• 한국분말야금학회:학술대회논문집
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• 한국분말야금학회 1999년도 춘계학술대회 및 발표대회 강연 및 발표논문 초록집
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• pp.5-5
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• 1999

The Principal deficiency of the existing notion about the sintering-mixtures consists in the fact that almost no attention is focused on the Phenomenon of alloy formation during sintering, its connection with dimensional changes of powder bodies, and no correct ideas on the driving force for the sintering process in the stage of establishing chemical equilibrium in a system are available as well. Another disadvantage of the classical sintering theory is an erroneous conception on the dissolution mechanism of solid in liquid. The two-particle model widely used in the literature to describe the sintering phenomenon in solid state disregards the nature of the neighbouring surrounding particles, the presence of pores between them, and the rise of so called arch effect. In this presentation, new basic scientific principles of the driving forces for the sintering process of a two-component powder body, of a diffusion mechanism of the interaction between solid and liquid phases, of stresses and deformation arising in the diffusion zone have been developed. The major driving force for sintering the mixture from components capable of forming solid solutions and intermetallic compounds is attributed to the alloy formation rather than the reduction of the free surface area until the chemical equilibrium is achieved in a system. The lecture considers a multiparticle model of the mixed powder-body and the nature of its volume changes during solid-state and liquid-phase sintering. It explains the discovered S-and V-type concentration dependencies of the change in the compact volume during solid-state sintering. It is supposed in the literature that the dissolution of solid in liquid is realised due to the removal of atoms from the surface of the solid phase into the melt and then their diffusicn transfer from the solid-liquid interface into the bulk of liquid. It has been shown in our experimental studies that the mechanism of the interaction between two components, one of them being liquid, consist in diffusion of the solvent atoms from the liquid into the solid phase until the concentration of solid solutions or an intermetallic compound in the surface layer enables them to pass into the liquid by means of melting. The lecture discusses peculimities of liquid phase formation in systems with intermediate compounds and the role of the liquid phase in bringing about the exothermic effect. At the frist stage of liquid phase sintering the diffusion of atoms from the melt into the solid causes the powder body to grow. At the second stage the diminution of particles in size as a result of their dissolution in the liquid draws their centres closer to each other and makes the compact to shrink Analytical equations were derived to describe quantitatively the porosity and volume changes of compacts as a result of alloy formation during liquid phase sinteIing. Selection criteria for an additive, its concentration and the temperature regime of sintering to control the density the structure of sintered alloys are given.

• 한국재료학회지
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• 제21권7호
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• pp.384-390
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• 2011

Ti-6Al-4V ELI (Extra Low Interstitial) alloy has been widely used as an alternative to bone due to its excellent biocompatibility. However, it still has many problems, including a high elastic modulus and toxicity. Therefore, nontoxic biomaterials with a low elastic modulus should be developed. However, the fabrication of a uniform coating is challenging. Moreover, the coating layer on Ti and Ti alloy substrates can be peeled off after implantation. To overcome these problems, it is necessary to produce bulk Ti and Ti alloy with hydroxyapatite (HA) composites. In this study, Ti, Nb, and Zr powders, which are biocompatible elements, were milled in a mixing machine (24h) and by planetary mechanical ball milling (1h, 4h, and 6h), respectively. Ti-35%Nb-7%Zr and Ti-35%Nb-7%Zr-10%HA composites were fabricated by spark plasma sintering (SPS) at $1000^{\circ}C$ under 70MPa using mixed and milled powders. The effects of HA addition and milling time on the biocompatibility and physical and mechanical properties of the Ti-35%Nb-7%Zr-(10%HA) alloys have been investigated. $Ti_2O$, CaO, $CaTiO_3$, and $Ti_xP_y$ phases were formed by chemical reaction during sintering. Vickers hardness of the sintered composites increases with increased milling time and by the addition of HA. The biocompatibilty of the HA added Ti-Nb-Zr alloys was improved, but the sintering ability was decreased.

