• 한국치위생학회지
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• 제7권4호
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• pp.471-479
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• 2007

The purpose of this study was to examine the optimum condition of impulse during the anodic spark oxidation applying pulse current as well as to find the excellent condition for HA precipitation the after electrochemical hydrothermal treatment by cathode reduction method. After anodic spark oxidation, the anodized specimen and the Pt plate connected cathode and anode, respectively. Hydrothermal treatment performed at 90, 120, $150^{\circ}C$ for 2 hours in the electrolyte containing $K_2HPO_4$, $CaCl_2{\cdot}2H_2O$, Tris(Hydroxymethyl)-$(CH_2OH)_3\;CNH_2$(Aminomethane), and NaCl. The optimum impulse voltage for anodic spark oxidation was 350V. The optimum pulse cycle measured at 10 mS. The HA crystals precipitated excellently by cathode reduction at $150^{\circ}C$ for 2 hours. The phases of anatase, rutile, and HA coating on the surface of modified titanium surface immersed in Hanks' solution for 3weeks were detected by XRD measurement and the intensity of HA crystal phase has increased by temperature and time of hydrothermal treatment. According to the our experiments, we found that Pure Ti will be good materials of bioactivity and biocompatibility.

• 한국전기전자재료학회논문지
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• 제28권9호
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• pp.561-564
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• 2015

Nano-size $BaTiO_3$ powder was synthesized by relatively simple hydrothermal reaction method. Finely dispersed Ti hydroxide precursor was first precipitated using $Ti(SO_4)_2$ and NaOH solution by applying ultrasonic power and washed thoroughly to remove $SO_4{^{2-}}$ and $Na^+$ ion. Then hydrothermal reaction was done at $160^{\circ}C$ for 6 hrs using solution prepared by washed Ti hydroxide precursor slurry and $Ba(OH)_2{\cdot}8H_2O$ with Ti:Ba mole ratio of 1:1. 200 ~ 500 nm size and uniform size distributed $BaTiO_3$ powder was synthesized by relatively low temperature and simple process.

• 한국결정성장학회지
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• 제26권5호
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• pp.175-180
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• 2016

본 연구에서는 수용액 상에서 침전법과 수열합성법을 이용하여 나노크기의 ZnO 분말을 합성하였다. 두 합성방법 모두 출발원료로는 Zn-nitrate hexahydrate($Zn(NO_3)_2{\cdot}6H_2O$)와 NaOH 수용액을 사용하였고, 이들의 혼합용액에 합성조건 즉 반응 pH, 온도 및 Zn precursor의 몰 농도를 달리하여 ZnO 분말을 얻을 수 있었다. 두 합성법 모두에서 단일 상 ZnO는 낮은 Zn 농도 높은 pH 및 높은 온도 조건에서 합성되기 쉬웠다. 합성된 분말의 형상은 flake(plate), multipod 및 rod 형태로 합성 조건에 따라 그 형태의 조절이 가능하였다. 침전법에 비해 수열합성법은 $100^{\circ}C$ 이하인 비교적 낮은 합성온도에서도, 본 연구의 Zn 농도 전 구간(0.1~1 M)과 넓은 pH 범위에서 결정성이 우수한 ZnO 단일 상을 합성할 수 있는 장점을 보여주었다.

• Korean Chemical Engineering Research
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• 제51권2호
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• pp.195-202
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• 2013

본 연구에서는 Titanium(IV) sulfate($Ti(SO_4)_2$)와 암모니아수로부터 수열합성법을 이용하여 비교적 낮은 합성온도($80{\sim}100^{\circ}C$)와 상압에서 소성과정을 거치지 않고 $TiO_2$ 분말을 제조하였고, $TiO_2$ 제조 시 반응온도, 반응물의 초기농도, 혼합용액의 pH와 같은 반응조건에 따른 $TiO_2$ 입자의 결정구조와 입자분포, 형상 등과 같은 물리적 특성을 고찰하였다. 제조한 시료는 UV 조사 하에 Brilliant Blue FCF(BB-FCF)의 광분해 실험을 실시하여 광분해 성능과 DRS 분석을 통해 광촉매 활성을 비교하였다. 제조한 시료의 물성은 XRD, SEM, PL, 입도분포 측정을 통하여 확인하였다. Titanium(IV) sulfate($Ti(SO_4)_2$)의 초기농도가 증가할수록 $TiO_2$의 평균 입자크기와 결정화도는 증가하였고 광촉매 활성은 감소하였다. 혼합용액의 pH가 높을수록 평균 입자크기는 감소하였고 광촉매 활성은 증가하였다. 반응온도가 높을수록 결정화도와 광촉매 활성은 증가하였다. 이상의 결과들로부터 $Ti(SO_4)_2$와 암모니아수를 이용한 비교적 낮은 합성온도와 상압에서의 수열합성법으로도 순수한 anatase 결정구조의 $TiO_2$가 제조됨을 확인할 수 있었다.

• 한국세라믹학회지
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• 제40권12호
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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.

