전기방사법을 이용해 제조된 NiZn ferrite 나노 섬유의 결정화
Crystallization of the NiZn ferrite nanofibers fabricated by electrospinning method
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초록
전기방사 공정을 이용하여 니켈, 아연, 철 전구체를 포함하는 Polyvinyl pyrrolidone 나노 섬유를 제조하였다. 이를 전자기파 차폐에 사용할 수 있는 Ni0.5Zn0.5Fe2O4 산화물 나노 섬유로 전환하기 위하여 열처리 조건을 제어하였다. 비정질카본 블랙이나 의도치 않은 제2상 등을 배제하고 1차원 미세구조를 유지하면서 산화물 나노 섬유로 만들기 위하여 열처리중 실시간으로 샘플을 채취해 공정 중 샘플 변화를 추적하였다. X-ray diffraction(XRD) 분석 결과 결정화된 Ni0.5Zn0.5Fe2O4의 회절 패턴은 300°C부터 나타나기 시작하였으나, energy dispersive spectroscopy(EDS) 결과 상 카본 블랙이 대부분 사라지기 위해서는 500°C 이상의 열처리를 필요로 하였다. 650°C 이상의 온도부터는 본격적으로 결정 핵 성장이 진행되어 섬유표면 상태가 매끄럽지 않아지므로, 적용 분야에 따라 선택적으로 열처리 조건을 결정해야 함이 확인되었다.
Abstract
Polyvinyl pyrrolidone nanofibers including nickel, zinc, and iron precursors were fabricated via the electrospinning method. To convert as-spun nanofibers to Ni0.5Zn0.5Fe2O4 oxide nanofibers which is c apable o f shielding a n electromagnetic wave, heat treatment conditions were optimized. To obtain the heat treatment condition that can exclude amorphous carbon black and secondary crystal phase, samples were taken at each temperature while the calcination process and analyzed. According to the X-ray diffraction (XRD) analysis, the Ni0.5Zn0.5Fe2O4 crystal phase started to appear from 300°C, but itwas confirmed through energy dispersive spectroscopy (EDS) analysis that heat treatment of 500°C or more was required to remove most of the carbon black. When the calcination temperature exceeds 650°C, crystal nuclei starts to grow and the fiber surface condition becomes rough, so it was confirmed that the heat treatment conditions should be selectively determined according to the application field.
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