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Development of Continuous Apparatus using Microreactor for Production of Nanoparticles in Supercritical Water

Research Project

Project/Area Number 15360416
Research Category

Grant-in-Aid for Scientific Research (B)

Allocation TypeSingle-year Grants
Section一般
Research Field Reaction engineering/Process system
Research InstitutionTohoku University

Principal Investigator

ARAI Kunio  Tohoku University, Graduate School of Environmental Studies, Professor, 大学院・環境科学研究科, 教授 (10005457)

Co-Investigator(Kenkyū-buntansha) NONAKA Toshiyuki  Tohoku University, Graduate School of Engineering, Lecturer, 大学院・工学研究科, 講師 (50237856)
WATANABE Masaru  Tohoku University, Graduate School of Engineering, Research Associate, 大学院・工学研究科, 助手 (40312607)
RUAN Jiongming  Tohoku University, Graduate School of Environmental Studies, Research Associate, 大学院・環境科学研究科, 助手 (80400456)
SUE Kiwamu  Nihon University, College of Industrial Technology, Research Associate, 生産工学部, 助手 (60333845)
Project Period (FY) 2003 – 2005
Project Status Completed (Fiscal Year 2005)
Budget Amount *help
¥14,500,000 (Direct Cost: ¥14,500,000)
Fiscal Year 2005: ¥2,900,000 (Direct Cost: ¥2,900,000)
Fiscal Year 2004: ¥5,200,000 (Direct Cost: ¥5,200,000)
Fiscal Year 2003: ¥6,400,000 (Direct Cost: ¥6,400,000)
KeywordsSupercritical water / Hydrothermal synthesis / Metal Oxides / Nanoparticles / Microreactor / Solubility / Flow-through apparatus / ナノサイズ微粒子
Research Abstract

Over the past ten years, a flow-through hydrothermal synthesis method with microreactor for continuous production of metal oxides have been established for forming micro or nano size metal oxide fine particles in subcritical and supercritical water. This method promises to heat starting solutions rapidly to the given temperature and to control reaction time exactly. When water in its near-critical or supercritical state is used, the hydrothermal reaction rate and metal oxide solubility can be controlled by changing temperature and pressure since the reaction solvent properties are strongly dependent on the conditions in these regions. Therefore, this method has great potential for producing nano-size metal oxide fine particles. There are many reports for producing nanoparticle by this method. However, there is no report that the controllability of the particle size is discussed on the basis of metal oxide solubility and supersaturation. In this work, to develop this method as a generic … More technology for producing nanocrystals we focus on the quantitative clarification of experimental conditions for producing single nano-sized metal oxide particles by this method and also its crystallinity on the basis of estimated metal oxide solubilities.
We carried out hydrothermal synthesis of metal oxides (AlO(OH), CuO, Fe2O3, NiO, ZrO2) nanoparticles from metal nitrates aqueous solution at 673 K and 30 MPa by this method. Particle size, phase and crystallinity of the obtained particles were characterized by TEM, XRD and TG, respectively. Effect of the difference of the metals in starting materials on particle size, conversion and crystallinity was analyzed on the basis of supersaturation, which was evaluated by estimated metal oxide solubilities. The result suggests that supersaturation should be set to higher than 104 in this method to obtain particles in single nanoscale. Further, crystallinity of the obtained particles was evaluated as weight loss through TG analysis. In addition that longer reaction time increased the crystallinity, it was found that smaller supersaturation also increased the crystallinity. This result can be explained that large supersaturation lead to include water molecule on the way to formation of particles. Less

Report

(4 results)
  • 2005 Annual Research Report   Final Research Report Summary
  • 2004 Annual Research Report
  • 2003 Annual Research Report
  • Research Products

    (15 results)

All 2006 2005 2004 Other

All Journal Article (11 results) Publications (4 results)

  • [Journal Article] One-Pot Synthesis of Nickel Particles in Supercritical Water2006

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Industrial and Engineering Chemistry Research 45

      Pages: 623-626

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2005 Annual Research Report 2005 Final Research Report Summary
  • [Journal Article] Continuous Production of Quinacridone Nanocrystals and Control of Crystal Form by High-Temperature Water Crystallization Method2006

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Japanese Journal of Applied Physics 45・1B(in press)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2005 Annual Research Report 2005 Final Research Report Summary
  • [Journal Article] Synthesis of Ni-Cu Particles by Hydrogen Reduction in Hot-compressed Water2005

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Chemistry Letters 35・1

      Pages: 50-51

    • NAID

      10016907719

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2005 Annual Research Report 2005 Final Research Report Summary
  • [Journal Article] 流通式超臨界水熱合成法によるナノ粒子設計2005

    • Author(s)
      陶 究
    • Journal Title

      Journal of the Society of Inorganic Materials, Japan 12

      Pages: 429-434

    • NAID

      10016379791

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2005 Annual Research Report 2005 Final Research Report Summary
  • [Journal Article] Synthesis of Ni-Cu Particles by Hydrogen Reduction in Hot-compressed Water2005

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Chemistry Letters 35, 1

      Pages: 50-51

    • NAID

      10016907719

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      2005 Final Research Report Summary
  • [Journal Article] Design of Nanoparticles in Supercritical Water using Flow-through Hydrothermal Synthesis Method2005

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Journal of the Society of Inorganic Materials, Japan 12

      Pages: 429-434

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      2005 Final Research Report Summary
  • [Journal Article] Rapid hydrothermal synthesis of ZnO nanorods without organics2004

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Materials Letters 58・26

      Pages: 3350-3352

    • Related Report
      2004 Annual Research Report
  • [Journal Article] Hydrothermal synthesis of ZnO nanocrystals using microreactor2004

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Materials Letters 58・25

      Pages: 3229-3231

    • Related Report
      2004 Annual Research Report
  • [Journal Article] Effect of cations and anions on properties of zinc oxide particles synthesized in supercritical water2004

    • Author(s)
      Kiwamu Sue
    • Journal Title

      The Journal of Supercritical Fluids 30・3

      Pages: 325-331

    • Related Report
      2004 Annual Research Report
  • [Journal Article] Hydrothermal synthesis of zinc oxide crystals in homogeneous mixture of carbon dioxide, hydrogen, and water2004

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Chemistry Letters 33・6

      Pages: 708-709

    • NAID

      10013105784

    • Related Report
      2004 Annual Research Report
  • [Journal Article] Continuous production of nickel fine particles by hydrogen reduction in near-critical water2004

    • Author(s)
      Kiwamu Sue
    • Journal Title

      Industrial and Engineering Chemistry Research 43・9

      Pages: 2073-2078

    • Related Report
      2004 Annual Research Report
  • [Publications] Kiwamu Sue: "Continuous production of nickel fine particles by hydrogen reduction in near-critical water"Industrial and Engineering Chemistry Research. (accepted). (2004)

    • Related Report
      2003 Annual Research Report
  • [Publications] Kiwamu Sue: "Effect of cations and anions on properties of zinc oxide particles synthesized in supercritical water"The Journal of Supercritical Fluids. (in press). (2004)

    • Related Report
      2003 Annual Research Report
  • [Publications] Kiwamu Sue: "Continuous synthesis of zinc oxide nanoparticles in supercritical water"Green Chemistry. 5(05). 659-662 (2003)

    • Related Report
      2003 Annual Research Report
  • [Publications] Yukiya Hakuta: "Continuous production of phosphor YAG : Tb nanoparticles by hydrothermal synthesis in supercritical water"Materials Research Bulletin. 38. 1257-1265 (2003)

    • Related Report
      2003 Annual Research Report

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Published: 2003-04-01   Modified: 2016-04-21  

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