Journal of the Ceramic Society of Japan
Online ISSN : 1882-1022
Print ISSN : 0914-5400
ISSN-L : 0914-5400
Volume 97, Issue 1129
Displaying 1-18 of 18 articles from this issue
  • Yoshihiro HIRATA, Shinichi MATSUSHITA, Susumu NAKAGAMA, Yoshimi ISHIHA ...
    1989 Volume 97 Issue 1129 Pages 881-887
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    Dispersion, rheology and consolidation of the colloidal suspension in the alumina powder-silicon nitride whisker system were studied to control the microstructure and density of the green compact. Al2O3 particles with an average diameter of 0.15μm and Si3N4 whiskers with an average size of 0.4μm×3.7μm were electrostatically dispersed in water in the pH range 3 to 10 and consolidated by filtration. Well-dispersed stable suspensions were obtained at low pH. Decreasing the viscosity and at the same time increasing the solid content of the suspension is the key step in making the green compact with high density and a narrow pore size distribution. Application of isostatic pressing to compacts consolidated by filtration increased green density and shifted the pore size distribution to smaller size. These green compacts by colloidal processing were densified to relative densities of 98.4-99.4% by hot-pressing at 1500°C at a pressure of 39MPa in N2 atmosphere.
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  • Yoshio ONODERA, Takashi IWASAKI, Hiromichi HAYASHI, Kazuo TORII
    1989 Volume 97 Issue 1129 Pages 888-894
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    A new inorganic titanium compound with high selective adsorbability for Li+ was prepared by acid-treatment of precursory Li2TiO3-rich products synthesized by heating an equimolar mixture of powdered Li2CO3 and TiO2 (anatase) in air at 450°-950°C. These products were examined by X-ray diffraction, chemical analysis, specific surface area (BET method), shape (TEM) and thermal (TG & DTA) analysis. For the examination of adsorbability for Li+ on the products, adsorption of Li+, Na+, K+ and Ca2+ for the acid-treated products was determined by a batch method in weakly basic media. The results are summarized as follows:
    (1) Crystalline Li2TiO3 transformed to a new crystalline phase (TOH), which was characterized by the XRD peaks at d=4.74, 4.53 and 2.45Å, on acid-treatment. But the conversion decreased with increasing preparation temperature of the precursory products.
    (2) Li+ was adsorbed selectively only on acid-treated products containing the TOH phase, suggesting that the TOH material contributed significantly to the selective adsorption of Li+.
    (3) As the TOH phase contains TiO2 and H2O in the 1:1 molar ratio, it is considered that lithium-free titanium oxide hydride, H2TiO3, was formed from Li2TiO3 by the acid-treatment.
    (4) When the TOH adsorbs Li+, a topotactic phase transformation to Li2TiO3 was observed. In the same manner as γ-MnO2, the following mechanism of cation exchange is supposed for the selective Li+-adsorption on the TOH phase: TOH(H2TiO3)+2Li+→←Li2TiO3+2H+.
    (5) The amount of adsorption of Li+ on TOH was influenced by the texture. The specific surface area (SSA) of the acid-treated products depended remarkably on the preparation conditions of the precursory products. The ratios of the amount of adsorbed Li+ to the exchange capacity increased with increasing SSA.
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  • Takeshi KUMAZAWA, Shigetoshi OHTA, Hideyo TABATA, Shuzo KANZAKI
    1989 Volume 97 Issue 1129 Pages 895-902
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    Mechanical properties of hot-pressed mullite-SiC whisker composites were studied in relation to the whisker content and chemical composition of matrix. Grain growth of mullite was suppressed by the existence of SiC whisker in the matrix, but the densification was not inhibited by the loading of whisker up to 30 vol%. The room temperature flexural strength of specimens was improved by the addition of SiC whisker in every chemical compositions of the matrix examined, more pronouced with increasing SiO2 content in the matrix. The high temperature strength was almost the same as that at room temperature up to 1300°C. In specimens containing a glassy grain-boundary phase, addition of SiC whisker to mullite did not significantly affect KIC value. Combination of single phase mullite (74 wt% Al2O3) and SiC whisker gave the best effect on the KIC value both at room temperature and elevated temperature. These phenomena can be explained by the presence of a glassy grain-boundary phase, which causes the matrix to the whisker bonding.
