• Title/Summary/Keyword: Vacuum annealing

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Development of the Ag/Cu Ingots for Mokumegane Jewelry (모꾸메가네 장신구를 위한 은/동 접합 잉곳 소재 개발)

  • Song, Oh-Sung;Kim, Jong-Ryul;Kim, Myung-Ro
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.9 no.1
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    • pp.9-15
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    • 2008
  • Mokumegane is one of the sophisticated metal craft techniques enabling wood grain surface effect. To embody the mokumegane, an ingot of well-bonded stacked metal plates has been required. Traditionally prepared mokumegane ingots were bonded using charcoal which enables reduction atmosphere, but sometimes end up with collapse of bonding interface due to the lack of reliable process control. We proposed a systematic vacuum direct bonding process for ingots. First, we confirmed copper//copper homogeneous plate bonding at $900^{\circ}C$ by applying uniaxial press of 2.5kg. We observed 80min required to obtain 90%-bonding ratio and the diffusion coefficient would be enhanced up to 100 times due to surface effect. Second, by considering enhanced diffusion behavior, we also obtained optimum bonding condition in copper/silver heterogeneous plates that ensures 90%-bonding ratio at $700^{\circ}C$ for 10min with apply uniaxial press. A 7-layered copper/silver ingot is prepared successfully, and eventually the prototype mokumegane cases for mobile phone were fabricated with these ingot.

Manufacturing of Cu Repair Coating Material Using the Kinetic Spray Process and Changes in the Microstructures and Properties by Heat Treatment (Kinetic spray 공정을 이용한 Cu repair 코팅 소재 제조 및 열처리에 따른 미세조직과 물성 변화)

  • Jeon, Min-Gwang;Kim, Hyung-Jun;Lee, Kee-Ahn
    • Journal of Powder Materials
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    • v.21 no.5
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    • pp.349-354
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    • 2014
  • This study is a basic research for repair material production which manufactured a Cu repair coating layer on the base material of a Cu plate using kinetic spray process. Furthermore, the manufactured material underwent an annealing heat treatment, and the changes of microstructure and macroscopic properties in the Cu repair coating layer and base material were examined. The powder feedstocks were sphere-shaped pure Cu powders with an average size of $27.7{\mu}m$. The produced repair coating material featured $600{\mu}m$ thickness and 0.8% porosity, and it had an identical ${\alpha}$-Cu single phase as the early powder. The produced Cu repair coating material and base material displayed extremely high adhesion characteristics that produced a boundary difficult to identify. Composition analysis confirmed that the impurities in the base material and repair coating material had no significant differences. Microstructure observation after a $500^{\circ}C/1hr$. heat treatment (vacuum condition) identified recovery, recrystallization and grain growth in the repair coating material and featured a more homogeneous microstructure. The hardness difference (${\Delta}H_v$) between the repair coating material and base material significantly reduced from 87 to 34 after undergoing heat treatment.

X-ray Scattering Study of Reactive Sputtered Ta-N/Ta/Si(001)Film as a Barrier Metal for Cu Interconnection (구리배선용 베리어메탈로 쓰이는 Ta-N/Ta/Si(001)박막에 관한 X-선 산란연구)

  • Kim, Sang-Soo;Kang, Hyon-Chol;Noh, Do-Young
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2001.05b
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    • pp.79-83
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    • 2001
  • In order to compare the barrier properties of Ta-N/Si(001) with those of Ta-N/Ta/Si(001), we studied structural properties of films grown by RF magnetron sputtering with various $Ar/N_2$ ratios. To evaluate the barrier properties, the samples were annealed in a vacuum chamber. Ex-situ x-ray scattering measurements were done using an in-house x-ray system. With increasing nitrogen ratio in Ta-N/Si(001), the barrier property of Ta-N/Si(001) was enhanced, finally failed at $750^{\circ}C$ due to the crystallization and silicide formation. Compared with Ta-N/Si(001), Ta-N/Ta/Si(001) forms silicides at $650^{\circ}C$. However it does not crystallize even at $750^{\circ}C$. With increasing nitrogen composition in Ta-N/Ta/Si(001), the formation of tantalum silicide was reduced and the surface roughness was improved. To observe the surface morphology of Ta-N/Ta/Si(001) during annealing, we performed an in-situ x-ray scattering experiment using synchrotron radiation of the 5C2 at Pohang Light Source(PLS). Addition of Ta layer between Ta-N and Si(001) improved the surface morphology and reduced the surface degradation at high temperatures. In addition, increasing $N_2/Ar$ flow ratio reduced the formation of tantalum silicide and enhanced the barrier properties.

