• Journal of the Korean Ceramic Society
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• v.24 no.1
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• pp.23-32
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• 1987

Synthesis of high purity ultrafine Si3N4 and ${\beta}$-Sialon powders was investigated via the simultaneous reduction and nitriding of amorphous SiO2, SiO2-Al2O3 system prepaerd by hydrolysis of alkoxides, using carbonablack as a reducing agent. In Si(OC2H5)4-C2H5 OH-H2 O-NH4OH system, hydrolysis rate increased with increasing reaction temperature and pH. Pure ${\alpha}$-Si3N4 was formed at 1350$^{\circ}C$ for 5 hrs in N2 atmosphere. In Si(OC2H5)4-Al(OC3H7)3-C6H6-H2 O-NH4OH system, weight loss increased as Si/Al ratio decreased. Single phase ${\beta}$-Sialon consisted of Si/Al=2 was formed at 1350$^{\circ}C$ in N2 and minor phases of ${\alpha}$-Si3N4, AIN, and X-phase were existed besides theSialon phase at other Si/Al ratios. The Si3N4 and Sialon powders synthesized from alkoxides consisted of uniform find particles of 0.05-0.2$\mu\textrm{m}$ in diameter, respectively.

• Proceedings of the Korean Ceranic Society Conference
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• 2003.04a
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• pp.61.2-61
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• 2003

• Journal of the Korean Ceramic Society
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• v.26 no.3
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• pp.341-346
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• 1989

In order to evaluate the oxidation behavior of $\beta$-Sialon, $\beta$-Sialon ceramics was prepared from Si3N4, Al2O3, AlN and Y2O3 system. The specimens were oxidized in an oxygen atmosphere at 1, 20$0^{\circ}C$ for 9days. Oxidation behavior was evaluated by weight gain oxidation process, surface roughness. Microscopy, EDX and X-ray diffraction analysis were also used for the evaluation. The weight and surface roughness ofoxidized specimens were increased with increasing the oxidation time. Oxidized products were mullite, $\alpha$-cristobalite, yttrium aluminum oxide and yttrium silicate oxide.

• Journal of the Korean Ceramic Society
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• v.29 no.5
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• pp.410-418
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• 1992

Si3N4, AlN and Y2O3 powder mixtures of the Y0.1(Si, Al)12(N, O)16 composition were hot-pressed at 1900℃ for 0 to 60 min under 30 MPa in order to fabricate the partially-stabilized α-Sialon ceramics (X=0.1). Room and high temperature flexural strengths of the specimens were compared with those of Si3N4-5 wt%Y2O3, Si3N4-5 wt%Y2O3-2 wt%Al2O3, and β-Sialon (Z=0.5) ceramics. The flexural strength of the α-Sialon ceramics which was hot-pressed for 15 min showed the highest value of 820 MPa at 1400℃ that is relatively higher temperature. It is guessed that a little amount of glassy phase existed in grain boundary because Y2O3 and AlN components were incoperated in Si3N4 grains, or transient liquid phase sintering, and microstructure with the smaller grain size and the interlocked grains of α'-and β-Si3N4 was obtained by the hot-pressing at high temperature of 1900℃ for the short time (15 min).

• Journal of the Korean Ceramic Society
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• v.21 no.1
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• pp.5-10
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• 1984

$eta$-Sialon synthesis was investigated via the simulataneous reduction and nitriding of Wando pyrophyllite. When Wando pyrophyllite-graphite-$Si_3N_4$ seed mixture was heated at 135$0^{\circ}C$ for as long as 10 hours in 80% $N_2$-20%$H_2$ atomsphere $eta$-$Si_3N_4$ solid solution was mainly formed together with a small amount of $\alpha$-$Si_3N_4$ The value z of the forming $Si_{6-x}Al_2O_2N{8-z}$ was decreased with heating time.

• Journal of the Korean Ceramic Society
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• v.37 no.3
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• pp.247-255
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• 2000

Silicon carbide with sialon was prepared by hot pressing and transient liquid-phase sintering, and the effects of sintering atmosphere and starting phases on their microstructural characteristics were investigated. The sintered SiC with Sialon composition(Y2O3, AlN, Si3N4) in argon atmosphere had high sintered density and large aspect ratio. But sintered specimens in nitrogen atmosphere showed low aspect ratio and small grian size, becuase of the retardation of phase transformation and grain growth. Addition of Y-Sialon powder to SiC also retarded the phase transformation to ${\alpha}$-SiC from ${\beta}$-SiC and densification. The SiC specimen prepared from the starting ${\beta}$-SiC powder with Sialon composition(Y2O3, AlN, Si3N4) showed the highest fracture toughness about 6.0 MPa$.$m1/2.

