• Korean Journal of Materials Research
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• v.13 no.4
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• pp.251-258
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• 2003

The effects of the salt and the precursor pH on the synthesizing behavior and the morphology of mullite have been studied. Two kinds of mullite precursor sols were prepared by the dissolution of two kinds of salt (aluminum nitrate enneahydrate, Al($NO_3$)$_3$ㆍ$9H_2$O; type I and aluminum sulfate 14∼18 water, (SO$Al_4$)$_3$$\cdot$$14∼18H_2$O; type II) into the mixture of colloidal silica sol, respectively. Precursor pH of the sols was controlled to the acidic (pH= 1.5∼2) and basic (pH= 8.5∼9) conditions. The co-products with nitrate and sulfate were completely eliminated at $500^{\circ}C$ and $850^{\circ}C$, respectively, which was confirmed by TG/DTA results. The synthesizing temperature of mullite phase was found to be above $1200^{\circ}C$ for pH= 1.5∼2 and above $1300^{\circ}C$ for pH= 8.5∼9 in type I. However, in type II, the synthesizing temperature of mullite was decreased to $850^{\circ}C$ for pH= 1.5∼2 and $1100^{\circ}C$ for pH= 8.5∼9. The grain size of the mullite synthesized at pH= 8.5∼9 was larger than that at pH= 1.5∼2 in overall heat-treated temperatures, showing smaller grain size in type II. Aspect ratio of the mullite grains was more increased at pH= 1.5∼2 than pH= 8.5∼9 in type I, showing similar aspect ratio at both pH conditions in type II. It was found that the synthesizing temperature and grain size were predominantly governed by the initial precursor pH and decomposition of the salt, with minor effect on the grain morphology.

• Journal of the Korean Ceramic Society
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• v.28 no.9
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• pp.667-674
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• 1991

In this study, Kaolin was carbonized at 1300~175$0^{\circ}C$ and its constituent mineral change was investigated. Carbonized kaolin at 1$650^{\circ}C$ was mixed with metallic silicon, formed and nitrified at 135$0^{\circ}C$ in N2-NH3 atmosphere. Properties of this product such as porosity, bulk density, MOR, nitrization rate and oxidation resistence were measured, and its mineralogical changes were investigated by XRD. The results were as follows; 1) $\beta$-SiC was initially synthesized at 150$0^{\circ}C$, and its amount was continuously increased with reaction temperature to 1$700^{\circ}C$. 2) At 1$600^{\circ}C$, mullite was rapidly decomposed and the amounts of $\beta$-SiC and $\alpha$-Al2O3 were increased simultaneously. 3) By adding alkali to kaolin, the decomposition temperature of mullite was dropped approximately 10$0^{\circ}C$, but the amount of $\alpha$-SiC was increased. 4) The highest values of their nitrization rate and MOR were obtained at the specimen of 35 wt% metallic silicon in nitrization reaction. 5) It seems that increment of $\alpha$-Si3N4 and $\alpha$-Al2O3 phase during nitrization was due to the decomposition of Al4SiC4 existed in carbonized kaolin. 6) Si3N4 bonded SiC-Al2O3 composite were fabricated from kaolin at relatively low temperature (135$0^{\circ}C$).

• Journal of Conservation Science
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• v.35 no.5
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• pp.392-402
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• 2019

This study interpreted the characteristics of the site and provenance of raw material by performing material characteristics analysis of the slags and tuyeres excavated from the Sinpung site in Wanju, Jeollabuk-do. The major chemical compositions suggested that the slags and tuyeres were created when Cu-Sn-Pb was alloyed. Metal microscope and scanning electron microscopy-energy dispersive spectrometer analyses revealed that the slags and tuyeres were by-products formed in the alloying process. This alloy, created by adding galena to copper and tin ingots, was an intermediary material used in making the finished products. According to the lead isotope ratio analysis result, slags could be made using galena of the southern Zone III region of Korea. Based on the decomposition of mica group minerals and the formation of mullite detected through X-ray diffraction analysis, it is possible to conclude that the tuyeres operated at approximately 1,000℃ as, the mullite was detected on the outside of the tuyeres.