• 한국재료학회지
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• 제5권2호
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• pp.151-156
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• 1995

$(Ba, Sr)TiO_{3}$계에 저융점의 Glass물질을 첨가하여 저온소결이 가능하며, 고유전율을 갖는 유전체 재료를 제조하여, 그 특성을 조사하였다. 본 연구에서는 고유전율의 $(Ba, Sr)TiO_{3}$계에 PbO함량이 서로 다른 Glass물질을 첨가하여 조성변화에 따른 저온소결거동 및 유전특성을 조사하였으며, 적층형 세라믹 Capacitor(MLCC)에 응용하기 위하여 다양한 조성으로 제조하였다. $PbO-ZnO-B_{2}O_{2}$계 Glass 성분을 첨가하여 소결온도를 $1350^{\circ}C$에서 $1050^{\circ}C$까지 낮출수 있었으며, 4wt% glass 첨가로 $1150^{\circ}C$ 이하에서 2시간 소결한 저온소결용 재료는 실온에서 8000정도의 높은 비유전율과 0.005의 낮은 유전손실 그리고 광역온도범위에서 유전상수의 안정성을 가진 우수한 특성을 나타내며, 입자크기가 1~3 $\mu$m 정도로 치밀한 미세구조를 가지고 있다. 본 연구의 저온소결용 유전체 재료는 Z5U 규격을 만족시키고 기존의 $BaTiO_{3}$계 재료에 비해 낮은 소결온도를 가지므로 MLCC에 응용시 내부전극으로 Ag-Pd alloy 사용이 가능한 것으로 밝혀졌다.

• 한국결정성장학회지
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• 제23권1호
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• pp.51-57
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• 2013

본 연구에서는 Heusler $Fe_2VAl$ 열전화합물을 제조하기 위하여 순금속 $Fe_{50}V_{25}Al_{25}$ 혼합분말을 기계적 합금화 처리하였다. $Fe_2VAl$ 열전화합물을 얻기 위하여 최적 볼밀조건 및 열처리 조건을 X선 회절분석과 시차주사 열량분석을 이용하여 조사하였다. $Fe_{50}V_{25}Al_{25}$ 혼합분말을 60시간까지 볼밀 처리한 경우 bcc 구조의 ${\alpha}$-(Fe,V,Al) 고용체가 얻어졌다. 단상의 Heusler $Fe_2VAl$ 화합물은 $Fe_{50}V_{25}Al_{25}$ 혼합분말을 60시간 동안 MA 처리 후 $700^{\circ}C$까지 열처리함으로써 얻을 수 있었다. MA 분말시료의 치밀화를 위하여 인가압력 60 MPa 및 소결온도 $900{\sim}1000^{\circ}C$에서 흑연다이를 사용하여 SPS 소결을 실시하였다. $1000^{\circ}C$에서 SPS 소결 후 얻어진 벌크체의 Vickers 경도는 870으로 매우 높은 값을 보였다. 또한 SPS 법으로 얻어진 벌크체의 밀도측정 결과, 모든 시료에서 상대밀도 90 % 이상의 금속광택을 나타내는 치밀한 소결체임을 알 수 있었다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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• pp.271-272
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• 2012

