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Relationship Between Crosslinking and Ordering for the Fabrication of Soft Templated Mesoporous Carbon Thin Films and Attempts Toward Time Efficient Fabrication of Mesoporous Carbon and Metal Oxides

Zhang, Yuanzhong
http://rave.ohiolink.edu/etdc/view?acc_num=akron1408366319

Abstract Details

2014, Master of Science in Engineering, University of Akron, Polymer Engineering.
The high specific surface area, large pore volume along with various surface and matrix chemical and electrochemical properties have granted ordered mesoporous materials the potential in a wide variety of applications, including adsorption and separation, energy storage and conversion and drug release. The soft template method which utilizes the cooperative self-assembly of amphiphilic block copolymers and various precursors to fabricate ordered mesoporous materials has allowed not only more flexibility and possibility in the control and tuning of morphology of these materials, but also simplified the procedure and lowered costs during manufacture. However, due to the required thermopolymerization step of precursors and subsequent template removal, which usually demand long period of heating, the fabrication of soft-template ordered mesoporous materials often takes hours to days. This can seriously hinder these materials’ potential of scaled-up manufacture in industry. Here, we describe 2 successful attempts in shortening the time of ordered mesoporous materials fabrication by introducing more efficient methods. First, we followed the chemical evolution of thermopolymerization of resol-type phenolic resin (in thin film geometry) which serves as a common carbon precursor to synthesize ordered mesoporous carbon. Both pure resol and Pluronic® F127 (a commercially available surfactant commonly used as templating agent) templated thin films were studied with FTIR quantitatively during thermopolymerization process at four different temperatures (100 °C, 120 °C, 140 °C, 160 °C). The majority of conversion (70%) can be achieved around 256 min, 60 min, 20 min and less than 5 min respectively for the four temperatures. In situ grazing incident small angle X-ray scattering (GISAXS) was performed at 100 °C and 120 °C, which showed that the formation of ordered mesostructure takes place within the first several minutes of thermopolymerization. Combining the information acquired, a step-wise 3 h procedure was developed to replace the traditional 24 h procedure of thermopolymerization without adversely impacting the final ordered mesoporous carbon product. Second, a micelle templated mesoporous cobalt oxide thin film material was synthesized using microwave heating method. The traditional procedure utilizing oven heating requires 2 h to solidify the precursor, remove template and transform the precursor into cobalt oxide, while microwave method allows the whole process to be finished within 2 min. FTIR and GISAXS showed that the chemical composition and mesostructure of pores were basically identical.
Bryan Vogt, Dr (Advisor)
Younjin MIn, Dr (Committee Member)
Kevin Cavicchi, Dr (Committee Member)
Polymers

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Citations

  • Zhang, Y. (2014). Relationship Between Crosslinking and Ordering for the Fabrication of Soft Templated Mesoporous Carbon Thin Films and Attempts Toward Time Efficient Fabrication of Mesoporous Carbon and Metal Oxides [Master's thesis, University of Akron]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=akron1408366319

    APA Style (7th edition)

  • Zhang, Yuanzhong. Relationship Between Crosslinking and Ordering for the Fabrication of Soft Templated Mesoporous Carbon Thin Films and Attempts Toward Time Efficient Fabrication of Mesoporous Carbon and Metal Oxides. 2014. University of Akron, Master's thesis. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=akron1408366319.

    MLA Style (8th edition)

  • Zhang, Yuanzhong. "Relationship Between Crosslinking and Ordering for the Fabrication of Soft Templated Mesoporous Carbon Thin Films and Attempts Toward Time Efficient Fabrication of Mesoporous Carbon and Metal Oxides." Master's thesis, University of Akron, 2014. http://rave.ohiolink.edu/etdc/view?acc_num=akron1408366319

    Chicago Manual of Style (17th edition)

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