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1999 Fiscal Year Final Research Report Summary

Preparation of Super-Hard Nitride Thin Films for Next Generation by High Density Plasma PVD

Research Project

Project/Area Number 09480091
Research Category

Grant-in-Aid for Scientific Research (B)

Allocation TypeSingle-year Grants
Section一般
Research Field プラズマ理工学
Research InstitutionOsaka University

Principal Investigator

MIYAKE Shoji  Osaka University, Joining and Welding Research Institute, Prof., 接合科学研究所, 教授 (40029286)

Co-Investigator(Kenkyū-buntansha) SHOJI Tatsuo  Nagoya University, Graduate School, School of Eng., Assoc.Prof., 大学院・工学研究科, 助教授 (50115581)
SETSUHARA Yuichi  Osask University, Joining and Welding Research Institute, Research Assoc., 接合科学研究所, 助手 (80236108)
MAKINO Yukio  Osask University, Joining and Welding Research Institute, Assoc.Prof., 接合科学研究所, 助教授 (20089890)
Project Period (FY) 1997 – 1999
Keywordshigh density plasma / PVD / super-hard material / thin film / helicon wave / carbon nitride film
Research Abstract

Research on the formation of β-C_3N_4 thin films as one of the most attractive super-hard nitride materials in the next generation has been conducted between 1997 and 1999. The first goal was settled to obtain films with stoichiometric composition for the first by developing a high density helicon-wave excited plasma sputtering source operated at low pressures, in which highly excited radicals and ions could easily be obtained. Results obtained within 3 years project are summarized as follows.
1) Using a simple helical coil antenna of several turns a high density plasma with a density reaching to 10^<13> cm^<-3> was obtained in Ar gas of 0.1 - 1 Pa in an external magnetic field with an RF power input of Several 100 W.Even in N_2 gas environment a plasma density of 10^2 cm^<-3> was also obtained easily.
2) Developing a sputtering machine based on this plasma, preparation of CN_x films were performed and it was found that increasing nitrogen flux brought an increase of N content in the films and succeeded in obtaining stoichiometric film composition by controlling C and N flux appropriately. Films were composed of mixture of sp^2 and sp^3 phases that increased with N content.
3) Micro-hardness of the films was not so high with a value of about 25 GPa in the condition of ion bombardment at a nearly stoichiometric composition. It was considered that softening of films was induced by the existence of graphite phase and impurity atoms such as O and/or H in the films causing polymer-like compound formation.

  • Research Products

    (22 results)

All Other

All Publications (22 results)

