• 제목/요약/키워드: Solid state sintering

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고상연소반응법에 의한 나노텅스텐분말의 합성 (Synthesis of nanometric tungsten powders by solid state combustion method)

  • ;이종현;원창환
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 2003년도 추계학술발표강연 및 논문개요집
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    • pp.93-93
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    • 2003
  • Tungsten and tungsten heavy alloys have widespread application as radiation shielding devices and heavy duty electrical contacts. High density and good room temperature mechanical properties have generated interest in evaluating tungsten and tungsten alloys as kinetic energy penetrators against armor. Nowdays ultra fine-grained tungsten powders are in great interest because higly dense structures can be obtained at low temperature, pressure and lower sintering time. Several physical md chemical methods are available for the synthesis of nanometric metal Powders: ball milling, laser abalation, vapor condensation, chemical precipitation, metallic wire explosion i.e. However production rates of the above mentioned methods are low and further efforts are needed to find out large-scale synthesis methods. From this point of view solid state combustion method ( known as SHS) represents undoubted interest.

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상 안정화제가 $Na^+$-Beta-Alumina 고체 전해질의 상 형성 및 소결밀도에 미치는 영향 (Effect of Phase Stabilizers on the Phase Formation and Sintering Density of $Na^+$-Beta-Alumina Solid Electrolyte)

  • 이기문;이성태;이대한;이상민;임성기
    • 공업화학
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    • 제23권6호
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    • pp.534-538
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    • 2012
  • $ Na^+$-beta-alumina 고체전해질을 고상반응법을 통해 합성하였으며, 두 종류의 안정화제 $Li_2O$와 MgO가 상 형성 및 소결밀도에 미치는 영향을 비교 분석하였다. 합성온도에 따른 ${\beta}/{\beta}^{{\prime}{\prime}}$-alumina 상 분율 분석을 위해, [$Na_2O$] : [$Al_2O_3$] = 1 : 5의 고정된 몰 비에서 하소온도를 $1200{\sim}1500^{\circ}C$로 변화하여, 각각 2 h동안 하소하였다. $Li_2O$를 안정화제로 사용한 경우에는 $1500^{\circ}C$에서 2차 상 전이가 발생해 ${\beta}^{{\prime}{\prime}}$-alumina 상 분율의 증가가 나타났지만, MgO를 첨가했을 때는 하소온도에 관계없이 상 분율이 유지되었다. 또한 disc 형태의 $Na^+$-beta-alumina 샘플을 $1550{\sim}1650^{\circ}C$의 온도에서 각각 30 min 소결한 후 상대 소결밀도, 상 변화 및 미세구조를 분석하였다. $Li_2O$를 안정화제로 사용하였을 때, 소결온도 $1600^{\circ}C$에서 ${\beta}^{{\prime}{\prime}}$-상 분율과 상대밀도가 각각 94.7%와 98%로 가장 높은 값을 나타냈으며, MgO를 안정화제로 사용하였을 경우, 소결온도의 증가에 따라 상대밀도가 크게 증가하는 결과를 보였다.

고상소결에 의한 방사성 희토류산화물의 고화 (Immobilization of Radioactive Rare Earth oxide Waste by Solid Phase Sintering)

  • 안병길;박환서;김환영;이한수;김인태
    • 방사성폐기물학회지
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    • 제8권1호
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    • pp.49-56
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    • 2010
  • Pyroprocessing에 의한 사용후핵연료 처리 과정에서 방사성 희토류 염화물이 포함된 폐용융염이 발생된다. 이러한 폐 용융염 내에 존재하는 방사성 희토류 염화물을 산화물로 침전시켜 회수함으로서 용융염을 재생할 수 있다. 최종적으로 발생되는 방사성 희토류 산화물의 저장과 처분에 적합한 monolithic 고화체를 제조하기 위한 연구를 수행하였다. 본 연구에서는 고상 소결에 의해 붕규산 유리에 의한 고화체 제조, 희토류 산화물을 모나자이트로 합성한 후 붕규산 유리에 의한 고화체 제조를 수행하였다. 또한 zinc titanate 세라믹이 주요성분인 고화 매질(ZIT)을 개발하여 고화체를 제조하였으며 각각의 고화체에 대한 침출 및 물리화학적 특성을 비교 평가하였다. 고상 소결에 의해 제조된 ZIT 매질 고화체는 내 침출성이 크며 밀도가 크고 열전도도가 우수한 특성을 나타내었다.