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Thermoelectric Properties of Co1-xNbxSb3 Prepared by Induction Melting (유도용해법으로 제조된 Co1-xNbxSb3의 열전특성)

  • Park J.B.;You S.W.;Cho K.W.;Jang K.W.;Lee J.I.;Ur S.C.;Kim I.H.
    • Korean Journal of Materials Research
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    • v.15 no.2
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    • pp.89-92
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    • 2005
  • The induction melting was employed to prepare Nb-doped $CoSb_3$ skutterudites and their thermoelectric properties were investigated. Single phase $\delta-CoSb_3$ was successfully obtained by induction melting and subsequent annealing at $400^{\circ}C$ for 2 hrs in vacuum. The positive signs of Seebeck coefficients for all the specimens revealed that Nb atoms acted as p-type dopants by substituting Co atoms. Electrical conductivity decreased and then increased with increasing temperature, indicating mixed conduction behavior. Electrical conductivity increased by Nb doping, and it was saturated at high temperature. Maximum value of the thermoelectric power factor was shifted to higher temperature with increasing the amount of Nb doping, mainly originated from the high Seebeck coefficient around mixed conduction temperature and high electrical conductivity.

Electrical and Mechanical Properties of Cu(Mg) Film for ULSI Interconnect (고집적 반도체 배선용 Cu(Mg) 박막의 전기적, 기계적 특성 평가)

  • 안재수;안정욱;주영창;이제훈
    • Journal of the Microelectronics and Packaging Society
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    • v.10 no.3
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    • pp.89-98
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    • 2003
  • The electrical and mechanical properties of sputtered Cu(Mg) films are investigated for highly reliable interconnects. The roughness, adhesion, hardness and resistance to thermal stress of Cu(Mg) film annealed in vacuum at $400^{\circ}C$ for 30min were improved than those of pure Cu film. Moreover, the flat band voltage(V$_{F}$ ) shift in the Capacitance-Voltage(C-V) curve upon bias temperature stressing(BTS) was not observed and leakage currents of Cu(Mg) into $SiO_2$ were three times less than those of pure Cu. Because Mg was easy to react with oxide than Cu and Si after annealing, the Mg Oxide which formed at surface and interface served as a passivation layer as well.

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Effects of Carbon Nitride Surface Layers and Thermal Treatment on Field-Emission and Long-Term Stability of Carbon Nanotube Micro-Tips (질화탄소 표면층 및 열처리가 탄소 나노튜브 미세팁의 전계방출 및 장시간 안정성에 미치는 영향)

  • Noh, Young-Rok;Kim, Jong-Pil;Park, Jin-Seok
    • Journal of the Semiconductor & Display Technology
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    • v.9 no.1
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    • pp.41-47
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    • 2010
  • The effects of thermal treatment on CNTs, which were coated with a-$CN_x$ thin film, were investigated and related to variations of chemical bonding and morphologies of CNTs and also properties of field emission induced by thermal treatment. CNTs were directly grown on nano-sized conical-type tungsten tips via the inductively coupled plasma-chemical vapor deposition (ICP-CVD) system, and a-$CN_x$ films were coated on the CNTs using an RF magnetron sputtering system. Thermal treatment on a-$CN_x$ coated CNT-emitters was performed using a rapid thermal annealing (RTA) system by varying temperature ($300-700^{\circ}C$). Morphologies and microstructures of a-$CN_x$/CNTs hetero-structured emitters were analyzed by FESEM and HRTEM. Chemical composition and atomic bonding structures were analyzed by EDX, Raman spectroscopy, and XPS. The field emission properties of the a-$CN_x$/CNTs hetero-structured emitters were measured using a high vacuum (below $10^{-7}$ Torr) field-emission measurement system. For characterization of emission stability, the fluctuation and degradation of the emission current were monitored in terms of operation time. The results were compared with a-$CN_x$ coated CNT-emitters that were not thermally heated as well as with the conventional non-coated CNT-emitters.

Effect of NbC Carbide Addition on Mechanical Properties of Matrix-Type Cold-Work Tool Steel (매트릭스(matrix)형 냉간금형강의 기계적 특성에 미치는 NbC 탄화물 첨가의 영향)

  • Kang, Jun-Yun;Kim, Hoyoung;Son, Dongmin;Lee, Jae-Jin;Yun, Hyo Yun;Lee, Tae-Ho;Park, Seong-Jun;Park, Soon Keun
    • Journal of the Korean Society for Heat Treatment
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    • v.28 no.5
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    • pp.239-249
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    • 2015
  • Various amount of NbC carbide was intentionally formed in a matrix-type cold-work tool steel by controlled amount of Nb and C addition. And the effect of NbC addition on the mechanical properties was investigated. Four alloys with different Nb and C contents were cast by vacuum induction melting, then hot forging and spheroidizing annealing were conducted. The machinability of the annealed specimens was examined with 3 different cutting tools. And tensile tests at room temperature were conducted. After quenching and tempering, hardness and impact toughness were measured, while wear resistance was evaluated by disk-on-plate type wear test. The increasing amount of NbC addition resulted in degraded machinability with increased strength, whereas the absence of NbC also led to poor machinability due to high toughness. After quenching and tempering, the additional NbC improved wear resistance with increasing hardness, whereas it deteriorated impact toughness. Therefore, it could be found that a moderate addition of NbC was desirable for the balanced combination of mechanical properties.

