• Title/Summary/Keyword: low-temperature hydrothermal synthesis

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Synthesis and Characterization of $CeO_2$ Powders by the Hydrothermal Process (수열합성법을 이용한 세륨산화물 나노분말의 특성 및 합성에 대한 연구)

  • Kong, Myung-Ho;Na, Han-Gil;Kim, Hyoun-Woo;Yang, Hack-Hui
    • Journal of the Semiconductor & Display Technology
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    • v.9 no.2
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    • pp.49-54
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    • 2010
  • We have successfully synthesized $CeO_2$ nanopowders by means of the hydrothermal method, in a low temperature range of $100-200^{\circ}C$. In order to investigate the structure and morphology of the nanopowders, scanning electron microscopy and X-ray diffraction have been employed. In addition, for exploring the optical properties, Raman spectroscopy, Fourier transform infrared spectroscopy, and photoluminescence spectroscopy have been used. In the optimized condition, with the pH, velocity, and time of 4.5, 600 rpm, and 60 h, the $CeO_2$ nanopowders with a diameter ranging from 50 to 150 nm have been synthesized. The nanopowders exhibited the visible emission mainly in the blue region. With comparing the reaction time, it is revealed that the extinction of functional groups at 60 h contributed to the growth and homogenization of the $CeO_2$ powders. Since the overgrowth and agglomeration of nanopowders were found, we suggest that the cracking/growth process is more favorable mechanism than the dissolution/precipitation process.

Hydrothermal Synthesis and Structural Characterization of x mol% Calcia-Stabilized ZrO2 Nanopowders (x mol% 칼시아-안정화 지르코니아 나노분말의 수열합성 및 구조적 특성평가)

  • Ryu, Je-Hyeok;Moon, Jung-In;Park, Yeon-Kyung;Nguyen, Tuan Dung;Song, Jeong-Hwan;Kim, Taik-Nam
    • Korean Journal of Materials Research
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    • v.22 no.5
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    • pp.220-226
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    • 2012
  • Pure zirconia and $x$ mol% calcia partially stabilized zirconia ($x$ = 1.5, 3, and 8) nanopowders were synthesized by hydrothermal method with various reaction temperatures for 24 hrs. The precipitated precursor of pure zirconia and $x$ mol% calcia doped zirconia was prepared by adding $NH_4OH$ to starting solutions; resulting sample was then put into an autoclave reactor. The optimal experimental conditions, such as reaction temperatures and times and amounts of stabilizer CaO, were carefully studied. The synthesized $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5, 3, and 8) powders were characterized by XRD, SEM, TG-DTA, and Raman spectroscopy. When the hydrothermal temperature was as low as $160^{\circ}C$, pure $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5 and 3) powders were identified as a mixture of monoclinic and tetragonal phases. However, a stable tetragonal phase of zirconia was observed in the 8 mol% calcia doped zirconia nanopowder at hydrothermal temperature above $160^{\circ}C$. To observe the phase transition, the 3 mol% CaO-$ZrO_2$ and 8 mol% CaO-$ZrO_2$ nanopowders were heat treated from 600 to $1000^{\circ}C$ for 2h. The 3 mol% CaO-$ZrO_2$ heat treated at above $1000^{\circ}C$ was found to undergo a complete phase transition from mixture phase to monoclinic phase. However, the 8 mol% calcia doped zirconia appeared in the stable tetragonal phase after heat treatment. The result of this study therefore should be considered as the preparation of 8 mol% CaO-$ZrO_2$ nanopowders via the hydrothermal method.

