• 한국재료학회지
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• 제13권4호
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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.

• 한국세라믹학회지
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• 제28권9호
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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$0^{\circ}C$).

• 한국세라믹학회지
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• 제14권3호
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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.

• 보존과학회지
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• 제35권5호
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• pp.392-402
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• 2019

전북 완주 신풍유적 출토 고려시대 슬래그와 송풍관을 대상으로 신풍유적의 야동기술(冶銅技術)성격을 확인하고, 납 원료산지를 추정하기 위해 납동위원소비를 실시하여 알아보았다. 성분분석 결과, Cu-Sn-Pb 삼원계 합금하는 과정에서 비롯된 슬래그와 송풍관으로 해석되었다. 금속현미경과 주사전자현미경(scanning electron microscopy-energy dispersive spectrometer) 분석결과, 동괴와 주석괴에 방연석을 첨가하여 완제품 제작을 위한 중간소재를 생성하는 합금단계에서 발생한 부산물로 추정된다. 납동위원소비분석 결과, 한국 남부 Zone III 지역의 광산에서 채굴된 방연석을 사용하여 합금한 것으로 판단된다. 송풍관은 송풍관의 외측으로 갈수록 Mullite가 검출되어, 1,000℃ 내외에서 조업이 이뤄졌을 가능성이 있다.

• 한국광물학회지
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• 제11권2호
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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.

• 한국세라믹학회지
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• 제29권5호
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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.

• 보존과학회지
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• 제26권1호
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• pp.1-12
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• 2010

초 록 부여 쌍북리 유적에서 출토된 백제시대 도가니는 유리와 금속의 용융에 사용했던 것으로서, 기질은 대체로 경질이며 담갈색, 회청색 및 회갈색의 색조를 보인다. 태토에는 다량의 석영과 파쇄된 토기가 혼입되어 있으며, 외부에는 정선된 석영입자를 도포하여 도가니에 내화성을 부여하였다. 이 도가니는 운모류의 분해와 뮬라이트의 형성 및 장석류의 관찰여부로 볼 때, 공통적으로 $1,000^{\circ}C$ 이상의 소성을 경험한 것으로 판단되며 일부 도가니는 $1,100^{\circ}C$ 이상에서 열적 변화가 수반된 것으로 사료된다. 그러나 검출된 광물상의 특성을 고려할 때 소성 및 용융시 최대 상한 온도는 $1,200^{\circ}C$를 넘지 않았을 것으로 판단된다. 전암대자율 측정과 지구화학적 특성 분석에서 도가니 시료는 크게 두 그룹으로 분류되었으며, 이는 적어도 두 종류 이상의 성인이 다른 태토로 제작되었음을 지시한다. 그러나 도가니의 태토와 유적을 구성하는 토양의 풍화정도가 유사하고 주성분원소의 분포 또한 대체로 동일한 것으로 보아 유적이 위치한 이 일대의 충적층은 두 암종의 풍화산물이 혼재할 가능성이 매우 높다. 따라서 도가니를 구성하는 태토는 모암이 다른 쌍북리 일대의 풍화토로 구성되었던 것으로 판단된다.