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Microstructural Analysis of Slags using Raman Micro Spectroscope
박수경,권인철,이수정,허일권,조남철 한국문화재보존과학회 2019 보존과학회지 Vol.35 No.2
The metal-manufacturing method and smelting temperature of ancient metal-production processes have been studied by analyzing the principal elements and microstructures of slag. However, the microstructure of slag varies according to the solidification cooling rate and types and relative amounts of various oxides contained within the smelting materials. Hence, there is a need for accurate analysis methods that allow slag to be distinguished by more than its composition or microstructure. In this study, the microstructures of slag discharged as a result of smelting iron sands collected from Pohang and Gyeongju, as well as the slag excavated from the Ungyo site in Wanju, were analyzed by using metalloscopy, scanning election microscopy-energy dispersine X-ray spectroscopy(SEM-EDS) and wavelength dispersive X-ray fluorenscence(WD-XRF). Furthermore, the microcrystals were accurately characterized by performing Raman micro-spectroscopy, which is a technique that can be used to identify the microcrystals of slags. SEM-EDS analysis of Pohang slag indicated that its white polygonal crystals could be Magnetite; however, Raman micro-spectroscopy revealed that these crystals were actually ulvöspinel. Raman micro-spectroscopy and SEM-EDS were also used to verify that the coarse white dendritic structures observed in the Gyeongju-slag were Wüstites. Additionally, the Wanju slag was observed to have a glassy matrix, which was confirmed by Raman micro-spectroscopy to be Augite. Thus, we have demonstrated that Raman micro-spectroscopy can accurately identify slag microcrystals, which are otherwise difficult to distinguish as solely based on their chemical composition and crystal morphology. Therefore, we conclude that it has excellent potential as a slag analysis technique.
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사철 제련을 통해 생산된 슬래그와 괴련철의 재료과학적 특성 비교
조성모,조현경,권인철,조남철 한국문화재보존과학회 2018 보존과학회지 Vol.34 No.1
This study replicated traditional smelting methods to produce iron blooms from sand iron. The metallurgical properties of the slag and the iron blooms were analyzed. The sand iron materials used in the smelting experiments, which were based on ancient documents, were collected from Gyeong-Ju and Pohang. Analysis by WD-XRF and XRD showed that Gyeong-Ju’s sand iron contains a high-titanium, with magnetite, and Pohang’s sand iron contains a low-titanium, which magnetite and ilmenite were mixed. Analysis of the slag with XRD, and the micro-structure with metal microscopes and SEM-EDS, confirmed that the major compounds in the slag of the Gyeong-Ju’s sand iron were fayalite and wüstite, and those in the slag of the Pohang’s sand iron were titanomagnetite and fayalite. The differences in the main constituents were confirmed according to the Ti quantity. Finally, we observed the microstructures of the iron blooms. In the case of the iron bloom produced from Gyeong-Ju’s sand iron, the outside was found to be dominantly a pearlite of eutectoid steel, while the inside was a hypo-eutectoid steel where ferrite and pearlite were mixed together. While, the major component of the iron bloom produced from Pohang’s sand iron was ferrite, which is almost like pure iron. However, there were many impurities inside the iron blooms. Therefore, this experiment confirmed that making ironware required a process that involved removing internal impurities, refining, and welding. It will be an important data to identify the characteristics of iron by-products and the site through traditional iron-making experiments under various conditions. 본 연구에서는 전통 제련법을 토대로 사철을 이용해 괴련철 생산을 재현하고 슬래그 및 괴련철을 분석하여 재료학적 특성을 알아보았다. 원료는 고문헌을 토대로 경주사철과 포항사철을 이용했다. WD-XRF 및 XRD 결과 경주사철은 저티탄사철의 Magnetite이며 포항사철은 고티탄사철의 Magnetite와 Ilmenite가 혼합됨을 확인하였다. 슬래그의 XRD 및 미세조직 분석결과 경주사철 슬래그는 Fayalite와 Wüstite, 포항사철 슬래그는 Titanomagnetite와 Fayalite가 확인되어 사철의 Ti 함량에 따른 조직의 차이를 확인하였다. 괴련철의 미세조직의 분석결과 경주사철 괴련철은 표면에 공석강에 가까운 탄소함량을 보이는 Pearlite가 우세하며, 내부는 Ferrite와 Pearlite가 혼재된 아공석강이었다. 포항사철 괴련철은 순철에 가까운 Ferrite이었다. 괴련철의 철물화를 위해서는 내부 불순물 제거, 조직을 치밀하게 하는 정련 및 단접이 필요함을 확인하였다. 향후 다양한 조건의 전통 제철 실험을 통해 제철부산물의 성격을 규명하고 제철 유적의 특징을 알아보는데 중요한 데이터로 활용 가능할 것이다.
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