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Preparation of Nanocrystalline ZrO2 Film by Using a Zirconium Naphthenate and Evaluation of Calcium Phosphate Forming Ability

지르코늄 나프테네이트를 이용한 나노결정질 ZrO2 박막의 제조와 칼슘 포스페이트 형성 능력의 평가

  • Oh, Jeong-Sun (Department of Chemistry, College of Natural Science, Chosun University) ;
  • Ahn, Jun-Hyung (School of Automotive and Mechanical Engineering and Institute of Manufacturing and Automation System, Nambu University) ;
  • Yun, Yeon-Hum (School of Automotive and Mechanical Engineering and Institute of Manufacturing and Automation System, Nambu University) ;
  • Kang, Bo-An (School of Automotive and Mechanical Engineering and Institute of Manufacturing and Automation System, Nambu University) ;
  • Kim, Sang-Bok (School of Automotive and Mechanical Engineering and Institute of Manufacturing and Automation System, Nambu University) ;
  • Hwang, Kyu-Seog (School of Automotive and Mechanical Engineering and Institute of Manufacturing and Automation System, Nambu University) ;
  • Shim, Yeon-A (Department of Ceramic Engineering, Chonnam National University)
  • 오정선 (조선대학교 화학과) ;
  • 안준형 (남부대학교 자동차기계공학부 생산 자동화 연구소) ;
  • 윤연흠 (남부대학교 자동차기계공학부 생산 자동화 연구소) ;
  • 강보안 (남부대학교 자동차기계공학부 생산 자동화 연구소) ;
  • 김상복 (남부대학교 자동차기계공학부 생산 자동화 연구소) ;
  • 황규석 (남부대학교 자동차기계공학부 생산 자동화 연구소) ;
  • 심연아 (전남대학교 세라믹공학과)
  • Published : 2002.01.01

Abstract

In order to investigate the calcium phosphate forming ability of nanocrystalline $ZrO_2$ film, we prepared $ZrO_2/Si$ structure by using a chemical solution deposition with a zirconium naphthenate as a starting material. Precursor sol was spin-coated onto the (100)Si substrate and prefired at 500$^{\circ}C$ for 10 min in air, followed by final annealing at 800$^{\circ}C$ for 30 min in air. Crystallinity of the annealed film was examined by X-ray diffraction analysis. Surface morphology and surface roughness of the film were characterized by field emission-scanning electron microscope and atomic force microscope. After annealing, nanocrystalline $ZrO_2$ grains were obtained on the surface of the film with a homogeneous interface between the film and substrate. After immersion for 1 or 5 days in a simulated body fluid, formation of calcium phosphate was observed on $ZrO_2$ film annealed at 800$^{\circ}C$ by energy dispersive X-ray spectrometer. The fourier transform infrared spectroscopy revealed that carbonate was substituted into the calcium phosphate.

나노 결정질 $ZrO_2$ 박막을 제조하여 박막의 표면에서 인산칼슘을 유도하는 능력을 편가하기 위하여, 지르코늄 나프테네이트를 출발물질로 사용하고 화학적 용액법을 이용하여, $ZrO_2/Si$ 구조를 제작하였다. 코팅용액을 (100)Si 기판 위에 스핀코팅한 후, 500$^{\circ}C$에서 10분간 전열처리와 800$^{\circ}C$에서 30분간 최종열처리를 행하였고, 모든 열처리는 공기분위기에서 실시하였다. X-ray diffraction analysis를 이용하여 열처리된 박막의 결정화도를 조사하였고, 표면의 미세구조와 표면 거칠기를 field emission-scanning electron microscope와 atomic force microscope를 이용하여 관찰하였다. 열처리 후의 박막은 표면에 미세한 $ZrO_2$ 나노 결정이 생성되어 있었으며, 박막의 계면은 매우 균질 하였다. 유사생채용액에 1일 및 5일간 침적된 샘플의 표면위에 형성된 인산칼슘을 energy dispersive X-ray spectrometer를 이용하여 관찰하였고, fourier transform infrared spectroscopy를 이용하여 인산칼슘에 카본이 치환되어 있음을 확인하였다.

Keywords

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