금속 알콕사이드로부터 Mullite 초미분체의 제조

임굉,임재석,김영호,Yim, Going,Yim, Chai-Suk,Kim, Young-Ho 한국재료학회 2006 한국재료학회지 Vol.16 No.12

Ultrafine mullite powder was prepared from aluminium-secbutoxide and tetraethyl orthosilicate(TEOS) in the molar $Al_2O_3/SiO_2$=3/2. Sol-gel method by partial hydrolysis technique, as it were, first, TEOS was partially hydrolysized and then mixed with Al-secbutoxide for complete hydrolysis was used. X-ray diffraction, infrared spectroscopy and transmission electron microscopy, etc. confirmed that the mullite powder prepared by this method is in the stoichiometric $Al_2O_3/SiO_2$ ratio. Al-Si spinel was formed at $980^{\circ}C$ and ultrafine mullite powder with about 20 nm particle size was obtained above $1,200^{\circ}C$. Also mullite powders calcined at $1,600^{\circ}C$ had a stoichiometric composition, $3Al_2O_3{\cdot}2SiO_2$ and the lattice constants of the mullite powders calcined above $1,200^{\circ}C$ were almost coincided with theoretical values.

알칼리 처리에 의한 Zeolite 광물의 물리화학적 특성

임굉,Yim, Going 배재대학교 자연과학연구소 1996 自然科學論文集 Vol.8 No.2

Zeolite인 mordenite 광물을 수산화나트륨용액으로 화학처리한 효과에 대해서 화학분석, X-선 분말회절, 열분석, 이산화탄소의 흡착측정 및 GC를 통하여 조사하였다. 출발원료로 mordenite 광물을 3시간동안 water bath 중 약 $95^{\circ}C$에서 NaOH 0.1-5N의 농도범위로 화학 처리한 결과, 시료중 함유된 모든 화학성분은 NaOH 0.5N 이하의 농도에서는 불용이고 mordenite 구조는 변화하지 않았으며 1N 이상의 농도에서는 실리카, 알루미나 등과 같이 성분들이 용해되었고 시료중 실리카의 용해비율이 알루미나의 용해보다 높으며 실리카와 알루미나의 비가 2-3N 농도 범위에서는 급격히 감소하였다.Mordenite 의 (202)면의 X-선 회절피크 강도와 $CO_2$ 흡착량은 1N 이상의 NaOH 농도가 증가함에 따라 감소하며 이로 인하여 mordenite 구조의 붕괴가 나타났다.산소, 질소 및 일산화탄소의 GC분리공정에서는 NaOH 용액 처리에 의한 영향을 받지 않으나 메탄과 크립톤의 용출피크가 넓어지는 경향이 나타나며 retention time 은 단축되었고 이 두 기체모두 용리피크는 산소 또는 질소와 중복되기 쉬운 경향을 보여주었다. The effect of sodium hydroxide treatment on some physicochemical properties of zeolite mordenite mineral was studied with chemical analyses, powder X-ray diffraction, thermal analyses, infrared analysis, measurement of carbon dioxide adsorption and gas chromatography. Mordenite mineral from tuffaceous rocks in Yeongil and Wolsung area was used as a starting material and treated with 0.1-5N NaOH aqueous solution at about $95^{\circ}C$ in the water bath for three hours.At the concentration of sodium hydroxide below 0.5N, all chemical compositions in the tuff were virtually insoluble and the mordenite structure did not change. At the concentration above 1N, the chemical compositions such as silica, alumina, etc., were dissolved. The dissolution ratio of silica was lager than that of alumina, and the ratio of silica to alumina in the tuff decreased sharply in the concentration range of 2 to 3N. Intensity of X-ray diffraction peak of mordenite (202) plane and the adsorbed amount of carbon dioxide also decreased with the increasing concentration of sodium hydroxide above 1N. These decreases corresponded to the degree of mordenite structure collapsed.The separation of gas chromatography of nitrogen, oxygen and carbon monoxide was not affected by the sodium hydroxide treatment, but elution peaks of methane and krypton tended to be broadened and their retention time was shortened. The elution peaks of both methane and krypton tended to be overlapped with those of nitrogen and oxygen.

