• Title/Summary/Keyword: Hydrothermal process

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Synthesis of 3D Nanostructured Flower-like ZnO Architecture on ZnO Thin-film by Hydrothermal Process (수열합성법에 의한 3차원 ZnO 나노구조체 합성)

  • Yoo, Beom-Keun;Park, Yong-Wook;Kang, Chong-Yoon;Kim, Jin-Sang;Yoon, Seok-Jin
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.22 no.10
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    • pp.884-889
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    • 2009
  • Recently, the control of size, morphology and dimensionality in inorganic materials has been rapidly developed into a promising field in materials chemistry. 3D nanostructured flower-like ZnO architecture with different size and shapes have been simply synthesized by hydrothermal process, using zinc acetate and ammonium hydroxide as reactants. In this study, the ZnO thin-films were deposited by RF magnetron sputtering in other to get high adhesion and uniformity of 3D nanostructured flower-like ZnO architecture on a $SiO_2$ substrate. The XRD patterns identified that the obtained the nanocrystallized ZnO architecture exhibited a wurtzite structure. SEM images illustrated that the flower-like ZnO bundles consisted of flower-like or chestnut bur, which were characterized by polycrystalline and (002) preferential orientation.

Magnetic Properties of Micron Sized Fe3O4 Crystals Synthesized by Hydrothermal Methods (수열합성을 이용하여 제작한 Fe3O4 결정입자의 자기적 특성)

  • Lee, Ki-Bum;Nam, Chunghee
    • Journal of Powder Materials
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    • v.26 no.6
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    • pp.481-486
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    • 2019
  • Iron oxides currently attract considerable attention due to their potential applications in the fields of lithiumion batteries, bio-medical sensors, and hyperthermia therapy materials. Magnetite (Fe3O4) is a particularly interesting research target due to its low cost, good biocompatibility, outstanding stability in physiological conditions. Hydrothermal synthesis is one of several liquid-phase synthesis methods with water or an aqueous solution under high pressure and high temperature. This paper reports the growth of magnetic Fe3O4 particles from iron powder (spherical, <10 ㎛) through an alkaline hydrothermal process under the following conditions: (1) Different KOH molar concentrations and (2) different synthesis time for each KOH molar concentrations. The optimal condition for the synthesis of Fe3O4 using Fe powders is hydrothermal oxidation with 6.25 M KOH for 48 h, resulting in 89.2 emu/g of saturation magnetization at room temperature. The structure and morphologies of the synthesized particles are characterized by X-ray diffraction (XRD, 2θ = 20°-80°) with Cu-kα radiation and field emission scanning electron microscopy (FE-SEM), respectively. The magnetic properties of magnetite samples are investigated using a vibrating sample magnetometer (VSM). The role of KOH in the formation of magnetite octahedron is observed.

Fabrication of ZnO Nanorod/polystyrene Nanosphere Hybrid Nanostructures by Hydrothermal Method for Energy Generation Applications (에너지 발생소자응용을 위한 수열합성법기반 ZnO 나노로드/Polystylene 하이브리드 나노구조 제조)

  • Baek, Seong-Ho;Park, Il-Kyu
    • Journal of Powder Materials
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    • v.22 no.6
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    • pp.391-395
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    • 2015
  • We report on the successful fabrication of ZnO nanorod (NR)/polystyrene (PS) nanosphere hybrid nanostructure by combining drop coating and hydrothermal methods. Especially, by adopting an atomic layer deposition method for seed layer formation, very uniform ZnO NR structure is grown on the complicated PS surfaces. By using zinc nitrate hexahydrate $[Zn(NO_3)_2{\cdot}6H_2O]$ and hexamine $[(CH_2)_6N_4]$ as sources for Zn and O in hydrothermal process, hexagonal shaped single crystal ZnO NRs are synthesized without dissolution of PS in hydrothermal solution. X-ray diffraction results show that the ZnO NRs are grown along c-axis with single crystalline structure and there is no trace of impurities or unintentionally formed intermetallic compounds. Photoluminescence spectrum measured at room temperature for the ZnO NRs on flat Si and PS show typical two emission bands, which are corresponding to the band-edge and deep level emissions in ZnO crystal. Based on these structural and optical investigations, we confirm that the ZnO NRs can be grown well even on the complicated PS surface morphology to form the chestnut-shaped hybrid nanostructures for the energy generation and storage applications.

