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Phase evaluation of Fe/Co pigments coated porcelain by rietveld refinement

리트벨트 정밀화법에 의한 Fe/Co 안료가 코팅된 도자기의 상분석

  • Nam-Heun Kim (Department of Art Ceramic, Kangwon National University) ;
  • Kyung-Nam Kim (Department of Materials Engineering, Kangwon National University)
  • 김남훈 (강원대학교 생활조형디자인학과) ;
  • 김경남 (강원대학교 신소재공학과)
  • Received : 2023.09.18
  • Accepted : 2023.10.04
  • Published : 2023.10.31

Abstract

Porcelain (white ware, celadon ware) coated with a ferrous sulfate and ferrous/cobalt sulfate was sintered at 1250℃. The specimens were investigated by HR-XRD, FE-SEM, HR-EDS, and UV-vis spectrophotometer. Through X-ray rietveld quantitative analysis, quartz and mullite were found to be the main phases for white ware, and mullite and plagioclase were found to be the main phases for celadon ware. When the pigment of ferrous/cobalt sulfate was applied, were identified as an andradite phase for celadon ware and a spinel phase for the white ware, and the amorphous phase, respectively. The L* value, which was the brightness of the specimen, was 72.01, 60.92 for white ware and celadon ware, respectively. The ferrous and ferrous/cobalt pigment coated porcelain had L* values of 44.89, 52.27 for white ware and celadon ware, respectively; with a* values of 2.12, 1.40, an d at b* values of 1.45 and 13.79. As for the color of the specimens, it was found that the L* value was greatly affected by the white ware, and the b* value differed greatly depending on the clay. It was thought to be closely related to the production of the secondary phase such as Fe2O3 and andradite phase produced in the surface layer.

본 연구는 백자와 청자 소지에 철/코발트 황하물의 안료를 시유하여 1250℃에서 소성한 도자기 표면의 상형성을 연구하였다. 시편의 특성은 X-선 회절분석기, 전계방사형 주사전자현미경, 에너지 분산형 엑스선분석기 및 UV-vis 분광계를 이용하였다. X-선 리트벨트 정밀화 분석으로 백자소지는 석영과 뮬라이트가, 청자소지는 뮬라이트와 plagioclase가 주 결정상이다. 백자와 청자소지에 철/코발트 황하물의 안료를 시유한 경우 백자는 스피넬상이 청자는 andradite 상의 이차상이 형성되었다. 시편 소지의 색상은 밝기인 L* 값은 백자와 청자소지가 72.01, 60.92이고 백자가 청자소지 보다는 백색도가 높다. 철/코발트 황하물의 안료를 도포한 시편에서 백자와 청자 시편의 경우, L* 값은 44.89, 52.27, a* 값은 2.12, 1.40, b* 값은 1.4 5, 13.79를 각각 보이고 있다. L* 값은 백자소지에 안료를 도포한 시편에서 큰 변화가 있으며, b* 값은 소지에 따라 크게 차이가 나는 것을 알 수가 있다. 이는 표면층에 생성되는 Fe2O3 상과 andradite 결정상 생성과 밀접한 관련이 있다.

Keywords

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