCCO2 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 approximately 450 °C) and by a SCCO 2 process for 25 and 55 wt% porogen loadings were evaluated. It is found that the SCCO2 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.",

author = "Lubguban, {J. A.} and S. Gangopadhyay and B. Lahlouh and T. Rajagopalan and N. Biswas and J. Sun and Huang, {D. H.} and Simon, {S. L.} and A. Mallikarjunan and Kim, {H. C.} and J. Hedstrom and W. Volksen and Miller, {R. D.} and Toney, {M. F.}",

year = "2004",

month = nov,

doi = "10.1557/JMR.2004.0413",

language = "English",

volume = "19",

pages = "3224--3233",

journal = "Journal of Materials Research",

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Lubguban, JA, Gangopadhyay, S, Lahlouh, B, Rajagopalan, T, Biswas, N, Sun, J, Huang, DH, Simon, SL, Mallikarjunan, A, Kim, HC, Hedstrom, J, Volksen, W, Miller, RD & Toney, MF 2004, 'Supercritical CO₂ extraction of porogen phase: An alternative route to nanoporous dielectrics', Journal of Materials Research, vol. 19, no. 11, pp. 3224-3233. https://doi.org/10.1557/JMR.2004.0413

Supercritical CO₂ extraction of porogen phase : An alternative route to nanoporous dielectrics. / Lubguban, J. A.; Gangopadhyay, S.; Lahlouh, B.; Rajagopalan, T.; Biswas, N.; Sun, J.; Huang, D. H.; Simon, S. L.; Mallikarjunan, A.; Kim, H. C.; Hedstrom, J.; Volksen, W.; Miller, R. D.; Toney, M. F.

In: Journal of Materials Research, Vol. 19, No. 11, 11.2004, p. 3224-3233.

Research output: Contribution to journal › Article

TY - JOUR

T1 - Supercritical CO2 extraction of porogen phase

T2 - An alternative route to nanoporous dielectrics

AU - Lubguban, J. A.

AU - Gangopadhyay, S.

AU - Lahlouh, B.

AU - Rajagopalan, T.

AU - Biswas, N.

AU - Sun, J.

AU - Huang, D. H.

AU - Simon, S. L.

AU - Mallikarjunan, A.

AU - Kim, H. C.

AU - Hedstrom, J.

AU - Volksen, W.

AU - Miller, R. D.

AU - Toney, M. F.

PY - 2004/11

Y1 - 2004/11

N2 - We present a supercritical CO2 (SCCO2) process for the preparation of nanoporous organosilicate thin films for ultralow dielectric constant materials. The porous structure was generated by SCCO2 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 approximately 450 °C) and by a SCCO 2 process for 25 and 55 wt% porogen loadings were evaluated. It is found that the SCCO2 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.

AB - We present a supercritical CO2 (SCCO2) process for the preparation of nanoporous organosilicate thin films for ultralow dielectric constant materials. The porous structure was generated by SCCO2 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 approximately 450 °C) and by a SCCO 2 process for 25 and 55 wt% porogen loadings were evaluated. It is found that the SCCO2 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.

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DO - 10.1557/JMR.2004.0413

M3 - Article

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SP - 3224

EP - 3233

JO - Journal of Materials Research

JF - Journal of Materials Research

SN - 0884-2914

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