• Title/Summary/Keyword: Solid state sintering

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Initial Sintering Behaviour of the Powder Injection Molded W-15wt%Cu Nanocomposite Powder (분말사출성형한 W-l5wt%Cu 나노복합분말의 초기소결거동)

  • 윤의식;유지훈;이재성
    • Journal of Powder Materials
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    • v.5 no.4
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    • pp.258-264
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    • 1998
  • The initial sintering behaviour of the powder injection molded (PIMed) W-l5wt%Cu nanocomposite powder was investigated. The W-Cu nanocomposite powder was produced by the mechanochemical process consisting of high energy ball-milling and hydrogen reduction of W blue powder-CuO mixture. Solid state sintering of the powder compacts was conducted at $1050^{\circ}C$ for 2~10 hours in hydrogen at mosphere. The sintering behaviour was examined and discussed in terms of microstructural developments such as W-Cu aggregate formation, pore size distribution and W grain growth. The volume shrinkage of PIM specimen was slightly larger than that of PM(conventional PM specimen), being due to fast local densification in the PIM. Remarkable decrease of carbon and oxygen in the PIM enhanced local densification in the early stage of solid state sintering process with eliminating very fine pores less than 10 nm. In addition, such local densiflcation in the PIM is presumably responsible for mitigating of W-grain growth in the initial stage.

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Various Master Sintering Curve Concepts and its Applications

  • Park, Seong-Jin;Blaine, Deborah C.;German, Randall M.
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2006.09a
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    • pp.66-67
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    • 2006
  • The master sintering curve (MSC) is derived from densification data over a range of heating rates and temperatures. To improve the accuracy, several modifications were proposed: multi-phase MSC for solid state sintering with phase changes, MSC for liquid phase sintering, and MSC with consideration of grain growth. The developed MSC models were applied to several material systems such as molybdenum, stainless steels, and tungsten heavy alloys (WHA), in order to evaluate the effect of compaction pressure, phase change, grain growth, and composition on densification, to classify regions having different sintering mechanism, and to help engineer design, optimize, and monitor sintering cycles.

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Electrical Properties of Rosen Type piezoelectric transformers using Low Temperature Sintering PMN-PNN-PZT ceramics (저온소결 PMN-PNN-PZT계 세라믹스를 이용한 Rosen형 압전변압기의 전기적 특성)

  • Lee, Sang-Ho;Yoo, Ju-Hyun;Kim, In-Sung;Song, Jae-Sung
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.53-53
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    • 2008
  • Piezoelectric transformers have been widely used such as DC-DC convertor, invertor, Ballast, etc. Because, the y have some merits compared with electro-magnetic transformers such as step-up ratio, high efficiency, small size and lg hit weight, etc. Piezoelectric transformer require high electromechanical coupling factor kp in order to induce a large out put power in proportional to applied electric field. And also, high mechanical quality factor Qm is required to prevent mechanical loss and heat generation. In general, PZT system ceramics should be sintered at high temperatures between 1200 and $1300^{\circ}C$ in order to obtain complete densification. Accordingly, environmental pollution due to its PbO evaporation. Hence, to reduce its sintering temperature, various kinds of material processing methods such as hot pressing, high energy mill, liquid phase sintering, and using ultra fine powder have been performed. Among these methods, liquid phase sintering is basically an effective method for aiding densification at low temperature. In this study, In order to comparis on low temperature sintering and solid state sintering piezoelectric transformers, rosen type transformers were fabricated u sing two PZT ceramics compositions and their electrical properties were investigated.

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Solid State Sintering of Calcium Phosphate Ceramic Composites and Their Cellular Response

  • Cho, Yeong-Cheol;Kong, Young-Min;Riu, Doh-Hyung
    • Korean Journal of Metals and Materials
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    • v.50 no.9
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    • pp.691-695
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    • 2012
  • Calcium phosphate ceramic composites, consisting of hydroxyapatite(HA) and tricalcium phosphate (TCP), were fabricated by solid state sintering in order to investigate the effect of their initial compositions on microstructural evolutions and biocompatibility. All the sintered calcium phosphate ceramics exhibited almost full densification, while the grain growth of the composites increased with an increasing TCP content in the green body. The TCP phase transformed into a Ca-deficient HA phase during sintering via the diffusion of calcium ions from the HA phase into the TCP phase. The phases formed in the composites significantly affected the biocompatibility of the composites. The HA-matrix ceramic composites with TCP had a better cellular response than the pure HA ceramics, presumably due to the newly formed Ca-deficient HA.

