• Title/Summary/Keyword: EPMA(Electron Probe Micro Analysis

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Characteristics of Plasma Damage and Recover in PZT Films by Dry Etching (건식식각에 의한 PZT 박막의 플라즈마 손상 및 회복특성)

  • 강명구;김경태;김동표;김창일
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.07a
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    • pp.375-378
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    • 2002
  • We investigated the reduction of etching damage by additive O$_2$ in etching gas and recovery of etching damage by O$_2$ annealing. The PZT thin films were etched using additive Ar or O$_2$ into Cl$_2$/CF$_4$ gas mixing ratio of 8/2. In order to recover ferroelectric properties of PZT thin films after etching, the etched PZT thin films were annealed at 600 C in O$_2$ atmosphere for 10 min. The remanent polarization is decreased seriously and fatigue is accelerated in the PZT sample etched in Ar/(C1$_2$+CF$_4$) plasma, whereas these characteristics are improved in O$_2$/(Cl$_2$/CF$_4$). From x-ray photoelectron spectroscopy (XPS) analysis, the intensities of Pb-O, Zr-O and Ti-O peaks are changed and the etch byproducts such as metal chloride and metal fluoride are reduced by O$_2$ annealing. From electron probe micro analyzer (EPMA) and auger electron spectroscopy(AES), O$_2$ vacancy is observed after etching. In x-ray diffraction (XRD), the structure damage in the additive O$_2$ into C1$_2$/CF$_4$ is reduced and the improvement of ferroelectric behavioral annealed sample is consistent with the increase of the (100) and (200) PZT peaks.

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Effect of Heat Treatment Conditions on the Microstructure and Wear Behavior of Ni-based Self-flux Alloy Coatings (니켈기 자융성 합금 코팅층의 미세구조 및 마모거동에 미치는 후열처리 조건의 영향)

  • Kim, K.T.;Oh, M.S.;Kim, Y.S.
    • Journal of Power System Engineering
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    • v.11 no.1
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    • pp.121-126
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    • 2007
  • This study aims at investigating the effect of heat treatment conditions on the dry sliding wear behavior of thermally sprayed Ni-based self-flux alloy coatings. Ni-based self-flux alloy powders were sprayed onto a carbon steel substrate and then heat-treated at 700, 800, 900 and $1000^{\circ}C$ for 30 minutes in a vacuum furnace. Dry sliding wear tests were performed using sliding speed of 0.4 m/s and applied load of 6 N. AISI 52100 ball(diameter 8 mm) was used as counterparts. Microstructure and wear behavior of both as-sprayed and heat-treated Ni-based self-flux alloy coatings were studied using a scanning electron microscope(SEM), energy dispersive X-ray spectroscopy(EDX), electron probe micro-analysis(EPMA) and X-ray diffraction(XRD). It was revealed that microstructure and wear behavior of thermally sprayed Ni-based self-flux alloy coatings were much influenced by heat treatment conditions.

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Enhancement of Hardness and Moderation of Surface Defects of 14K, 18K Yellow Gold Alloy by Heat Treatment (열처리에 의한 14K, 18K yellow gold alloy의 경도 향상 및 표면 결함 완화)

  • Ahn, Ji-Hyun;Seo, Jin-Kyo;Ahn, Yoeng-Gil;Park, Jong-Wang
    • Journal of Surface Science and Engineering
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    • v.43 no.2
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    • pp.86-90
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    • 2010
  • In this study, we conducted heat treatment on 14K, 18K yellow gold alloy at various temperature conditions for improving their hardness and moderating their surface defects. Also after the heat treatment we used EPMA (Electron Probe Micro Analyzer), XRF (x-ray Fluorescence spectroscopy) for qualitative analysis and OM (optical microscope), SEM (scanning electron microscope) to investigate the changes of surface grain boundary. We used Vickers hardness tester to verify the changes of hardness. After the heat treatment, 14K, 18K gold alloys showed improved hardness and moderated surface defects at specific temperatures and duration.