Preparation and Characterization of Hydrothermal BaTiO3 Powders and Ceramics (수열합성법에 의한 BaTiO3분말합성 및 소결체의 제조)

  • 이병우;최경식;신동우
    • Journal of the Korean Ceramic Society
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    • v.40 no.6
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    • pp.577-582
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    • 2003
  • BaTiO$_3$ fine powders were synthesized by hydrothermal process from peroxo-coprecipitate precursors. The peroxo-coprecipitates were obtained by addition of the BaCl$_2$, TiCl$_4$, and $H_2O$$_2$ aqueous solution to an ammonium solution. Hydrothermal reaction was conducted at various reaction temperatures, times and pH ranges. Unlike the conventional hydrothermal synthesis which needs highly alkaline condition over pH 13 with KOH or NaOH, the present method offered well-developed crystalline (perovskite) BaTiO$_3$ powders synthesized below pH 12 with use of ammonium solution. It was found that the phase-pure fine powders were formed at temperatures as low as 11$0^{\circ}C$ and the properties of the powders synthesized over 13$0^{\circ}C$ were almost same regardless of the reaction time. BET surface area of the prepared powder was as high as 76 $m^2$/g and the calculated particle (particulate) size was below 20 nm. The ultrafine particulates formed weak agglomerates. The microstructure and dielectric properties of BaTiO$_3$ ceramics sintered at the temperature range of 1150~125$0^{\circ}C$ were evaluated.

Synthetic study of Zeolites from Some Glassy Rocks (I) L Low-Temperature Hydrothermal Synthesis of Zeolites Na-P, Na-X, and Na-A (유리질 암석으로부터 제올라이트 합성에 광한 연구 (I) : Na-P, Na-X 및 Na-A 제올라이트의 저온 수열 합성)

  • 노진환
    • Journal of the Mineralogical Society of Korea
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    • v.3 no.1
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    • pp.7-17
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    • 1990
  • 화산 유리질 암석을 출발 물질로 사용하여 저온 ($80^{\circ}C$)에서 수열 처리하여 Na-P Na-X 및 Na-A 제올라이트를 합성하였다. 합성과정은 (1) 유리질 분말 시료와 알칼리 용액과의 용해.변질 반응에 의한 1차적인 Na-P의 합성 방식과 (2) 여기서 잔류된 규산질 모액에 Al(OH)3나 NaAlO2의 수용액을 공급하여 보다 고순도의 Na-P, Na-X 및 Na-A를 효과적으로 합성할 수 있었다. 원암의 암상과 조성은 제올라이트들의 화학 조성과 순도 및 백색도같은 물리적 특성에는 영향을 주지만, 합성된 제올라이트의 광물종을 규제하는 주된 요인은 아닌 것으로 해석된다. 합성된 제올라이트의 광물상은 반응 용액의 pH, Al(OH)4 및 Na+에 대한 농도 조건에 주로 의존되는 경향을 나타낸다. 또한 화산 유리질 암석을 제올라이트 합성원료로 활용하는 데에 있어서 (2)와 같음 합성 방안이 보완적으로 시행되면 그 생산성과 효율성을 제고시킬 수 있을 것으로 여겨진다.

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Influence of RTA treatments on optical properties of ZnO nanorods synthesized by wet chemical method

  • Shan, Qi;Ko, Y.H.;Lee, H.K.;Yu, J.S.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.190-190
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    • 2010
  • Zinc oxide is the most attractive material due to the large direct band gap (3.37 eV), excellent chemical and thermal stability, and large exciton binding energy (60 meV). Recently, ZnO nanorods were used as the high efficient antireflection coating layer of solar cells based on silicon (Si). In this reports, we studied the effects of rapid thermal annealing (RTA) treatment on optical properties of ZnO nanorods. For fabrication of ZnO nanorods, there are many methods such as hydrothermal method, sol-gel method, and metal organic chemical vapor deposition method. Among of them, we used the conventional wet chemical method which is simple and low temperature growth. In order to synthesize the ZnO nanorods, the ZnO films were deposited on Si substrate by RF magnetron sputtering at room temperature and the samples were dipped to aqua solution containing the zinc nitrate and hexamethylentetramines (HMT). The synthesis process was achieved in keeping with temperature of $90-95^{\circ}C$ and under constant stirring. The morphology of ZnO nanorods on glass and Si was characterized by scanning electron microscopy. For the analysis of antireflection performance, the reflectance and transmittance were measured by spectrophotometer. And for analyzing the effects of RTA treatment on ZnO nanorods, crystalline properties were investigated by X-ray diffraction measurements and optical properties was estimated by photoluminescence spectra.