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  • Kohei ODA, Tetsuo YOSHIO
    1989 Volume 97 Issue 1129 Pages 903-910
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
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    The leaching behavior of hot-pressed and pyrolytic boron nitride (BN) was studied under hydrothermal conditions at 150°C and 0.48MPa for 1-10 days. A large degree of weight loss was observed in the hot-pressed BN specimens at the initial stage, due to dissolution of a grain boundary phase. The weight of the pyrolytic BN specimen decreased slowly with increasing time. SEM observation and EPMA of leached specimens and chemical analyses of leached solutions revealed that BN reacted with H2O to produce H3BO3 and NH3, and the grain boundary phase was rapidly dissolved, and the hydrated layer was not left. These results suggested that the chemical stability of h-BN ceramics under hydrothermal conditions depends on the difference in the grain boundary structure, though BN is fairly stable.
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  • Influence of pH
    Shin-ichi TAKEDA, Shinji NAKADA, Isao TARI
    1989 Volume 97 Issue 1129 Pages 911-915
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    Post-indentation slow crack growth in soda-lime-silica glass in various aqueous solutions was investigated. Measurements of crack length and streaming potential at the glass/solution interface were carried out in order to understand the mechanism of slow crack growth of glass. The crack growth depended on the pH of electrolyte, and was enhanced by the change of pH from 1 to 10. This behavior was in good agreement with the prediction obtained from the charged state at the interface. These results were discussed in terms of the charged state at glass/solution interface and its effect on the stress corrosion reaction in electrolytes.
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  • Toshio TSUCHIYA, Kazuhide YAMASHIRO, J. D. MACKENZIE
    1989 Volume 97 Issue 1129 Pages 916-922
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
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    Thins film of magnetoplumbite type ferrite (MFe12O19, M=Ba, Sr) have been prepared by the dip-coating method from solgel process. Ferric nitrates, other metal nitrate and titaniumoxiacetylacetonate were used as law materials, and glycerol was used as solvent. A film was prepared by dipping a silica glass plate. The magnetoplumbite type ferrite was obtained by heattreatment at 750°C for 5h in air. The film thickness was about 0.08μm. The coercive forces (Hc) of the film and powder with the composition of 15BaO⋅85Fe2O3 was 3300 and 3050 Oe by heat-treatment at 850°C for 48h respectively. These films were shown to have much larger Hc than the powder. The effect of substitution of titanium and cobalt ion in barium hexaferrite films and powders were investigated. The saturation magnetization of the powder in the system 15BaO⋅85 [(100-2x) Fe2O3⋅xTiO2⋅xCoO] was almost constant in the range of 0≤x≤8.33. But the Hc changed drastically with increasing titanium and cobalt ion content. The Hc of the powder was controllable in the range of 50 Oe and 3050 Oe by changing the substitution contents for the same system. The Hc of the films was controllable in the range of 300 Oe and 3300 Oe for the same system.
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  • Masahiro YOSHIMURA, Naotoshi MORITA, Masao NISHIOKA, Shigeyuki SOMIYA
    1989 Volume 97 Issue 1129 Pages 923-928
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    Reactions among Si3N4, SiC, ZrC, ZrN and C were investigated under 1 atm N2 at 1650°C. Compatibility relations among the compounds coexisting with 1 atm N2 in the system Si-Zr-C-N were determined. Equilibrium states were confirmed by the fact that reaction products obtained from nitridation reactions were identical with those from decomposition of nitrides and by thermochemical calculation. The reaction products obtained from the starting sample of ZrC-Si3N4 were zirconium carbonitride and SiC, and those from ZrN-SiC were zirconium carbonitride and Si3N4. The lattice parameter of the zirconium carbonitride varied with the composition of the starting sample. The isobaric and isothermal section of the system Si-Zr-C-N includes 2 three-phase triangles: the area [I] ZrCxN1-x (x=0.43)+C+SiC, the area [III] ZrCyN1-y (y=0.32)+SiC+Si3N4 and 2 two-phase regions: the area [II] ZrC1-bNb (0.32<1-b<0.43)+SiC, the area [IV] ZrCcN1-c (0≤c<0.32)+Si3N4. On the assumption that zirconium carbonitride might be a regular solution between ZrC and ZrN, the interaction parameter of zirconium carbonitride was estimated to be -6--10kcal/mol from thermochemical calculation.
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  • Yoshihito KONDO, Akira TSUKUDA, Shojiro OKADA
    1989 Volume 97 Issue 1129 Pages 929-934
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    In order to make clear the grindability of ceramics, a series of alumina-zirconia composite ceramics was ground using diamond grinding wheel, because the physical properties of this kind of ceramics vary greatly. Grinding force was adopted as a criterion of grindability, and bending strength, elastic modulus, Knoop hardness and fracture toughness were also measured as properties related to material removal mechanism. The results are summarized as follows:
    (1) The grindability was dominated by hardness and fracture toughness in plastic deformation and in brittle fracture, respectively.
