• Title/Summary/Keyword: Sintering densification

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Application of Mechanochemical Processing for Preparation of Si3N4-based Powder Mixtures

  • Sopicka-Lizer, Malgorzata;Pawlik, Tomasz
    • Journal of the Korean Ceramic Society
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    • v.49 no.4
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    • pp.337-341
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    • 2012
  • Mechanochemical processing (MCP) involves several high-energy collisions of powder particles with the milling media and results in the increased reactivity/sinterability of powder. The present paper shows results of mechanochemical processing (MCP) of silicon nitride powder mixture with the relevant sintering additives. The effects of MCP were studied by structural changes of powder particles themselves as well as by the resulting sintering/densification ability. It has been found that MCP significantly enhances reactivity and sinterability of the resultant material: silicon nitride ceramics could be pressureless sintered at $1500^{\circ}C$. Nevertheless, a degree of a silicon nitride crystal lattice and powder particle destruction (amorphization) as detected by XRD studies, is limited by the specific threshold. If that value is crossed then particle's surface damage effects are prevailing thus severe evaporation overdominates mass transport at elevated temperature. It is discussed that the cross-solid interaction between particles of various chemical composition, triggered by many different factors during mechanochemical processing, including a short-range diffusion in silicon nitride particles after collisions with other types of particles plays more important role in enhanced reactivity of tested compositions than amorphization of the crystal lattice itself. Controlled deagglomeration of $Si_3N_4$ particles during the course of high-energy milling was also considered.

Thermal and Dielectric Properties of LiF-Doped MgO Ceramics (LiF첨가 MgO 세라믹스의 열적·유전적 특성)

  • Kim, Shin;Kim, So-Jung;Nam, Kyung-Jin;Cha, Hansol;Yoon, Sang-Ok
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.28 no.7
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    • pp.419-423
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    • 2015
  • Sintering, microstructure, thermal conductivity and microwave dielectric properties of xLiF-(1-x)MgO ceramics (x=0.03~0.10 mol) were investigated. The high density was obtained in the specimens of $x{\geq}0.06$, i.e., 0.04 LiF-0.96 MgO in mol, whereas the amount of 0.03 mol LiF was insufficient to densify. From the result that the contact flattening in the sintered specimen was observed, the densification occurred through the liquid-phase sintering. The specimen of x=0.06 showed the highest room-temperature thermal conductivity. Relative density, thermal conductivity, dielectric constant, and quality factor ($Q{\times}f$) of the specimen for x=0.06 sintered at $900^{\circ}C$ for 4 h were 97.8%, $39.2Wm^{-1}K^{-1}$, 9.45, and 14,671 GHz, respectively.

Homogeneous Mixing of Si3N4 with Sintering Additives by Coprecipitation Method (질화규소의 소결첨가제의 공침법에 의한 균일혼합)

  • 김지순
    • Journal of the Korean Ceramic Society
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    • v.30 no.10
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    • pp.829-837
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    • 1993
  • Chemically and geometrically homogeneous mixing of Si3N4 powders with sintering additives(YAG, 3Y2O3$.$5Al2O3) was attempted via coprecipitation method. X-ray dot maps for the additive elements(Al and Y) showed that the additives are evenly distributed in the powder mixture prepared by coprecipitation method(CP). TEM observation of the coprecipittion-treated Si3N4 powders revealed that they are covered with extremely fine crystallites of additive. The shift in isoelectric point(IEP) of Si3N4 powders from pH 6.7 to pH 7.9 after coprecipitation mixing gave another evidence for coating of Si3N4 powders with YAG additives. SIMS analysis for composition on the surface and in the matrix of mixed powders showed that the YAG additives are highly enriched on the surface of coprecipitation-treated Si3N4 powders. Especially when a small amount of additive was used, the effect of homogeneous additive distribution on densification was preceptible: After pressureless-sintering of powder compacts containing 5 mol% YAG at 1800$^{\circ}C$ for 0.5h, a sintered density of 96.5% theoretical was obtained from the specimens prepared bycoprecipitation in comparison with 93.8% from the mechanically-mixed one.