기.고 크로마토그래피법에 의한 이산화질소 측정

임굉,Yim, Going,Serth Robert W. 배재대학교 공학연구소 1997 공학논문집 Vol.2 No.1

이산화질소는 Linde Molecular Sieve 칼럼에 흡수된 물에 의해 일산화질소로 급속히 전환된다. 합성된 파형은 칼럼에 도입된 순수 일산화질소의 것과 구별할 수 없는 것이다. 따라서 저비점 일산화질소로 전환함으로써 유기분배액의 산화의 복잡성은 미연에 방지된다. Nirogen dioxide is rapidly converted to nitric oxide by the water absortbed on a Linde Molecular Sieve column. The resultant wave form is indistinguishable from that of pure nitric oxide introduced to the column. Thus, by conversion to the low boiling nitric oxide, the complication of oxidation of organic partitioning liquids is obviated.

Tricalcium silicate의 수화반응에 따른 $T1_2CO_3$의 영향

임굉,Yim, Going 배재대학교 자연과학연구소 1991 自然科學論文集 Vol.4 No.-

규산삼석회$(C_3S)$의 수화반응에 있어서 $T1_2CO_3$의 농도변화에 따른 영향에 대해서 Isothermal microcalorimeter 등을 이용하여 조사한 결과, $T1_2CO_3$의 존재로 인하여 $C_3S$의 수화반응은 촉진되고 $C_3S$의 농도가 급격히 감소된다. 또 $T1_2CO_3$의 농도증가로 인해서 수화반응속도도 증가하고 있다. $T1_2CO_3$ 첨가에서 수화된 $C_3S$의 분석결과로는 반응초기에 $CaCO_3$가 나타나고 있으며, $T1_2CO_3$의 촉진작용이 수화반응의 초기에 있어서만 더욱 분명하게 나타나고 있음을 $C_3S$의 비휘발성 수분함량과 수화도로서 알수 있고 $C_3S$ paste와 접촉하고 있는 액상의 조성은 $T1_2CO_3$의 존재로 인하여 $Ca^(++)$이온과 $OH^-$ 이온의 농도가 상당히 변화하고 있음을 알 수 있다. The influences of various concentrations of thallium carbonate on the hydration of tricalcium silicate which is widely used to the inorganic materials have been studied using an isothermal microcalorime-ter. The experimental results indicate that the hydration of tricalcium silicate is accelerated in the presence of thallium carbonate, namely the concentration of thallium carbonate is increased, the rate of hydration is also increased. The x-ray diffraction analysis shows that the concentration of tricalcium silicate decreases rapidly in the presence of thallium carbonate. Differential thermal analysis of tricalcium silicate hydrated in the persence of thallium carbonate indicates the presence of calcium carbonate. The nonevaporable water content and the degree of hydration of tricalcium silicate show that the accelerating action of thallium carbonate is more pronounced only during the early period of hydration. Analytical results of the liquid phase in contact with the tricalcium silicate paste indicate that the concentrations of calcium and hydroxyl ions are changed considerably in the presence of thallium carbonate.

