• Journal of Conservation Science
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• v.6 no.1 s.7
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• pp.3-14
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• 1997

Twelve Punchong sherds collected in Hakbongni, Kongju where the well known iron-painted on white slip were manufactured from late 15C to early 16C were analyzed for their composition and microstructure. The composition of the body was analyzed by X-ray fluorescence and that of glaze by electron probe micro-analyzer. Microstructure was observed by optical microscope, polarizing microscope, EPMA, and X-ray diffractometer. The results of composition of body and glaze of Hakbongni were compared with those of Punchong from Yongsuri, Boryong which was close to Hakbongni. The composition of body and glaze of these two areas were compared by principal component analysis using SPSS program. Hakbongni bodies have higher silica and flux materials but lower alumina and their glaze have higher silica, soda, iron oxide but lower alumina, calcia. Hakbongni punchong itself is divided into two groups. Their glaze is lime type. There are many remnant minerals, such as quartz, large feldspar mass with partially melted surrounding area, albite, biotite, and iron-oxide. From such a microstructure we can assume that preparation of raw material was rather crude and firing temperature quite low. Iron-painted material is identified as Mg/Fe/Al spinel by composition analysis and XRD pattern.

• Korean Journal of Metals and Materials
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• v.47 no.12
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• pp.811-818
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• 2009

In order to meet increasingly complex and rigorous technical specifications, extensive effort has been devoted to fabricate clad materials with multi-layered metal plates. In this study, novel stainless steel/aluminum/copper (STS/Al/Cu) three-ply clad materials were fabricated by a hot rolling process for cookware applications. The effect of the testing temperature on the mechanical properties of the clad materials and on each component metal was investigated during the tensile tests. The interface properties of the clad materials were also examined by optical microscopy (OM) and an electron probe micro-analyzer (EPMA). The best mechanical and interfacial properties for a warm working process were found in a sample annealed at a temperature of $300^{\circ}C$. For the sample annealed at $400^{\circ}C$, the results of the tensile test indicated that interface delamination occurred only in the region of the Al/Cu interfaces. This was due to the formation of the thick and brittle intermetallic compound of $Al_2Cu$ in the Al/Cu interface. In contrast, no interface delamination was observed in the STS/Al interface, most likely due to its strong bond strength.

• Journal of the korean academy of Pediatric Dentistry
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• v.37 no.3
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• pp.288-297
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• 2010

The purpose of this study was to evaluate the effect of light cured fluoride-releasing materials on the inhibition of demineralization. In addition, the pattern of fluoride uptake of adjacent tooth structure was analyzed with EPMA. Eighty intact premolars were restored with $Filtek^{TM}$ Z250(control group, composite), Fuji Filling $LC^{TM}$(RMGI), Dyract $AP^{(R)}$ (compomer) and Beautifil II(giomer). Restored teeth were stored in distilled water for 30 days. Then sixty teeth(n=15) were exposed to demineralizing solution(pH 4.3). Demineralized teeth were bisected and polished. The specimens were observed with confocal laser scanning microscope. The depth of outer lesion and the thickness of inhibition zone were measured. Remained twenty teeth(n=5) were bisected for fluoride uptake analysis. The fluoride analysis were taken at enamel-restoration interface and dentin-restoration interface by electron probe micro-analyzer. The results are as follows: 1. The depth of outer lesion of Fuji Filling $LC^{TM}$ Dyract AP, Beautifil II was shallower than that of $Filtek^{TM}$ Z250 at the margin of restoration(p<0.05). 2. The thickness of caries inhibition zone of Fuji Filling $LC^{TM}$, Dyract AP, Beautifil II was greater than that of $Filtek^{TM}$ Z250 at the margin of restoration(p<0.05). 3. Fuji Filling $LC^{TM}$, Dyract AP, Beautifil II groups showed the greater fluoride uptake into enamel and dentine around restoration than $Filtek^{TM}$ Z250 group. 4. In dentin the difference of fluoride concentration were greater than in enamel, and Dyract AP showed the greatest fluoride concentration in dentin.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.109-110
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• 2014