    (2) A normal force increased with grinding time. The increasing rate was closely connected with the wear of abrasive grain and influenced by the nature of work material.
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  • Tian-quan LIU, Osamu SAKURAI, Nobuo KIEDA, Nobuyasu MIZUTANI, Masanori ...
    1989 Volume 97 Issue 1129 Pages 935-940
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    Polysilazanes, high potential precursors for Si3N4 materials, were synthesized from trichlorosilane and methyldichlorosilane. The molecular weight of these polysilazanes increased as the mixing ratio of trichlorosilane to methyldichlorosilane increased. Their pyrolysis behavior were studied by TG, DTGA (Differential Thermal Gas Analysis) and Mass spectrometer. The major chemical species of gas evolved from samples in He atmosphere was ammonia at 350°C, and methane at 570°C. Moreover, on heating the samples in N2, the DTGA curve showed that the reaction occurred from 400° to 950°C, and especially two DTGA peaks appeared at 570° and 750°C. When these polysilazanes were heated at 1300°C in N2, α-Si3N4 formed, but a mixture of α-Si3N4 and β-SiC was obtained by heating them at 1400°C in Ar.
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  • Kazuhiro NONAKA, Toyohiko YANO, Nozomu OTSUKA
    1989 Volume 97 Issue 1129 Pages 941-946
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    Fine powders of partially stabilized zirconia containing 2mol% Y2O3 were synthesized from water-alcohol solutions of ZrO(NO3)2⋅2H2O and YCl3⋅6H2O with various concentrations, [Zr4++Y3+]=0.25-0.9mol/l, by the spray pyrolysis technique using a 2-fluids nozzle. The powders obtained were calcined between 1100° and 1300°C and milled for 12h. The powders so obtained were characterized by crystallite size and specific surface area measurements, TEM and SEM observations. On the basis of these results, the influence of powder properties such as primary particle size, degree of agglomeration, and green density on the density of the ceramic bodies (Y-TZP) fabricated by pressureless sintering at 1300° to 1500°C was investigated. The green density increased with an increase in calcining temperature, but was slightly affected by the concentration of solutions. With decreasing calcining temperature and/or decreasing concentration of solution, the size and degree of aggregation of primary particles decreased. Sintered bodies with 98% T. D. was obtained from the powders prepared in the present method by firing at 1300°C. The sinterability of the powders at 1400°C was almost independent of the concentration of solution, and 98% T. D. was obtained from the powder prepared from a concentrated solution of 0.9mol/l.
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  • Akira KAMIYA, Kikuo NAKANO, Hiroshi OKUDA
    1989 Volume 97 Issue 1129 Pages 947-953
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    SiC whisker-reinforced NbC composites were fabricated by the hot-pressing method. NbC, SiC whisker (Vf=10-30%) and 1wt% Cr7C3 were mixed with a ball mill, then hot-pressed at 1600°C, 330kg/cm2 for 1h in Ar atmosphere. Flexural strength (σf), fracture toughness (KIC) and Vickers hardness (Hv) were measured at room temperature. All of these mechanical properties were improved by whisker reinforcement. For the composite having Vf=30%, σf, KIC and Hv were 880MPa, 5.74MPa√m and 24.7GPa, respectively. Crack deflection and grain growth inhibition of the matrix were observed as a result of whisker incorporation.
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  • Masafumi KOBUNE, Kiyoshi AMAKAWA, Hiroshi NAKAYAMA, Mitsuyoshi ONODA
    1989 Volume 97 Issue 1129 Pages 954-959
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
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    Electrical properties of PbTiO3-MgTiO3 (MgO=2000-6000ppm) single crystals grown by the flux cooling method were studied. Arrhenius plots of σdc for PbTiO3-MgTiO3 (MgO=4000-6000ppm) exhibited high linearity. The apparent activation energy Ua and conductivity σ obtained were 0.9eV and (3.0-3.4)×103 exp (-0.9/kT)Ω-1·cm-1, respectively. I-V characteristic curve was separated into two ranges at the temperature above 300°C independent of the quantity of doped MgO. Thermal breakdown of specimens caused by joule heat was frequently observed in the high field range. The relationship between the quantity of doped MgO and temperature dependence of EH showed that the effects of doped Mg2+ ions remarkably decrease with increasing temperature. It is possible to apply the poling dc-electric field approximately 30-50V/cm by the electric field cooling method in the range from high temperature above Tc to room temperature.