Hydrothermal Synthesis and Mechanical Characterization of 3mol%Y2O3-ZrO2 by Urea Contents (우레아 첨가량 변화에 따라 수열합성법으로 제조 된 3mol%Y2O3-ZrO2 분말의 합성 및 기계적 특성 평가)

  • Lee, Hak-Joo;Go, Myung-Won;Kim, Taik-Nam
    • Korean Journal of Materials Research
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    • v.21 no.8
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    • pp.425-431
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    • 2011
  • The industrial manufacturing of YSZ products can be summarized as a three step process: a) hydrolysis of zirconyl chloride and mixing of other solutions, b) precipitation, and c) calcination. The addition of ammonia or OH- is essential in the precipitation process. However, a strong agglomeration was observed in the results of an ammonia or OH- addition. Thus, it is necessary to disperse the powders smoothly in order to improve the mechanical strength of YSZ. In this study, YSZ was synthesized using the urea stabilizer and hydrothermal method. YSZ powders were synthesized using a hydrothermal method with Teflon Vessels at $180^{\circ}C$ for 24 h. The mole ratio of urea to Zr was 0, 0.5, 1, and 2. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens ($33\;mm{\times}8\;mm{\times}1{\pm}0.5\;mm$) for three-point bend tests were used in the mechanical properties evaluation. The crystalline of YSZ powders observed a tetragonal phase in the sample with a ratio of Zr:urea = 1:2 addition and a hydrothermal reaction time of 24 h. The average primary particle size of YSZ was measured to be 9 nm to 11 nm. The agglomerated particle size was measured from 15 nm to 30 nm. The three-point bending strength of the YSZ samples was 142.47 MPa, which is the highest value obtained for the Zr:urea = 1:2 ratio addition YSZ sample.

Characteristics of Zirconia Nanoparticles with Hydrothermal Synthesis Process (수열합성법으로 제조된 지르코니아의 나노분말 특성)

  • Cho, Chi Wook;Tai, Weon Pil;Lee, Hak Sung
    • Applied Chemistry for Engineering
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    • v.25 no.6
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    • pp.564-569
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    • 2014
  • Zirconia nanoparticles were synthesized by hydrothermal process, and experimental parameters such as reaction temperature, reaction time, kind and concentration of precipitator, kind of precursor were varied. Particle sizes and crystalline phases of each synthesized nanoparticles were analyzed with X-ray diffraction and FE-scanning electron microscope (SEM). The particle size and crystallization of zirconia increased with increasing concentration of precipitator. The growth rate of particle sizes when NaOH as a precipitator was used also increased more than that of KOH. Therefore, the use of KOH rather than NaOH was more effective in the control of particle sizes. An amorphous zirconia nanoparticle was found in 4 h of hydrothermal reaction, but the monoclinic zirconia nanoparticle was found in 8 h and over of hydrothermal reaction, and the width of nanoparticles was slightly slimmed and the length of nanoparticles was slightly extended with increasing reaction time. The smallest particle size was produced at the same synthesis condition when zirconium chloride among the precursors such as zirconium (IV) acetate, zirconium nitrate and zirconium chloride was used.

SURFACE CHARACTERISTICS AND BIOLOGICAL RESPONSES OF HYDROXYAPATITE COATING ON TITANIUM BY HYDROTHERMAL METHOD: AN IN VITRO STUDY

  • Kim, Dong-Seok;Kim, Chang-Whe;Jang, Kyung-Soo;Lim, Young-Jun
    • The Journal of Korean Academy of Prosthodontics
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    • v.43 no.3
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    • pp.363-378
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    • 2005
  • Statement of problem. Hydroxyapatite(HA) coated titanium surfaces have not yet showed the reliable osseointegration in various conditions. Purpose. This study was aimed to investigate microstructures, chemical composition, and surface roughness of the surface coated by the hydrothermal method and to evaluate the effect of hydrothermal coating on the cell attachment, as well as cell proliferation. Material and Methods. Commercially pure(c.p.) titanium discs were used as substrates. The HA coating on c.p. titanium discs by hydrothermal method was performed in 0.12M HCl solution mixed with HA(group I) and 0.1M NaOH solution mixed with HA(group II). GroupⅠ was heated at 180 $^{\circ}C$ for 24, 48, and 72 hours. GroupⅡ was heated at 180 $^{\circ}C$ for 12, 24, and 36 hours. And the treated surfaces were evaluated by Scanning electron microscopy(SEM), Energy dispersive X-ray spectroscopy(EDS), X-ray photoelectron spectroscopy(XPS), X-ray diffraction method(XRD), Confocal laser scanning microscopy(CLSM). And SEM of fibroblast and 3-(4,5- dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide(MTT) assay were used for cellular responses of the treated surfaces. Results. The color of surface changed in both groups after the hydrothermal process. SEM images showed that coating pattern was homogeneous in group II, while inhomogeneous in group I. H72 had rosette-like precipitates. The crystalline structure grew gradually in group II, according to extending treatment period. The long needle-like crystals were prominent in N36. Calcium(Ca) and phosphorus(P) were not detected in H24 and H48 in EDS. In all specimens of group II and H72, Ca was found. Ca and P were identified in all treated groups through the analysis of XPS, but they were amorphous. Surface roughness did not increase in both groups after hydrothermal treatment. The values of surface roughness were not significantly different between groups I and II. According to the SEM images of fibroblasts, cell attachments were oriented and spread well in both treated groups, while they were not in the control group. However, no substantial amount of difference was found between groups I and II. Conclusions. In this study during the hydrothermal process procedure, coating characteristics, including the HA precipitates, crystal growth, and crystalline phases, were more satisfactory in NaOH treated group than in HCl treated group. Still, the biological responses of the modified surface by this method were not fully understood for the two tested groups did not differ significantly. Therefore, more continuous research on the relationship between the surface features and cellular responses seems to be in need.