고상반응식을 이용한 석회-석영의 수열반응속도와 반응메카니즘

임굉,Lim, Going 배재대학교 공학연구소 1998 공학논문집 Vol.3 No.1

고상반응식을 이용한 석회와 석영과의 수열반응속도 및 반응메카니즘에 관하여 연구하였다. 출발물질로 석영과 수산화칼슘 CaO/$SiO_2$몰비 0.8-1.0로 혼합하고 $180-200^{\circ}C$, 0.5-8시간동안 포화증기압하에서 오토클레이브로 수열반응을 행하였다. 수열반응속도는 총 석회의 양과 총 석영의 양에 대한 미반응 석회의 양과 미반응 석영의 양의 비로 구하였다. 반응속도는 Jander의 식 $[1-(1-\alpha)^{1/3}]^N=Kt$를 이용하여 얻은 결과, 석회의 반응속도는 N=1로서 주로 용해속도에 의해 지배되고 석영의 반응속도는 $N\risingdotseq2$로서 확산에 의해 주로 지배된다. 규산칼슘수화물계의 수열반응속도는 반응물 입자주위에 형성된 생성물층을 통한 물질전달에 의해 율속되는 것으로 추정되고 전체 수열반응의 속도식은 대략 $N=1-2$로서 경계층으로부터 확산에 의해 율속과정으로 전환된다. The kinetic and mechanism of the hydrothermal reaction between lime and quartz used solid state reaction equations have been investigated. Hydrothermal reaction on the starting materials was carried out in an autoclave that quartz mixed with calcium hydroxide in CaO/$SiO_2$ ratio of 0.8-1.0 for 0.5-8 hour at saturated steam pressure of $180-200^{\circ}C$. The rate of reaction was given from the ratio of uncombined lime and quartz content to the total lime and quartz content. The rate of reaction was obtained the results by the Jander's equation $[1-(1-\alpha)^{1/3}]^N=Kt$. The reaction of lime is controlled mainly by the dissolution such as N=1, and the reaction of quartz is controlled mostly by the diffusion such as $N\risingdotseq2$. The rate of hydrothermal reaction in the calcium silicate hydrates system is suggested to be determined generally by the mass transfer through the product laver formed around the reactant particles. The rate equation for whole hydrothermal reaction is shown that it is converted into the rate determining step by the diffusion from the boundary reaction such as approximately $N=1-2$.

화학처리에 의한 천연 Zeolite의 Gas 분리

임굉,Im, Goeng 배재대학교 자연과학연구소 1992 自然科學論文集 Vol.5 No.1

결정성 aluminosilicate 광물의 일종인 천연 zeolite는 광물학적 특성과 화학적 표면활성으로 인하여 다방면의 공업화학적 이용가치가 매우 높고 광물중 특히 가장 높은 양이온교환능을 가지고 있어 기체분자에 대한 선택적 흡착력이 큰 molecular sieve로써 흡착분리제로는 물론, 건조제, 흡습제, 이온교환체, 촉매, 증량제 그리고 폐수처리제, 경수의 연화제등으로 이용도가 날로 증가하고 있다. 국내산 천연 zeolite를 IN HCL용액과 NaCl용액으로 화학처리하여 다공성을 증가시켜 column충전제로 사용한 결과, 혼합기체 Ar, $N_2$ CO및 $CH_4$의 분리특성에 관해서 HCL용액으로 처리한 mordenite 시료는 활성화온도가 $300^{\circ}C$일 경우, CO와 $CH_4$의 분리는 곤란하나 $350^{\circ}C$에서는 분리가 용이하였고 NaCl용액으로 처리한 시료는 미처리한 것과 거의 유사하였다. Ar과 $N_2$와의 분리에는 산 또는 알칼리로 화학처리한 시료에도 별로 효과가 없었으나 HCL용액과 NaCl용액을 연속적으로 처리한 천연 zeolite는 합성 zeolite의 특성에 견줄만한 정도로 기체분리효과와 HETP값을 보여주었다. 한편 시료의 화학처리에 의한 Ar과 CO의 흡착열의 변화는 극성기체인 CO의 경우, 별로 변화가 없지만 무극성기체인 Ar은 영향을 받기가 용이하였다. 또한 carrier gas He의 유속이 대략 20~30ml min범위일때 최소의 HETP값을 가지며 column의 효능이 좋았다. In the our country, especially in Yeongil and Wolsung area, abundant authigenic zeolites are found from the tuffaceous sediments and volcanic rocks of Miocene age showing wide variation in their mineralogy and abundance from horizon to horizon. The principal zeolite species identified are clinopti-lolite. mordenite. heulandite. ferrierite, and erionite. etc. Zeolite minerals are widely used in many countries in the following applications; (a) in air separation adsorption processes; (b)as desiccants; (c)in inorganic building materials; (d)in papermaking; (e)in fertilizers; (f)as soilconditioners-this application is based upon the ability of the zeolite to ion exchange with soil nutrients; (g)in the treatment of radioactive wastes; and (h)as adsorbents for toxic gases, etc. In the present paper, using natural zeolite mordenite treated with IN hydrochloric acid or IN sodium chloride solution as column packings, separation characteristics of argon, nitrogen, carbon monoxide, and methane gases have been studied by gas chromatography. By the use of mordenite treated with hydrochloric acid solution, the tailing peak of methane showed from untreated mordenite was satisfactorily reduced, although it was difficult to separate it from carbon monoxide with a column activated at $300^{\circ}C$. Using a column activated at $350^{\circ}C$, methane could be separated from carbon monoxide easily but only carbon monoxide eluted as a bad defined peak. Mordenite treated with sodium chloride solution was generally similar to chromatograms obtained by using the untreated mordenite. Both the above chemical treatments of mordenite had little effect on the separations of argon and nitrogen. The separations and the HETP values obtained from natural zeolite mordenite treated with continuously hydrochloric acid and sodium chloride solutions were almost identical with those obtained with synthetic molecular sieve 5A zeolite. On the other hand, the efficiency of column was good in the range 20~3Oml/min of the carrier helium gas rate.

