• Title/Summary/Keyword: low-temperature densification

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Transmission Electron Microscopy Investigation of Hot-pressed ZrB2-SiC with B4C Additive

  • Kim, Seongwon;Chae, Jung-Min;Lee, Sung-Min;Oh, Yoon-Suk;Kim, Hyung-Tae;Jang, Byung-Koog
    • Journal of the Korean Ceramic Society
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    • v.52 no.6
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    • pp.462-466
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    • 2015
  • This paper reports the microstructure of hot-pressed $ZrB_2$-SiC ceramics with added $B_4C$ as characterized by transmission electron microscopy. $ZrB_2$ has a melting point of $3245^{\circ}C$, a relatively low density of $6.1g/cm^3$, and specific mechanical properties at an elevated temperature, making it a candidate for application to environments with ultra-high temperatures which exceed $2000^{\circ}C$. Due to the non-sinterability of $ZrB_2$-based ceramics, research on sintering aids such as $B_4C$ or $MoSi_2$ has become prominent recently. From TEM investigations, an amorphous layer with contaminant oxide is observed in the vicinity of $B_4C$ grains remaining in hot-pressed $ZrB_2$-SiC ceramics with $B_4C$ as an additive. The effect of a $B_4C$ addition on the microstructure of this system is also discussed.

Micro Structure and Surface Characteristics of NiCr Thin films Prepared by DC Magnetron Sputter according to Annealing Conditions (DC 마그네트론 스퍼터링 NiCr 박막의 열처리 조건에 따른 미세구조 및 표면특성)

  • Kwon, Yong;Kim, Nam-Hoon;Choi, Dong-You;Lee, Woo-Sun;Seo, Yong-Jin;Park, Jin-Seong
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.18 no.6
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    • pp.554-559
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    • 2005
  • Ni/Cr thin film is very interesting material as thin film resistors, filaments, and humidity sensors because their relatively large resistivity, more resistant to oxidation and a low temperature coefficient of resistance (TCR). These interesting properties of Ni/Cr thin films are dependent upon the preparation conditions including the deposition environment and subsequent annealing treatments. Ni/Cr thin films of 250 nm were deposited by DC magnetron sputtering on $Al_2O_3/Si$ substrate with 2-inch Ni/Cr (80/20) alloy target at room temperature for 45 minutes. Annealing treatments were performed at $400^{\circ}C,\;500^{\circ}C,\;and\;600^{\circ}C$ for 6 hours in air or $H_2$ ambient, respectively. The clear crystal boundaries without crystal growth and the densification were accomplished when the pores were disappeared in air ambient. Most of surface was oxidic including NiO, $Ni_2O_3$ and $Cr_xO_y$(x=1,2, y=2,3) after annealing in air ambient. The crystal growth in $H_2$ ambient was formed and stabilized by combination with each other due to the suppression of oxidized substance on film surface. Most oxidic Ni was restored when the oxidic Cr was present due to its stability in high-temperature $H_2$ ambient.

Effect of $Ga_2O_3$ and $GeO_2$ Additives on Sintering of Magnesia (Magnesia 소결에 미치는 $Ga_2O_3$$GeO_2$ 첨가의 경향)

  • 이종한;박철원
    • Journal of the Korean Ceramic Society
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    • v.20 no.2
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    • pp.99-106
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    • 1983
  • This experiment has been carried out for the purpose of investigating the effect of $Ga_2O_3$ and $GeO_2$ additivies on sintering of magnesium oxide over the temperature range of 130$0^{\circ}C$~150$0^{\circ}C$. The effect of calcining temperature on the bulk densities of fired compacts prepared from this material was observed MgO powder has been obtained by calcining extra reagent grade magnesium carbonate(basic fired) at 90$0^{\circ}C$ for 30 minutes $Ga_2O_3$and GeO2 were added in the ratio of 1, 2, and 3 wt% to MgO and mixed with calcined MgO. The specimens were prepared by compression with pressure of $700kg/cm^2$ than fired at 130$0^{\circ}C$~150$0^{\circ}C$ for 0-5hrs. Sintering behaviour and microstructure of the fired specimens were examined. The optimum calcination temperature of magnesium carbonate was 90$0^{\circ}C$. Densification rates obeyed the equation D=K in t+c. Theoretical density in the case of addition of $Ga_2O_3$ was 23.1 kcal/mole in the case of the additive $GeO_2$ was 14.176kcal/mole. This low value would appear to support a machanism of grain boundatry diffusion The range of average grain size in the case of addition of $Ga_2O_3$ and $GeO_2$ was 21$\mu\textrm{m}$-31$\mu\textrm{m}$.