• Journal of the Korean Ceramic Society
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• v.14 no.3
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• pp.163-168
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• 1977

As a wet chemical drying process "hot petroleum drying method" was applied and developed for preparing uniformly fine oxide powder with high purity and sinterreactivity. Using this method solution of sulfates was dried in hot petroleum bath (~17$0^{\circ}C$) to sulfate powder from which corresponding mullite doped by Fe3+ ion was formed. Particle size, shape, decomposition by heat, and phase identification of sulfate andoxide powders determined by DTA, TGA, X-ray diffraction, analysis and electron microscopy: sulfate powder prepared by this drying method is an intimate mixture of the amorphous form of uniformly and finely distributed spherical particles (0.05-0.1$\mu$). Mullitization with the sulfate powder occurs at 110$0^{\circ}C$ in air. The morphology of mullite particle made by firing the sulfate powder at 135$0^{\circ}C$ in oxygen atmosphere is granular of 0.1-0.3$\mu$ in size. This drying process proved to be a very effective method for preparing fine, homogeneous, and highly sinterreactive multicomponent oxide powder without conventional ceramic process of mixing, milling, and granulating. This process can be also applied for preparing electronic ceramic materials which are requisite for high purity and homogeneity.mogeneity.

• Journal of the Mineralogical Society of Korea
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• v.11 no.2
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• pp.85-96
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• 1998

The sericite ore is formed by the hydrothermal alteration of rhyodacitic welded tuff. The alteration zone of the host rock can be classified into four types based on the mineral assemblages ; sericite, quartz-sericite, silicified and propylite zone. The sericite ore mainly occurs as vein types and fault clay along the fault plane in the quartz-sericite zone. Mineral components of the sericite ore are mainly sericite with minor diaspore, corundum and pyrite. The sericitic porcelaineous ore is mainly composed of quartz and sericite. Accessory minerals are muscovite, diaspore, sphene, corundum, pyrite, iron-oxides and etc. The chemical compositions of K2O, Al2O3, and ignition loss in the sericite ore increase largely than that of the host rock, while the compositions of SiO2, Na2O and Fe2O3 decrease. XRD patterns of the heat-treated sericite ores show the formation of mullite at $1,200^{\circ}C$. and the diaspore-bearing sericite ore forms mullite and corundum at $1,200^{\circ}C$. The differential thermal analysis of the sericite ores show small endothermic peak at 645~668$^{\circ}C$. and the diaspore-bearing sericite ore shows a strong endothermic peak at $517^{\circ}C$. It indicates that the decomposition of diaspore appear at lower temperature than that of sericite. The thermal expansivity of the sericite ores show the similar pattern. The sericite ores show the thermal expansivity of 3.3~4.7% at 900$^{\circ}C$ and 0.39~0.75% at 1,20$0^{\circ}C$, respectively. DTA-TG curves of the sericite ores show closely relations with the thermal expansivity.

• 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 Conservation Science
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• v.26 no.1
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• pp.1-12
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• 2010

The crucibles of Baekje Kingdom from the Ssangbukri Site which were used for glass and metal melting had light brown, grayish blue and grayish brown colored bodies. In thin section, the crucibles contained numerous quartz grains and pottery fragments. The surface was covered with fine grained quartz for thermal resistance. Based on decomposition of mica group minerals and formation of mullite detected by X-ray diffraction analysis, it was inferred that all crucibles have been fired over $1,000^{\circ}C$. It was also found that firing temperature has exceeded $1,100^{\circ}C$ in some crucibles because feldspar was not detected. The maximum temperature was assumed at $1,200^{\circ}C$. The magnetic susceptibility values and geochemical characteristics sorted out the crucibles into two groups that differed from the characteristics of the local soils. This reflected geological setting of the site where the alluvium was formed from two kinds of surrounding rock masses, granite gneiss and biotite granite. However, the local soils had similarities with the crucibles in weathering degree and geochemical behavior of major elements. In consequence, it was considered that the raw clay of the crucibles was supplied from the local area of the site.