AN EXPERIMENTAL STUDY OF THE EFFECT OF ION EXCHANGE ON STRENGTHENING OF DENTAL PORCELAIN (이온교환법에 의한 치과용도재의 강도증진 효과에 관한 실험적 연구)

  • Lee Young-Kook;Lee Sun-Hyung;Yang Jae-Ho
    • The Journal of Korean Academy of Prosthodontics
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    • v.29 no.3
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    • pp.75-86
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    • 1991
  • Ion exchange strengthening is a chemical process whereby large alkali ions(such as potassium) are substituted for smaller ions(sodium) within the surfaces of glasses and ceramics, thereby reducing the thermal expansion coefficient of this surface region, and creating beneficial state of compressive stress within the near surface region. The purpose of this study was to determine the effects of ion exchange and etching treatments on the strength of some dental porcelains. Two feldspathic dental porcelains(Vitadur-N, G-Cera) were used in this study. A commercial ion exchange paste and etching gel containing 8% hydrofluoric acid were used for surface conditioning. Transverse strength was measured using a universal testing machine and the technique of EPMA(electron probe micro analysis) was used to access the potassium contents. The results were as follows: 1. Improvement in strength was only obtained by treating the surface placed in tension. 2. No changes in the dimensions of the treated specimens were detected when samples were measured with a micrometer. 3. There was significant increase in transverse strength of G-Cera IV group treated with etching and ion exchange, compared with G-Cera II group only treated with ion exchange. 4. From the results of EPMA test, increase in potassium contents was observed on the surface treated with ion exchange paste.

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Underwater Explosive Welding of Stainless Steel and Magnesium Alloy (수중 충격파를 이용한 스테인레스 스틸과 마그네슘합금의 폭발용접에 관한 연구)

  • Lee, Joon-Oh;Kim, Young-Kook;Cho, Sang-Ho
    • Tunnel and Underground Space
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    • v.22 no.3
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    • pp.221-225
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    • 2012
  • Magnesium is one of the light weight materials, which can improve fuel economy and reduce emissions in automotive industry. Recently, magnesium alloys have gained considerable attention due to good mechanical properties. In this work, we have performed an explosive welding using the magnesium alloys (AZ31) and stainless steel (SUS 304). As a result, SUS304/AZ31 were successfully combined each other; however, a resolidified interlayer was observed at the point of welded layer. To reduce the resolidified interlayer, we have changed the thickness (0.5 mm and 1 mm) of stainless steel, distance (45 mm and 60 mm) between explosive and the center of materials and initial angle ($20^{\circ}$ and $30^{\circ}$) of explosive. In the case of the thickness 0.5 mm and angle of $30^{\circ}$, the resolidfied interlayer was not observed due to the increase of distance from the explosive. To accurately estimate the resolidified interlayer, electron probe micro-analyzer (EPMA) method and hardness were used. For the EPMA analysis, mixed materials were confirmed at the resolidified interlayer, and the measurement exhibited the middle value compared with the AZ31 and SUS304.

