• Title/Summary/Keyword: Hydrothermal precipitation method

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Synthesis of Yttria Stabilized Zirconia by Sol-gel Precipitation Using PEG and PVA as Stabilizing Agent

  • Bramhe, Sachin N.;Lee, Young Pil;Nguyen, Tuan Dung;Kim, Taik-Nam
    • Korean Journal of Materials Research
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    • v.23 no.8
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    • pp.441-446
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    • 2013
  • There is increasing interest in zirconia as a dental material due to its aesthetics, as well as the exceptionally high fracture toughness and high strength that are on offer when it is alloyed with certain oxides like yttria. In recent years, many solution based chemical synthesis methods have been reported for synthesis of zirconia, of which the sol-gel method is considered to be best. Here, we synthesize zirconia by a sol gel assisted precipitation method using either PEG or PVA as a stabilizing agent. Zirconia sol is first synthesized using the hydrothermal method. We used NaOH as the precipitating agent in this method because it is easy to remove from the final solution. Zirconium and yttrium salts are used as precursors and PEG or PVA are used as stabilizers to separate the metal ions. The resulting amorphous zirconia powder is calcined at $900^{\circ}C$ for 2 h to get crystallized zirconia. XRD analysis confirmed the partially stabilized zirconia synthesis in all the synthesized powders. SEM was taken to check the morphology of the powder synthesized using either PEG or PVA as a stabilizing agent and finally the transparency was calculated. The results confirmed that the powder synthesized with 10 % PVA as the stabilizing agent had highest percentage of transparency among all the synthesized powder.

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.

Synthesis of plate powder coated nano sized ZnO by hydrothermal precipitation method

  • Lee, Dong-Kyu;Lee, Jin-Hwa
    • Journal of the Korean Applied Science and Technology
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    • v.24 no.4
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    • pp.369-376
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    • 2007
  • 우리는 마이카, boron nitride, bismuthoxychloride와 같은 판상 분체에 ZnO 나노입자를 코팅한 고 기능성 무기 분체를 합성하였다. 본 실험에서 우리는 수열침전법을 이용하여 합성 분체를 합성하였다. 출발물질은 $ZnCl_2$를 사용하였고 침전제로는 hexamethylenetetramine(HMT)와 urea를 사용하였다. 본 실험의 반응변수로는 출발물질의 농도, 침전제 및 반응온도를 변화시켜 실험하였다. 합성물의 형태, 결정성 및 UV-차단능은FE-SEM, XRD, FT-IR, TGA-DTA, in vitro SPF 테스트를 활용해 분석하였다. 본 실험의 결과, 나토입자 크기를 갖는 ZnO는 동일한 최적의 합성조건하에서 다양한 판상 분체의 종류에 관계없이 균일하게 코팅되었다.

Synthesis and spectroscopic characterization of zinc ferrite nanoparticles

  • Arora, Shefali;Nandy, Subhajit;Latwal, Mamta;Pandey, Ganesh;Singh, Jitendra P.;Chae, Keun H.
    • Advances in nano research
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    • v.13 no.5
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    • pp.437-451
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    • 2022
  • Synthesis approaches usually affect the physical and chemical properties of ferrites. This helps ferrite materials to design them for desired applications. Some of these methods are mechanical milling, ultrasonic method, micro-emulsion, co-precipitation, thermal decomposition, hydrothermal, microwave-assisted, sol-gel, etc. These methods are extensively reviewed by taking example of ZnFe2O4. These methods also affect the microstructure and local structure of ferrite which ultimately affect the physical and chemical properties of ferrites. Various spectroscopic techniques such as Raman spectroscopy, Fourier Transform Infrared spectroscopy, Ultra Violet-Visible spectroscopy, Mossbauer spectroscopy, extended x-ray absorption fine structure, and electron paramagnetic resonance are found helpful to reveal this information. Hence, the basic principle and the usefulness of these techniques to find out appropriate information in ZnFe2O4 nanoparticles is elaborated in this review.