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Microwave Dielectric Properties of (1-x)CaTiO3-xYAIO3 and its Low Temperature Densification by CaB2O4 Addition ((1-x)CaTiO3-xYAIO3계의 마이크로파 유전특성과 CaB2O4첨가제의 영향)

  • 강보경;김경용;김범수;김주선;김병호
    • Journal of the Korean Ceramic Society
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    • v.40 no.1
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    • pp.81-86
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    • 2003
  • Microwave dielectric properties have been investigated in the$(1-x)CaTiO_3-xYAlO_3$ (x=0.1~1.0) solid solution system. The mixtures of $CaTiO_3$ and $YalO_3$using solid state method were sintered at various temperatures. Their dielectric constants and related temperature coefficients were strongly depend on the composition of the solid solution. The optimum properties were recorded as for ${\varepsilon}_r=47,$ $Q{\times}f_0$=35000 and ${\tau}_f=+11ppm/^{\circ}C$ without sintering agent. Even at $1200^{\circ}C$ full densification has been achieved with addition of $CaB_2O_4$ in the $0.75CaTiO_3-0.25YalO_3$ composition. The sample of $0.3 wt%-CaB_2O_4$ added $ 0.75CaTiO_3-0.25YalO_3$ sintered at $1300^{\circ}C$ for 3 h showed optimum microwave dielectric properties of ${\varepsilon}_r=47$, $Q{\time}f_0=37000$ and ${\tau}_f=+17ppm/^{\circ}C$, which demonstrates the promising candidates for microwave dielectric materials covering 5~7 GHz range.

Effect of NiO on Microstructure and Properties of PMN-PT-BT Ceramics Prepared by Mixed Oxide Method

  • Han, Kyoung-Ran;Jung, Jung-Woong;Kim, Chang-Sam
    • Journal of the Korean Ceramic Society
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    • v.41 no.12 s.271
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    • pp.884-888
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    • 2004
  • Effects of NiO were studied in aspects of dielectric properties and microstructure of $0.96(0.91Pb(Mg_{1/3}Nb_{2/3})O_3-0.09PbTiO_3)­0.04BaTiO_3$ (PMN-PT-BT, PBT). The PBT was prepared by a conventional mixed oxide method using $(MgCO_3)_4{\cdot}Mg(OH)_2$ instead of MgO through Lewis acid-base interaction. NiO was added in the range of 0.5 to $3.0\;wt\%$ as thermally decomposable $2NiCO_3{\cdot}3Ni(OH)_2$ and it seemed to enhance densification to a large extent below $1000^{\circ}C$. But all the systems gave rise to ceramics with almost same relative sintered density of 96% by sintering at $1000^{\circ}C$ for 2 h. But it turned out that the addition of NiO was detrimental to dielectric constant but beneficial to the loss of dielectric constant.

Relization of Low Temperature Oxide Using Porous Silicon (다공질 실리콘을 이용한 저온 산화막의제조)

  • Ryu, Chang-U;Sim, Jun-Hwan;Lee, Jeong-Hui;Lee, Jong-Hyeon;Bae, Yeong-Ho;Heo, Jeung-Su
    • Korean Journal of Materials Research
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    • v.6 no.5
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    • pp.489-493
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    • 1996
  • 다공질 실리콘층(Porous Silicon LayerLPSL)을 사용하여 저온 열산화 (50$0^{\circ}C$, 1시간)와 급속 열산화공정(rapid thermal oxidationLRTO)(115$0^{\circ}C$, 1분)을 통하여 저온 산화막을 제조하였다. 제조된 산화막의 특성을 IR흡수 스펙트럼, C-V 곡선, 절연파괴전압, 누설전류, 그리고 굴절률을 조사함으로써 알아보았다. 절연파괴전압은 2.7MV/cm, 누설전류는 0-50V 범위에서 100-500pA의 값을 보였다. 산화막의 굴절률은 1.49의 값으로서 열산화막의 굴절률에 근접한 값을 나타냈다. 이 결과로부터 다공질 실리콘층을 저온산화막으로 제조할 때, RTO공정이 산화막의 치밀화(densification)에 크게 기여함을 알 수 있었다.

