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Synthesis of ultrafine carbon cryogel microspheres using a homogenizer

Authors

  • Apinan Soottitantawat,

    1. National Nanotechnology Center (NANOTEC), National Science and Technonology Development Agency (NSTDA), Klong Luang, Patumthani 12120, Thailand
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  • Takuji Yamamoto,

    Corresponding author
    1. Research Institute for Innovation in Sustainable Chemistry, National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba 305-8565, Japan
    • Research Institute for Innovation in Sustainable Chemistry, National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba 305-8565, Japan
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  • Akira Endo,

    1. Research Institute for Innovation in Sustainable Chemistry, National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba 305-8565, Japan
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  • Takao Ohmori,

    1. Research Institute for Innovation in Sustainable Chemistry, National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba 305-8565, Japan
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  • Masaru Nakaiwa

    1. Research Institute for Innovation in Sustainable Chemistry, National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba 305-8565, Japan
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Abstract

Ultrafine carbon cryogel (UCC) microspheres of diameter <5 μm with desirable mesopores were successfully synthesized using a homogenizer during the inverse emulsion polymerization of a resorcinol–formaldehyde (RF) aqueous solution in an organic solvent as a continuous phase (CP) containing nonionic surfactant, SPAN80 as an emulsifier, followed by solvent exchange, freeze-drying, and pyrolysis in an Ar atmosphere. The curing time of RF solution before emulsification is a significant factor in controlling the size of the microspheres without changing their porosity. Both the mesoporosity and the size of the microspheres decreased on increasing SPAN80 and RF solution concentration in an inverse emulsion, which showed the possibility of controlling the mesoporosity and the size of the UCC microspheres. Furthermore, hexane could also be used as the continuous phase in the emulsion polymerization. The mean diameter of the UCC microspheres increased and their mesopore volume decreased with increasing pyrolysis temperature. © 2006 American Institute of Chemical Engineers AIChE J, 2007

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