알루미나가 11Å Tobermorite의 수열합성에 미치는 영향

임굉,임재석,Yim Going,Yim Chai Suk 한국재료학회 2005 한국재료학회지 Vol.15 No.2

[ $11\AA$ ] tobermorite$(5CaO{\cdot}6SiO_2{\cdot}5H_2O)$ is synthesized from the mixtures of calcium hydroride and quartz using alumina in a molar ratio $Ca(OH)_2/SiO_2$ of 0.8 at $180^{\circ}C$ for 8 and 24 hrs under saturated steam pressure. The influence of alumina on the formation of $11\AA$ tobermorite was investigated by X-ray diffraction, differential thermal analysis and infrared spectroscopy. $11\AA$ tobermorite containing increasingly larger amounts of aluminum showed a shift of the basal spacing from 11.3 to $11.6\AA$. In general, there was a direct linear relation between the basal spacing and added content of alumina. The differential thermal analysis curves showed that $11\AA$ tobermorite with increasing alumina contents exhibited the exothermic peak at high temperature, namely $11\AA$ tobermorite containing aluminum gave a sharp exothermic peak at temperature around $850\~860^{\circ}C$ in the case of $S_3\~S_5$. The absorption band at $1607\~1620cm^{-1}$ is attributed to the bending vibration of water, and the position of the main O-H stretching and Si-O lattice vibration of $11\AA$ tobermorite at 3500 and $965cm^{-1}$ respectively is not altered. Consequently the existence of alumina accelerates the crystallization of $11\AA$ tobermorite, and that the aluminum ion appears to substitute for the silicon ion in $11\AA$ tobermorite structure. Al-containing tobermorite is distinguished from Al-free tobermorite.

