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알루미나와 실리콘 지지체에 종자결정에 의한 제올라이트 MFI 필름의 합성
고태석,Ko, Tae-Seog 한국결정성장학회 2008 韓國結晶成長學會誌 Vol.18 No.1
c-축 배향을 갖는 MFI 제올라이트 필름$(<35{\mu}m)$을 종자결정 성장법을 이용하여 실리카라이트-1 종자결정이 도포된 알루미나와 실리콘 지지체 위에 성장시켰다. 지지체 표변에서 성장된 필름은 전자현미경과 X- 회절 분석을 이용하여 조사하였다. 지지체 표면의 거친 정도에 따른 필름의 성장에 미치는 영향에 대해서 조사하였으며 c- 축 배향을 갖는 필름과 종자결정 성장법에서 나타나는 특징적인 돔 형태의 결함구조의 생성과 반응기구에 대해서 설명하였다. 지지체 표면의 거친 정도가 c- 축 배향에 중요한 역할을 하였다. Contiuous c-oriented zeolite MFI films $(<35{\mu}m)$ were prepared by hydrothermal secondary growth of silicalite-1 seed crystal in the surface of alumina porous substrate and silicon substrate. The supported films were characterized with scanning electron microscopy and X-ray diffraction. Effect of substrate surface roughness were investigated and a mechanism for c-oriented film formation and characteristic dom-like defects formation which is observed after seeding growth was discussed. The roughness of substrate plays an important role.
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고태석,이기완 東新大學校 1998 論文集 Vol.10 No.-
Kaolinite has been hydrothermally synthesized at 220℃ for 15 days with various acidic solution using a mixture of silica monomer and gibbsite or boehmite with a Si/Al ration =1. Acid solution treatment for kaolinite synthesis promotes the dissolution of the starting materials and leads to crystallization in short induction periods. Kaolinite synthesized with gibbsite treated with nitric acid was synthesized in short induction period and 10 ㎛ cubic form crystal, but gave a lower crystallinity due to disordering of unit cell to crystal, whereas Kaolinite synthesized with gibbsite treated with chloric acid gave a higher crystallinity and 0.5 ㎛ hexagonal plate form crystal.
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고태석 東新大學校 工業技術硏究所 1998 工業技術硏究 Vol.4 No.-
Kaolinite was synthesized through the acid treatment of mixture which consisted of alumina sources and colloidal silica in hydrothermal reaction at 220℃ under autogeneous vapor pressure. Cubic shape of kaolinite whose size are 10 μm has been synthesized from the mixture of gibbsite and silica treated with 0.1 N nitric acid. Sperules were formed surrounding the cubic shape of kaolinite through disruption of the cubic shape of kaolinite. Spherules were associated in groups composed of very great number of individuals which grew to platy kaolinite. For kaolinte synthesis from the mixture of boehmite and silica monomer treated with chloric acid, we identified that spherical aggregates from amorphous gel were formed and grew to lath and platy kaolinites.
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Pseudoboehmite를 출발물질로한 kaolinite의 수열 합성
고태석 한국결정성장학회 2001 韓國結晶成長學會誌 Vol.11 No.1
$213^{\circ}C$에서 깁사이트와 pseudoboehmite를 출발물질로 하여 산성도를 변화시켜 수열합성법에 의해서 카올리나이트를 합성하였다. 합성된 카올리나이트는 X-선회절 분석기와 적외선 분광광도계를 이용하여 결정화 과정을 조사하였으며 Hinckley 지수를 계산하였다. 산을 이용한 카올리나이트 합성은 출발물질의 용해를 촉진시켜 결정화하였다. 결정화 속도와 적층결함은 음이온의 종류, 산성도와 출발물질에 의존하였다. Kaolinite was synthesized through th acid treatment of mixture which consisted of psudoboehmite and colloidal silica in hydrothermal reaction at $213^{\circ}C$ under autogeneous vapor pressure. Crystallization process was characterized by X-ray powder diffraction pattern, IR spectra and Hinckley index was calculated. The synthesis in acidic solution promotes the dissolution of the starting materials and leads to crystallization of kaolinite. The rate of crystallization to kaolinite and stacking defect were found to e affected by kind of anion, acidity and starting materials.