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  • 1989 Volume 97 Issue 1129 Pages 959
    Published: 1989
    Released on J-STAGE: August 06, 2010
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  • Residual Stress Effect
    Mitsuo YODA
    1989 Volume 97 Issue 1129 Pages 960-964
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    For comparing crack growth characteristics, subcritical crack growth data for soda-lime glass subjected to sustained load in water were obtained using conventional CT specimens with long crack and bend specimens with small Knoop indented crack. The relation between crack velocity V and stress intensity factor KI obtained from as-indented specimens containing indentation crack shows that there is residual stress effect which increases crack growth in the region of lower KI values. In addition, the slopes of the V-KI curves for the as-indented specimens are much less than those for the CT specimens. However, the V-KI curve for the indented and subsequently annealed specimen shows almost the same trend as that for the CT specimens. Thus, the effective stress intensity factor KIeff including the residual stress effect can be used to explain the anomalous growth of the indentation crack in its as-indented state.
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  • Isao KONDOH, Nobuyuki TAMARI, Makoto KINOSHITA
    1989 Volume 97 Issue 1129 Pages 965-967
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
    JOURNAL FREE ACCESS
    Tricalcium phosphate (TCP) was HIP'ed in a glass capsule at 800°-1100°C and 100MPa for 30min. Soda-lime glass was more suitable than Pyrex glass as a capsule material because of less thermal expansion mismatch from HIP-sintered TCP. Alumina powder was suitable as a barrier layer between glass capsule and sample, but boron nitride powder seemed to be reacted with the sample. The dense and transparent TCP ceramics were obtained by HIPing above 1000°C. In the comparison with pressureless sintering, the HIP treatment lowered the densification temperature as much as 200°C and also improved mechanical properties, 120MPa for bending strength and 0.8MPa·m1/2 for fracture toughness.
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  • Hiroshi TODOROKI, Shoichi OKAMOTO
    1989 Volume 97 Issue 1129 Pages 968-971
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
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    The superconducting properties of the Bi-Sr-Ca-Cu-O ceramics has been studied in terms of the microstructure. The powders were uniaxially hot pressed at 5t/cm2, 500°C for 5min. Then the compacts were heated and sintered again at 870°C in air for 10 and 100h, followed by furnace cooling. Resistivity of the specimens was measured by standered four-probe method. Zero resistivity was observed at 80.0K when the compact was heated at 870°C for 10h, while after heated for 100h the off-set was at high as 105.5K. The critical current density at 77K was very low as 168.4mA/cm2. The specimens simply heated and sintered at 870°C for 10 and 100h after cold pressing at 5t/cm2 (without hot pressing) showed very low off-set temperatures. It was found, however, that the prolonged heating at 870°C with or without hot pressing increased the formation of the high Tc phase in the Bi-Sr-Ca-Cu-O ceramics. The hot pressing prior to the heating at 870°C increased the bulk density and the grain sizes of the specimens. The improvement of the sintering behavior may assist the formation of superconducting contacts among the grains of the high Tc phase in the Bi-Sr-Ca-Cu-O ceramics.
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  • Masaaki SUZUKI, Yoshinori NAKATA, Takeshi OKUTANI, Akio KATO
    1989 Volume 97 Issue 1129 Pages 972-975
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
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    Preparation of SiC ultrafine particles from SiH2Cl2-C2H4 mixtures by using CO2 laser was investigated. Powders with specific surface areas of 8 to 150m2/g, were obtained by irradiating CO2 laser beam to SiH2Cl2-C2H4 gas mixture at atmospheric pressure. The power density of laser beam was 3.66kW/cm2 and wave length was 10.6μm. XRD of the products showed that Si, β-SiC and free carbon were produced and that the composition of powders depended on the C2H4/SiH2Cl2 ratio. Reaction temperature changed with the power density of laser beam and C2H4/SiH2Cl2 ratio. Hysteresis was observed between reaction temperature and power density of laser beam.
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  • Kazuo NAKAMURA, Takeshi KUMAZAWA, Nobuyuki AZUMA, Shuzo KANZAKI
    1989 Volume 97 Issue 1129 Pages 976-979
    Published: September 01, 1989
    Released on J-STAGE: August 06, 2010
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    Oxidation behavior of mullite composites containing 10 to 30vol% of SiC-whisker (SiC-w) has been studied at 1300°C in dry air. As the volume fraction of SiC-w increased, the weight gain increased. The weight gain curve obeyed the parabolic law for the SiC-w content of 10vol% and at the oxidation time shorter than 200h. However, the weight gain of the specimen containing more than 20vol% SiC-w was accelerated when the oxidation time exceeded 200h. It was found that impurities such as Na2O, K2O and CaO, originally contained in the SiC-w, were concentrated near the surface of the specimen. The acceleration of the weight gain for longer oxidation duration is explained in terms of corrosion of mullite and SiC-w by the liquid phase formed through the reaction between oxidized SiC-w and the impurities.
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