• Title/Summary/Keyword: Hydrothermal deposition

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Selective Growth of Nanosphere Assisted Vertical Zinc Oxide Nanowires with Hydrothermal Method

  • Lee, Jin-Su;Nam, Sang-Hun;Yu, Jung-Hun;Yun, Sang-Ho;Boo, Jin-Hyo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.252.2-252.2
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    • 2013
  • ZnO nanostructures have a lot of interest for decades due to its varied applications such as light-emitting devices, power generators, solar cells, and sensing devices etc. To get the high performance of these devices, the factors of nanostructure geometry, spacing, and alignment are important. So, Patterning of vertically- aligned ZnO nanowires are currently attractive. However, many of ZnO nanowire or nanorod fabrication methods are needs high temperature, such vapor phase transport process, metal-organic chemical vapor deposition (MOCVD), metal-organic vapor phase epitaxy, thermal evaporation, pulse laser deposition and thermal chemical vapor deposition. While hydrothermal process has great advantages-low temperature (less than $100^{\circ}C$), simple steps, short time consuming, without catalyst, and relatively ease to control than as mentioned various methods. In this work, we investigate the dependence of ZnO nanowire alignment and morphology on si substrate using of nanosphere template with various precursor concentration and components via hydrothermal process. The brief experimental scheme is as follow. First synthesized ZnO seed solution was spun coated on to cleaned Si substrate, and then annealed $350^{\circ}C$ for 1h in the furnace. Second, 200nm sized close-packed nanospheres were formed on the seed layer-coated substrate by using of gas-liquid-solid interfacial self-assembly method and drying in vaccum desicator for about a day to enhance the adhesion between seed layer and nanospheres. After that, zinc oxide nanowires were synthesized using a low temperature hydrothermal method based on alkali solution. The specimens were immersed upside down in the autoclave bath to prevent some precipitates which formed and covered on the surface. The hydrothermal conditions such as growth temperature, growth time, solution concentration, and additives are variously performed to optimize the morphologies of nanowire. To characterize the crystal structure of seed layer and nanowires, morphology, and optical properties, X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), Raman spectroscopy, and photoluminescence (PL) studies were investigated.

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Hydroxyapatite Coating on Al2O3 by Hydrothermal Process

  • Ha, Jung-Soo
    • Journal of the Korean Ceramic Society
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    • v.40 no.12
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    • pp.1154-1158
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    • 2003
  • Hydrothermal deposition of hydroxyapatite coatings on $Al_2$O$_3$ substrates was studied using aqueous solutions of Ca(NO$_3$)$_2$ㆍ4$H_2O$ and (NH$_4$)$_2$HPO$_4$ containing EDTA disodium salt as a chelating agent for $Ca^{2+}$. For the precipitation of the coatings the EDTA-Ca$^{2+}$ chelates were dissociated thermally at 20$0^{\circ}C$ or decomposed by oxidation with $H_2O$$_2$ at 9$0^{\circ}C$. Scanning electron microscopy and X-ray diffraction were used to investigate the deposition behavior and the phase of the coatings. Hydroxyapatite coatings were not deposited with the thermal dissociation method, whereas uniform deposition of the coatings (about 0.7 $\mu\textrm{m}$ thickness) was obtained with the oxidative decomposition method. The coatings consisted of fine rod-like hydroxyapatite crystals (hexagonal structure) with 60-80 nm diameters, having some preferred orientation with their length (i.e., the c axis) perpendicular to the substrate.ate.

Density control of ZnO nanorod arrays using ultrathin seed layer by atomic layer deposition

  • Shin, Seokyoon;Park, Joohyun;Lee, Juhyun;Choi, Hyeongsu;Park, Hyunwoo;Bang, Minwook;Lim, Kyungpil;Kim, Hyunjun;Jeon, Hyeongtag
    • Journal of Ceramic Processing Research
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    • v.19 no.5
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    • pp.401-406
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    • 2018
  • We investigated the effect of ZnO seed layer thickness on the density of ZnO nanorod arrays. ZnO has been deposited using two distinct processes consisting of the seed layer deposition using ALD and subsequent hydrothermal ZnO growth. Due to the coexistence of the growth and dissociation during ZnO hydrothermal growth process on the seed layer, the thickness of seed layer plays a critical role in determining the nanorod growth and morphology. The optimized thickness resulted in the regular ZnO nanorod growth. Moreover, the introduction of ALD to form the seed layer facilitates the growth of the nanorods on ultrathin seed layer and enables the densification of nanorods with a narrow change in the seed layer thickness. This study demonstrates that ALD technique can produce densely packed, virtually defect-free, and highly uniform seed layers and two distinctive processes may form ZnO as the final product via the initial nucleation step consisting of the reaction between $Zn^{2+}$ ions from respective zinc precursors and $OH^-$ ions from $H_2O$.