주사전자현미경(Scanning Electron Microscopy: SEM)은 고체상태에서 미세조직과 형상을 관찰하는 데에 가장 다양하게 쓰이는 분석기기로서 최근에 판매되고 있는 고분해능 SEM은 수 나노미터의 분해능을 가지고 있다. 그리고 SEM의 초점심도가 크기 때문에 3차원적인 영상의 관찰이 용이해서 곡면 혹은 울퉁불퉁한 표면의 영상을 육안으로 관찰하는 것처럼 보여준다. 활용도도 매우 다양해서 금속파면, 광물과 화석, 반도체 소자와 회로망의 품질검사, 고분자 및 유기물, 생체시료 nnnnnnnnn와 유가공 제품 등 모든 산업영역에 걸쳐 있다(Fig. 1). 입사된 전자빔이 시료의 원자와 탄성, 비탄성 충돌을 할 때 2차 전자(secondary electron)외에 후방산란전자(back scattered electron), X선, 음극형광 등이 발생하게 되는 이것을 통하여 topography (시료의 표면 형상), morphology(시료의 구성입자의 형상), composition(시료의 구성원소), crystallography (시료의 원자배열상태)등의 정보를 얻을 수 있다. SEM은 2차 전자를 이용하여 시료의 표면형상을 측정하고 그 외에는 SEM을 플랫폼으로 하여 EDS (Energy Dispersive X-ray Spectroscopy), WDS (Wave Dispersive X-ray Spectroscope), EPMA (Electron Probe X-ray Micro Analyzer), FIB (Focus Ion Beam), EBIC (Electron Beam Induced Current), EBSD (Electron Backscatter Diffraction), PBMS (Particle Beam Mass Spectrometer) 등의 많은 분석장치들이 SEM에 부가적으로 장착되어 다양한 시료의 측정이 이루어진다. 이 중 결정구조, 조성분석을 쉽고 효과적으로 할 수 있게 하는 X선 분석장치인 EDS를 SEM에 일체화시킨 장비와 EDS 및 PBMS를 SEM에 장착하여 반도체 공정 중 발생하는 나노입자의 형상, 성분, 크기분포를 측정하는 PCDS(Particle Characteristic Diagnosis System)에 대해 소개하고자 한다. - EDS와 통합된 SEM 시스템 기본적으로 SEM과 EDS는 상호보완적인 기능을 통하여 매우 밀접하게 사용되고 있으나 제조사와 기술적 근간의 차이로 인해 전혀 다른 방식으로 운영되고 있다. 일반적으로 SEM과 EDS는 별개의 시스템으로 스캔회로와 이미지 프로세싱 회로가 개별적으로 구현되어 있지만 로렌츠힘에 의해 발생하는 전자빔의 왜곡을 보정을 위해 EDS 시스템은 SEM 시스템과 연동되어 운영될 수 밖에 없다. 따라서, 각각의 시스템에서는 필요하지만 전체 시스템에서 보면 중복된 기능을 가지는 전자회로들이 존재하게 되고 이로 인해 SEM과 EDS에서 보는 시료의 이미지의 차이로 인한 측정오차가 발생한다(Fig. 2). EDS와 통합된 SEM 시스템은 중복된 기능인 스캔을 담당하는 scanning generation circuit과 이미지 프로세싱을 담당하는 FPGA circuit 및 응용프로그램을 SEM의 회로와 프로그램을 사용하게 함으로 SEM과 EDS가 보는 시료의 이미지가 정확히 일치함으로 이미지 캘리브레이션이 필요없고 측정오차가 제거된 EDS 측정이 가능하다. - PCDS 공정 중 발생하는 입자는 반도체 생산 수율에 가장 큰 영향을 끼치는 원인으로 파악되고 있으며, 생산수율을 저하시키는 원인 중 70% 가량이 이와 관련된 것으로 알려져 있다. 현재 반도체 공정 중이나 반도체 공정 장비에서 발생하는 입자는 제어가 되고 있지 않은 실정이며 대부분의 반도체 공정은 저압환경에서 이루어지기에 이 때 발생하는 입자를 제어하기 위해서는 저압환경에서 측정할 수 있는 측정시스템이 필요하다. 최근 국내에서는 CVD (Chemical Vapor Deposition) 시스템 내 파이프내벽에서의 오염입자 침착은 심각한 문제점으로 인식되고 있다(Fig. 3). PCDS (Particle Characteristic Diagnosis System)는 오염입자의 형상을 측정할 수 있는 SEM, 오염입자의 성분을 측정할 수 있는 EDS, 저압환경에서 기체에 포함된 입자를 빔 형태로 집속, 가속, 포화상태에 이르게 대전시켜 오염입자의 크기분포를 측정할 수 있는 PBMS가 일체화 되어 반도체 공정 중 발생하는 나노입자 대해 실시간으로 대처와 조치가 가능하게 한다.

