Economic and Environmental Geology (자원환경지질)

The Korean Society of Economic and Environmental Geology (대한자원환경지질학회)
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In-situ Phase Transition Study of Minerals using Micro-focusing Rotating-anode X-ray and 2-Dimensional Area Detector

집속 회전형 X-선원과 이차원 검출기를 이용한 광물의 실시간 상전이 연구

  • 성동훈 (연세대학교 이과대학 지구시스템과학과) ;
  • 이용문 (연세대학교 이과대학 지구시스템과학과) ;
  • 이용재 (연세대학교 이과대학 지구시스템과학과)
  • Received : 2012.03.26
  • Accepted : 2012.04.23
  • Published : 2012.04.28
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Abstract

The increased brightness and focused X-ray beams now available from laboratory X-ray sources facilitates a variety of powder diffraction experiments not practical using conventional in-house sources. Furthermore, the increased availability of 2-dimensional area detectors, along with implementation of improved software and customized sample environmental cells, makes possible new classes of in-situ and time-resolved diffraction experiments. These include phase transitions under variable pressure- and temperature conditions and ion-exchange reactions. Examples of in-situ and time-resolved studies which are presented here include: (1) time-resolved data to evaluate the kinetics and mechanism of ion exchange in mineral natrolite; (2) in-situ dehydration and thermal expansion behaviors of ion-exchanged natrolite; and (3) observations of the phases forming under controlled hydrostatic pressure conditions in ion-exchanged natrolite. Both the quantity and quality of the in-situ diffraction data are such to allow evaluation of the reaction pathway and Rietveld analysis on selected dataset. These laboratory-based in-situ studies will increase the predictability of the follow-up experiments at more specialized beamlines at the synchrotron.

최근 개발된 상용 X-선원들은 기존 선원들에 비하여 비약적으로 증가된 휘도와 집속율을 보임으로써 다양한 형태의 연구실 규모의 분말회절 분석을 가능하게 하고 있다. 더욱이, 개선된 소프트웨어 및 시료환경 장치와 더불어 2차원 검출기의 성능향상은 다양한 온도, 압력하에서의 상전이 현상 및 이온교환 반응과 같은 새로운 형태의 실시간 및 시간분해 회절실험을 가능하게 하고 있다. 본 논문에서는 (1) 나트로라이트의 이온교환 특성에 관한 실시간 측정, (2) 이온교환된 나트로라이트의 탈수 및 열팽창 특성에 관한 실시간 측정, (3) 이온교환된 나트로라이트의 정수압(靜水壓) 하에서의 상전이 현상의 관찰 등의 내용을 소개하고자 한다. 측정된 회절자료의 양과 품질은 각 반응의 진행경로를 확인할 수 있게 하고 선택된 자료의 리트벨트 분석을 통해 구조해석까지 가능케 한다. 이와 같은 형태의 개별 연구실 기반 실시간 회절분석 연구는 추후 연관되어 수행될 방사광가속기를 이용한 보다 특화된 실험에 대한 사전 예측성을 더욱 증가시킬 것으로 사료된다.

Keywords

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