Hydrothermal Coating of Hydroxyapatite on ZrO2 Ceramics

  • Ha, Jung-Soo
    • Journal of the Korean Ceramic Society
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    • v.43 no.8 s.291
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    • pp.463-468
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    • 2006
  • Hydrothermal deposition of hydroxyapatite coatings on two types of $ZrO_2$ substrates (3 mol% $Y_2O_3$-doped and 13 mol% $CeO_2$-doped tetragonal $ZrO_2s$) was studied using aqueous solutions of $Ca(NO_3)_2\;4H_2O$ and $(NH_4)_2HPO_4$ containing EDTA (ethylene diamine tetra acetic acid) disodium salt as a chelating agent for $Ca^{2+}$ ions. For the precipitation of the coatings, the $EDTA-Ca^{2+}$ chelates were decomposed by oxidation with $H_2O_2$ at $90^{\circ}C$. The deposition behavior, morphology, and orientation of the coatings were investigated while varying the solution pH using scanning electron microscopy and X-ray diffractometry. For the two sub-strates, sparse deposition of the coating was obtained at pH 5.5, whereas a uniform deposition was obtained at pH 7.1, 9.8, and 11.4 with a denser microstructure for the higher pH. The coating consisted of thin needle-like or plate-like crystals ($1-2{\mu}m$ length or diameter) at pH 7.1, but fine rod-like crystals ($1-2{\mu}m$ length, $0.1{\mu}m$ diameter) at pH 9.8 and 11.4. The coatings were $1-3{\mu}m$ thick and showed a preferred orientation of the hydroxyapatite crystals with their c axis (i.e., the elongated direction) perpendicular to the substrate surface especially for pH 9.8 and 11.4.

Synthesis of Aligned ZnO Nanorod Arrays via Hydrothermal Route (수열합성법에 의한 정렬된 ZnO 나노로드 구조의 합성)

  • Koo, Jin Heui;Lee, Byeong Woo
    • Journal of the Korean institute of surface engineering
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    • v.49 no.5
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    • pp.472-476
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    • 2016
  • The nano-array of the vertically aligned rod-like particles grown on ZnO coated glass-substrates was obtained via hydrothermal process. ZnO thin film coatings were prepared on the glass substrates using a MOD (metallorganic deposition) dip-coating method with zinc chloride dihydrate as starting material and 2-ethylhexanol as solvent. ZnO nanorods were synthesized on the seeded substrates by hydrothermal method at $80^{\circ}C$ using zinc-nitrate hexahydrate as a Zn source and sodium hydroxide as a mineralizer. Under the hydrothermal condition, the rod-like nanocrystals were easily attaching on the already ZnO seeded (coated) glass surface. It has been shown that the hydrothermal synthesis parameters are key factors in the nucleation and growth of ZnO crystallites. By controlling of hydrothermal parameters, the ZnO particulate morphology could be easily tailored. Rod-shaped ZnO arrays on the glass substrates consisted of elongated crystals having 6-fold symmetry were predominantly developed at high Zn precursor concentration in the pH range 7~11.

Crack-Free Fabrications of Yttria-Stabilized Zirconia Films Using Successive-Ionic-Layer-Adsorption-and-Reaction and Air-Spray Plus Method

  • Taeyoon Kim;Sangmoon Park
    • Korean Journal of Materials Research
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    • v.34 no.2
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    • pp.79-84
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    • 2024
  • Thin films of yttria-stabilized zirconia (YSZ) nanoparticles were prepared using a low-temperature deposition and crystallization process involving successive ionic layer adsorption and reaction (SILAR) or SILAR-Air spray Plus (SILAR-A+) methods, coupled with hydrothermal (175 ℃) and furnace (500 ℃) post-annealing. The annealed YSZ films resulted in crystalline products, and their phases of monoclinic, tetragonal, and cubic were categorized through X-ray diffraction analysis. The morphologies of the as-prepared films, fabricated by SILAR and SILAR-A+ processes, including hydrothermal dehydration and annealing, were characterized by the degree of surface cracking using scanning electron microscopy images. Additionally, the thicknesses of the YSZ thin films were compared by removing diffusion layers such as spectator anions and water accumulated during the air spray plus process. Crack-free YSZ thin films were successfully fabricated on glass substrates using the SILAR-A+ method, followed by hydrothermal and furnace annealing, making them suitable for application in solid oxide fuel cells.

