• 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.

• Journal of the Korean Ceramic Society
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• v.33 no.2
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• pp.169-176
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• 1996

The specimens which were prepared from $\alpha$-Si3N4 with additions of YAG(3Y2O3.5Al2O3)-10 wt% and various AlN contents were sintered in N2 atmosphere at 1$700^{\circ}C$ The effect of $\alpha$,$\beta$-solid solution contents and sintering time on mechanical properties were investigated. As the content of $\beta$-solid solution and sintering time increased the hardness is reduced but the hardness of specimen sintered over 10 hours is constant irrespective of sintering time. While the fracture toughness increased with increasing of $\beta$-solid solution and sintering time. The fracture toughness of specimen with 80% $\beta$-solid solution content increased from 3.89 to 6.66 MPam1/2 with sintering sintering up to 20 hours/ But the amount of increased fracture toughness of specimen with below 20% $\beta$-solid solution content is not significant.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2006.09b
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• pp.866-867
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• 2006

This work will report a highly textured ${\beta}-Si_3N_4$ ceramic by aqueous slip casting in a magnetic field and subsequent pressureless sintering, Effects of the sintering aids, polymer dispersant, pH and stirring time on the stability of the $Si_3N_4$ slurries were studied. The textured ${\beta}-Si_3N_4$ with 97 % relative density could be obtained by slip casting in a magnetic field of 12 T and subsequent sintering at $1800^{\circ}C$ for 1 h. The textured microstructure is featured by the alignment of c-axis of ${\beta}-Si_3N_4$ crystals perpendicular to the magnetic field, and the Lotgering orientation factor, f, is determined to be 0.8.

• Journal of the Korean Ceramic Society
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• v.33 no.8
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• pp.871-876
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• 1996

It is believed that fly ash could be suitable for preparing the sialon by carbothermal reduction method because the total amount of SiO2 and Al2O3 is above 80% and the unburned residual carbon is above 5% within the fly ash. The effects of reaction temperature (1350, 1400, 145$0^{\circ}C$) reaction time (1, 5, 10 hours) and the amount of carbon additions (C/SiO2=2, 3, 4 mole) on the $\beta$-sialon synthesis were obserbed, It was conformed that $\beta$-sialon (Z=2.15~2.18) was formed as major phase under all of the synthesis conditions and small amount of Si2ON2 SiC, AlN and Si3N4 was formed depending on the synthesis conditions. FeSix intermetal-lic compound was formed above 140$0^{\circ}C$ reaction temperature due to the large amount of iron oxides within the raw fly ash.

• Journal of the Korean Ceramic Society
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• v.25 no.5
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• pp.561-569
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• 1988

Mixtures of very small amounts of additive, carbon and silica(about 0.46${\mu}{\textrm}{m}$) which synthesized by the hydrolysis of ethyl silicate, the molar ratio of SiO2/C was fixed to 1/10, was nitrided at 145$0^{\circ}C$. It was considered that the optimum amount of additive to promote the nitridation reaction was below 2.0wt%. By the addition of additive, the nitridation reaction was promoted and formation of $\beta$-Si3N4 was promoted at 145$0^{\circ}C$ for 1hour, but, the nitridation reaction was decreased and the ratio of $\alpha$/$\beta$ of Si3N4, was increased at 145$0^{\circ}C$ for 5 hours. The crystal phase was $\alpha$ phase and the nitridation reaction was promoted and the particle size of silicon nitride was become smaller by the addition of $\alpha$-Si3N4, but silicon nitride of whisker-like form was produced by the addition of transition elements. There was a difference in the lattice constants of $\alpha$-Si3N4, but no difference in its of $\beta$-Si3N4 according to kinds of added substance and reaction time.

• Proceedings of the Korean Ceranic Society Conference
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• 2003.04a
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• pp.61.1-61
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• 2003

• Proceedings of the Korean Ceranic Society Conference
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• 2002.10a
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• pp.177.2-177
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• 2002

• Korean Journal of Materials Research
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• v.14 no.5
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• pp.358-362
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• 2004

$Si_3$$N_4$ ceramics have been identified as one of the promising structural ceramics. This study has been carried out to investigate of the synthetic behaviors of $Si_3$$N_4$ derived from domestic silica-stone by direct nitriding method. The silicon nitridation reaction has been studied in the temperature range of $1300～1550^{\circ}C$. Below the $1400^{\circ}C$, the nitriding rate was measured to be 16%. For the temperatures higher than the $1400^{\circ}C$, $\beta$-$Si_3$$N_4$ phase was formed mainly, and the nitriding rate showed above 98%. With the increasing of sample weight of silicon powder, the nitriding rate and $\beta$-$Si_3$$N_4$ phase increased at $1400^{\circ}C$ for 2 hours. The shape and particle size of$ Si_3$$N_4$ powder synthesized at $1400^{\circ}C$ for 2 hours showed the irregular angular-type and 10 $\mu\textrm{m}$, respectively.

• Journal of the Korean Ceramic Society
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• v.38 no.5
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• pp.405-411
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• 2001

Compacts of a mixture of fine $\alpha$-Si$_3$N$_4$powders, 6% $Y_2$O$_3$and 1% $Al_2$O$_3$were attrition milled time on phase and microstructural development in silicon nitride ceramics. The sintered surface and the interior showed different behaviors in phase and microstructral developments. Increased oxygen content with increased milling time of powder mixture leads to the formation of Si$_2$$N_2$O phase at temperatures as low as 155$0^{\circ}C$. Si$_2$$N_2$O is stable in the interior of the samples but unstable in the surface region of the specimen sintered at higher temperature. This results in a duplex structure where the interior consists of Si$_2$$N_2$O grains dispersed in $\beta$-Si$_3$N$_4$matrix and a surface which contains only $\beta$-Si$_3$N$_4$. The alpha to beta phase transformation and the microstructural development are shown to be influenced by the formation and decomposition of the Si$_2$$N_2$O.

• Journal of the Korean Ceramic Society
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• v.31 no.2
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• pp.129-136
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• 1994

Si3N4 with 6w/o Y2O3 and 1.5w/o Al2O3 has been gas pressure sintered and its densification behavior and the effect of the sintering variables on the microstructure and mechanical properties were investigated. Densification rate was higher at temperature below 1775$^{\circ}C$ and between 187$0^{\circ}C$ and 195$0^{\circ}C$ than between 1775$^{\circ}C$ and 187$0^{\circ}C$. The faster densification at temperature between 187$0^{\circ}C$ and 195$0^{\circ}C$ was thought to be due to the increased amount of liquid phase resulting from the increased amount of Si3N4 dissolving in the liquid. $\beta$-Si3N4 and Y-disilicate at temperatures below 1775$^{\circ}C$, and only $\beta$-Si3N4 at 187$0^{\circ}C$ and above were detected by XRD analysis. Three different two-step schedules were employed to obtain sintered body with above 99% theoretical density and to investigate the effect of the sintering variables on the density, the microstructure and the mechanical properties of the sintered body. The sintered density did not change with the heating rate, and the microstructure became coarser as the temperature increased. The strength decreased with the width of $\beta$-Si3N4 grain, while the fracture toughness increased with the square root of it. A ceramic cutting tool made of the sintered body showed an uniform flank wear after the cutting test.