Journal of Sol-Gel Science and Technology

, Volume 67, Issue 2, pp 406–413 | Cite as

Gelation behavior and phase separation of macroporous methylsilsesquioxane monoliths prepared by in situ two-step processing

  • Xingzhong Guo
  • Wenyan Li
  • Hui Yang
  • Kazuyoshi Kanamori
  • Yang Zhu
  • Kazuki Nakanishi
Original Paper


An in situ two-step processing using an initial acid catalysis step accompanied by an epoxide-mediated condensation step in the presence of ammonium chloride (NH4Cl) is reported, and macroporous cocontinuous methylsilsesquioxane (MSQ) monoliths have been successfully prepared by this processing. We explain the hydrolysis, gelation behavior and phase separation of MTMS(methyltrimethoxysilane)-MeOH(methanol)-HCl-PO(propylene oxide) system and the in situ effect of NH4Cl, and examine the macroporous morphology and pore structures of MSQ monoliths obtained under different conditions. Macroporous MSQ monolith under optimized conditions possesses a narrow macropore size distribution between 3 to 10 μm, surface area as high as 366 m2·g−1 and minimal shrinkage of only 1 %.


Methylsilsesquioxane Monolith Sol–gel process Phase separation Ammonium chloride 


  1. 1.
    Nakanishi K (1997) J Porous Mater 4:67CrossRefGoogle Scholar
  2. 2.
    Dong H, Brennan JD (2006) Chem Mater 18:541CrossRefGoogle Scholar
  3. 3.
    Dong H, Brook MA, Brennan JD (2005) Chem Mater 17:2807CrossRefGoogle Scholar
  4. 4.
    Dong H, Brennan JD (2006) Chem Mater 18:4176CrossRefGoogle Scholar
  5. 5.
    Dong H, Reidy RF, Brennan JD (2005) Chem Mater 17:6012CrossRefGoogle Scholar
  6. 6.
    Kanamori K, Yonezawa H, Nakanishi K, Hirao K, Jinnai H (2004) J Sep Sci 27:874CrossRefGoogle Scholar
  7. 7.
    Kanamori K, Nakanishi K, Hanada T (2006) J Sep Sci 29:2463CrossRefGoogle Scholar
  8. 8.
    Kanamori K, Kodera Y, Hayase G, Nakanishi K, Hanada T (2011) J Colloid Interface Sci 357:336CrossRefGoogle Scholar
  9. 9.
    Kanamori K, Aizawa M, Nakanishi K, Hanada T (2007) Adv Mater 19:1589CrossRefGoogle Scholar
  10. 10.
    Popp M, Sulyok M, Rosenberg E (2007) J Sep Sci 30:2888CrossRefGoogle Scholar
  11. 11.
    Shiu JY, Kuo CW, Chen P, Mou CY (2004) Chem Mater 16:561CrossRefGoogle Scholar
  12. 12.
    Padovani AM, Rhodes L, Riester L, Lohman G (2001) Electrochem Solid-State Lett 4:F25CrossRefGoogle Scholar
  13. 13.
    Yin G, Yuan Q, Ning Z (2012) J Electroceram 28:70Google Scholar
  14. 14.
    Rosezin R, Meier M, Trellenkamp S, Kügeler C, Waser R (2010) Microelectron Eng 87:1531CrossRefGoogle Scholar
  15. 15.
    Crouzet L, Leclercq D, Mutin PH, Vioux A (2003) J Sol-Gel Sci Technol 26:335CrossRefGoogle Scholar
  16. 16.
    Gash AE, Tillotson TM, Satcher JH, Poco JF, Hrubesh LW (2001) Chem Mater 13:999CrossRefGoogle Scholar
  17. 17.
    Gash AE, Satcher JH, Simpson RL (2003) Chem Mater 15:3268CrossRefGoogle Scholar
  18. 18.
    Tokudome Y, Fujita K, Nakanish K, Miura K, Hirao K (2007) Chem Mater 19:3393CrossRefGoogle Scholar
  19. 19.
    Kido Y, Nakanishi K (2012) Chem Mater 24:2071CrossRefGoogle Scholar
  20. 20.
    Kaji H, Nakanishi K, Soga N (1993) J Sol-Gel Sci Technol 1:35CrossRefGoogle Scholar
  21. 21.
    Nakanishi K (2006) Bull Chem Soc Jpn 79:673CrossRefGoogle Scholar
  22. 22.
    Nakanishi K, Tanaka N (2007) Acc Chem Res 40:863CrossRefGoogle Scholar
  23. 23.
    Nakanishi K, Komura H, Ryoji T, Soga H (1994) Bull Chem Soc Jpn 67:1327CrossRefGoogle Scholar
  24. 24.
    Nakanishi K, Soga H (1997) Bull Chem Soc Jpn 70:587CrossRefGoogle Scholar
  25. 25.
    Amatani T, Nakanishi K, Hirao K, Kodaira T (2005) Chem Mater 17:2114CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2013

Authors and Affiliations

  • Xingzhong Guo
    • 1
  • Wenyan Li
    • 1
  • Hui Yang
    • 1
  • Kazuyoshi Kanamori
    • 2
  • Yang Zhu
    • 2
  • Kazuki Nakanishi
    • 2
  1. 1.Department of Materials Science and EngineeringZhejiang UniversityHangzhouChina
  2. 2.Department of Chemistry, Graduate School of ScienceKyoto UniversityKyotoJapan

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