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2000 Fiscal Year Final Research Report Summary

Preparation of Amorphous Solid Electrolytes by Mechanical Milling

Research Project

Project/Area Number 11450336
Research Category

Grant-in-Aid for Scientific Research (B).

Allocation TypeSingle-year Grants
Section一般
Research Field 無機工業化学
Research InstitutionOsaka Prefecture University

Principal Investigator

TATSUMISAGO Masahiro  Osaka Prefecture Univ., Prof., 工学研究科, 教授 (50137238)

Co-Investigator(Kenkyū-buntansha) MATSUDA Atsunori  Osaka Prefecture Univ., Lecturer., 大学院・工学研究科, 講師 (70295723)
TADANAGA Kiyoharu  Osaka Prefecture Univ., Assoc.Prof., 大学院・工学研究科, 助教授 (90244657)
MINAMI Tsutomu  Osaka Prefecture Univ., Prof., 大学院・工学研究科, 教授 (80081313)
Project Period (FY) 1999 – 2000
KeywordsMechanical milling / Amorphous / Ion conduction / Oxysulfide / Ball milling / Conductivity / Solid electrolyte / Solid state battery
Research Abstract

1.Amorphous materials with various compositions in the oxysulfide system Li_2S-SiS_2-LixMOy (LixMOy=Li_4SiO_4, Li_3PO_4) were obtained by mechanical milling (MM) of crystalline starting materials in a dry N_2 atmosphere at room temperature. The pelletized samples exhibited high conductivities in the order of 10^<-4> Scm^<-1> at 25℃. It was found that the transport number of lithium ions of the amorphous materials was almost unity and the potential window as solid electrolytes was wider than 10V.
2.Several spectroscopic measurements like MAS NMR and XPS revealed that the local structure of the amorphous oxysulfide powders prepared by MM was very close to thata of the corresponding melt quenched glass. Furthermore, the formation of continuous amorphous phase with the inrease of milling tive incresed conductivity grastically from 10^<-10> to 10^<-4> Scm^<-1> at room temperature.
3.The amorphous Li_2S-P_2S_5 sample prepared by MM exhibited high conductivity of 9x10^<-5> S cm^<-1> at room temperature. After the sample was heated up to the crystallization temperature, the conductivity decreased with a smaller slope in the cooling process. The conductivity of the heated sample was 6x10^<-4> S cm^<-1> at room temperature. It was revealed that the conductivity improvement with forming the. 80Li_2S・20P_2S_5 glass-ceramics was brought about by the softening of glassy powders and the formation of highly conductive Li_7PS_6 crystal.
4.Electrochemical cells were constructed using amorphous matterials in the system Li_2S-SiS_2-Li_4SiO_4 obtained by MM as an electrolyte, LiCoO_2 as a positive electrode and indium as a negative electrode. The charge-discharge capacity decreased gradually from 90 to 70 mAhcm^<-2> till about the 10th cycle and became stable after the 10th cycle.

  • Research Products

    (32 results)

All Other

All Publications (32 results)