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수열반응에 의한 알루미나 지지체에 제올라이트 A 박막의 합성
고태석,Ko, Tae-Seog 한국결정성장학회 2007 한국결정성장학회지 Vol.17 No.3
The synthesis of NaA zeolite membrane on a porous alumina support from clear solution by using hydrothermal reaction was investigated. Effects of reaction temperature, reaction time and seeding for transformation of zeolite A membrane and powder which are produced in the reactor were monitored through X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM). The transformation process of producing Zeolite A membrane starts from the formation of the compact and continuous membrane on the surface of porous support from clear solution. The large Zeolite A poly-crystal was then farmed through the dissolution process. Finally, the process was advanced from sodalite to amorphous. In case of powder, sodalite is formed in the early stage of reaction because of surrounding space difference between membrane and powder crystal. Discrete surrounding space of powder crystal makes easy to transform to sodalite. From Zeolite A to amorphous through transformed product was rapidly advanced at high temperature while the membrane with somewhat low coverage was obtained at low temperature. A compact and continuous zeolite A membrane was synthesized at $120^{\circ}C$ in 12-hour period. 수열합성 장치를 이용하여 종자 결정이 도포된 알루미나 지지체 위에 제올라이트 박막을 합성하였다. X-선 회절 분석과 전자현미경 사진을 이용하여 반응기 내에 생성된 제올라이트 A 분말과 제올라이트 A박막의 생성과 전이 생성물에 대해 합성온도, 합성시간, 종자결정의 영향에 대해서 고찰하였다. 제올라이트 A박막의 생성은 지지체 표면에 도포된 종자 결정에서 치밀한 연속적인 박막이 형성된 다음 용해과정을 거쳐 결정의 크기가 큰 다결정 층을 형성하고, 최종적으로 소다라이트를 거쳐 무정형으로 진행하였다. 반면에 분말에서는 반응초기부터 소다라이트가 관찰되는데 고정된 제올라이트 A 박막과 다르게 결정주위의 공간적인 차이에 의해 소다라이트가 생성하기에 용이한 공간을 갖기 때문에 소다라이트가 쉽게 생성되는 것으로 생각된다. 합성온도가 높으면 짧은 시간 내에 전이 생성물을 거쳐 무정형으로 진행하였고 온도가 낮으면 합성 시간이 길고 피복도가 다소 낮은 제올라이트 A 박막을 얻었다. $120^{\circ}C$, 12시간에서 피복도가 높은 치밀한 제올라이트 A박막을 합성하였다.
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고정층 반응기에서 HZSM-5 제올라이트 촉매를 사용한 올레핀의 전환반응
고태석,김나현 東新大學校 1995 論文集 Vol.7 No.-
Conversion reactions of ethylene, propylene and 1-butene over HZSM-5 zeolite and phosphorus-impregnated catalyst were studied. Conversion of lower olefin was increased with the order of ethylene<propylene<1-butene, showed maxima at 300∼350 ℃. Selectivity to lower olefin increased with reaction temperature, while higher olefins decreased. The decrease patterns of reactant concentration with space time are different. The decreasing rate of reactant is low at short space time in the conversion of ethylene, while the rate is high in the conversion of 1∼butene at short space time. For the conversion of propylene, autocatalytic characteristics is observed. The reaction of lower olefin described very well with proposed reaction path, which composed of adsorption of olefin, oligomerization of gaseous olefin with adsorbed olefin, cracking of oligomerization olefin to various hydrocarbons. The difference in reactivities of lower olefins, the reduction of activity with phosphorus impregnation, and lower conversion at higher temperature can be explaned in terms of surface concentration of adsorbed reactant and interaction between catalyst and reactant.
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고태석,서곤 ( Tae Seog Ko,Gon Seo ) 한국공업화학회 1992 공업화학 Vol.3 No.1
Three solid acid catalysts developed recently are reviewed. Cloverite is a gallophosphate molecular sieve with very large pore, titanium silicate has a specific structure compared with conventional molecular sieves, and Envirocat is prepared for the replacement of aluminium chloride catalyst.
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