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A New Process for Liquid Phase Sintering of W-Cu Composite; Fluidized Beds Reductio Method (W-Cu 합금의 액상소결을 위한 새로운 공정의 개발:유동층 환원법)

  • Ihn, Tae-Hyoung;Lee, Seok-Woon;Joo, Seung-Ki
    • Korean Journal of Materials Research
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    • v.4 no.4
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    • pp.393-400
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    • 1994
  • A new process for uniform coating of copper to submicron tungsten powder has been developed. W-Cu alloy where copper can be uniformly distibuted has been made by the liquid phase sintering of thus prepared tungsten powder. It has been found that copper content can be lowered less than IOwt. % in our new process, maintaining the uniform distribution of copper in W-Cu alloy. Relative density above 96% was obtained after the liquid phase sintering when small amount of cobalt was added. It was revealed that the rapid increase of densification rate was due to the enhancement of wettability between tungsten particle and liquid copper.

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Fabrication of ZnS-SiO2 Composite and its Mechanical Properties (방전플라즈마 소결법을 이용한 ZnS-SiO2 복합재료의 제조와 기계적 특성)

  • Shin, Dae-Hoon;Kim, Gil-Su;Lee, Young-Jung;Cho, Hoon;Kim, Young-Do
    • Journal of Powder Materials
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    • v.15 no.1
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    • pp.1-5
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    • 2008
  • ZnS-$SiO_2$ composite is normally used for sputtering target. In recent years, high sputtering power for higher deposition rate often causes crack formation of the target. Therefore the target material is required that the sintered target material should have high crack resistance, excellent strength and a homogeneous microstructure with high sintered density. In this study, raw ZnS and ZnS-$SiO_2$ powders prepared by a 3-D mixer or high energy ball-milling were successfully densified by spark plasma sintering, the effective densification method of hard-to-sinter materials in a short time. After sintering, the fracture toughness was measured by the indentation fracture (IF) method. Due to the effect of crack deflection by the residual stress occurred by the second phase of fine $SiO_2$, the hardness and fracture toughness reached to 3.031 GPa and $1.014MPa{\cdot}m^{1/2}$, respectively.

The Fabrication and Sinterability of $Al_2O_3/Cu$ Nanocomposite Powder ($Al_2O_3/Cu$ 나노복합분말의 제조 및 소결 특성)

  • 홍대희;오승탁;김지순;김영도;문인형
    • Journal of Powder Materials
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    • v.6 no.4
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    • pp.301-306
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    • 1999
  • Mechanical properties of oxide based materials could be improved by nanocomposite processing. To investigate optimum route for fabrication of nanocomposite enabling mass production, high energy ball milling and Pulse Electric Current Sintering (PECS) were adopted. By high energy ball milling, the $Al_2O_3$-based composite powder with dispersed Cu grains below 20 nm in diameter was successfully synthesized. The PECS method as a new process for powder densification has merits of improved sinterability and short sintering time at lower temperature than conventional sintering process. The relative densities of the $Al_2O_3$-5vol%Cu composites sintered at $1250^{\circ}C$ and $1300^{\circ}C$ with holding temperature of $900^{\circ}C$ were 95.4% and 95.7% respectively. Microstructures revealed that the composite consisted of the homogeneous and very fine grains of $Al_2O_3$ and Cu with diameters less than 40 nm and 20 nm respectively The composite exhibited enhanced toughness compared with monolithic $Al_2O_3$. The influence of the Cu content upon fracture toughness was discussed in terms of microstructural characteristics.

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Preparation of Ce0.8Gd0.2O1.9 Powder Using CeO2 Powder and Gd Precipitation and Effect of CoO doping on Sintering

  • Sim, Soo-Man
    • Journal of the Korean Ceramic Society
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    • v.52 no.6
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    • pp.521-526
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    • 2015
  • $Ce_{0.8}Gd_{0.2}O_{1.9}$(GDC20) powder was prepared from a mixture of submicron-sized $CeO_2$ powder and Gd precipitates using ammonium carbonate $((NH_4)_2CO_3)$ as a precipitant. The mixture was calcined at $700^{\circ}C$ for 4 h followed by ball-milling that resulted in the GDC powder with an average particle size of $0.46{\mu}m$. The powder had a very uniform particle size distribution with particle sizes ranging from $0.3{\mu}m$ to $1{\mu}m$. Sintering of undoped GDC samples did not show a relative density of 99.2% until the temperature was increased to $1500^{\circ}C$, whereas GDC samples doped with 5 mol% CoO exhibited a significant densification at lower temperature reaching a relative density of 97.6% at $1100^{\circ}C$ and of 98.8% at $1200^{\circ}C$.

