• Title/Summary/Keyword: homogeneous precipitation method

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Preparation of in situ Patterned ZnO Thin Films by Microcontact Printing (Microcontact Printing을 이용한 미세패턴 ZnO 박막 제조)

  • 임예진;윤기현;오영제
    • Journal of the Korean Ceramic Society
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    • v.39 no.7
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    • pp.649-656
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    • 2002
  • In situ patterned zinc oxide thin films were prepared by precipitation of Zn(NO$_3$)$_2$ aqueous solution containing urea and by microcontact printing using Self-Assembled Monolayers(SAMs) on A1/SiO$_2$/Si substrates. The visible precipitation of Zn(OH)$_2$ that was formed in the Zn(NO$_3$)$_2$ aqueous solution containing urea was enhanced with an increase of the reaction temperature and the amount of urea. As the reaction time of Zn(NO$_3$)$_2$ with urea was prolonged, the thickness and grain size of Zn(OH)$_2$ thin layers were increased, respectively. The optimum precipitation condition was at 80$\^{C}$ for 1 h for the solution with the ratio of Zn(NO$_3$)$_2$ to urea of 1 : 8. Homogeneous ZnO thin films were fabricated by the heat treatment of 600$\^{C}$ for 1 h of Zn(OH)$_2$ precipitation on Al/SiO$_2$/Si substrate. This was available to the in-situ patterned ZnO thin films with uniform grain size. Hydrophobic SAM, Octadecylphosphonic Acid(OPA) and hydrophilic SAM, 2-Carboxyethylphosphonic Acid(CPA) were applied on the Al/SiO$_2$/Si substrate by microcontact printing method. In situ patterned ZnO thin film was successfully prepared by the heat treatment of Zn(OH)$_2$ precipitated on the surface of hydrophilic SAM, CPA.

Effect of Water and Aluminum Sulfate Mole Ratio on Pore Characteristics in Synthesis of AlO(OH) Nano Gel by Homogeneous Precipitation (균일침전에 의한 AlO(OH) 나노 겔 합성에서 물/황산알루미늄의 몰 비가 세공특성에 미치는 영향)

  • Choe, Dong-Uk;Park, Byung-Ki;Lee, Jung-Min
    • Journal of the Korean Ceramic Society
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    • v.43 no.9 s.292
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    • pp.564-568
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    • 2006
  • AlO(OH) nano gel is used in precursor of ceramic material, coating material and catalyst. For use of these, not only physiochemical control for particle morphology, pore characteristic and peptization but also studies of synthetic method for preparation of advanced application products were required. In this study, AlO(OH) nano gel was prepared through the aging and drying process of aluminum hydroxides gel precipitated by the hydrolysis reaction of dilute NaOH solution and aluminum sulfate solution. In this process, optimum synthetic condition of AlO(OH) nano gel having excellent pore volume as studying the effect of water and aluminum sulfate mole ratio on gel precipitates has been studied. Water and aluminum sulfate mole ratio brought about numerous changes on crystal morphology, surface area, pore volume and pore size. Physiochemical properties were investigated as using XRD, TEM, TG/DTA, FT-IR, and $N_2$ BET method.

Morphology of Barium Titanyl Oxalate Produced by Homogeneous Precipitation from Acidic Solution of Dimethyl Oxalate (Dimethyl Oxalate에 의한 균일 침전법으로 생성된 Barium Titanyl Oxalate의 형태학적 연구)

  • Min, Chonkyu;Lee, Chul
    • Analytical Science and Technology
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    • v.10 no.3
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    • pp.203-208
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    • 1997
  • Barium titanyl oxalate(BTO) was precipatated by utilizing the thermal decomposition of dimethyl oxalate in acidic aqueous solution having $BaCl_2$ and $TiCl_4$. Particle morphology of BTO was influeneced by the various experimental factors. i.e.. the faster rate to nucleation with higher temperature and the higher ratio of [DMO]/[$Ba^{2+}+Ti^{4+}$] was found to correspond to the faster rate of transformation of particle size distribution from unimodal to broad unimodal through bimodal. The BT powder obtained by calcination at $900^{\circ}C$ in air consists of larger particles than BT generated by general coprecipitation method and shows tetragonal symmetry. The stirring during reaction was also found to have much effect upon characteristics of BTO and BT.