Bulk Metallic Glasses (BMGs or amorphous alloy) exhibit high strength and good corrosion resistance. Applications of thin films and micro parts of BMGs have been used a lot since its inception in the research of BMGs. However, Application and fabrication of BMGs are limited to make structural materials. Thin films of BMGs which is sputtered on the surface of structural materials by sputtering process is used to improve limits about application of BMGs. In order to investigate the difference of properties between designed alloys and thin films, we identified that thin films deposited on the surface that have the characteristic of the amorphous films and the composition of designed alloys. Zr-Cu (Cu=30, 35, 38, 40, 50 at.%) and Zr-Cu-Al (Al=10 at.% fixed, Cu=26, 30, 34, 38 at.%) alloys were fabricated with Zr (99.7% purity), Cu (99.997% purity), and Al (99.99% purity) as melting 5 times by arc melting method before rods 2mm in diameter was manufactured. In order to analyze GFA (Glass Forming Ability), rods were observed by Optical Microscopy and SEM and $T_g$, $T_x$, ($T_x$ is crystallization temperature and $T_g$ is the glass transition temperature) and Tm were measured by DTA and DSC. Powder was manufactured by Gas Atomizer and target was sintered using powder in large supercooled liquid region ($=T_x-T_g$) by SPS(Spark Plasma Sintering). Amorphous foil was prepared by RSP process with 5 gram alloy button. The composition of the foil and sputtered thin film was analyzed by EDS and EPMA. In the result of DSC curve, binary alloys ($Zr_{62}Cu_{38}$, $Zr_{60}Cu_{40}$, $Zr_{50}Cu_{50}$) and ternary alloys ($Zr_{64}Al_{10}Cu_{26}$, $Zr_{56}Al_{10}Cu_{34}$, $Zr_{52}Al_{10}Cu_{38}$) have $T_g$ except for $Zr_{70}Cu_{30}$ and $Zr_{60}Al_{10}Cu_{30}$. The compositions with $T_g$ made into powders. Figure shows XRD data of thin film showed similar hollow peak.

• 한국분말재료학회지
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• 제23권1호
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• pp.49-53
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• 2016

The present study demonstrates the effect of freezing conditions on the pore structure of porous Cu-10 wt.% Sn prepared by freeze drying of $CuO-SnO_2$/camphene slurry. Mixtures of CuO and $SnO_2$ powders are prepared by ball milling for 10 h. Camphene slurries with 10 vol.% of $CuO-SnO_2$ are unidirectionally frozen in a mold maintained at a temperature of $-30^{\circ}C$ for 1 and 24 h, respectively. Pores are generated by the sublimation of camphene at room temperature. After hydrogen reduction and sintering at $650^{\circ}C$ for 2 h, the green body of the $CuO-SnO_2$ is completely converted into porous Cu-Sn alloy. Microstructural observation reveals that the sintered samples have large pores which are aligned parallel to the camphene growth direction. The size of the large pores increases from 150 to $300{\mu}m$ with an increase in the holding time. Also, the internal walls of the large pores contain relatively small pores whose size increases with the holding time. The change in pore structure is explained by the growth behavior of the camphene crystals and rearrangement of the solid particles during the freezing process.

• 한국재료학회지
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• 제13권5호
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• pp.292-296
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• 2003

In an attempt to enhance phase transformation and homogenization of Mn-doped $FeSi_2$, mechanical alloying of elemental powders was applied. Cold pressing and sintering in vacuum were carried out to produce a dense microstructure, and then isothermal annealing was employed to induce a phase transformation to the $\beta$-$FeSi_2$semiconductor. Phase transitions in this alloy system during the process were investigated by using XRD, EDS and SEM. As-milled powders after 100 h of milling were shown to be metastable state. As-sintered iron silicides consisted of untransformed mixture of $\alpha$-$Fe_2$$Si_{5}$and $\varepsilon$-FeSi phases. $\beta$-$FeSi_2$phase transformation was induced by subsequent isothermal annealing at $830^{\circ}C$, and near single phase of $\beta$-$FeSi_2$was obtained after 24 h of annealing. Thermoelectric properties in terms of Seebeck coefficient, and electrical conductivity were evaluated and correlated with phase transformation. Seebeck coefficient electrical resistivity and hardness increased with increasing annealing time due to $\beta$ phase transformation.

• 한국세라믹학회지
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• 제39권8호
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• pp.769-774
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• 2002

금속 산화물 상태으 혼합분말을 수소 환원하여 $Al_2O_3$ 분말 표면에 20 nm 크기의 Fe-Ni 합금이 균일하게 분산된 복합분말을 합성하였다. 상압소결을 이용하여 제조한 $Al_2O_3$/Fe-Ni 나노복합재료는 전 소결 온도 범위에서 단지 $Al_2O_3$와 ${gamma}$-Fe-Ni 상만으로 구성되어 있었고, $1350^{\circ}C$ 이상의 소결 온도에서 98% 이상의 치밀화를 이루었다. 최대 파괴강도와 파괴인성은 각각 574 MPa과 3.9 MP$a{\cdot}m1/2$로서 동일한 소결 조건의 순수 $Al_2O_3$ 보다 약 20% 증가하였다. 나노복합재료는 강자성 거동을 보였으며 분산상의 평균 입자 크기가 감소함에 따라 증가된 보자력 값을 나타내었다.