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Synthesis of TiO2/active carbon composites via hydrothermal process and their photocatalytic performance (수열합성법에 의한 TiO2/active carbon 복합체의 제조 및 광촉매특성)

  • Kim, Dong Jin;Lee, Jin Hee;Lee, Byeong Woo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.5
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    • pp.241-245
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    • 2013
  • Granular bamboo-derived active carbons (AC) were impregnated (or coated) with $TiO_2$ nano crystalline powders. The photocatalytic activity of the $TiO_2$-impregnated active carbons ($TiO_2$/AC) were determined on the basis of the degradation rate of methylene-blue aqueous solution under UV irradiation. The active compounds of $TiO_2$ were impregnated onto the AC under moderate hydrothermal conditions (${\leq}200^{\circ}C$, pH 11). The mean size of $TiO_2$ particles calculated from BET surface area were found to be as 50 nm. The $TiO_2$ precipitates were coated on the cavities or pores on the surfaces of highly activated carbons. Since the hydrothermal process led to a lowering of the on-set temperature of the anatase-to-rutile transition of $TiO_2$ as low as $200^{\circ}C$, $TiO_2$ crystallites of a pure anatase or a mixed form with rutile were successfully coated on the AC depending on the synthesis temperatures.

Synthesis and characterization of potassium titanate whisker by hydrothermal process (수열합성법을 이용한 티탄산칼륨 휘스커의 합성과 특성)

  • Choi, Yeon-Bin;Son, Jeong-hun;Lee, Je Kyun;Bae, Dong-Sik
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.1
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    • pp.9-17
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    • 2017
  • $K_2Ti_6O_{13}$ whisker have been synthesized by hydrothermal process at low temperature and pressure condition. The average length of the synthesized $K_2Ti_6O_{13}$ whisker was about in the range of 300 nm to $1.5{\mu}m$. The average diameter of the synthesized $K_2Ti_6O_{13}$ whisker was 15 nm to 60 nm. The aspect ratio of the synthesized $K_2Ti_6O_{13}$ whisker was below 12. The average length and diameter of the synthesized $K_2Ti_6O_{13}$ whisker can be controlled by reaction temperature and time, KOH molar ratio. $K_2Ti_6O_{13}$ whisker was synthesized from more than $210^{\circ}C$ and 4 h at reaction temperature and time. The length of the whisker is increased with increasing reaction temperature. Characterization of the synthesized $K_2Ti_6O_{13}$ whisker was carried out using the XRD and FE-SEM.

Green Synthesis of Multifunctional Carbon Nanodots and Their Applications as a Smart Nanothermometer and Cr(VI) Ions Sensor

  • Li, Lu;Shao, Congying;Wu, Qian;Wang, Yunjian;Liu, Mingzhu
    • Nano
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    • v.13 no.12
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    • pp.1850147.1-1850147.14
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    • 2018
  • In this work, water-soluble and blue-emitting carbon nanodots (CDs) were synthesized from apple peels for the first time via one-step hydrothermal method. The synthetic route is facile, green, economical and viable. The as-prepared CDs were characterized thoroughly by transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman, Fourier transform infrared (FT-IR), X-ray photoelectron (XPS), fluorescence and UV-Vis absorption spectroscopy in terms of their morphology, surface functional groups and optical properties. The results show that these CDs possessed ultrasmall size, good dispersivity, and high tolerance to pH, ionic strength and continuous UV irradiation. Significantly, the CDs had fast and reversible response towards temperature, and the accurate linear relationship between fluorescence intensity and temperature was used to design a novel nanothermometer in a broad temperature range from 5 to $65^{\circ}C$ facilely. In addition, the fluorescence intensity of CDs was observed to be quenched immediately by Cr(VI) ions based on the inner filter effect. A low-cost Cr(VI) ions sensor was proposed employing CDs as fluorescent probe, and it displayed a wide linear range from 0.5 to $200{\mu}M$ with a detection limit of $0.73{\mu}M$. The practicability of the developed Cr(VI) sensor for real water sample assay was also validated with satisfactory recoveries.

