• Proceedings of the Korea Association of Crystal Growth Conference
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• 1996.06b
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• pp.219-222
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• 1996

수열법은 밀폐용기중에서 10$0^{\circ}C$이상의 가열, 가압된 수용액이 반응에 관여하는 것으로써, 수정, CaCO3, AlPO4, GaPO4 등과 같은 단결정의 육성 뿐만 아니라 균일분산계로부터 균일한 결정성의 미립자 합성에도 폭넓게 이용되고 있다. 세라믹분말의 합성에 있어서, 이 방법은 특히 형상, 입자크기의 제어가 용이할 뿐만 아니라 고상법, 졸-겔법, 공침법에서와 같은 열처리, 분쇄과정이 필요없기 때문에 고순도의 초미립자를 얻을 수 있는 장점이 있다. 근년 미국, 일본에서는 수열법을 이용한 유전, 압전체 등 세라믹분말의 일부가 공업적인 규모로 대량 생산되고 있다. 그러나 이에 대한 국내 기술은 아직 초기단계에 이르고 있는 실정이다. 따라서 본 연구실에서는 수열법에 의한 단결정 육성 (예; 자수정, CaCO3, AlPO4, GaPO4, KTP, Emerald 등), 박막제조 (예; GaP, PbTiO3, BaTiO3 등), 정제 (고령토, 장석, 도석 등), 원석처리 (진주, 인공 emerald, 비취 등) 그리고 각종 세라믹분말의 합성 등과 같은 다양한 기반기술의 축적과 동시에 공업화에 대응한 수열장치를 위하여 반응용기의 대형화, 엄밀한 밀폐방식, 실용적인 수열조건 등을 개발해 오고 있다. 본 발표에서는 현재까지의 연구개발 내용 중에서 결정성 미립자에 관련한 세라믹분말의 합성에 대한 일부의 결과들을 보고한다. 일반적으로 수열장치는 전기로, 반응용기, 온도 및 압력제어계 등을 기본으로 하고 있으며 시판용의 대부분이 교반기가 부착된 수직형 (vertical type)이다. 이와 같은 방식에 있어서는 엄밀한 밀폐가 곤란, 반응온도의 한계성 (25$0^{\circ}C$ 이하), 증진율의 한계성 (소량생산) 등과 같은 점이 있기 때문에 본 연구실에서는 개폐식 전기로내에 엄밀한 밀폐가 가능한 수평식(horizontal type)의 반응용기를 채택한 뒤 이를 회전 또는 시이소(seesaw)식으로 움직일 수 있도록 하여 연속공정화, 온도구배의 자율조절 그리고 보다 저온에서도 인위적인 이온의 확산을 효율적으로 유도할 수 있도록 하였다. 이와 같은 방식은 기존의 방식과 비교하여 반응용기 내에 응집현상과 미반응물이 존재하지 않으며 또한 단분산으로 결정성 미립자를 대량적으로 얻을 수 있는 장점이 있었다. 다음은 이상과 같이 본 연구실에서 자체 개발한 수열장치를 이용하여 PbTiO3, (Pb,La)TiO3Mn, BaTiO3, ZnSiO4:Mn, CaWO4 등과 같은 세라믹분말에 대한 합성 실험의 결과이다. 압전성, 초전성이 우수한 PbTiO3 및 (Pb,La)TiO3:Mn 분말의 수열합성은 PbO, TiO2, La2O3 등의 분말을 출발원료로 하여 합성도도 25$0^{\circ}C$부근의 알카리성 용액중에서 결정성 PbTiO3 및 (Pb,La)TiO3:Mn 미립자를 단상으로 얻었으며 입자의 형상 및 크기는 합성온도와 수열용매의 종류에 의존하였다. 유전체로서 폭넓게 응용되고 있는 BaTiO3 분말은 Ba(OH)2.8H2O, TiO2와 같은 최적의 출발원료를 선택함으로써 15$0^{\circ}C$ 부근의 저온영역에서도 용이하게 합성할 수 있었다. 특히 본 연구에서는 수용성인 Ba(OH)2.8H2O를 사용함으로써 host-guest적인 반응을 유도시키는데 있어 물의 가장 실용적이고 효과적인 수열용매임도 알았다. ZnSiO4:Mn, CaWO4, MgWO4와 같은 형광체 분말은 공업적으로 고상반응 또는 습식법에 의해 얻어지고 있으나 이들 방법에 있어서는 분쇄공정으로 인한 형광특성의 저하와 같은 문제점이 있다. 따라서 본 연구에서는 수열법을 이용하여 이들 화합물의 합성을 시도하였으며 그 결과 합성온도 30$0^{\circ}C$ 부근의 알칼리성 용액중에서 수열적으로 얻어짐을 알았다. 여기서의 합성분말을 이용하여 실제 조명램프로 제조한 결과 녹색, 청색 발광용 형광체로서 우수한 형광특성을 나타내었다. 천연에서 소량 산출되고 있는 고가의 (Li,Al)MnO2(OH)2:Co 분말은 도자기의 전사지용 청색안료로써 이용되고 있다. 본 연구실에서는 LiOH.H2O, Al(OH)3, MnO2 등의 분말을 출발원료로 하고 24$0^{\circ}C$ 온도 부근 그리고 물을 수열용매로 하여 천연산에 필적하는 (Li,Al)MnO2(OH)2:Co 분말을 인공적으로 합성하였다.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.3 no.1
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• pp.12-17
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• 1993