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Densification and Dielectric Properties of Ba0.5Sr0.5TiO3-Glass Composites for LTCC Applications

  • Shin, Hyun-Ho;Byun, Tae-Hun;Yoon, Sang-Ok
    • Journal of the Korean Ceramic Society
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    • v.49 no.1
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    • pp.100-104
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    • 2012
  • Barium zincoborate (BZB) glass was added to $Ba_{0.5}Sr_{0.5}TiO_3$, and sintered at $875^{\circ}C$ for 2 h in air. When the BZB glass was added in quantities ranging from 15 to 20 wt%, the relative bulk density ranged from 93.1% to 94.2%, while the density decreased to roughly 81% thereafter up to 30 wt% glass addition. Quantitative XRD analysis showed that the $Ba_{0.5}Sr_{0.5}TiO_3$ filler was significantly dissolved into the BZB glass. However, no secondary phase was identified by XRD up to 30 wt% glass addition. The dielectric constant was about 130 to 140 at 1MHz up to 20 wt% BZB glass addition, while it decreased to about 60 thereafter, which may be ascribed to decreased density, partial dissolution of the $Ba_{0.5}Sr_{0.5}TiO_3$, and associated changes in the glass composition. The dielectric loss of the 20 wt% glass added specimen was 0.008.

Deposition Of $TiB_2$ Films by High Density Plasma Assisted Chemical Vapor Deposition (고밀도 플라즈마 화학 증착 장치를 이용한 $TiB_2$ 박막 제조)

  • Lee S. H.;Nam K. H.;Hong S. C.;Lee J. J.
    • Journal of the Korean institute of surface engineering
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    • v.38 no.2
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    • pp.60-64
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    • 2005
  • The ICP-CVD (inductively coupled plasma chemical vapor deposition) process was applied to the deposition of $TiB_2$ films. For plasma generation, 13.56 MHz r.f. power was supplied to 2-turn Cu coil placed inside chamber. And the gas mixture of $TiCl_4,\;BCl_3,\;H_2$ and Ar was used for $TiB_2$ deposition. $TiB_2$ films with high hardness (<40 GPa) were obtained at extremely low deposition temperature $(250^{\circ}C)$, and the films hardness increased with ICP power and gas flow ratio of $TiCl_4/BCl_3$. The film structure was changed from (100) preferred orientation to random orientation with increasing RF power. It is supposed that the enhanced hardness of films was caused by a strong Ti-B chemical bonding of stoichiometric $TiB_2$ films and film densification induced by high density plasma.

Synthesis of Nanocrystalline Ceria for IT-SOFC by Glycine Nitrate Combustion Process (연소합성을 이용한 저온형 고체산화물 연료전지용 나노구조 세리아계 전해질 제조)

  • Jo, Seung-Hwan;Kim, Jong-Ho;Kim, Do-Kyung
    • Journal of the Korean Ceramic Society
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    • v.42 no.12 s.283
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    • pp.821-826
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    • 2005
  • Gadolinia-doped ceria nanopowder was prepared by glycine-nitrate combustion method with different glycine/nitrate mixing ratio. The characteristics of the synthesized powder were investigated by X-ray diffraction method, transmission electron microscopy, thermal gravity, differential thermal analysis and thermo-mechanical analysis. The smallest powder was obtained with glycine/nitrate ratio 1.00 and the lowest organic and water vapor contained powder was made with glycine/nitrate ratio 1.75. According to dilatometry, fast densification was occurred around $1000^{\circ}C$ and shows full density over $1300^{\circ}C$. Finally near-fully dense ceria electrolyte was fabricated with conventional sintering technique. Glycine-nitrate process yields fine nanopowders which enable low temperature sintering and fabrication of fully dense and nanostructured oxide electrolyte.

Effects of the SiC Particle Size and Content on the Sintering and Mechanical Behaviors of $Al_2O_3$/SiC Particulate Composites

  • Ryu, Jung-Ho;Lee, Jae-Hyung
    • The Korean Journal of Ceramics
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    • v.3 no.3
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    • pp.199-207
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    • 1997
  • $Al_2O_3$/SiC particulate composites were fabircated by pressureless sintering. The dispersed phase was SiC of which the content was varied from 1.0 to 10 vol%. Three SiC powders having different median diameters from 0.28 $\mu\textrm{m}$ to 1.9 $\mu\textrm{m}$ were used. The microstructure became finer and more uniform as the SiC content increased except the 10 vol% specimens, which were sintered at a higher temperature. Under the same sintering condition, densification as well as grain growth was retarded more severly when the SiC content was higher or the SiC particle size was smaller. The highest flexural strength obtained at 5.0 vol% SiC regardless of the SiC particle size seemed to be owing to the finer and more uniform microstructures of the specimens. Annealing of the specimens at $1300^{\circ}C$ improved the strength in general and this annealing effect was good for the specimens containing as low as 1.0 vol% of SiC. Fracture toughness did not change appreciably with the SiC content but, for the composites containing 10 vol% SiC, a significantly higher toughness was obtained with the specimen containing 1.9$\mu\textrm{m}$ SiC particles.

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