  • [Publications] R.Sakamoto: "Preparation of Fast Lithium Ion Conducting Glasses in the System Li_2S-SiS_2-Li_3N"J.Phys.Chem.B.. 103・[20]. 4029-4031 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] H.Morimoto: "Mechanochemical Synthesis of New Amorphous Materials of 60Li_2S・40SiS_2 with High Lithium Ion Conductivity"J.Am.Ceram.Soc.. 82・[5]. 1352-1354 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] A.Hayashi: "Structural Change Accompanying Crystallization in the Lithium Ion Conductive Li_2S-SiS_2-Li_3PO_4 Oxysulfide Glasses"J.Ceram.Soc.Jpn.. 107・[6]. 510-516 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] A.Hayashi: "High-Resolution Solid-State NMR Studies of Ionically Conductive Li_2S-SiS_2-Li_2O-P_2O_5 Oxysulfide Glasses"Phys.Chem.Glasses. 40[3]. 140-145 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 南努: "超イオン伝導ガラス(総説)"電池技術. 11. 131-138 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] A.Hayashi: "Electrochemical Properties for the Lithium Ion Conductive (100-x)(0.6Li_2S・0.4SiS_2)・xLi_4SiO_4 Oxysulfide Glasses"J.Electrochem.Soc.. 146・[9]. 3472-3475 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] H.Morimoto: "Mechanical Synthesis and Anode Properties of SnO-Based Amorphous Materials"J.Electrochem.Soc.. 146・[11]. 3970-3973 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] A.Hayashi: "Crystallization of Li_2S-SiS_2 Based Lithium Ion Conducting Glasses"Phys.Chem.Glasses. 40・[6]. 333-338 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] H.Morimoto: "Mechanochemical Synthesis of the High Lithium Ion Conductive Amorphous Materials in the Systems Li_2S-SiS_2 and Li_2S-SiS_2-Li_4SiO_4"J.Ceram.Soc.Jpn.. 108・[2]. 128-131 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 林晃敏: "硫化物系リチウムイオン伝導ガラスの作製とキャラクタリゼーション(総説)"金属. 70・[7]. 550-558 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.Tatsumisago: "Preparation and Structure of Amorphous Solid Electrolytes Based on Lithium Sulfide"J.Non-Cryst.Solids. 274・[1-3]. 30-38 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] A.Hayashi: "Crystallization Process of Lithium Oxysulfide Glasses"J.Non-Cryst.Solids. 276・[1-3]. 27-34 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] A.Hayashi: "Development of Lithium Ion Conducting Oxysulfide Glasses"Proc.7th Asian Conf.on Solid State Ionics. 177-186 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] H.Yamashita: "Formation Process of 60Li_2S・40SiS_2 Amorphous Materials with High Lithium Ion Conductivity Prepared by Mechanical Milling"J.Ceram.Soc.Jpn.. 108・[11]. 973-978 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.Tatsumisago: "Preparation of Amorphous Solid Electrolytes in the System Li_2S-SiS_2-Li_4SiO_4 by Mechanical Milling"Solid State Ionics. 136-137. 483-488 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Minami: "Preparation and Characterization of Lithium Ion-Conducting Oxysulfide Glasses"Solid State Ionics. 136-137. 1015-1023 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] R.Sakamoto: "Preparation of Fast Lithium Ion Conducting Glasses in the System Li_2S-SiS_2-Li_3N"J.Phys.Chem.B.. 103 [20]. 4029-4031 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] H.Morimoto: "Mechanochemical Synthesis of New Amorphous Materials of 60Li_2S-40SiS_2 with High Lithium Ion Conductivity"J.Am.Ceram.Soc.. 82 [5]. 1352-1354 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Hayashi: "Structural Change Accompanying Crystallization in the Lithium Ion Conductive Li_2S-SiS_2-Li_3PO_4 Oxysulfide Glasses"J.Ceram.Soc.Jpn.. 107 [6]. 510-516 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Hayashi: "High-Resolution Solid-State NMR Studies of Ionically Conductive Li_2S-SiS_2-Li_2-P_2O_5 Oxysulfide Glasses"Phys.Chem.Glasses.. 40 [3]. 140-145 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Minami: "Superionic Conducting Glasses"Denchi-Gijutsu. 11. 131-138 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Hayashi: "Electrochemical Properties for the Lithium Ion Conductive (100-x)(0.6Li_2S・0.4SiS_2)・xLi_4SiO_4 Oxysulfide Glasses"J.Electrochem.Soc.. 146 [9]. 3472-3475 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] H.Morimoto: "Mechanical Synthesis and Anode Properties of SnO-Based Amorphous Materials"J.Electrochem.Soc.. 146 [11]. 3970-3973 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Hayashi: "Crystallization of Li_2S-SiS_2 Based Lithium Ion Conducting Glasses"Phys.Chem.Glasses. 40 [6]. 333-338 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] H.Morimoto: "Mechanochemical Synthesis of the High Lithium Ion Conductive Amorphous Materials in the Systems Li_2S-SiS_2 and Li_2S-SiS_2-Li_4SiO_4"J.Ceram.Soc.Jpn.. 108 [2]. 128-131 (2000)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Hayashi: "Preparation and Characterization of Lithium-Ion-Conducting Sulfide Glasses"Kinzoku. 70 [7]. 550-558 (2000)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.Tatsumisago: "Preparation and Structure of Amorphous Solid Electrolytes Based on Lithium Sulfide"J.Non-Cryst.Solids. 274 [1-3]. 30-38 (2000)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Hayashi: "Crystallization Process of Lithium Oxysulfide Glasses"J.Non-Cryst.Solids. 276 [1-3]. 27-34 (2000)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Hayashi: "Development of Lithium Ion Conducting Oxysulfide Glasses"Proc.7th Asian Conf.on Solid State Ionics. 177-186 (2000)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] H.Yamashita: "Formation Process of 60Li_2S-40SiS_2 Amorphous Materials with High Lithium Ion Conductivity Prepared by Mechanical Milling"J.Ceram.Soc.Jpn.. 108 [11]. 973-978 (2000)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.Tatsumisago: "Preparation of Amorphous Solid Electrolytes in the System Li_2S-SiS_2-Li_4SiO_4 by Mechanical Milling"Solid State Ionics. 136-137. 483-488 (2000)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Minami: "Preparation and Characterization of Lithium Ion-Conducting Oxysulfide Glasses"Solid State Ionics. 136-137. 1015-1023 (2000)

    • Description
      「研究成果報告書概要(欧文)」より

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Published: 2002-03-26  

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