주조방법에 따른 주얼리 제품(14K yellow gold alloy)의 특성비교 및 열처리 전과 후 특성변화

  • Yun, Don-Gyu;Seo, Jin-Gyo;Sin, So-Ra;An, Yong-Gil;Park, Jong-Wan
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.238-238
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    • 2012
  • 현재 국내 주얼리(gold alloy) 제품을 생산함에 있어 주조 방법은 크게 대기 중 주조(흡입주조) 방법과 진공주조 방법으로 나누어진다. 국내 주얼리 제조업체의 약 90%이상이 대기 중에서 주조하는 흡입주조방법을 통해 제품을 제작하고 있고, 국외의 경우, 대다수 진공주조방법을 통해 제품을 제작하고 있다. 본 연구에서는 주얼리 제품을 생산할 때 사용되는 합금재료(master alloy)가 동일한 조건에서 주조방법을 달리하여 각각 24개씩 총 48개의 14K yellow gold alloy 제품을 제작한 후 열처리를 통해 각각의 기계적, 물리적 특성분석을 비교 분석하였다. EPMA (Electron Probe Micro Analysis)분석을 통해 합금재료 및 제품의 구성성분을 조사하였고, ICP-MS (Inductively Coupled Plasma Mass Spectroscopy)를 사용하여 성분에 대한 정량분석을 실시하였다. 용체화처리(solid solution treatment)는 $700^{\circ}C$, 30분의 조건으로 실시하였고, 시효경화처리(age-hardening)는 $200{\sim}300^{\circ}C$의 온도범위에서 $50^{\circ}C$ 간격으로 실시하였다. 열처리 전과 후 시료의 grain 들의 배열 및 size 변화를 관찰하기 위해 식각 후 OM (optical microscope) 및 SEM (Scanning Electron Microscope)를 통해 분석하였다. 열처리 전 제품의 경도측정결과 대기 중 흡입주조방법 및 진공 주조방법을 통해 제작된 제품이 각각 119 Hv, 126 Hv로 나타났고, 용체화 처리 후 98 Hv, 92 Hv로 감소하였다. 시효경화 처리 후의 경도변화는 대기 중 흡입주조 및 진공주조방법을 통해 제작된 제품 모두 $270^{\circ}C$에서 각각 154 HV, 166 HV로 가장 높은 경도 값을 나타내었고, $270^{\circ}C$ 이상에서는 과시효(over aging)현상으로 인해 경도 값이 다시 감소하는 경향을 나타내었다. EPMA mapping 분석을 통해 주조방법에 따라 각각 제품의 구성성분분포도를 확인하였다. 이를 통해 열처리 전 다소 불균일하게 분포되었던 성분들이 열처리 후 균일해짐을 확인할 수 있었다.

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Analysis of Chemical Composition, Microstructure and Hydroxyapatite Structure for Mouse Teeth (생쥐 치아의 화학적 조성, 미세구조 및 Hydroxyapatite 구조 분석)

  • Kim, Eun-Kyung;Jeon, Tae-Hoon;Kim, Chang-Yeon;Nam, Seung-Won;Song, Kyung;Lee, Sang-Gil;Kim, Youn-Joong
    • Applied Microscopy
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    • v.40 no.3
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    • pp.147-154
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    • 2010
  • The aim of this study is to determine microstructure, chemical composition and crystal structure of hydroxyapatite for mouth teeth using optical microscopy and electron microscopy as well as electron probe micro-analysis (EPMA). Enamel, a protective cover to the teeth, consisted of rods oriented in regular and had relatively higher crystallinity and Ca component. In contrast, dentin showed a sponge-like microstructure with circular holes which were passages of dentinal tubules, and had higher Mg component than the enamel region due to its higher organic content. Hydroxyapatite crystals appeared as large rods in enamel, but as small needles in dentin. Their electron diffraction patterns were different by their crystallinity as well as by the organic content of the matrix.

A Study on the Degradation Mechanism of ZnO Ceramic Varistor Manufactured by Ambient Sintering-Process (분위기 소결공정에 의해 제조된 ZnO 세라믹 바리스터의 열화기구 연구)

  • 소순진;김영진;박춘배
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.13 no.5
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    • pp.383-389
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    • 2000
  • The relationship between the DC degradation characteristics of the ZnO varistor and the ambient sintering-process is investigated in this study. ZnO varistors made o matsuoka’s composition were fabricated by standard ceramic techniques. The ambient sintering-process is performed at the extraordinary electrical-furnace which is equipped with the vacuum system. Gases used in sintering process were oxygen nitrogen argon and air. Using XRD and SEM the phase and microstructure of samples were analyzed respectively. The conditions of DC degradation tests were conducted at 115$\pm$2$^{\circ}C$ for 13 h. Current-voltage analysis is used to determine nonlinear coefficients($\alpha$). Frequency analysis are performed to understand electrical properties as DC degradation test. From above analysis it is found that the ZnO varistor sintered in oxygen atmosphere showed superior properties at the DC degradation test and degradation phenomenon of ZnO varistor is caused by the change of electrical properties in grain boundary. These results are in accordance with Gupta’s degradation model.