• 한국결정성장학회:학술대회논문집
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• 한국결정성장학회 2000년도 Proceedings of 2000 International Nano Crystals/Ceramics Forum and International Symposium on Intermaterials
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• pp.35-58
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• 2000

The demand for sub-micrometer or nanometer functional ceramic powders with a better suspension behavior in aqueous media in increasing. Redispersible barium titanate (BT) nanocrystals, green light emitting Mn2+ doped Zn$_2$SiO$_4$ and ZnS nanoparticle phosphors were synthesized by a hydrothermal method or chemical precipitation with surface modification. The nanoparticle redispersibility for BT was achieved by using a polymeric surfactant. X-ray diffraction(XRD) results indicated that the BT particles are of cubic phase with 80 nm in size. XRD results of zinc silicate phosphor indicate that seeds play an important role in enhancing the nucleation and crystallization of Zn$_2$SiO$_4$ crystals in a hydrothermal condition. This paper describes and discuss the methods of surface modification, and the resulting related properties for BT, zinc silicate and zinc sulfide.

• 한국분말재료학회지
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• 제14권5호
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• pp.309-314
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• 2007

Zirconia powders with nano size pores and high specific surface areas were synthesized via aqueous precipitation and hydrothermal synthetic method using $ZrOCl_28H_2O$ and $NH_4OH$ under pH=11 and ambient condition. By this reaction. zirconia hydrate $(ZrO_x(OH)_{4-2x})$ was primarily synthesized and the obtained zirconia hydrate was heat treated hydrothermally using an autoclave at various temperatures under pH=11. X-ray diffraction, Scanning electron microscopy, Energy dispersive X-ray spectroscopy, FT-IR, Raman, Particle size analysis, DTA-TG, and BET techniques were used for the characterization of the powder. The synthesized zirconia showed an amorphous phase, however, the phase was transformed to the crystalline state during the hydrothermal process. The observed crystalline phase above $160^{\circ}C$ was a mixed phase of monoclinic and tetragonal zirconia. By the BET analysis, it was found that the specific surface area was ranged in $126{\sim}276m^2/g$ and the zirconia had the cylindrical shaped pores with average diameter of $2{\sim}7nm$.

• 한국세라믹학회지
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• 제32권5호
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• pp.543-548
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• 1995

Li-ferrite powders were prepared from mixture of Fe and Li salts using a hydrothermal method. Their crystal structure, microstructure and magnetic property were investigated with X-ray diffraction analysis, chemical analysis, SEM, and VSM. In the case of using FeCl3 as a precursor, Li-ferrite powders were synthesized. However, Fe3O4 was formed when the precursor was a divalented Fe2SO4 or FeCl2. The precipitation rate of Li-ferrite was increased as the reaction temperature increased. The optimum conditions of synthesis were the mole ratio of Fe+++/Li+=2, pH 13, the reaction temperature of 25$0^{\circ}C$ and the reaction time of 120min. With this condition, the spherical particles with good dispersion were obtained with average particle size of 0.4${\mu}{\textrm}{m}$ and saturation magnetization of 65 emu/g.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2006년도 하계학술대회 논문집 Vol.7
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• pp.545-546
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• 2006

This study was performed to investigate the surface properties of electrochemically oxidized pure titanium by anodic spark discharging method. Commercially pure titanium plates of $10{\times}20{\times}1[mm]$ in dimensions were polished sequentially emery paper. Anodizing was performed at current density of $76.2\;[mA/cm^2]$, application voltage of 290, 350, 400 [V] using a regulated DC power supply, which allowed automatic transition constant current when a preset maximum voltage has been reached. The Ti surface oxided films was characterized by scanning electron microscope(SEM). The precipitation of HA(Hydroxyapatite) crystals on anodized surface was greatly accelerated by hydrothermal treatment. The concentrations of DL-$\alpha$-Glycerolphosphate Magnesiurn(DL-$\alpha$-GP-Mg) salt and Ca acetate in an electrolyte was highly affected the precipitation of HA crystals converted by Ti Anodized oxide films by Shape of Impulse Voltage.

• Korean Chemical Engineering Research
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• 제54권2호
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• pp.152-156
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• 2016

Brilliant blue FCF에 대한 분해 특성이 우수한 광촉매를 제조하는 연구를 수행하였다. 먼저 전구체인 titanium (IV) sulfate와 zinc acetate에 침전제로 각각 NaOH, $NH_4OH$를 첨가하여 비교적 낮은 온도와 상압에서 중간상 형성 없이 1단계의 수열합성법으로 $TiO_2$와 ZnO를 제조하였다. $TiO_2$의 경우 제조과정에 양이온성 계면활성제인 CTAB을 첨가하여 제조하기도 하였다. 제조된 $TiO_2$와 ZnO의 결정성, 입자크기, 흡광도 등과 같은 물리적 특성을 확인하기 위해 XRD, Zeta-potential meter, DRS 등을 사용하여 분석하였다. 광촉매적 특성을 확인하기 위해 회분식 반응장치를 이용하여 UV 조사 하에서 brilliant blue FCF의 광분해 특성을 조사하였다. CTAB을 첨가하지 않은 경우, $TiO_2$가 ZnO보다 입자가 작고 흡광도와 광촉매 반응의 초기속도가 큰 것을 확인할 수 있었다. 그리고 동일한 제조조건에서 CTAB을 전구체인 $Ti(SO_4)_2$ 농도의 1/10 첨가하여 제조한 $TiO_2$는 CTAB을 첨가하지 않은 것보다 brilliant blue FCF의 최종 제거율이 약 15% 정도 우수하였다.