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2004.06a
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• pp.353-354
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• 2004

사용후 핵연료의 조성을 분석하거나 또는 반사전자상과 2차 전자상 등으로 시료를 관찰하기 위해서는 핫셀(Hot cell)에 증착기(coater)를 설치하여 시료표면을 전도성 물질인 탄소 등으로 증착시켜야 한다. 그러나 원격조정기를(manipulator)를 이용하여 수행되는 핫셀에서의 증착작업은 사용후 핵연료 시험의 선진분석기술을 갖고 있는 원자력 선진국에서도 핫셀내에 설치되어 있는 증착기의 탄소봉을 교체하는 작업과 진공장치의 성능 유지가 까다로워 시료표면에 균질하게 전도성 물질을 증착시키는 작업에 많은 어려움을 겪고 있다. 본 연구는 통상적으로 이용되는 증착기를 사용하지 않고 Silver Paint를 사용하여 사용후 핵연료를 분석할 수 있는 새로운 방법에 대한 연구를 수행하였다. 산화물 핵연료는 전기전도도가 매우 낮아($3{\times}10^{-1}~4{\times}10^{-8}/ohm{\cdot}cm$)입사된 전자의 이동이 원활하지 못해 일어나는 들뜸(Charging)현상이 발생한다. 그러나 Silver Paint 에 사용후 핵연료를 접착하면 모세관(capillary)현상에 의해 시료 주위와 핵연료의 결정립계로 Silver가 스며들어 입사된 전자의 이동이 원활해져 전도성이 극히 낮은 시료의 분석이 가능하게 된다. 본 시험에 사용된 EPMA는 (Electron Probe Micro Analyzer, SX-50R, CAMECA, Paris, France) 고 방사능을 띤 조사 핵연료의 시험을 수행할 수 있도록 기기의 적절한 부위에 납과 텅스텐으로 차폐되어 시편의 방사능 세기가 $3{\times}10^{10}Bq$까지 시험 가능한 기기이다. 그림 1은 JAERI 에 설치 운영중인 증착기 설비 사진이다. 그림에서 핫셀에 설치된 증착기의 진공을 유지하기 위해 핫셀 벽을 관통하여 증착기 본체까지 연결된 배출관의 형상과 복잡한 주변장치들을 볼 수 있다. 그림 2는 비조사 핵연료 시편을 Silver Pain떼 접착한 사진이다. 그림은 시료주위와 시료 표면까지 Silver Paint가 도포된 모습을 보여주고 있다. 상용발전소에서 연소도가 50,000 Mwd/tU인 사용후 핵연료를 상기와 같은 방법으로 만든 시편의 표면을 관찰한 사진을 그림 3~8에 나타내었다. 그림 3은 핵연료 중앙부위의 결정립을 나타낸 그림이다. Silver Paint만으로 접착한 시료의 표면관찰 및 정량분석이 그림에서 보듯이 가능함을 확인하였다. 그림 4는 사용후 핵연료시료를 중앙부위에서 가장자리까지를 다섯 부위로 나누어 그 중 중앙부위(1/5) 지점의 입계 및 형상을 관찰한 사진이다. 결정립의 크기가 다른 부위보다 상대적으로 크고, 결정립에 생성된 기공이 발달되어 있음을 볼 수 있다. 그림 5와 6과 7은 중심부위와 rim부위 사이 지점을 관찰한 사진으로서 결정립과 기공의 분포가 비슷한 형상을 나타내고 있음을 관찰할 수 있었다. 그림 8은 rim 부위 사진으로 전형적인 rim 영역 현상을 관찰할 수 있었다. 표 1은 그림 2와 같이 비조사 산화물 핵연료를 Silver Paint로 접착한 시편을 정량 분석한 결과이다. 시편의 조성은 33.6 at% U, 66.4 at% O의 결과를 얻었다. 산화물 핵연료의 표면 관찰 및 정량 분석 시험시 시편 표면을 전도성 물질로 증착시키지 않고, Silver Paint 에 시편을 접착하는 방법으로도 만족한 시험 결과를 얻을 수 있었다.