임의의 벽면온도에 따른 수평채널에서의 비정상 자연대류운동

임굉,Im, Goeng 배재대학교 공학연구소 1997 공학논문집 Vol.1 No.1

실내를 따뜻하게 하기위한 고온의 라디에이터, 냉동코일, 변압기, 전기가열장치 및 전자장비에서와 같이 자연대류에 의한 에너지전달은 여러 공업분야에 응용되고 있다. 일반적으로 임의의 벽면온도에 따른 수평채널에서의 비정상자연대류흐름과 수학적.물리적 대류이동에 관한 기본법칙을 고찰하였다. 전달문제에 관한 물리적 의미있는 엄밀해는 표준유한정현변환기법을 적용함으로써 폐쇄형에 있어서 얻어진다. 또한 최종 정상상태의 유동과 열전달을 초래하는 Pr수와 Ra수 등 기본매개변수의 영향에 대해서 각각 검토하였다. 축방향의 평균속도를 측정하는 Pr수가 Pr>1 과 Pr<1 일 경우 각각 시간차에 접근하고 또한 축방향의 온도구배를 대표하는 함수는 기본매개변수가 없으므로 영향을 받는 것이라 본다. 그러나 정상상태의 유동현상은 Ra수에 따라서만 영향을 받게된다. 자연대류는 여러 가지 전기기구들은 물론이고 파이프장치 등의 열전달에 큰 영향을 미친다. 또한 열전달과정이 포함되는 바다와 대기의 운동과 같은 지구의 환경과학에도 중요하다. Energy transfer by free convection arises in many engineering applications, such as a hot steam radiator for heating a room, refrigeration coils, electric transformers, heating elements and electronic equipments. Generally unsteady natural convection flow in a horizontal channel with arbitrary wall temperatures and the mathematical and physical basis of convection transport has been considered in general. A physically meaningful exact solution of the problem has been obtained in a closed form by the application of the standard finite sine transform technique. Influences of the governing parameters, the Prandtl number and the Rayleigh number, to bring the flow and heat transfer to final steady states have been discussed separately. For constant values of the arbitray wall temperatures and of the function, determining the average axial velocity, the final steady state is approached in different times respectively for the cases when the Prandtl number Pr>1 and Pr<1. It is also seen that the function, representing the axial temperature gradient, is influenced by none of the governing parameters : but the steady state flow is influenced only by the Rayleigh number. There are, of course, many applications. Free convection strongly influences heat transfer from pipes and transmission lines, as well as from various electronic devices. It is also relevant to the environmental sciences, where it is responsible for oceanic and atmospheric motions, as well as related heat transfer processes.

Potassium Chloride로부터 Nitrogen Dioxide 반응에 의한 Potassium Nitrate로의 전환

임굉,Yim, Going 배재대학교 자연과학연구소 1996 自然科學論文集 Vol.8 No.2

염화물을 이산화질소기체로 반응시킬때와 같이 고체 염화칼륨으로부터 고체 질산칼륨으로의 직접적인 전환이 질산칼륨의 생성을 암시하고 있음을 확인하였다. 또 열역학적 추정에 있어서 자유에너지 변화는 상온에서 유리하며 발열반응을 보여준다. 그리고 높은 수율과 함께 적은양의 물존재로 인하여 상온에서 반응이 일어나며 반응생성물에서 염화니트로실이 동시에 생성되고 있다. The direct conversion of solid potassium chloride to solid potassium nitrate by the reaction of the chloride with gaseous nitrogen dioxide is suggested for the preparation of potassium nitrate. Thermodynamic calculations indicate that the free energy change is favorable at ordinary temperatures and that the reaction is exothermic. Experiments are described in which it was found that the reaction takes place at ordinary temperatures in the presence of a small amount of water with good yield. Nitrosyl chloride is produced simultaneously.

B_2O_3 添加劑에 의한 BaFe_12O_19의 製造 및 磁氣特性

任宏,梁重植 慶熙大學校 1989 論文集 Vol.18 No.-

The-barium ferrite. BaFe_12O_19 of magnetoplumbite structure is chemically stable and have excellent magnetic properties. The ferrite BaFe_12O_19 is widely used in permanent magnets because of its large coercive force and saturation magnetization, which is derived from the large magnetocrystalline anisotropy, and its fine grain structure. In the present paper, BaFe_12O_19 powders were prepared by the solid state reaction technique of iron oxides and barium carbonate at low temperature without milling by using the boric oxide as a additive, and then magnetic properties with various starting materials, influence of additive on formation, and physical properties of powders, and the formation process were studied. The homogeneous and fine particles which have excellent magnetic properties were formed by heating at 900℃ for two hours with 3wt% B_2O_3 addition to Fe_3O_4. The typical values of the saturation magnetization, coercivity, and remanence ratio of the obtained powders are 42.5emu per gram, 2650 oersted, and 0.57, respectively. The average grain size for BaFe_12O_19 is about 0.2 micron. The obtained BaFe_12O_19 fine particles would be appreciated as perpendicular magnetic recording media. The results considered together successfully account for the effects of B_2O_3 on the growth of barium ferrite particles. The mechanism of the formation of the Ba-Ferrite thus take place in the following two step processes regardless of the type of Fe_2O_3 used in the mixtures. BaCO_3 + 6Fe_2O_3 → BaFe_2O_4 + 5Fe_2O_3 + CO_2 BaFe_2O_4 + 5Fe_2O_3 → BaFe_12O_19