Influence of Ga Content on the Ionic Conductivity of Li1+XGaXTi2-X(PO4)3 Solid-State Electrolyte Synthesized by the Sol-Gel Method

  • Seong-Jin Cho;Jeong-Hwan Song
    • Korean Journal of Materials Research
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    • v.34 no.4
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    • pp.185-193
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    • 2024
  • In this study, NASICON-type Li1+XGaXTi2-X(PO4)3 (x = 0.1, 0.3 and 0.4) solid-state electrolytes for all-solid-state batteries were synthesized through the sol-gel method. In addition, the influence on the ion conductivity of solid-state electrolytes when partially substituted for Ti4+ (0.61Å) site to Ga3+ (0.62Å) of trivalent cations was investigated. The obtained precursor was heat treated at 450 ℃, and a single crystalline phase of Li1+XGaXTi2-X(PO4)3 systems was obtained at a calcination temperature above 650 ℃. Additionally, the calcinated powders were pelletized and sintered at temperatures from 800 ℃ to 1,000 ℃ at 100 ℃ intervals. The synthesized powder and sintered bodies of Li1+XGaXTi2-X(PO4)3 were characterized using TG-DTA, XRD, XPS and FE-SEM. The ionic conduction properties as solid-state electrolytes were investigated by AC impedance. As a result, Li1+XGaXTi2-X(PO4)3 was successfully produced in all cases. However, a GaPO4 impurity was formed due to the high sintering temperatures and high Ga content. The crystallinity of Li1+XGaXTi2-X(PO4)3 increased with the sintering temperature as evidenced by FE-SEM observations, which demonstrated that the edges of the larger cube-shaped grains become sharper with increases in the sintering temperature. In samples with high sintering temperatures at 1,000 ℃ and high Ga content above 0.3, coarsening of grains occurred. This resulted in the formation of many grain boundaries, leading to low sinterability. These two factors, the impurity and grain boundary, have an enormous impact on the properties of Li1+XGaXTi2-X(PO4)3. The Li1.3Ga0.3Ti1.7(PO4)3 pellet sintered at 900 ℃ was denser than those sintered at other conditions, showing the highest total ion conductivity of 7.66 × 10-5 S/cm at room temperature. The total activation energy of Li-ion transport for the Li1.3Ga0.3Ti1.7(PO4)3 solid-state electrolyte was estimated to be as low as 0.36 eV. Although the Li1+XGaXTi2-X(PO4)3 sintered at 1,000 ℃ had a relatively high apparent density, it had less total ionic conductivity due to an increase in the grain-boundary resistance with coarse grains.

Effect of Li3BO3 Additive on Densification and Ion Conductivity of Garnet-Type Li7La3Zr2O12 Solid Electrolytes of All-Solid-State Lithium-Ion Batteries

  • Shin, Ran-Hee;Son, Sam-Ick;Lee, Sung-Min;Han, Yoon Soo;Kim, Yong Do;Ryu, Sung-Soo
    • Journal of the Korean Ceramic Society
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    • v.53 no.6
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    • pp.712-718
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    • 2016
  • In this study, we investigate the effect of the$Li_3BO_3$ additive on the densification and ionic conductivity of garnet-type $Li_7La_3Zr_2O_{12}$ solid electrolytes for all-solid-state lithium batteries. We analyze their densification behavior with the addition of $Li_3BO_3$ in the range of 2-10 wt.% by dilatometer measurements and isothermal sintering. Dilatometry analysis reveals that the sintering of $Li_7La_3Zr_2O_{12}-Li_3BO_3$ composites is characterized by two stages, resulting in two peaks, which show a significant dependence on the $Li_3BO_3$ additive content, in the shrinkage rate curves. Sintered density and total ion conductivity of the system increases with increasing $Li_3BO_3$ content. After sintering at $1100^{\circ}C$ for 8 h, the $Li_7La_3Zr_2O_{12}-8$ wt.% $Li_3BO_3$ composite shows a total ionic conductivity of $1.61{\times}10^{-5}Scm^{-1}$, while that of the pure $Li_7La_3Zr_2O_{12}$ is only $5.98{\times}10^{-6}Scm^{-1}$.

Low Temperature Sintering of $Mg_{3-x}Co_x(VO_4)_2$ Microwave Dielectric Ceramics for LTCC Applications (저온소결 $Mgx_{-3}Cox(VO_4)_2$ 세라믹스의 마이크로파 유전특성)

  • Lee, Ji-Hun;Bang, Jae-Cheol
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2005.11a
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    • pp.220-223
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    • 2005
  • We studied the effect of composition, processing, and sintering temperature on the microwave properties of $Mg_{3-x}Co_x(VO_4)_2$ system which is applicable to LTCC. When $Mg_{3-x}Co_x(VO_4)_2$ was fabricated by solid-state reaction process and sintered at the temperature range of $800\sim910^{\circ}C$, it was found that the optimum composition of x was 2 at which microwave properties of 910$^{\circ}C$-sintered one were as follows: $Q\times f_0\sim55,200GHz$ and $\varepsilon_r\sim10$. When $(MgCo_2)(VO_4)_2$ was fabricated by sol-gel process and sintered at 800$^{\circ}C$, $Q\timesf_0$was 34,400GHz which is much high compared to those fabricated by solid-state reaction process at the same sintering temperature.