• Economic and Environmental Geology
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• v.30 no.1
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• pp.61-65
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• 1997

Cadmium occurs as a minor element in sphalerite ((Zn, Fe)S) from the Boseong-Jangheung gold-silver mine district. We analyzed the abundance of cadmium in sphalerite using an electron probe micro analyzer (EPMA) and discussed the natural sources of cadmium in terms of bedrock geochemistry, in order to preliminarily reconnoiter the potential cadmium contamination in mine districts. Cadmium contents of sphalerites from the Au-Ag mines (Bodeok, Mundeok, Jeonbo, Boknae, Keumsan) in the Boseong-Jangheung district are considerably high, compared with cadmium contents of sphalerites (average = 0.5 wt.% Cd, maximum = 4.4 wt.% Cd) in the world. Sphalerites from the Keumsan mine (average = 9.49 wt.% Cd, maximum=11.22 wt. Cd) are highly enriched in cadmium. Our data suggest that the Boseong-Jangheung area is an important potential site of cadmium contamination in Korea. Based on bedrock geochemistry, natural causes of cadmium enrichment in sphalerite from the mine district are thought to be the mixing of cadmium leached from organic-rich, metasedimentary rocks (including coal) and/or black shales. From this study, we propose that the pinpointing of potential sites of pollution by toxic heavy metals can be done effectively through detailed reconnaisance study on mineralogical compositions of ore minerals such as sphalerite from the mine area.

• Journal of Conservation Science
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• v.34 no.5
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• pp.433-442
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• 2018

In this study, metal properties were compared by preparingthree iron knives from steel ingots produced via traditional iron-making, and ingot which jointed the steel of modern times. Metal microscope and SEM-EDS analysis revealed fine ferrite and pearlite structures of the hypo-eutectoid steel of Fe-C alloys. All samples also exhibited martensite on the blade of the knife. By Vicker's hardness analysis, the hardness of the sand iron knife (K1) was 533.38 HV, sand iron-nickel steel knife (K3) was 514.8 HV, and sand iron-carbon steel knife (K2) was 477.02 HV. The mass reduction due to wear was 0.058% for K1, 0.059% for K3, and 0.144% for K2. EPMA(Electron probe micro-analyzer) analysis of the surface pattern of the specimens confirmed that the patterns were exposed due to differences in the content of C or the chemical composition. Additional research on heat treatment processes is needed to increase the abrasion resistance of blades. Traditional steel ingots could produce high-quality steel if combined with nickel steel.

• Economic and Environmental Geology
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• v.51 no.4
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• pp.323-343
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• 2018

This study defines the mineralogical, micro-textural and geochemical characteristics for the carbonate rocks and discusses the fluids that have affected the depositional environment of the Lower Makgol Formation in Seokgaejae section. Based on analysis of X-ray Diffraction (XRD), Scanning Electron Microscope-Energy Dispersive X-ray Spectrometry (SEM-EDS), Electron Probe Micro Analyzer-Wavelength Dispersive X-ray Spectrometry (EPMA-WDS) and Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS), carbonate miorofacies in the basal and the lower members of the Makgol Formation are distinguished and classified into four types. Type 1 dolomite (xenotopic interlocking texture) and Type 2 dolomite (idiotopic interlocking texture) have relatively high Mg/Ca ratio, flat REE pattern, low Fe and Mn. Extensively interlocking textures in these dolomites indicate constant supply of Mg ion from hypersaline brine. Type 3 and Type 4 dolomite (scattered and loosely-aggregated texture) have relatively moderate Mg/Ca ratio, MREE enriched pattern, low to high Fe and Mn. These partial dolomitization indicate limited supply of Mg ion under the influx of meteoric water with seawater. Also, the evidence of Fe-bearing minerals, recrystallization and relatively high Fe and Mn in Type 4 indicates the influence of secondary diagenetic fluids under suboxic conditions. Integrating geochemical data with mineralogical and micro-textural evidence, the discrepancy between the basal and the lower members of the Makgol Formation indicates different sedimentary environment. It suggest that hypersaline brine have an influence on the basal member, while mixing meteoric water with seawater have an effect on the lower member of the Makgol Formation.