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METAL SURFACE CHANGES BY HEAT TREATMENT OF Ni-Cr ALLOYS (열처리에 의한 도재용 Ni-Cr합금 표면의 변화에 관한 연구)

  • Kim, Young-Han;Lee, Sun-Hyung;Yang, Jae-Ho;Jung, Heon-Young
    • The Journal of Korean Academy of Prosthodontics
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    • v.27 no.2
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    • pp.219-248
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    • 1989
  • The purposes of this study were to analyze the microstructural and compositional changes of metal surfaces following different conditions of preoxidizing heat treatment, to investigate the composition of metal oxides, and to evaluate the effect of preoxidation and removal of surface oxides on microstructure and diffusion profiles. The techniques of EDAX (energy-dispersive analysis of x-ray), ESCA (electron spectroscopy for chemical analysis), and EPMA (electron probe micro analysis) were used, along with SEM (scanning electron microscopy). The obtained results were as follows : 1. A surface of the specimen became rough and the amount of the metal oxides increased with increasing the heat treatment time and temperature and the partial pressure of oxygen. 2. At an air pressure of 28' vacuum, the higher the temperature and the longer the time of preoxidation, the higher Ni concentration was detected. 3. Cr concentration in the specimen heat treated with air was higher than that of with vacuum. 4. The oxides in the specimens were mainly composed of Ni and Cr oxides. On the globular growth particles, significant rises in Al concentration of Rexillium III and Ti concentration of Verabond were noted. 5. Atomic diffusion occurred at the ceramic-metal interface, furthermore the amount of the flux was increased with preoxidation heat treatment.

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A histomorphometric study on the effect of surface treatment on the osseointegration (티타늄 임플란트의 표면처리가 골유착에 미치는 영향에 관한 조직형태계측학적 연구)

  • Choi, Woong-Jae;Cho, In-Ho
    • The Journal of Korean Academy of Prosthodontics
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    • v.47 no.4
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    • pp.445-456
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    • 2009
  • Statement of problem: Many studies have been conducted to improve the primary stability of implants by providing bioactive surfaces via surface treatments. Increase of surface roughness may increase osteoblast activity and promote stronger bonding between bone and implant surface and it has been reported that bioactive surface or titanium can be obtained through alkali and heat treatment. Purpose: The purpose of this study was to evaluate the stability of alkali and heat treated implants via histomorphometric analysis. Material and methods: Specimens were divided into three groups; group 1 was the control group with machined surface, the other groups were treated for 24 hours in 5 M NaOH solution and heat treated for 1 hour at $600^{\circ}C$ in the atmosphere (group 2) and vacuum (group 3) conditions respectively. Surface characteristics were analyzed and fixtures were implanted into rabbits. The specimens were histologically and histomorphometrically compared according to healing periods and change in bone composition were analyzed with EPMA (Electron Probe Micro Analyzer). Results: 1. Groups treated with alkali and heat showed increase of oxidization layer and Na ions. Groups 2 which was heat treated in atmosphere showed significant increase of surface roughness (P<.05). 2. Histomorphometric analysis showed significant increase in BIC (bone to implant contact) according to increase in healing period and there was significant increases in groups 2 and 3 (P<.05). 3. BA(bone area) ratio showed similar results as contact ratio, but according to statistical analysis there was significant increase according to increase in healing period in group 2 only (P<.05). 4. EPMA analysis revealed no difference in gradation of bone composition of K, P, Ca, Ti in surrounding bone of implants according to healing periods but groups 2 and 3 showed increase of Ca and P in the initial stages. Conclusion: From the results above, it can be considered that alkali and heat treated implants in the atmosphere have advantages in osseointegration in early stages and may decrease the time interval between implantation and functional adaptation.