• Korean Journal of Materials Research
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• v.24 no.2
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• pp.111-115
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• 2014

Titanium and its alloys are useful for implant materials. In this study, porous Ti-Nb-Zr biomaterials were successfully synthesized by powder metallurgy using a $NH_4HCO_3$ as space holder and $TiH_2$ as foaming agent. Consolidation of powder was accomplished by spark plasma sintering process(SPS) at $850^{\circ}C$ under 30 MPa condition. The effect of high energy milling time on pore size and distribution in Ti-Nb-Zr alloys with space holder($NH_4HCO_3$) was investigated by optical microscope(OM), scanning electron microscope(SEM) & energy dispersive spectroscopy(EDS) and X-ray diffraction(XRD). Microstructure observation revealed that, a lot of pores were uniformly distributed in the Ti-Nb-Zr alloys as size of about $30-100{\mu}m$ using mixed powder and milled powders. In addition, the pore ratio was found to be about 5-20% by image analysis, using an image analyzer(Image Pro Plus). Furthermore, the physical properties of specimens were improved with increasing milling time as results of hardness, relative density, compressive strength and Young's modulus. Particularly Young's modulus of the sintered alloy using 4h milled powder reached 52 GPa which is similar to bone elastic modulus.

• Journal of the Korean Ceramic Society
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• v.51 no.6
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• pp.549-553
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• 2014

$CoSb_3$-based skutterudite compounds are candidate materials for thermoelectric power generation in the mid-temperature range (600 - 900 K) because their thermoelectric properties can be enhanced by doping and filling. The joining property of thermoelectric module electrodes containing thermoelectric materials is of great importance because it can dominate the efficiency of the thermoelectric module. This study examined the properties of $CoSb_3$/Al/Ti/CuMo joined by the spark plasma sintering technique. Titanium thin foil was used to prevent the diffusion of copper into $CoSb_3$ and Aluminum thin foil was used to improve the adhesion between $CoSb_3$ and Ti. The insertion of an Aluminum interlayer between the Ti and $CoSb_3$ was effective for joining $CoSb_3$ to Ti by forming an intermediate layer at the Al-$CoSb_3$ boundary without any micro cracks. Specifically, the adhesion strength of the Ti/Al/$CoSb_3$ joining interface showed a remarkable improvement compared with our previous results, without deterioration of electrical property in the interface.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.08a
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• pp.237.1-237.1
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• 2013

Ti 와 Al 은 금속간의 화합물이 내산화성에 우수한 성질을 가지고 있으며 낮은 밀도와 고온에도 큰 변화가 없는 성질을 가지고 있다. 그리하여 내식 및 부식 관련 연구나 고온재료를 필요로 하는 우주, 엔진 제품 등에 많은 연구가 진행되고 있다. 또한 Ti-Al-N 박막은 경도가 우수하여 고속 공구 부품에 널리 사용되고 있으며 최근 Ti-Al-N 에 Si 첨가로 인하여 40 GPa 이상의 고경도와 1,000도 이상의 산화온도를 지닌 나노 혼합물 코팅을 형성 시키는 것으로 알려져 있다. 본 연구에서는 Ti, Al, Si 원분말을 PBM (Planetary Ball Milling) 방법을 사용하여 Ti-Al-Si 혼합분말로 제조하고, 제조된 분말들은 SPS (Spark Plasma Sintering) 공정을 통하여 Ti-Al-Si 합금타겟을 제작하였다. 제작된 Ti-Al-Si 합급타겟을 사용한 Sputtering 공정을 수행하여 Ti-Al-Si 3원계 박막을 증착하였다. 그 결과 기존 Ti (82 ${\mu}m$), Al (32 ${\mu}m$), Si (16 ${\mu}m$) 크기의 원분말들이 PBM (Planetary Ball Milling) 공정 후 Ti-Al-Si (18 ${\mu}m$) 로 입도가 작아진 것을 확인 할 수 있었고, 소결 후 타겟이 99% 이상의 높은 밀도를 가졌으며 원분말의 조성과 동일한 조성을 가진 타겟이 제작되었음을 확인하였다. Ti-Al-Si 타겟의 경도는 약 1,000 Hv 이상의 값을 보였으며, Ti-Al-Si-N 박막의 경우 타겟의 조성과 동일하였고 경도는 약 35 GPa 로 높은 경도 값을 가지는 것을 확인하였다. 내산화 테스트 결과 Ti-Al-Si-N 박막은 1,000도 에서도 박막의 손상이 가지 않았다.