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Development of Internal Reforming Catalysts and Catalysts Forming Method using Homogeneous Precipitation (균일용액침전법을 이용한 내부개질촉매의 개발과 성형방법에 대한 연구)

  • Jung, Youshick;Rhee, Youngwoo;Koo, Keeyoung;Jung, Unho;Youn, Wanglai;seo, Yongseog
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.223.2-223.2
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    • 2010
  • 용융탄산염 연료전지(MCFC)는 $650^{\circ}C$에서 작동하는 고온형 연료전지 시스템이다. 이 시스템은 천연가스 등을 개질하여 생산된 수소를 바로 전기로 생산할 수 있는 시스템으로 열효율이 높으며, 현재 대체 발전시스템으로 각광을 받고 있다. MCFC는 개질방식에 따라 내부개질 방식과 외부개질 방식이 있다. 내부개질 방식은 수소를 생산하는 개질기가 스택내부에 장착된 형식으로 천연가스를 스택내부에서 개질하여 바로 전기를 생산하는 방식이다. 이 내부개질반응에 사용되는 촉매로는 알루미나에 담지된 니켈(Ni) 계열촉매이 주로 쓰이고 있다. 또한 내부개질촉매의 형태는 작은 원주형의 촉매형태로 성형되어 사용된다. 이 성형된 촉매의 크기가 바로 내부개질 스택의 크기를 결정하는 중요한 요소이다. 그래서 촉매의 크기는 되도록이면 작게 성형하는 것이 중요하다. 그러나 촉매의 크기가 너무 작으면 촉매를 성형하는데 큰 어려움이 생기게 된다. 본 연구에서는 니켈 촉매를 공침법이 아닌 균일용액침전법을 이용하여 제조하였으며, 이 촉매를 이용하여 지름이 약 2 mm 이하로 촉매를 압출성형하는 방법을 연구하였다. 먼저 요소(urea)를 이용한 균일용액침전법으로 촉매를 제조하였다. 최적의 촉매 합성조건을 살펴보기 위해서, 반응 온도를 80, 85, 90, 95, $100^{\circ}C$로 변화 시키면서 제조된 촉매의 특성을 살펴보았다. 그리고 촉매의 적절한 니켈 양을 알아보기 위해서 니켈의 양을 30, 40, 50, 60, 70 wt%로 변화 시켰으며, 조촉매로 사용되는 MgO 양을 5, 10, 15, 20 wt%로 변화 시켜서 제조된 촉매의 특성을 살펴보았다. 물성을 비교하기 위해서, X-선 회절분석(XRD) 및 TPR, 물리화학흡착을 하였다. 그 결과 침전반응온도가 $80^{\circ}C$에서 촉매가 가장 좋은 물성을 보였으며, 우수한 개질성능을 보였다. 그리고 촉매 활성물질인 니켈의 함량은 50 wt% 정도가 가장 적절한 함량이었으며, MgO의 함량이 15 wt%일 때 가장 우수한 물성과 개질 성능을 보여주었다. 이 촉매들은 공침법으로 제조된 상용촉매와 비교하였을 때, 보다 우수한 물성과 개질성능 보였다. 그래서 이 촉매를 균일침전법을 이용하여 대량으로 제조한 다음 압출성형 방법을 이용하여 촉매를 원주형으로 제조하였다. 먼저 제조된 촉매는 별도의 분쇄작업(볼밀 혹은 제트밀)을 거치지 않아도 입자사이즈가 약 $4{\mu}m$ 수준이 나오도록 촉매 제조조건을 조절 하였다. 그리고 소량의 Methyl cellulose(MC) 바이더와 물만 사용하여 촉매를 혼합한 다음 스크류 압출기를 이용하여 촉매를 성형하였다. 이 촉매는 지름이 약 2 mm 이하로 제조할 수 있었으며, 기계적 강도는 타정기로 성형한 상용촉매보다 우수하였다. 그리고 촉매 성능 또한 상용촉매와 비교하였을 때, 우수한 성능 보였다. MCFC용 내부개질 촉매로 균일용액침전법을 사용한 촉매가 적합하다고 판단되며, 압출성형에도 적합하다고 판단되었다.

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The effect of MgO content on highly active Ni-MgO-$Al_2O_3$ catalysts prepared by homogeneous precipitation method (균일용액침전법으로 제조한 MgO 함량에 따른 고활성 Ni-MgO-$Al_2O_3$ 촉매에 대한 연구)