Preparation and Sintering Characteristics of Ce0.8Gd0.2O1.9 Powder by Ammonium Carbonate Co-precipitation (탄산암모늄 공침을 이용한 Ce0.8Gd0.2O1.9 분말의 합성 및 소결특성)

  • Yoo, Young-Chang;Chung, Byung-Joo;Sim, Soo-Man
    • Journal of the Korean Ceramic Society
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    • v.49 no.1
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    • pp.118-123
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    • 2012
  • GDC20($Ce_{0.8}Gd_{0.2}O_{1.9}$) powder was synthesized from Ce and Gd nitrate solutions using ammonium carbonate($(NH_4)_2CO_3$) as a precipitant. Attrition-milling of the powder, which had been calcined at $700^{\circ}C$ for 4 h, decreased an average particle size of 2.2 ${\mu}m$ to 0.5 ${\mu}m$. The milled powder consisted of nano-sized spherical primary particles. Due to the excellent sinterability of the powder, sintering of the powder compacts for 4 h showed relative densities of 80% at 1000 $^{\circ}C$ and 96.5% at $1200^{\circ}C$, respectively. Densification was found to almost complete at $1300^{\circ}C$, resulting in a dense and homogeneous microstructure with a relative density of 99.5%. The grains of ~0.2 ${\mu}m$ in size at $1200^{\circ}C$ grew to ~1 ${\mu}m$ in size at $1300^{\circ}C$ as a result of a rapid grain growth.

Fabrication of Ultra fine WC-Ni Hard Materials by Rapid Sintering Process

  • Kim Hwan-Cheol;Oh Dong-Young;Shon In-Jin
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2004.11a
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    • pp.98-99
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    • 2004
  • (1) Using high-frequency induction heating sintering and spark plasma sintering method, the densification of WC-Ni hard materials was accomplished using ultra fine power of Ni and WC. (2) Nearly fully dense WC-Ni could be obtained within 1 min. (3) Relative density and mechanical properties of WC-Ni obtained by HFIHS were high than those obtained by SPS. And WC grain size made by HFIHS was smaller than that made by SPS. (4) The fracture toughness and hardness values of WC-8Ni, WC-10Ni, and WC-12Ni made by HFIHS were $13MPa{\cdot}m^{1/2}\;and\;1950kg/mm^2,\;13.5Mpa{\cdot}m^{1/2}\;and\;1810kg/mm^2,\;14.4MPa{\cdot}m^{1/2}\;and\;1690kg/mm^2$, respectively for 60MPa and an induced current for 90% output of total capacity, 15KW. (5) The fracture toughness and hardness values of WC-8Ni, WC-10Ni, and WC-12Ni made by SPS were $12.2MPa{\cdot}m^{1/2}\;and\;1796kg/mm^2,\;12.9MPa{\cdot}m^{1/2}\;and\;1725kg/mm^2,\;13.6MPa{\cdot}m^{1/2}\;and\;1597kg/mm^2$, respectively for 60MPa and the electric current of 2500 A

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Carbon Dioxide Sorption Properties and Sintering Behavior of Lithium Zirconate Prepared by Solid-State Reaction (고상반응에 의하여 제조된 Li2ZrO3의 이산화탄소 흡수 및 소결 특성)

  • Woo, Sang-Kuk;Lee, Shi-Woo;Yu, Ji-Haeng
    • Journal of the Korean Ceramic Society
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    • v.43 no.5 s.288
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    • pp.309-314
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    • 2006
  • We synthesized lithium zirconate using solid-state reaction and analyzed thermal properties (TG/DTA) of starting materials and the synthesized one. When $Li_2ZrO_3$ powder was exposed to $CO_2$ environment at $500^{\circ}C$, 93% of the theoretical absorption weight was gained within 280 min with fairly high sorption rate. Almost all the absorbed $CO_2$ was generated by heating the sample to $800^{\circ}C$. We also investigated densification behavior of $Li_2ZrO_3$ under $CO_2$ environment. By sintering $Li_2ZrO_3$ at $760^{\circ}C$ using 2-step process, we obtained dense product, composed mainly of $Li_2ZrO_3\;and\;ZrO_2$, with relative density of 92%.