Growth runs of KTP single crystals were carried out by the hydrothermal method. KTP powders used for the crystal growth were prepared as a single phase by the solid state reaction of a stoichiometric mixture of $KH_2PO_4 and TiO_2$ at TEX>$800^{\circ}C$ and subsequently by the hydrothermal treatment at $250^{\circ}C$ 4m KF solution. The most effective solvents for the crystal growth of KTP were KF and K $K_2HPO_4$ solutions. Solubilities of KTP in these solutions were positive over the range $350~450^{\circ}C$.Seed crystals of good quality could be obtained by the horizontal temperature gradient method at temperatures over the range 380~430^{\circ}C$ in these solutions. The hydrothermal conditions for the high growth rates of seed crystals are as follows: growth method; vertical temperature gradient method, solvent; 4m KF or $K_2HPO_4$ solution, temperature region; $400~450^{\circ}C$, pressure region; $1000~1500kg/cm^2$, where solubility of KTP was large enough to proceed the growth. Under such conditions, seed crystals of KTP are grown at a rate of approximately 0.06-0.08mm/day in the direction of the c-axis. Morphologies of grown crystals tended to be bounded by (100), (011) and (201) faces.

• Journal of Hydrogen and New Energy
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• v.29 no.2
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• pp.170-180
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• 2018

After $MoS_2$ catalyst was prepared at 1, 30, and 70 atm, the hydrothermal pressure effect over preparation of $MoS_2$ was investigated in terms of catalyst characterization and direct methanation. Multifaceted characterization techniques such as XRD, BET, SEM, TPR, EDS, and XPS were used to analyze and investigate the effect of high pressure over the preparation of surface and bulk $MoS_2$ catalyst. Result from XRD, SEM, and BET demonstrated that $MoS_2$ was more dispersed as preparation pressure was increased, which resulted finer $MoS_2$ crystal size and higher surface area. EDS result confirmed that bulk composition was $MoS_2$ and XPS result showed that S/Mo mole ratio of surface was about 1.3. TPR showed that $MoS_2$ prepared at 30 atm possessed higher active surface sites than $MoS_2$ prepared at 1 atm and these sites could contribute to higher CO yield during methanation. Direct methanation was used to evaluate the CO conversion of the both catalysts prepared at 1 atm and 30 atm and reaction condition was at feed mole ratio of $H_2/CO=1$, GHSV=4800, 30 atm, temperature($^{\circ}C$) of 300, 350, 400, and 450. $MoS_2$ prepared at 30 atm showed more stable and higher CO conversion than $MoS_2$ prepared at 1 atm. Faster deactivation was occurred over $MoS_2$ prepared at 1 atm, which indicated that preparation pressure of $MoS_2$ catalyst was the dominant factor to improve the yield of direct methanation.

• Journal of the Korean Society for Geothermal and Hydrothermal Energy
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• v.16 no.1
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• pp.9-16
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• 2020

In this study, a numerical study was conducted to evaluate the performance improvement when CuO nanofluid was used in the plate heat exchanger. As a result, the heat transfer amount is increased by 5.45% when 2 vol% CuO nanofluid is used. The influence on the CuO nanofluid on the performance of heat exchanger is decreased by increasing the flow rate of working fluid. In addition, the overall heat transfer coefficient using 2 vol% CuO nanofluid decreased compared to the base fluid. However, the pressure drop and the consumption of the pump power is increased as the concentration of CuO nanofluid increased because the increase of the viscosity. These are increased up to 15.4% compared to those of the base fluid. Moreover, the performance index of CuO nanofluid is decreased by 12.6% compared to that of the base fluid.

• Journal of the Korean Society for Geothermal and Hydrothermal Energy
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• v.15 no.4
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• pp.46-54
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• 2019

In this study, the performance of a shell and tube heat exchanger (STHE) and welded plate heat exchanger (WPHE) was measured experimentally. The pass numbers of the STHE was changed by 1, 2 and 4. As a result, the WPHE showed 2.1 times higher heat exchange capacity than that of the STHE. In case of pressure drop, the STHE with 1 and 2 pass number has a lower pressure drop than the WPHE, while the STHE with 4 pass presented higher pressure drop than the WPHE. The performance index considering the heat exchange capacity and pump consumption power, showed in oder of STHE_Pass1 > STHE_Pass2 > W PHE > STHE_Pass4 under the same flow rate. Therefore, when the WPHE was designed optimally under same operating condition with STHE, the maintenance fee and space can be reduced effectively by using the WPHE.