Sol-Gel법에 의한 Li1.5Al0.5Ti1.5(PO4)3 고체전해질 제조 및 chelating agent의 영향 (Effect of Chelating Agent on Li1.5Al0.5Ti1.5(PO4)3 Particles by Sol-gel Method and Densification)

  • 류성준;최슬기;원종호;양민호
    • 한국분말재료학회지
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    • 제30권5호
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    • pp.394-401
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    • 2023
  • Li1.5Al0.5Ti1.5(PO4)3 (LATP) is considered to be one of the promising solid-state electrolytes owing to its excellent chemical and thermal stability, wide potential range (~5.0 V), and high ionic conductivity (~10-4 S/cm). LATP powders are typically prepared via the sol-gel method by adding and mixing nitrate or alkoxide precursors with chelating agents. Here, the thermal properties, crystallinity, density, particle size, and distribution of LATP powders based on chelating agents (citric acid, acetylacetone, EDTA) are compared to find the optimal conditions for densely sintered LATP with high purity. In addition, the three types of LATP powders are utilized to prepare sintered solid electrolytes and observe the microstructure changes during the sintering process. The pyrolysis onset temperature and crystallization temperature of the powder samples are in the order AC-LATP > CA-LATP > ED-LATP, and the LATP powder utilizing citric acid exhibits the highest purity, as no secondary phase other than LiTi2PO4 phase is observed. LATP with citric acid and acetylacetone has a value close to the theoretical density (2.8 g/cm3) after sintering. In comparison, LATP with EDTA has a low sintered density (2.2 g/cm3) because of the generation of many pores after sintering.

Sintering Effects on Fe/Mo Ordering and Magnetoresistance in Double Perovskite Sr2FeMoO6

  • Kim, J;Park, B.J;Lee, B.W
    • Journal of Magnetics
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    • 제9권1호
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    • pp.9-12
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    • 2004
  • We have investigated sintering effects on Fe/Mo ordering and magnetoresistance (MR) in double perovskite-reflection lines due to $Sr_2FeMoO_6$ (SFMO). Polycrystalline samples have been prepared by the conventional solid-state reaction by sintering in a stream of 5% $H_2/Ar$ gas. All samples are single phase and exhibit a series of superstructurecation ordering at Fe and Mo sites. As sintering temperature increases from 900 to $1300^{\circ}C$, the degree of Fe/Mo ordering increases from 82 to 92%, magnetization (15 K, 7 kOe) increases from 1.6 to 2.7 ${\mu}_B/f.u.,$ and Curie temperature increases at a rate of 4.3 K/% with the increase of Fe/Mo ordering ratio. The magnitude of MR measured at 5 K is 19% for sample prepared at $1000^{\circ}C$ with magnetic fields of 7 kOe. The observed MR is proportional to the square of magnetization indicating that the MR feature in SFMO is explained by the spin-polarized tunneling at grain boundaries.

PLZT(8/65/35) 세라믹스의 소결온도에 따른 유전 및 전기열량 특성 (Dielectric and Electrocaloric Characteristics of PLZT(8/65/35) Ceramics as a Function of Sintering Temperature)

  • 김유석;한종대;류주현;정영호
    • 한국전기전자재료학회논문지
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    • 제29권10호
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    • pp.608-612
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    • 2016
  • In this study, in order to develop relaxor ferroelectric ceramics for refrigeration device application with large electrocaloric effect and low sintering temperature, PLZT(8/65/35) ceramics was fabricated using conventional solid-state method with the variation of sintering temperature ($1,050^{\circ}C$, $1,100^{\circ}C$, $1,200^{\circ}C$). The XRD pattern of all specimens indicated general perovskite structure with secondary phase. From the results of temperature dependence of dielectric constant, the $T_C$ (ferroelectric-paraelectric phase transition temperature) was shifted toward high temperature with increasing sintering temperature. When the specimen was sintered at $1,100^{\circ}C$, the optimal value of ${\Delta}T{\sim}0.349^{\circ}C$ in ambient temperature of $215^{\circ}C$ was appeared. It is considered that PLZT(8/65/35) ceramics possess the possibility of refrigeration device application.

Cu, Zn, Sn, Se 혼합 분말의 소결특성에 미치는 볼밀링 영향 (Effects of Ball Milling Condition on Sintering of Cu, Zn, Sn and Se Mixed Powders)

  • 안종헌;정운화;장윤정;이성헌;김규호
    • 한국분말재료학회지
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    • 제18권3호
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    • pp.256-261
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    • 2011
  • In order to make a $Cu_2ZnSnSe_4$ (CZTSe) sputtering target sintered for solar cell application, synthesis of CZTSe compound by solid state reaction of Cu, Zn, Sn and Se mixed powders and effects of ball milling condition on sinterability such as ball size, combination of ball size, ball milling time and sintering temperature, was investigated. As a result of this research, sintering at $500^{\circ}C$ after ball milling using mixed balls of 1 mm and 3 mm for 72 hours was the optimum condition to synthesis near stoichiometric composition of $Cu_2ZnSnSe_4$ and to prepare sintered pellet with high density relatively.