• Journal of the Korean Ceramic Society
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• v.21 no.1
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• pp.11-18
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• 1984

$eta$-Sialon synthesis was investigated via the simultaneous reduction and nitridation of Hadong Pink Kaolin using the graphite as a reducing agent at 135$0^{\circ}C$ under 80% $N_2-20%H_2$ atmosphere. When Hadong Pink Kaolin-graphite-silicon nitride seed(molar ratio ; $SiO_2:C:Si_3N_4$=1;3.5:0.05) mixture was heated at 135$0^{\circ}C$ for as long as 20h in 80%$N_2-20%H_2$ atmosphere a homogeneous $eta$-Sialon$(Si_{3.5}Al_{2.5}O_{2.5}N_{2.5})$ was mainly formed together with a small amount of $\alpha$-$Si_3N_4$.

• Journal of the Korean Ceramic Society
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• v.29 no.5
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• pp.347-356
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• 1992

Various kaolin samples with different alumina content were prepared from calcined admixture of kaolin and ammonium sulfate by varying the treatment time in sulfuric acid. Samples were nitridated under N2 or N2-H2 atmosphere with changing the amount of added carbon, the reaction time and temperature. As the alumina content lowered, the size of kaolin particles decreased and the specific surface area increased. XRD analysis indicated that ${\alpha}$-quartz remained by decomposition of halloysite and meta-halloysite. Experimental results of nitridation behavior are summerized as follows; 1) Nitridation under N2 atmosphere. With the increase of C/SiO2 ratio and with the decrease of Al2O3 content, disappearance of XRD pattern peaks of mullite, ${\alpha}$-quartz and ${\alpha}$-Al2O3 were accelerated at 1300$^{\circ}C$. SiC was the main phase in the reaction product of acid-treated kaolin samples nitridated at 1300$^{\circ}C$ for 10 hours regardless of C/SiO2 ratio. But the XRD peak intensities of ${\beta}$-Si3N4, ${\beta}$-sialon and SiC did not show much difference when untreated raw kaolin was fired at the same condition. When the ratio of C/SiO2 was 3.5, ${\beta}$-sialon and ${\beta}$-Si3N4 existed in the reaction product of about 22% alumina containing kaolin sample fired at 1350$^{\circ}C$ for 7 hours. Only ${\beta}$-sialon existed in the same sample fired at 1400$^{\circ}C$ for 10 hours. ${\beta}$-sialon was obtained from all of the acid-treated kaolin samples fired at 1400$^{\circ}C$ for 40 hours, but AlN and SiC remained in the untreated kaolin sample. Z value of the ${\beta}$-sialon obtained from the 22% alumina containing kaolin sample fired at 1400$^{\circ}C$ for 40 hours was about 1.3(XRD) and 1.5(EDS). 2) Nitridation under 80N2+2OH2 mixed gas atmosphere with the C/SiO2 ratio of 1 Mullite was not found, but ${\alpha}$-Si3N4, and ${\beta}$-sialon were present in the reaction product of about 22% alumina containing kaolin sample fired at 1300$^{\circ}C$ for 10 hours. When untreated kaolin sample was nitridated at the same condition, mullite remained. AlN and SiC were not found in the reaction product of about 22% alumina containing kaolin sample fired at 1350$^{\circ}C$ for 5 hours. On the other hand, AlN and SiC remained in the product of untreated kaolin fired at the same condition.

• The Korean Journal of Ceramics
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• v.1 no.1
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• pp.45-54
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• 1995

Four kinds of silicon nitride based ceramic materials have been hot pressed. Effect of the sintering additives on the phase transformation, microstructural development and mechanical properties was investigated. While sintering under the same condition a big difference among the microstructures of the specimens, they appeared alike if sintered to have a similiar $\alpha$-$\beta$ phase ratio. The specimen of the stoichiometric $\alpha$-$\beta$ sialon composition showed very limited amount of the intergranular glassy phase and a significant degree of the residual stress. It exhibited almost no strength degradation up to $1300^{\circ}C$, and the strength of the specimen degraded more as its composition deviated from the stoichiometry.

• Journal of the Korean Ceramic Society
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• v.28 no.3
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• pp.189-196
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• 1991

Si(OC2H5)4, commercial AlN and Y2O3 powder were used as the precusor of Si3N4, AlN, Y2O3, respectively. After Si3N4 powder was synthesized by carbothermal reduction and nitridation at 135$0^{\circ}C$ for 13h in N2 atmosphere, characteristics of synthesized powder and the ceramics sintered at 178$0^{\circ}C$ for 1h under 30MPa were investigated. In order to evaluate the reliability of sintered body, Weibull modulus was investigated. Premixing of carbon black as a reduction agent had no effect on Si(OH)4 formation, and Si3N4 powder synthesized from Si(OC2H5)4 was $\alpha$-Si3N4 single phase. Mechanical properties of sintered body were measured as follows : flexural strength ; 750MPa, fracture toughness ; 3.71Mn/3/2, hardness : 17.4GPa, thermal shock resistence temperature ; $600^{\circ}C$. Flexural strength at room temperature was 750MPa and was retained up to 110$0^{\circ}C$. The Weibull modulus of sintered body was 10.7.