  • Jung, Youshick;Rhee, Youngwoo;Koo, Keeyoung;Jung, Unho;Youn, Wanglai;Seo, Yongseog
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.05a
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    • pp.155-155
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    • 2011
  • 용융탄산염 연료전지(MCFC)는 $650^{\circ}C$에서 작동하는 고온형 연료전지 시스템이다. 이 시스템은 천연가스 등을 개질하여 생산된 수소를 바로 전기로 생산할 수 있는 시스템으로 열효율이 높으며, 현재 대체 발전시스템으로 각광을 받고 있다. MCFC는 개질방식에 따라 내부개질 방식과 외부개질 방식이 있다. 내부개질 방식은 수소를 생산하는 개질기가 스택내부에 장착된 형식으로 천연가스를 스택내부에서 개질하여 바로 전기를 생산하는 방식이다. 이 내부개질반응에 사용되는 촉매로는 알루미나에 고함량 (약 50 wt.%)으로 담지된 니켈(Ni) 계열촉매이 주로 쓰이고 있다. 이 고함량으로 담지된 촉매는 대부분 높은 활성을 보인다. 비교적 낮은 온도 운전조건 (약 $580{\sim}620^{\circ}C$)을 가지는 MCFC 내부개질에 적용하기 위해서는 활성점인 니켈을 최대한 담지체에 고르게 분산 시켜야한다. 이를 위해서 MgO를 이용하여 촉매의 활성점을 높게 분산시키는 연구를 진행 하였다. 촉매를 제조하는 방법으로 요소(urea)를 이용한 균일용액침전법을 이용하였다. 니켈함량은 50 wt.%로 고정을 한 다음, MgO 양과 $Al_2O_3$ 양을 각각 0 ~ 45 wt.%와 5 ~ 50 wt.%로 조절하면서 촉매를 제조하여 그 특성들을 분석하였다. 물성을 비교하기 위해서, X-선 회절분석 (XRD) 및 TPR, 물리화학흡착 실험을 하였다. 촉매의 활성을 살펴보기 위해서, fresh 상태 및 피독 상태에서 메탄수증기 개질활성 실험을 실시하였다. MgO 함량이 없거나 적은 촉매에서는 높은 BET surface area와 작은 NiO, metallic Ni 결정 크기가 나타났다. 반면 MgO 함량이 높은 촉매에서 낮은 BET surface area와 비교적 큰 NiO, metallic Ni 결정 크기가 나타났다. 또한 XRD 분석에서 MgO 함량이 증가할 수 록 MgO 결정 피크가 명확히 나타났으며, $MgAl_2O_4$ 피크는 나타나지 않았다. TPR 분석에서 촉매들의 환원 피크를 측정한 결과, 저함량의 MgO를 포함한 촉매는 $700^{\circ}C$ 부근에 환원 피크가 관찰되었고 MgO가 고함량인 촉매는 환원 피크가 $400^{\circ}C$ 부근에서 관찰되었다. 촉매의 초기 fresh 상태에서의 활성은 고함량 MgO를 포함한 Ni-90M10A 샘플을 제외하고 모든 촉매가 거의 비슷하게 나타났다. 그러나 $K_2CO_3$ 피독 상태에서는 MgO 함량이 증가할 수 록 활성이 좋지 않았음을 알 수 있었다. 따라서 MgO가 소량 포함된 촉매의 경우 fresh 상태에서는 우수한 물성과 활성을 보이지만, 피독상태에서는 MgO가 포함되지 않은 Ni-$Al_2O_3$ 촉매가 우수한 활성을 보였다.

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Multi-scale agglomerates and photocatalytic properties of ZnS nanostructures

  • Man, Min-Tan;Lee, Hong-Seok
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.267.2-267.2
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    • 2016
  • Semiconductor photo-catalysis offers the potential for complete removal of toxic chemicals through its effective and broad potential applications. Various new compounds and materials for chemical catalysts were synthesized in the past few decades. As one of the most important II-VI group semiconductors, zinc sulfide (ZnS) with a wide direct band gap of 3.8 eV has been extensively investigated and used as a catalyst in photochemistry, environmental protection and in optoelectronic devices. In this work, the ZnS films and nanostructures have been successfully prepared by wet chemical method. We show that the agglomerates with four successive scales are always observed in the case of the homogeneous precipitation of zinc sulfide. Hydrodynamics plays a crucial role to determine the size of the largest agglomerates; however, other factors should be invoked to interpret the complete structure. In addition, studies of the photocatalytic properties by exposure to UV light irradiation demonstrated that ZnS nanocrystals (NCs) are good photo-catalysts as a result of the rapid generation of electron-hole pairs by photo-excitation and the highly negative reduction potentials of excited electrons. A combination of their unique features of high surface-to volume ratios, carrier dynamics and rich photo-catalytic suggests that these ZnS NCs will find many interesting applications in semiconductor photo-catalysis, solar cells, environmental remediation, and nano-devices.

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A Study on the Crystallization Behavior of Al85Ce5Ni10 Amorphous Ribbon (Al85Ce5Ni10 비정질 리본의 결정화 거동에 관한 연구)

  • Moon, J.T.;Jo, W.M.;Shin, B.M.;Lee, Y.H.
    • Journal of the Korean Society for Heat Treatment
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    • v.8 no.3
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    • pp.236-243
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    • 1995
  • Since amorphous alloys have been known to have better mechanical and chemical properties than crystalline alloys of the same composition, a great number of studies on the formation of Al-based amorphous alloys have been carried out actively. However, little has been obtained about the effect of Rare-Earth metal and Transition metal addition on amorphous phase formed by melt spinning method. This study included fabrication of amorphous alloy $Al_{85}Ce_5Ni_{10}$ by melt spinning methods and DTA, XRD, TEM analysis to determine crystalization behavoir. Annealing treatments were carried out in Ar atmosphere under isothermal and nonisothermal conditions. The diffraction pattern of non-heated ribbons showed broad form characteristic of glass metallic alloy. The crystallization of amorphous $Al_{85}Ce_5Ni_{10}$ takes place eutedtoidly by homogeneous formation of Al and MS-1, followed by precipitation of the $Al_{11}Ce_3$ and later $MS-1{\rightarrow}Al_3Ni$ transformation.