• Journal of the Korean Society for Geothermal and Hydrothermal Energy
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• v.6 no.2
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• pp.15-22
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• 2010

The natural refrigerants have used into HVAC equipments because the CFCs and HFCs have some environmental problems like high ODP and GWP. The carbon dioxide has small effect on the environmental problem but also good thermodynamics properties. In this study, the simulation study on the performance and characteristics of a $CO_2$ gascooler and evaporator using a fin-tube and microchannel heat exchanger has been conducted. Besides, the comparison of performance with operating condition was carried out in order to apply to the $CO_2$ heat pump system. As a result, the front sizes of a gascooler and evaporator using a microchannel were decreased by 63% and 58%, respectively, compared to those using a fin-tube. The performance of the fin-tube gascooler and evaporator were more responsive to the variation of operating conditions compared to that of microchannel. The pressure drop of a fin-tube heat exchanger was higher than that of a microchannel one.

• Journal of the Korean Society for Geothermal and Hydrothermal Energy
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• v.7 no.2
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• pp.23-29
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• 2011

The objectives of this paper are to study the characteristics of heat transfer and pressure drop of the plate heat exchanger with corrugation height by numerical analysis. Plate heat exchanger of three types was designed, which was corrugation height 3.1mm, 2.8mm and 2.5mm. The plate heat exchanger was numerically investigated for Reynolds number in a range of 950~3,380. The temperatures of the hot side were performed at $14.5^{\circ}C$ while that of the cold side was conducted at $4.5^{\circ}C$. The results show that the performance of heat transfer coefficient for corrugation height 2.5mm increases about 9.5~17.1% compared to that of corrugation height 3.1mm. On the other hand, the performance of pressure drop for corrugation height 2.5mm is remarkably higher than that of corrugation height 3.1mm, about 65.7~86.0%.

• Journal of the Korean Society for Geothermal and Hydrothermal Energy
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• v.17 no.2
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• pp.20-29
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• 2021

In this study, it is proposed that an analysis method using charatersistics curve of PICV in the CFD simulation for hydronic system. From the results, the pressure drop characteristics appeared in the region of PICV at a specified flow rate. And the CFD results are in good agreement with the experimental results. Proposed analysis method is proved that the characteristics of PICV applied to the hydronic system were properly applied in the flow analysis. This result can be applied to PICV in the complex hydronic systems. Therefore, the optimal selection of PICV in hydronic system contribute the building energy saving.

• Journal of the Mineralogical Society of Korea
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• v.19 no.4 s.50
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• pp.301-310
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• 2006

Smectites were synthesized from Na-P type and Na-A type zeolites by the hydrothermal synthetic method, and their physicochemical properties were studied. The optimal synthetic conditions for producing smectite were $290^{\circ}C$, 72 hr and $75{\sim}100kgf/cm^2$ in autogenous pressure. pHs of initial reaction solutions for the synthesis of smectites from Na-P type and Na-A type zeolite s were pH 6 and pH 10, respectively. The synthetic smectite was confirmed as $12{\AA}$-beidellite by a series of analysis such as X-ray diffraction analysis with random and oriented mounts, ethylene glycol treatment, and Greene-Kelly test, and their several physicochemical properties were studied.

• Journal of Energy Engineering
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• v.23 no.4
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• pp.141-149
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• 2014

In the present study, pure RHO zeolite was hydrothermally synthesized by using 18-crown-6 ether as a structure directing agent(SDA), and the small gases adsorption was investigated. Synthesized RHO zeolite was a cube shape particle of which average edge length was around $1.2{\mu}m$ and composed of primary crystallites having a diameter of around 100 to 200 nm. RHO zeolite structure was stable under 3h calcination at $600^{\circ}C$. Water adsorption data announced that RHO zeolite has a specific surface area of 483.32 m2/g and its micropore diameter was about 4 A. Gas adsorption was studied in the pressure range of 50 to 500 kPa for $CO_2$, $N_2$, $O_2$ and $H_2$. It was evident that RHO zeolite showed a strong $CO_2$ adsorption behavior. Especially, RHO zeolite showed a transient $CO_2$ adsorption behavior. The 3h $CO_2$ up-take at 50 kPa and 500 kPa was 1.283 and 3.357 mmol/g, respectively. The $CO_2/H_2$ selectivity was around 16 at 500 kPa. Compared with gas adsorption data for some representative microporous adsorbents, it was certain that RHO zeolite is a beneficial adsorbent for $CO_2/H_2$ separation.