Oxidative Dehydrogenation of n-Butenes over BiFe0.65MoP0.1 Oxide Catalysts Prepared with Various Synthesis Method (다양한 합성 방법으로 제조된 BiFe0.65MoP0.1 산화물 촉매 상에서 n-부텐의 산화탈수소화 반응)

  • Park, Jung-Hyun;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.53 no.3
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    • pp.391-396
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    • 2015
  • To investigate the effect of the catalyst synthesis method on the oxidative dehydrogenation (ODH) of nbutenes, $BiFe_{0.65}MoP_{0.1}$ oxide catalysts were prepared with various synthesis methods such as co-precipitation, citric acid method, hydrothermal method, and surfactant templated method. The catalysts were characterized by X-ray Diffraction (XRD), $N_2$ sorption, and $NH_3/1$-butene-temperature programmed desorption ($NH_3/1$-butene-TPD) to correlate with catalytic activity in ODH reaction. Among the catalysts studied here, $BiFe_{0.65}MoP_{0.1}$ oxide catalyst prepared with co-precipitation method marked the highest activity showing 1-butene conversion, 79.5%, butadiene selectivity, 85.1% and yield, 67.7% after reaction for 14 h. From the result of $NH_3$-TPD, the catalytic activity is closely related to the acidity of the $BiFe_{0.65}MoP_{0.1}$-x oxide catalyst and acidity of the $BiFe_{0.65}MoP_{0.1}$ oxde catalyst prepared with co-precipitation method was higher than that of other catalysts. In addition, combined with the 1-butene TPD, the higher catalytic activity is closely related to the amount of weakly adsorbed intermediate (< $200^{\circ}C$) and the desorbing temperature of strongly adsorbed intermediates (> $200^{\circ}C$).

Synthesis and Characterization of High Surface Area of Zirconia: Effect of pH (고비표면적 지르코니움 산화물의 제조 및 특성 분석: pH 영향)

  • Jeong, Ye-Seul;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.57 no.1
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    • pp.133-141
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    • 2019
  • High specific surface area zirconia with acid-basic property was synthesized by precipitation using reflux method or hydrothermal synthesis method using ammonium hydroxide solution as precipitant in the range of pH of Zr solution from 2 to 10. The prepared zirconia was characterized by the nitrogen adsorption, X-ray diffraction (XRD), isopropanol temperature programmed desorption (IPA-TPD), scanning electron microscopy and X-ray photoelectron spectroscopy, and the catalytic activity in the IPA decomposition reaction was correlated with the acid-basic properties. When using reflux method, high pH of Zr solution was required to obtain high fraction of tetragonal zirconia, and pure tetragonal zirconia was possible at pH 9 or higher. High pH was required to obtain high specific surface area zirconia, and the hydrous zirconia synthesized at pH 10 had high specific surface area zirconia of $260m^2g^{-1}$ even after calcination at $600^{\circ}C$. However, hydrothermal synthesis with high pressure under the same conditions resulted in very low specific surface area below $40m^2g^{-1}$ and monoclinic phase zirconia was synthesized. High pH of the solution was required to obtain high specific surface area tetragonal phase zirconia. In hydrothermal synthesis requiring high pressure, monoclinic zirconia was produced irrespective of the pH of the solution, and the specific surface area was relatively low. Zirconia with high specific surface area and tetragonal phase was predominantly acidic compared to basicity and only propylene, which was observed as selective dehydration reaction in IPA decomposition reaction, was produced.

Preparation of hydroxyapatite/$TiO_2$ biocomposite powders by wet chemical method (습식화학법에 의한 수산화아파타이트/$TiO_2$ 생체용 복합분말의 제조)

  • 정항철;이종국
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.3
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    • pp.83-89
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    • 2004
  • In this work, HA/$TiO_2$ biocomposite to get high mechanical properties with biocompatibility were prepared. HA/$TiO_2$ biocomposite powders were prepared by mixing $TiO_2$ and HA powders which were synthesized through sol-gel, precipitation and hydrothermal methods. The mixing ratio was fixed at 1:1 ratio (HA/$TiO_2$, wt%). HA/$TiO_2$ biocomposite powders showed different microstructures depending on their particle size and shape. The smaller particles were coated on the surface of larger particles, whereas they were well mixed and dispersed when both $TiO_2$ and HA were nanocrystallites. HA/$TiO_2$ biocomposite powders with homogeneous microstructure showed high sintered density and good mechanical properties.