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Microwave Dielectric Properties of Low-temperature Sintered $MgCo_2(VO_4)_2$ Ceramics Synthesized by Sol-Gel process (졸-겔 공정에 의해 제조된 저온소결 $MgCo_2(VO_4)_2$ 세라믹스의 마이크로파 유전특성)

  • Lee, Ji-Hun;Bang, Jae-Cheol
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2006.06a
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    • pp.288-289
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    • 2006
  • We studied the effect of sol-gel processing and sintering temperature on the microwave properties of $MgCo_2(VO_4)_2$ system(MCV) which is applicable to LTCC(low-temperature cofired ceramics). The MCV was synthesized by sol-gel process using solution that contains precursor molecules for Mg, Co, and V. SEM analysis shows that the average particle size is ${\sim}1{\mu}m$ and size distribution is very uniform compared to the one prepared by conventional solid-state reaction process. Highly dense samples were obtained at the sintering temperature range of $750^{\circ}C{\sim}930^{\circ}C$. The maximum $Q{\times}f_0$ value of 55,700GHz, dielectric constant(${\varepsilon}_r$) of 10.41 and temperature coefficient(${\tau}_f$) of $-85ppm/^{\circ}C$ was obtained at the sintering temperature of $930^{\circ}C$. The superior microwave properties of sol-gel processed MCV relative to conventional solid-state reaction processed one is remarkable especially at lower sintering temperatures such as $750^{\circ}C$ and $800^{\circ}C$.

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Synthesis of Ultrafine LaAlO$_3$ Powders with Good Sinterability by Self-Sustaining Combustion Method Using (Glycine+Urea) Fuel ((Glycine+Urea) 혼합연료를 이요한 자발착화 연소반응법에 의한 우수한 소결성의 초미분체 LaAlO$_3$ 분말 합성)

  • Nam, H.D.;Choi, W.S.;Lee, B.H.;Park, S.
    • Journal of the Korean Ceramic Society
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    • v.36 no.2
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    • pp.203-209
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    • 1999
  • LaAlO3d single phase used as the butter layer on Si wafer for YBa2Cu3O7-$\delta$ superconductor application were prepared by solid state reaction method and by self-sustaining combustion process. The microstructure and crystallity of synthesiszed LaAlO3 powder studied using scanning electron microscope (SEM) and X-ray diffractometer(XRD), specific surface area and sintering characteristics fo powder were investigated by Brunauer-Emmett-Teller (BET) method and dilatometer respectively. In solid state reaction method, it is difficult to obtain LaAlO3 single phase up to 150$0^{\circ}C$ period. However, in self-sustaining combustion process, it is to easy to do it only $650^{\circ}C$. Based on the results of analysis of dilatometer it is easier to obtain high sintering density (98.87%) in self-sustaining combustion process than in the solid state reaction method. This reason is that the average particle size prepared by self-sustaining combustion process is nano crystal size and has high specific surface are value(56.54 $m^2$/g) compared with that by solid state reaction method. Also, LaAlO3 layer on the Si wafer has been achieved by screen printing and sintering method. Even though the sintering temperature is 130$0^{\circ}C$, the phenomena of silicon out diffusion in LaAlO3/Si interphase are not observed.

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Research progress of oxide solid electrolytes for next-generation Li-ion batteries (차세대 리튬이차전지를 위한 산화물 고체전해질의 연구동향)

  • Kang, Byoungwoo;Park, Heetaek;Woo, Seungjun;Kang, Minseok;Kim, Abin
    • Ceramist
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    • v.21 no.4
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    • pp.349-365
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    • 2018
  • Since the electrification of vehicles has been extended, solid-state batteries have been attracting a lot of interest because of their superior safety. Especially, polymer, sulfide, and oxide based materials are being studied as solid electrolytes, and each type of materials has advantaged and disadvantages over others. Oxide electrolytes has higher chemical and electrochemical stability compared to the other types of electrolytes. However, ionic conductivity isn't high enough as much as that of organic liquid electrolytes. Also, there are many difficulties of fabricating solid-state batteries with oxide based electrolytes because they require a sintering process at very high temperature (above ${\sim}800^{\circ}C$). Herein, we review recent studies of solid-state batteries with oxide based electrolytes about the ionic conductivity, interfacial reactions with Li metal, and preparation of solid-state cell.