A study on the synthesis of tin oxide crystalline by the liquid reduction precipitation method and hydrothermal process (액상환원침전법 및 수열반응법을 이용한 주석산화물 결정 합성에 관한 연구)

  • Park, Il-Jeong;Kim, Geon-Hong;Kim, Dae-Weon;Choi, Hee-Lack;Jung, Hang-Chul
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.3
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    • pp.95-100
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    • 2016
  • In this work, tin oxides were obtained by the liquid reduction precipitation method and hydrothermal process using $SnCl_2{\cdot}2H_2O$, $N_2H_4$, and NaOH. Tin oxide crystals having different sizes and morphologies could be achieved. The powders were characterized by X-ray diffraction (XRD) and Field Emission Scanning Electron Microscopy (FE-SEM). Depending on the molar ratio of the raw materials, tin oxide crystalline with the spherical and rectangular plate-like shape could be obtained, the crystal phase was SnO and $Sn_6O_4(OH)_4$. And the obtained SnO crystals by a hydrothermal reaction showed various shapes, such as, spherical, plate-like and flower-like architectures depending on the temperature conditions.

Conversion of Wood Waste into Solid Biofuel Using Catalytic HTC Process (촉매 열수탄화(Hydrothermal carbonization)공정을 이용한 폐목재의 고형연료 제조 및 특성 연구)

  • Joo, Bokyoung;Yeon, Hyejin;Lee, Sangil;Ahn, Soojeung;Lee, Kyeongjae;Jang, Eunsuk;Won, JongChoul
    • New & Renewable Energy
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    • v.10 no.2
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    • pp.12-18
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    • 2014
  • The objective of this work is to produce solid biofuel from sawdust using the HTC (Hydrothermal carbonization) process. The HTC process of feedstock involves the raw material coming into contact with high temperature and pressurized water. The HTC process could produce gaseous, liquefied and solid products, but this study focused on solid product only as an alternative to coal. In this study, sawdust used for a feedstock and its moisture content was under 5%. Water was added with the feedstock to raise moisture content to 80% and also used catalysts. The HTC process was performed at temperature range from 200 to $270^{\circ}C$ and reaction time was 15 to 120 min. Rising temperature resulted in increasing the higher heating value (HHV) of HTC product. In case of adding catalyst, HHV of solid biofuel was higher and reaction occurred at lower temperature and pressure. Also, HTC solid product had been characterized and found to be hydrophobic, increased HHV (over 40%), and pelletized easily compared to raw material.

Synthesis and characterization of $BaTiO_3$ fine particles by hydrothermal process (수열합성법에 의한 미립의 $BaTiO_3$ 분말합성 및 특성)

  • 배동식;주기태;한경섭;최상흘
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.4
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    • pp.563-566
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    • 1998
  • $BaTiO_3$ fine particles were prepared by hydrothermal process from titanium tetra-isoproproxide ($Ti(OiPr)_4$) and barium hexa-hydroxide ($Ba(OH)_2{cdot}8H_2O$) as raw materials. The fine particles were obtained at the temperature range of 160 to $185^{\circ}C$. The properties of $BaTiO_3$ particles were studied as a function of various parameters such as reaction temperature, reaction time and Ba/Ti ratio, etc. The average particle size of $BaTiO_3$ increased with increasing reaction temperature and time. After hydrothermal treatment at $170^{\circ}C$ for 8 h, the average particle size of $BaTiO_3$ was about 30 nm and the particle size distribution was narrow.

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Characteristics and Preparation of Gas Sensor Using ZnO Nanorods Grown by Hydrothermal Process (수열합성법으로 성장된 ZnO 나노로드 가스 센서의 제작 및 특성 연구)

  • Jong, Jong-Hun;Yu, Il
    • Korean Journal of Materials Research
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    • v.21 no.4
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    • pp.232-235
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    • 2011
  • ZnO nanorods for gas sensors were prepared by a hydrothermal method. The ZnO gas sensors were fabricated on alumina substrates by a screen printing method. The gas-sensing properties of the ZnO nanorods were investigated for $CH_4$ gas. The effects of growth time on the structural and morphological properties of the ZnO nanorods were investigated by X-ray diffraction and scanning electron microscope. The XRD patterns of the nanocrystallized ZnO nanorods showed a wurtzite structure with the (002) predominant orientation. The diameter and length of the ZnO nanorods increased in proportion to the growth time. The sensitivity of the ZnO sensors to 5 ppm $CH_4$ gas was investigated for various growth times. The ZnO sensors exhibited good sensitivity and rapid response-recovery characteristics to $CH_4$ gas, and both traits were dependent on the growth time. The highest sensitivity of the ZnO sensors to $CH_4$ gas was observed with the growth time of 7 h. The response and recovery times were 13 s and 6 s, respectively.