Effect of Support Geometry on Catalytic Activity of Pt/CeO2 Nanorods in Water Gas Shift Reaction (Water Gas Shift 반응에서 Pt/CeO2 촉매의 지지체구조에 따른 촉매활성 연구)

  • Im, Hyo Been;Kwon, Soon Jin;Byun, Chang Ki;Ahn, Hee Sung;Koo, Kee Young;Yoon, Wang Lai;Yi, Kwang Bok
    • Transactions of the Korean hydrogen and new energy society
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    • v.25 no.6
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    • pp.577-585
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    • 2014
  • Nanorod and particle shape $CeO_2$ were synthesized via hydrothermal process and precipitation method, respectively, and used as supports of Pt catalyst for water gas shift (WGS) reaction. Three different durations (12, 48, and 96h) for hydrothermal process were applied for the preparation of nanorod type $CeO_2$. 1.0 wt% of Pt was loaded on the prepared supports with incipient wetness method prior to the catalytic activity tests that were carried out at a GHSV of $95,541h^{-1}$, and a temperature range of 200 to $360^{\circ}C$. Varying duration of hydrothermal process led to the difference in physical characteristics of $CeO_2$ nanorods, such as aspect ratio, BET surface area, pore diameter, and pore volume. Consequently, the catalytic activities of Pt/$CeO_2$ nanorods were affected by the physical characteristics of the supports and appeared to be in the order of Pt/$CeO_2$(12) > Pt/$CeO_2$(48) > Pt/$CeO_2$(96). The comparison of the catalytic activities and results of the analysis (XPS, XRD, SEM, BET and TPR) for the supports revealed that the activity of the catalysts depends on chemical states of the Pt and the support materials in the temperature range that is lower than $280^{\circ}C$. However, the activity is rather dependent on the physical characteristic of the supports because the increased gas velocity limits the mass transfer of reactants in micropores of the supports.

Synthesis, Characterization and Photocatalytic Activity of Reduced Graphene Oxide-Ce/ZnO Composites

  • Zhang, Wenjun;Zhao, Jinfeng;Zou, Xuefeng
    • Korean Chemical Engineering Research
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    • v.54 no.1
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    • pp.127-134
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    • 2016
  • A series of Ce-doped ZnO (Ce/ZnO) nanostructures were fabricated using the co-precipitation method, then a simply nontoxic hydrothermal approach was proposed for preparation of reduced graphene oxide (rGO)-Ce/ZnO composites. The synthesized composites were investigated by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), photoluminescence spectroscopy (PL), electrochemical impedance spectroscopy (EIS), UV-vis diffuse reflectance spectroscopy (DRS) techniques and Raman pattern. The as-synthesized rGO-Ce/ZnO composites showed high photodecomposition efficiency in comparison with the rGO-ZnO, Ce/ZnO, pure ZnO under UV, visible-light and sunlight irradiation. The degradation of methylene blue (MB) (10 mg/L, 100ml) by 95.8% within 60 min by using rGO-2 (10 mg) under sunlight irradiation was observed. The repeated use of the rGO-2 was investigated, and the results showed almost no decay in the catalytic activity.

Physicochemical Properties of MnO2 Catalyst Prepared via Hydrothermal Process and its Application for CO Oxidation (수열방법으로 합성된 이산화망간의 물리화학적 특성과 일산화탄소 산화반응)

  • Lee, Young-Ho;Jeon, Su A;Park, Sang-Jun;Youn, Hyun Ki;Shin, Chae-Ho
    • Clean Technology
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    • v.21 no.4
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    • pp.248-256
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    • 2015
  • MnO2 was prepared by a hydrothermal process method in the range of 120-200 ℃ and 0.5-5 h, calcined at 300 ℃ after induction of precipitation using KMnO4 and MnCl2・4H2O, and its catalytic activity was compared for CO oxidation. The catalysts were characterized using by X-ray diffraction, N2-sorption, scanning electron microscopy, and temperature programmed reduction of H2 or CO. The crystalline structure of pure α-MnO2 or hybrid α/β-MnO2 was controlled by the preparation conditions. The pure α-MnO2 showed better catalytic activity and thermal stability than hybrid α/β-MnO2. Especially, α-MnO2 prepared at 150 ℃ for 1 h has the highest specific surface area 214 m2 g-1, reducibility and labile lattice oxygen species analyzed by H2, CO-TPR, respectively. It also showed the best CO oxidation activity in both conditions of temperature programmed and isothermal reaction. The results came from the physicochemical properties of catalysts like the crystalline structure, specific surface area, reducibility and lattice oxygen species, and which are correlated with catalytic performance.