Magnetic Properties of YBCO Superconductor Bulk Materials (YBCO 초전도체 Bulk 소재에 대한 자기적 특성)

  • Lee, Sang-Heon
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.33 no.2
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    • pp.147-150
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    • 2020
  • Relatively pure YBCO was first synthesized by heating a mixture of metal carbonates at temperatures between 1,000 and 1,300 K, resulting in the reaction: 4BaCO3+Y2(CO3)3+6CuCO3+(1/2-x)O2 → 2YBa2Cu3O7-x+1/3CO2. Modern syntheses of YBCO use the corresponding oxides and nitrates. The superconducting properties of YBa2Cu3O7-x are sensitive to the value of x, i.e., its oxygen content. Only those materials with 0≤x≤0.65 are superconducting below Tc, and when x ~ 0.07, the material superconducts at the highest temperature, i.e., 95 K, or in the highest magnetic fields, i.e., 120 T and 250 T when B is perpendicular and parallel to the CuO2 planes, respectively. In addition to being sensitive to the stoichiometry of oxygen, the properties of YBCO are influenced by the crystallization methods applied. YBCO is a crystalline material, and the best superconductive properties are obtained when crystal grain boundaries are aligned by careful control of annealing and quenching temperature rates. However, these alternative methods still require careful sintering to produce a quality product. New possibilities have arisen since the discovery of trifluoroacetic acid, a source of fluorine that prevents the formation of undesired barium carbonate (BaCO3). This route lowers the temperature necessary to obtain the correct phase at around 700℃. This, together with the lack of dependence on vacuum, makes this method a very promising way to achieve a scalable YBCO bulk.

Purification of Si using Catalytic CVD

  • Jo, Chul-Gi;Lee, Kyeong-Seop;Song, Min-Wu;Kim, Young-Soon;Shin, Hyung-Shik
    • 한국신재생에너지학회:학술대회논문집
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    • 2009.11a
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    • pp.383-383
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    • 2009
  • Silicon is commercially prepared by the reaction of high-purity silica with wood, charcoal, and coal, in an electric arc furnace using carbon electrodes, so called the metallurgical refining process, which produces ~98% pure Si (MG-Si). This can be further purified to solar grade silicon (SoG-Si) by various techniques. The most problematic impurity elements are B and P because of their high segregation coefficients. In this study, we explored the possibility of the using Cat-CVD for Si purification. The existing hot-wire CVD was modified to accommodate the catalyzer and the heating source. Mo boat (1.5 cm ${\times}$ 1 cm ${\times}$ 0.2 cm) was used as a heating source. Commercially available Si was purchased from Nilaco corporation (~99% pure). This powder was kept in the Mo-boat and heated to the purification temperature. In addition to the purification by cat-CVD technique, other methods such as thermal CVD, plasma enhanced CVD, vacuum annealing was also tried. It is found that the impurities are reduced to a great extent when treated with cat-CVD method.

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Electronic Structure of Ce-doped ZrO2 Film: Study of DFT Calculation and Photoelectron Spectroscopy

  • Jeong, Kwang Sik;Song, Jinho;Lim, Donghyuck;Kim, Hyungsub;Cho, Mann-Ho
    • Applied Science and Convergence Technology
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    • v.25 no.1
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    • pp.19-24
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    • 2016
  • In this study, we evaluated the change of electronic structure during redox process in cerium-doped $ZrO_2$ grown by sol gel method. By sol-gel method, we could obtain cerium-doped $ZrO_2$ in high oxygen partial pressure and low temperature. After post annealing process in nitrogen ambient, the film is deoxidized. We used spectroscopic and theoretical methods to analysis change of electronic structure. X-ray absorption spectroscopy (XAS) for O K1-edge and Density Functional Theory (DFT) calculation using VASP code were performed to verify the electronic structure of the film. Also, high resolution x-ray photoelectron spectroscopy (HRXPS) for Ce 3d was carried out to confirm chemical bond of cerium doped $ZrO_2$. Through the investigation of the electronic structure, we verified as followings. (1) During reduction process, binding energy of oxygen is increase. Simultaneously, oxidation state of cerium was change to 4+ to 3+. (2) Cerium 4+ and cerium 3+ states were generated at different energy level. (3) Absorption states in O K edge were mainly originated by Ce 4+ $f_0$ and Ce 3+, while occupied states in valance band were mainly originated from Ce 4+ $f_2$.