• Journal of the Mineralogical Society of Korea
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• v.23 no.2
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• pp.125-139
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• 2010

Behavior of heavy metals and arsenic in the tailings of Songcheon Au-Ag mine was characterized via both mineralogical and geochemical methods. Mineral composition of the tailings was investigated by X-ray diffractometry, energy-dispersive spectroscopy, and electron probe micro-analyzer (EPMA) and total concentrations of heavy metals and arsenic and their chemical forms were analyzed by total digestion of aqua regia and sequential extraction method, respectively. The results of mineralogical study indicate that the tailings included mineral particles of resinous shape mainly consisting of galena, sphalerite, pyrite, quartz, and scorodite, and specifically socordite was identified in the form of matrix. EPMA quantitative analyses were performed to evaluate the weatherability of each mineral, and the results suggest that it decreased in the sequence of arsenopyrite > galena > sphalerite > pyrite. The weathering pattern of galena was observed to show distinctive zonal structure consisting of secondary minerals such as anglesite and beudantite. In addition, almost all of arsenopyrite has been altered to scorodite existing asmatrix and galena, sphalerite, and pyrite which have lower weatherability than arsenopyrite were identified within the matrix of scorodite. During the process of alteration of arsenopyrite into scorodite, it is likely that a portion of arsenic was lixiviated and caused a great deal of detrimental effects to surrounding environment. The results of EPMA quantitative analyses verify that the stability of scorodite was relatively high and this stable scorodite has restrained the weathering of other primary minerals within tailings as a result of its coating of mineral surfaces. For this reason, Songcheon tailings show the characteristics of the first weathering stage, although they have been exposed to the surface environment for a long time. Based on the overall results of mineralogical and geochemical studies undertaken in this research, if the tailings are kept to be exposed to the surface environment and the weathering process is continuous, not only hazardous heavy metals, such as lead and arsenic seem to be significantly leached out because their larger portions are being partitioned in weakly-bound (highly-mobile) fractions, but the potential of arsenic leaching is likely to be high as the stability of scorodite is gradually decreased. Consequently, it is speculated that the environmental hazard of Songcheon mine is significantly high.

• Economic and Environmental Geology
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• v.50 no.2
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• pp.117-128
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• 2017

Occurrence characteristics and existing forms of U-Th containing minerals in KURT (KAERI Underground Research Tunnel) granite are investigated to understand long-term behavior of radionuclides in granite considered as a candidate rock for the geological disposal of high-level radioactive waste. KURT granite primarily consists of quartz, feldspar and mica. zircon, REE(Rare Earth Element)-containing monazite and bastnaesite are also identified. Besides, secondary minerals such as sericite, microcline and chlorite including quartz vein and calcite vein are observed. These minerals are presumed to be accompanied by a post-hydrothermal process. U-Th containing minerals are mainly observed at the boundaries of quartz, feldspar and mica, mostly less than $30{\mu}m$ in size. Quantitative analysis results using EPMA (Electron Probe Micro-Analyzer) show that 74.2 ~ 96.5% of the U-Th containing minerals consist of $UO_2$ (3.39 ~ 33.19 wt.%), $ThO_2$ (41.61 ~ 50.24 wt.%) and $SiO_2$ (15.43 ~ 18.60 wt.%). Chemical structure of the minerals calculated using EPMA quantitative analysis shows that the U-Th minerals are silicate minerals determined as thorite and uranothorite. The U-Th containing silicate minerals are formed by a magmatic and hydrothermal process. Therefore, KURT granite formed by a magmatic differentiation is accompanied by an alteration and replacement owing to a hydrothermal process. U-Th containing silicate minerals in KURT granite are estimated to be recrystallized by geochemical factors and parameters such as temperature, pressure and pH owing to the hydrothermal process. By repeated dissolution/precipitation during the recrystallization process, U-Th containing silicate minerals such as thorite and uranothorite are formed according to the variation in the concentrated amount of U and Th.