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Effects of Coating Conditions on the Thickness and Morphology of Alumina- or Carbon-Coated Layers on SiC Whiskers (알루미나 또는 카본 코팅 SiC 휘스커의 코팅층 두께 및 형상에 미치는 코팅조건의 영향)

  • 배인경;장병국;조원승;최상욱
    • Journal of the Korean Ceramic Society
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    • v.36 no.5
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    • pp.513-520
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    • 1999
  • Alumina-coated SiC whiskers wee prepared by the calcination (1150$^{\circ}C$, 1h, Ar) of the alumina hydrate layer which was precipitated homogeneously on whisker surface from a solution of Al2(SO4)3 and urea as a precipitant. In addition carbon coated SiC whiskers were prepared by the pyrolysis (1000$^{\circ}C$, 4h Ar) of phenolic resin coated whisker. The effects of coating conditions on the thickness and morphology of the coated layers were examined by SEM and TEM. It was found that Al2O3-coating layers become thinner and more uniform with decreasing the Al2(SO4)3 concentration. Thin (0.075-0.1$\mu\textrm{m}$) and uniformly alumina-coating layers were obtained at the Al2(SO4)3 concentration 0.010mol/l. On the other han carbon-coating layers were uniform but very thin (5-16 nm) in thickness. For thicker carbon-coating layers ethanol as a disperse medium was found to be more efficient compared tousing acetone.

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The Influence of Global Sea Surface Temperature Anomalies on Droughts in the East Asia Monsoon Region

  • Awan, Jehangir Ashraf;Bae, Deg-Hyo
    • Proceedings of the Korea Water Resources Association Conference
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    • 2015.05a
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    • pp.224-224
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    • 2015
  • The East Asia monsoon is one of the most complex atmospheric phenomena caused by Land-Sea thermal contrast. It plays essential role in fulfilling the water needs of the region but also poses stern consequences in terms of flooding and droughts. This study analyzed the influence of Global Sea Surface Temperature Anomalies (SSTA) on occurrence of droughts in the East Asia monsoon region ($20^{\circ}N-50^{\circ}N$, $103^{\circ}E-149^{\circ}E$). Standardized Precipitation Index (SPI) was employed to characterize the droughts over the region using 30-year (1978-2007) gridded rainfall dataset at $0.5^{\circ}$ grid resolution. Due to high variability in intensity and spatial extent of monsoon rainfall the East Asia monsoon region was divided into the homogeneous rainfall zones using cluster analysis method. Seven zones were delineated that showed unique rainfall regimes over the region. The influence of SSTA was assessed by using lagged-correlation between global gridded SSTA ($0.2^{\circ}$ grid resolution) and SPI of each zone. Sea regions with potential influence on droughts in different zones were identified based on significant positive and negative correlation between SSTA and SPI with a lag period of 3-month. The results showed that SSTA have the potential to be used as predictor variables for prediction of droughts with a reasonable lead time. The findings of this study will assist to improve the drought prediction over the region.

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Synthesis of nano-crystalline slaked lime using design of experiment (실험계획법을 이용한 나노 결정 소석회 합성)

  • Kim, Jin-Seong;Kim, Jung-Woo;Lee, Hee-Soo;Kim, Yong-Nam;Shin, Hyun-Gyoo;Kim, Hwan
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.4
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    • pp.174-178
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    • 2008
  • Nano-crystalline slaked lime was synthesized using design of experiment. In order to synthesize slaked lime, calcium chloride $(CaCl_2)$ and urea were used as starting materials. Calcium chloride solution and urea solution were mixed and heated in vessel that calcium carbonate was precipitated during heating. Precipitates were filtered, washed several times using D.I.water and ethanol and finally dried in oven. Slaked lime $(Ca(OH)_2)$ has been fabricated by the hydration of calcined $CaCO_3$. Design of experiment (Taguchi method) was used to optimize parameter, to minimize noise factors of experiment and to statistically analyze the results. Slaked lime having about 50 nm in optimized crystallite size could be obtained by calcination of $CaCO_3$ at $1000^{\circ}C$ for 0.5 h and hydration with D.I water containing ethanol and oxalic acid.