• Journal of Powder Materials
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• v.26 no.4
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• pp.299-304
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• 2019

Nb-Si-B alloys with Nb-rich compositions are fabricated by spark plasma sintering for high-temperature structural applications. Three compositions are selected: 75 at% Nb (Nb0.7), 82 at% Nb (Nb1.5), and 88 at% Nb (Nb3), the atomic ratio of Si to B being 2. The microstructures of the prepared alloys are composed of Nb and $T_2$ phases. The $T_2$ phase is an intermetallic compound with a stoichiometry of $Nb_5Si_{3-x}B_x$ ($0{\leq}x{\leq}2$). In some previous studies, Nb-Si-B alloys have been prepared by spark plasma sintering (SPS) using Nb and $T_2$ powders (SPS 1). In the present work, the same alloys are prepared by the SPS process (SPS 2) using Nb powders and hypereutectic alloy powders with composition 67at%Nb-22at%Si-11at%B (Nb67). The Nb67 alloy powders comprise $T_2$ and eutectic ($T_2+Nb$) phases. The microstructures and hardness of the samples prepared in the present work have been compared with those previously reported; the samples prepared in this study exhibit finer and more uniform microstructures and higher hardness.

• Current Applied Physics
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• v.18 no.12
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• pp.1540-1545
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• 2018

SiGe alloy is widely used thermoelectric materials for high temperature thermoelectric generator applications. However, its high thermoelectric performance has been thus far realized only in alloys synthesized employing mechanical alloying techniques, which are time-consuming and employ several materials processing steps. In the current study, for the first time, we report an enhanced thermoelectric figure-of-merit (ZT) ~ 1.1 at $900^{\circ}C$ in ntype $Si_{80}Ge_{20}$ nano-alloys, synthesized using a facile and up-scalable methodology consisting of rapid solidification at high optimized cooling rate ${\sim}3.4{\times}10^7K/s$, employing melt spinning followed by spark plasma sintering of the resulting nano-crystalline melt-spun ribbons. This enhancement in ZT > 20% over its bulk counterpart, owes its origin to the nano-crystalline microstructure formed at high cooling rates, which results in crystallite size ~7 nm leading to high density of grain boundaries, which scatter heat-carrying phonons. This abundant scattering resulted in a very low thermal conductivity ${\sim}2.1Wm^{-1}K^{-1}$, which corresponds to ~50% reduction over its bulk counterpart and is amongst the lowest reported thus far in n-type SiGe alloys. The synthesized samples were characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy, based on which the enhancement in their thermoelectric performance has been discussed.

• Korean Journal of Materials Research
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• v.31 no.7
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• pp.392-396
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• 2021

Expensive PCBN or ceramic cutting tools are used for processing of difficult-to-cut materials such as Ti and Ni alloy materials. These tools have the problem of breaking easily due to their high hardness but low fracture toughness. To solve these problems, cutting tools that form various coating layers are used in low-cost WC-Co hard material tools, and research on various tool materials is being conducted. In this study, binderless-WC, WC-6 wt%Co, WC-6 wt%Co-1 wt% Mo₂C, and WC-6 wt%Co-2.5 wt% Mo₂C hard materials are densified using horizontal ball milled WC-Co, WC-Co-Mo₂C powders, and spark plasma sintering process (SPS process). Each SPSed Binderless-WC, WC-6 wt%Co-1 wt% Mo₂C, and WC-6 wt%Co-2.5 wt% Mo₂C hard materials are almost completely dense, with relative density of up to 99.5 % after the simultaneous application of pressure of 60 MPa and almost no significant change in grain size. The average grain sizes of WC for Binderless-WC, WC-6 wt%Co-1 wt% Mo₂C, and WC-6 wt%Co-2.5 wt% Mo₂C hard materials are about 0.37, 0.6, 0.54, and 0.43 ㎛, respectively. Mechanical properties, microstructure, and phase analysis of SPSed Binderless-WC, WC-6 wt%Co-1 wt% Mo₂C, and WC-6 wt%Co-2.5 wt% Mo₂C hard materials are investigated.