• 한국수소및신에너지학회논문집
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• 제6권1호
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• pp.1-9
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• 1995

$V_{0.9}Ti_{0.1}$ 합금은 많은 양의 수소를 흡수할 수 있으나 KOH 전해질내에서 방전이 되지 않기 때문에 Ni-MH 전지의 음극재료로 사용할 수 없었다. 이와 같은 $V_{0.9}Ti_{0.1}$ 합금을 전해질내에서 수소흡수/방출에 대한 촉매효과를 갖도록 Ni 분말과 소결하였다. Ni 분말과 소결한 모든 시편은 KOH 전해질내에서 10 Cycle 이내에 활성화 되었다. 방전용량은 소결시 첨가된 Ni 분말의 양에 따라 maximum 거동을 보였다. 가장 높은 방전용량을 보여준 전극의 경우는 소결시 첨가된 Ni 분말의 양이 25wt.%이며 그 방전용량은 302mAh/g이었다. SEM과 EDS 그리고 XRD 분석결과 소결시 $VNi_3$가 형성됨을 알 수 있었다. $V_{0.9}Ti_{0.1}$ 합금의 표면에 형성된 $VNi_3$는 전극의 최적방전조건과 밀접한 관련이 있음을 알 수 있었다. Brewer-Engel 이론에 의하면 $VNi_3$는 수소의 evolution에 대한 전기적 촉매효과가 매우 높다고 보고하고 있으며, 이러한 효과는 본 실험결과 교환전류밀도의 증가와 방전시 과전압의 감소로써 나타났다. 본 연구에서는 수소의 저장용량은 크나 KOH 전해질내에서 방전되지 않는 합금을 사용하여 Ni-MH 전지용 음극개발을 하기 위해 Ni분말과 소결하여 합금의 표면을 변화시키는 새로운 방법을 제안하고자 한다.

• The Journal of Advanced Prosthodontics
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• 제4권3호
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• pp.162-169
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• 2012

PURPOSE. Fracture of the veneering material of zirconia restorations frequently occurs in clinical situations. The purpose of this in vitro study was to compare the fracture strengths of zirconia crowns veneered with various ceramic materials by various techniques. MATERIALS AND METHODS. A 1.2 mm, $360^{\circ}$ chamfer preparation and occlusal reduction of 2 mm were performed on a first mandibular molar, and 45 model dies were fabricated in a titanium alloy by CAD/CAM system. Forty-five zirconia copings were fabricated and divided into three groups. In the first group (LT) zirconia copings were veneered with feldspathic porcelain by the layering technique. In the second group (HT) the glass ceramic was heat-pressed on the zirconia coping, and for the third group (ST) a CAD/CAM-fabricated high-strength anatomically shaped veneering cap was sintered onto the zirconia coping. All crowns were cemented onto their titanium dies with Rely $X^{TM}$ Unicem (3M ESPE) and loaded with a universal testing machine (Instron 5583) until failure. The mean fracture values were compared by an one-way ANOVA and a multiple comparison post-hoc test (${\alpha}$= 0.05). Scanning electron microscope was used to investigate the fractured interface. RESULTS. Mean fracture load and standard deviation was $4263.8{\pm}1110.8$ N for Group LT, $5070.8{\pm}1016.4$ for Group HT and $6242.0{\pm}1759.5$ N for Group ST. The values of Group ST were significantly higher than those of the other groups. CONCLUSION. Zirconia crowns veneered with CAD/CAM generated glass ceramics by the sintering technique are superior to those veneered with feldspathic porcelain by the layering technique or veneered with glass ceramics by the heat-pressing technique in terms of fracture strength.