열처리조건이 두 NASICON 조성의 소결 및 전기적특성에 미치는 영향 (Effects of Heat-treatment Condition on the Characteristics of Sintering and Electrical Behaviors of Two NASICON Compounds)

  • 강희복;조남희;김윤호
    • 한국세라믹학회지
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    • 제34권7호
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    • pp.685-692
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    • 1997
  • Effects of sintering temperature and time on the phase formation, the characteristics of sintering and electrical behaviors of NASICON compounds with Na3Zr2Si2PO12 and Na3.2Zr1.3Si2.2P0.8O10.5 compositions synthesized by solid state reaction were investigated. Maximum relative densities of 96% and 91% were obtained for Na3Zr2Si2PO12 and Na3.2Zr1.3Si2.2P0.8O10.5 compounds, respectively. Complex impedance analysis in a frequency range below 4 MHz was performed to measure the ionic conductivity and migration barrier height of the compounds at RT-30$0^{\circ}C$. The maximum ionic conductivity and the minimum migration barrier height were 0.45 ohm-1cm-1 and 0.07 eV, respectively. The migration barrier height of the high temperature form (space group : R3c) is about 30-40% of that of the low temperature form (space group : C2/c) in two NASICON compounds. Ionic conductivity increases with increasing sinterability, and the presence of glass phase in Na3.2Zr1.3Si2.2P0.8O10.5 compounds lowers significantly ionic conductivity at temperatures above 14$0^{\circ}C$.

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Effect of Nickel Addition on Sintering Behavior and Electrical Conductivity of BaCe0.35Zr0.5Y0.15O3-δ

  • An, Hyegsoon;Shin, Dongwook;Ji, Ho-Il
    • 한국세라믹학회지
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    • 제56권1호
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    • pp.91-97
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    • 2019
  • The effect of different Ni-containing additives on the sintering behavior and electric conductivity of the proton conducting electrolyte $BaCe_{0.35}Zr_{0.5}Y_{0.15}O_{3-{\delta}}$ (BCZY5) was investigated. Ni-doped, NiO-added, and $BaY_2NiO_5$(BYN)-added (all 4 mol%) BCZY5 samples were prepared by the solid state synthesis method and sintered at $1400^{\circ}C$ for 6 h. Among the three samples, the onset of densification was observed at the lowest temperature for NiO-added BCZY5, which is attributed to the formation of an intermediate phase at a low melting temperature. The BYN-added sample, where no consumption of the constitutional elements of the electrolyte was expected during sintering, exhibited the highest electrical conductivity whereas the doped sample had the lowest conductivity. The electrical conductivities at $500^{\circ}C$ under humid argon atmosphere were measured to be 2.0, 4.8, and $6.2mS{\cdot}cm^{-1}$ for Ni-doped and NiO- and BYN-added samples, respectively.

냉간 압축 성형한 Mg3Sb2 열전재료의 고상 반응 소결 (Solid state reactive sintering of cold pressed thermoelectric Mg3Sb2)

  • 김인기;장경욱;오한준
    • 한국결정성장학회지
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    • 제24권4호
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    • pp.176-182
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    • 2014
  • 상온 압축 성형 후 고상 반응 소결 공정을 통하여 $Mg_3Sb_2$ 소결체를 제조하고자 하였다. Mg과 Sb의 성분의 몰비와 반응온도에 따른 결정상의 변화를 조사하였다. 773~843 K에서 얻어진 고상반응 소결체들은 전형적인 $Mg_3Sb_2$ 결정상을 형성하였으나 소결체의 위치에 따라 약간 다른 상적 구성을 보였다. 소결체 하단 부위에서 전형적으로 얻어지는 결정상이 얻어졌으며 823 K 온도에서는 Mg : Sb = 3.15 : 1.85 조성일 때, 843 K 온도에서는 Mg의 몰 수가 3.10 이상인 모든 조성에서 ${\alpha}-Mg_3Sb_2$ 상과 정확히 일치하는 결정상이 얻어졌다. 미량 남아있는 Mg 성분은 응고 후 냉각 시 ${\alpha}-Mg_3Sb_2$ 상으로부터 석출된 것으로 보인다.