• Journal of Powder Materials
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• v.29 no.3
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• pp.219-225
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• 2022

An alternative fabrication method for carburizing steel using spark plasma sintering (SPS) is investigated. The sintered carburized sample, which exhibits surface modification effects such as carburizing, sintered Fe, and sintered Fe-0.8 wt.%C alloys, is fabricated using SPS. X-ray diffraction and micro Vickers tests are employed to confirm the phase and properties. Finite element analysis is performed to evaluate the change in hardness and analyze the carbon content and residual stress of the carburized sample. The change in the hardness of the carburized sample has the same tendency to predict hardness. The difference in hardness between the carburized sample and the predicted value is also discussed. The carburized sample exhibits a compressive residual stress at the surface. These results indicate that the carburized sample experiences a surface modification effect without carburization. Field emission scanning electron microscopy is employed to verify the change in phase. A novel fabrication method for altering the carburization is successfully proposed. We expect this fabrication method to solve the problems associated with carburization.

• Nuclear Engineering and Technology
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• v.53 no.7
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• pp.2289-2294
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• 2021

In the present study, an original spark plasma sintering-reactive synthesis (SPS-RS) method for minerallike ceramic materials based on SrAl₂Si₂O₈ feldspar-like skeleton structure was used for the first time, promising solid-state matrices for reliable immobilization of high-energy ⁹⁰Sr. The method is based on the "in-situ" reaction of a mixture of SrO, Al₂O₃ and SiO₂ oxides when heated by a unipolar pulsed current under compacting pressure. The phase and elemental composition structure were studied. The dynamics of the consolidation of the reaction mixture of oxides was studied in the range of 900-1200 ℃. The study found the temperature of the high-speed (minutes) SPS-RS formation of single-phase SrAl₂Si₂O₈ composition ceramic in the absence of intermediate reaction products with a relative density of up to 99.2% and compressive strength up to 145 MPa and a strontium leaching rate of 10^-4g/cm²·day.

• Nuclear Engineering and Technology
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• v.53 no.8
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• pp.2582-2590
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• 2021

The high-energy milling is one of the most extended techniques to produce Oxide dispersion strengthened (ODS) powder steels for nuclear applications. The consequences of the high energy mill process on the final powders can be measured by means of deformation level, size, morphology and alloying degree. In this work, an ODS ferritic steel, Fe-14Cr-5Al-3W-0.4Ti-0.25Y₂O₃-0.6Zr, was fabricated using two different mechanical alloying (MA) conditions (M_std and M_act) and subsequently consolidated by Spark Plasma Sintering (SPS). Milling conditions were set to evidence the effectivity of milling by changing the revolutions per minute (rpm) and dwell milling time. Differences on the particle size distribution as well as on the stored plastic deformation were observed, determining the consolidation ability of the material and the achieved microstructure. Since recrystallization depends on the plastic deformation degree, the composition of each particle and the promoted oxide dispersion, a dual grain size distribution was attained after SPS consolidation. M_act showed the highest areas of ultrafine regions when the material is consolidated at 1100 ℃. Microhardness and small punch tests were used to evaluate the material under room temperature and up to 500 ℃. The produced materials have attained remarkable mechanical properties under high temperature conditions.

• Nuclear Engineering and Technology
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• v.56 no.7
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• pp.2584-2594
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• 2024

A novel approach to incorporating oxide formers into ferritic ODS production has been developed using the co-precipitation technique. This method enables the tailored design of complex nano-oxides, integrated during Mechanical Alloying (MA) and precipitated during Spark Plasma Sintering (SPS) consolidation. Findings illustrate that co-precipitation effectively produces nano-powders with customised compositions, enriching Y, Ti, and Zr in the ferritic grade to condition subsequent oxide precipitation. While the addition of Y-Ti-Zr-O nano-oxides did not prevent the formation of Y-Al-O and Al-containing nano-oxides, these were refined thanks to the presence of well-dispersed Zr. Additionally, the Spark Plasma Sintering (SPS) parameters were optimised to tailor the bimodal grain size distribution of the ODS steels, aiming for favourable strength-to-ductility ratios. Comprehensive microstructural analyses were performed using SEM, EDS, EBSD, and TEM techniques, alongside mechanical assessments involving microtensile tests conducted at room temperature and small punch tests carried out at room temperature, 300 ℃, and 500 ℃. The outcomes yielded promising findings, showcasing similar or better performance with conventionally manufactured ODS steels. This reinforces the effectiveness and success of this innovative approach.