Hydrothermal Antimony Deposits of the Hyundong Mine : Geochemical Study (현동 광산의 열수 안티모니 광화작용 : 지화학적 연구)

  • Seong-Taek Yun
    • Economic and Environmental Geology
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    • v.32 no.5
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    • pp.435-444
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    • 1999
  • The antimony deposits of the Hyundong mine, located in the northeastern part of the Sobaegsan massif, occur as hydrothermal quartz+carbonate veins and stockworks which fill the fault fractures developed in Precambrian metamOlphic rocks (mainly, granitic gneiss). Hydrothermal alteration occurs commonly in the vicinity of mineralized veins and is characterized by sericitization and silicification. A K-Ar age of alteration sericite is 139.2$\pm$ 4.4 Ma, implying the early Cretaceous age of mineralization, possibly in association with intrusion of nearby acidic dikes (mainly, quartz porphyry). The hydrothermal mineralization occurred in five mineralization stages. These are: (I) stage I, characterized by deposition of chalcedonic quartz; (2) stage II, deposition of quartz with base-metal sulfides and stibnite; (3) stage III, deposition of quartz and carbonates (calcite, dolomite, ankerite, rhodochrosite) with various antimony-bearing minerals such as stibnite, polybasite, berthierite, native antimony, gudmundite and ullmannite; (4) stage IV, deposition of calcite with stibnite; and (5) stage V, deposition of barren calcite. Antimony occurs mostly as stibnite within stages II to IV veins, which has various habits including disseminated, veinlets and euhedral coarse crystals. Fluid inclusion studies indicate that hydrothermal mineralization at Hyundong occurred from the fluids with temperature and salinity of $330^{\circ}$C to 120 and 5.3 wI. % equiv. NaCI. The temperature and salinity of ore fluids systematically decreased with elapsed time in the course of mineralization, possibly due to the influx of larger amounts of meteoric groundwater. The deposition of antimony-bearing minerals occurred at low temperatures «$250^{\circ}$C), mainly due to the cooling and dilution of fluids. Based on the evidence of fluid boiling during the early stage II mineralization, the mineralization occurred under low pressure conditions (about 80 bars, corresponding to depths of about 350 m under hydrostatic pressure regime). Thermodynamic considerations of ore . mineral assemblages indicate that antimony deposition also occurred as the results of decreases in temperature and sulfur fugacity of hydrothermal fluids. Calculated sulfur isotope composition of ore fluids ($\delta^{34}S_{\Sigma s}$=5.4 to 7.8$\textperthousand$) indicates an igneous source of sulfur.

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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.

The growth of ZnO nanorods by hydrothermal method on organic substrates (유기 기판 위에 수열 합성법으로 성장된 ZnO 나노 막대의 특성 연구)

  • Kim, Ah-Ra;Lee, Ji-Yeon;Lee, Ju-Young;Kim, Hong-Seung;Park, Hyun-Kook
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.281-281
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    • 2010
  • In this study, ZnO nanorod arrays are grown on organic substrates by hydrothermal method which requires a low temperature, simple process, and no vacuum. The structure properties of ZnO nanorods were examined by field emission scanning electron microscopy and X-ray diffraction. To detect the optical transmission, ultraviolet visible spectrophotometer was also used. From results, the ZnO nanorods were grown the horizontal growth on the organic substrates had the length of over $10\;{\mu}m$. After deposition of ZnO seed layer, the ZnO nanorod arrays had uniformity orientation and length.

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Evaluation of Biocompatibility of Anodized and Hydrothermally Treated Pure Niobium Metal (양극산화와 열수처리한 순수 니오비움 금속의 생체활성 평가)

  • Won, Dae-Hee;Choi, Un-Jae;Lee, Min-Ho;Bae, Tae-Sung
    • Journal of Technologic Dentistry
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    • v.27 no.1
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    • pp.79-88
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    • 2005
  • This study was performed to investigate the surface properties of electrochemically oxidized pure niobium by anodic oxide and hydrothermal treatment technique. Niobium specimens of $10\times10mm$ in dimension were polished sequentially from #600, #800, #1000 emery paper. The surface pure niobium specimens were anodized in an electrolytic solution that was dissolved calcium and phosphate in water. The electrolytic voltage was set in the range of 250 V and the current density was 10 $mA/cm^2$. The specimen was hydrothermal treated in high-pressure steam at 300$^{\circ}C$ for 2 hours using an autoclave. Then, specimens were immersed in the Hanks' solution with pH 7.4 at 37$^{\circ}C$ for 30 days. The surface of specimen was characterized by scanning electron microscope(SEM), energy dispersive X-ray microanalysis(EDX), potentiostat/galvanostat test, and cytotoxicity test. The results obtained was summarized as follows; According to the result of measuring corrosion behavior at 0.9% NaCl, corrosion resistance was improved more specimens treated with anodic oxide than in hydrothermal treated ones. The multi-porous oxide layer on surface treated through anodic oxidation showed a structure that fine pores overlap one another, and the early precipitation of apatite was observed on the surface of hydrothermal treated samples. According to the result of EDX after 30 days deposition in Hanks' solution, Ca/P was 1.69 in hydrothermal treated specimens. In MTT test, specimens treated through anodic oxidation and hydrothermal treated ones showed spectrophotometer similar to that of the control group. Thus no significant difference in cytotoxicity was observed (P>0.05).

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