  • [Publications] J.Q.Zhang,Y.Setsuhara,S.Miyake and B.Kyoh: "Formation of Carbon Nitride Films by Helicon Wave Plasma Enhanced DC Sputtering"Jpn.J.Appl.Phys.. Vol.36, Pt.1, No.11. 6894-6899 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] Y.Ohtsu,G.Tochitani,H.Fujita,J.Zhang,Y.Setsuhara and S.Miyake: "Measurements of Ion Energy Distribution Functions in a Radical Frequency Plasma Excited with an m=0 Mode Helical Antenna and Thin Film Preparation"Jpn.J.Appl.Phys.. 36. 4620-4624 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] S.Miyake: "Trend in Super-Hard Materials Coating by Plasma and Ion Beam Processes"Proc.of Int.Conf.on Surface Eng.. 243-249 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 三宅正司: "プラズマ・イオンを利用した超硬質被膜の形成"溶射. 141-146 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 三宅正司: "プラズマ・イオンプロセスによる窒化物超硬質薄膜の合成"第2回関西大学先端科学技術シンポジウム講演集. 1-7 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] S.Miyake,Y.Setsuhara,M.Kumagai,K.Ogata,Y.Sakawa and T.Shoji: "Sputter Deposition of Carbon Nitride Films by Reactive High-Density Plasmas w* Excitation of m=0 Mode Helicon Wave"Proc.of 4th Int.Conf.on Reactive Plasmas(ICRP4)/51st Annual Gaseous Electronics Conf.(GEC51). 87-88 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] S.Miyake: "Materials Coating by Ion and Plasma Technology"Proc.of The Japan-China Bilaterial Symposium on Advanced Materials Engineering. 39-45 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 節原 裕一、三宅 正司: "イオン・プラズマプロセスによる硼素、炭素、窒素系超硬質薄膜の合成"応用物理. Vol.67, No.6. 659-663 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] S.Miyake,Y.Setsuhara,K.Shibata,M.Kumagai,Y.Sakawa and T.Shoji: "Formation of Carbon Nitride Films by Reactive High-Density Plasma Sputtering with Excitation of m=0 Mode Helicon Wave"Surf.Coat.Technol.. 116-119. 11-17 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] Y.Takaki,Y.Setsuhara,S.Miyake,M.Kumagai,Y.Sakawa and T.Shoji: "Formation of Superhard Nitride Films by High-Density Helicon-Plasma Sputtering"Proc.17th Symp.on Plasma Processing. 383-386 (2000)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] Y.Setsuhara,Y.Sakawa,T.Shoji,M.Kumagai and S.Miyake: "Synthesis of Carbon Nitride Films by High-Density Helicon-Wave Excited Plasma Sputtering"Surf.& Coat.Technol.. (in press).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 1. J.Q.Zhang, Y.Setsuhara, S.Miyake and B.Kyoh: "Formation of Carbon Nitride Films by Helicon Wave Plasma Enhanced DC Sputtering"Jpn.J.Appl.Phys.. Vol.36, Pt.1, No.11. 6894-6899 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 2. Y.Ohtsu, G.Tochitani, H.Fujita, J.Zhang, Y.Setsuhara and S.Miyake: "Measurements of Ion Energy Distribution Functions in a Radical Frequency Plasma Excited with an m=0 Mode Helical Antenna and Thin Film Preparation"Jpn.J.Appl.Phys.. Vol.36. 4620-4624 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 3. S.Miyake: "Trend in Super-Hard Materials Coating by Plasma and Ion Beam Processes"Proc.of Int.Conf.on Surface Eng.(CSE'97), Nov., Shanghai, China. 243-249 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 4. S.Miyake: "Super-Hard Materials Coating by Plasma and Ion Beam Processes"Yousha. 141-146 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 5. S.Miyake: "Preparation of super-hard nitride thin films with Plasma・Ion Process"Proc.2^<nd> Symp.of Advanced Science and Technol.of Kansai University.

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 6. S.Miyake, Y.Setsuhara, M.Kumagai, K.Ogata, Y.Sakawa and T.Shoji: "Sputter Deposition of Carbon Nitride Films by Reactive High-Density Plasmas with Excitation of m=0 Mode Helicon Wave"Proc.of 4th tnt.Conf.on Reactive Plasmas (ICRP4)/51st Annual Gaseous Electronics Conf.(GEC51) Maui, USA. 87-88 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 7. S.Miyake: "Materials Coating by Ion and Plasma Technology"Proc.of The Japan-China Bilaterial Symposium on Advanced Materials Engineering, Tokyo, Japan. 39-45 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 8.Y.Setsuhara and S.Miyake: "Ion-beam and plasma processing techniques for thin-film synthesis of superhard materials in boron-carbon-nitrogen system"Ouyou Butsuri. Vol.67, No.6. 659-663 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 9. S.Miyake, Y.Setsuhara, K.Shibata, M.Kumagai, Y.Sakawa and T.Shoji: "Formation of Carbon Nitride Films by Reactive High-Density Plasma Sputtering with Excitation of m=O Mode Helicon Wave"Surf.Coat.Technol.. 116-119. 11-17 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 10. Y.Takaki, Y.Setsuhara, S.Miyake, M.Kumagai, Y.Sakawa and T.Shoji: "Formation of Superhard Nitride Films by High-Density Helicon-Plasma Sputtering"Proc.17th Symp.on Plasma Processing, Nagasaki, Japan. 383-386 (2000)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] 11.Y.Setsuhara, Y.Sakawa, T.Shoji, M.Kumagai and S.Miyake: "Synthesis of Carbon Nitride Films by High-Density Helicon-Wave Excited Plasma Sputtering"Surf.& Coat.Technol.. (in press).

    • 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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