Low Temperature Selective Catalytic Reduction of NO with $NH_3$ over Mn/$CeO_2$ and Mn/$ZrO_2$ (Mn/$CeO_2$와 Mn/$ZrO_2$ 촉매 상에서 $NH_3$를 사용한 NO의 선택적 촉매 산화 반응)

  • Ko, Jeong Huy;Park, Sung Hoon;Jeon, Jong-Ki;Sohn, Jung Min;Lee, See-Hoon;Park, Young-Kwon
    • Applied Chemistry for Engineering
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    • v.23 no.1
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    • pp.105-111
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    • 2012
  • Manganese (Mn) catalysts were generated using $CeO_2$ and $ZrO_2$supports synthesized by the supercritical hydrothermal method and two different Mn precursors, aimed at an application for a low-temperature selective catalytic reduction process. Manganese acetate (MA) and manganese nitrate (MA) were used as Mn precursors. Effects of the kind and the concentration of the Mn precursor used for catalyst generation on the NOx removal efficiency were investigated. The characteristics of the generated catalysts were analyzed using $N_2$ adsorption-desorption, thermo-gravimetric analysis, X-ray diffraction, and X-ray photoelectron spectroscopy. De-NOx experiments were carried out to measure NOx removal efficiencies of the catalysts. NOx removal efficiencies of the catalysts generated using MA were superior to those of the catalysts generated using MN at every temperature tested. Analyses of the catalyst characteristics indicated that the higher NOx removal efficiencies of the MA-derived catalysts stemmed from the higher oxygen mobility and the stronger interaction with support material of $Mn_2O_3$ produced from MA than those of $MnO_2$ produced from MN.

Synthetic Study of Zeolites from Some Glassy Rocks (II) : Dissolution Behavior of Perlite and Zeolite Synthesis in Alkaline Aqueous Solution (유리질 암석으로부터 제올라이트 합성에 관한 연구(Ⅱ) : 알칼리 용액에서 진주암의 용해 거동과 제올라이트의 합성)

  • Noh, Jin-Hwan
    • Journal of the Mineralogical Society of Korea
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    • v.5 no.2
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    • pp.61-71
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    • 1992
  • Through the low-temperature(60-150${\circ}C$) hydrothermal treatment of perlite with the alkaline solution at various NaOH concentrations, the mode of volcanic glass alteration and resultant zeolite formation were investigated in a closed system. At a temperature of 80${\circ}C$ and alkalinities of pH range 8 to 12, corresponding to the natural environments of diagenetic zeolite formation, only weak dissolution of perlitic glass occurs without zeolite formation despite the residence time of 100 days. Activities of Si and Al increase progressively, as a consequence of increasing pH, whereas activity ratios of Si/Al decrease. Zeolites were synthesized from perlite in the alkaline solution at above 0.1M NaOH concentrations. Below the temperature of 100${\circ}C$ Na-P was mainly formed, whereas analcime was the dominant zeolite at the temperature range of 100-150${\circ}C$. During Na-P synthesis chabazite and Na-X were also formed as by-products in case of lower proportion of solution/sample(<10ml/g) and higher NaOH concentraion (>3M), respectively. The alteration modes of perlite in the zeolite synthesis reflect that the formation of synthetic zeolites occurs as an incongruent dissolution likely with the diagenetic formation of natural zeolites from volcanic glass. Considering much difference in reaction kinetics between natural and synthetic systems, however, the evaluated synthetic conditions in these experiments were not directly applicable to the natural diagenetic system.

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