• 공업화학
• /
• 제25권6호
• /
• pp.564-569
• /
• 2014

지르코니아 나노분말을 수열합성법으로 제조하였으며, 반응온도, 반응시간, 침전제의 종류 및 농도, 전구체의 종류를 실험 변수로 하였고, 각각의 제조된 분말을 X-선 회절(XRD)과 주사전자현미경(FE-SEM)을 통해 입자크기 및 결정상을 측정하였다. 침전제의 농도 증가에 따라 지르코니아 입자크기가 증가하였으며, 입자의 결정화도도 높아졌고, KOH 보다 NaOH 침전제를 사용하였을 경우, 입자 성장 속도가 증가하였다. 이는 입자의 크기 컨트롤에 있어 NaOH를 사용하는 경우보다 KOH를 사용하는 것이 더 효과적이었다. 4 h의 수열반응시간에서는 4 h의 수열반응시간에서는 비정질의 지르코니아 입자가 발견되었지만, 8 h 이상 합성 시, 단사정상의 지르코니아 입자가 생성됨을 확인하였고, 반응시간이 길어짐에 따라 지르코니아 입자의 폭이 소폭으로 줄어들고, 길이는 소폭 늘어남을 확인하였다. 동일한 합성 조건에서 전구체로서 zirconium (IV) acetate, zirconium nitrate, zirconium chloride 중에서 zirconium chloride를 사용하여 합성하였을 경우, 입자의 크기가 가장 작게 형성되었다.

• 대한치과보철학회지
• /
• 제43권3호
• /
• pp.363-378
• /
• 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.

• 한국재료학회지
• /
• 제20권5호
• /
• pp.262-266
• /
• 2010

ZnO nanostructures were grown on an Au seed layer by a hydrothermal method. The Au seed layer was deposited by ion sputter on a Si (100) substrate, and then the ZnO nanostructures were grown with different precursor concentrations ranging from 0.01 M to 0.3M at $150^{\circ}C$ and different growth temperatures ranging from $100^{\circ}C$ to $250^{\circ}C$ with 0.3 M of precursor concentration. FE-SEM (field-emission scanning electron microscopy), XRD (X-ray diffraction), and PL (photoluminescence) were carried out to investigate the structural and optical properties of the ZnO nanostructures. The different morphologies are shown with different growth conditions by FE-SEM images. The density of the ZnO nanostructures changed significantly as the growth conditions changed. The density increased as the precursor concentration increased. The ZnO nanostructures are barely grown at $100^{\circ}C$ and the ZnO nanostructure grown at $150^{\circ}C$ has the highest density. The XRD pattern shows the ZnO (100), ZnO (002), ZnO (101) peaks, which indicated the ZnO structure has a wurtzite structure. The higher intensity and lower FWHM (full width at half maximum) of the ZnO peaks were observed at a growth temperature of $150^{\circ}C$, which indicated higher crystal quality. A near band edge emission (NBE) and a deep level emission (DLE) were observed at the PL spectra and the intensity of the DLE increased as the density of the ZnO nanostructures increased.

• 한국결정성장학회지
• /
• 제30권3호
• /
• pp.91-95
• /
• 2020

본 연구는 BaTiO₃ 나노입자의 용액 공정의 분산성을 확보하기 위해 합성 시간과 온도 증가를 통한 입자들의 핵생성 속도 및 확산 속도를 동시에 증가시켜 수열합성을 진행하였다. 상대적으로 연구가 부족했던 20 nm 이하 균일한 크기의 BaTiO₃ 나노입자를 oleic acid 리간드를 매개로 180℃, 30시간의 조건에서 추가 공정 없이 합성하였다. 수열합성을 저온에서 짧은 시간 동안 진행하였을 시 입자의 응집과 크기의 불균일함을 확인하였으며, 고온에서 장시간 진행하였을 시 입자가 잘 분산되고 크기가 균일한 것을 확인하였다. 이는 고온에서 TiO₂ 입자의 핵 생성 속도와 Ba²⁺ 이온의 확산 거리 증가에 기인한다. 비극성 용매인 mesitylene에서 향상된 분산도를 보여준 BaTiO₃ 나노입자의 크기와 결정도 및 흡광도는 투과전자 현미경과 X-ray diffraction 및 자외/가시선 분광광도계를 통해 분석하였다. 본 연구 결과로 수열합성을 통한 BaTiO₃ 나노입자의 크기의 균일성과 분산성을 개선하고 다양한 전자소자에 응용 가능할 것이라 예상한다.

• 미생물학회지
• /
• 제48권1호
• /
• pp.42-47
• /
• 2012

열수구(Hydrothermal vent)는 빛이 없는 환경에서 생명체의 진화가 일어나는 독특한 환경을 유지하고 있다. 남태평양 Tonga의 Tofua arc의 열수구로부터 퇴적물을 채취하여 산화철[iron(III)], 황(elemental sulfur, $S^0$) 그리고 질산염을 전자수용체로 사용하고, 수소($H_2$), yeast extract를 전자공여체로 사용하여 배양에 의한 미생물의 다양성을 연구하였다. 배양 온도는 각각 $65^{\circ}C$와 $80^{\circ}C$였으며, 연속희석배양법과 16S rRNA 유전자의 PCR-Denaturing Gradient Gel Electrophoresis를 분석하고, 검출된 염기서열의 정보분석을 통하여 고세균을 동정하였다. 16S rRNA 유전자의 계통분류학적 분석 결과 배양된 대부분의 고세균은 Thermococcus 속(T. alcaliphilius, T. litoralis, T. celer, T. barossii, T. thoreducens, T. coalescens)에 속하며 그들과 98-99%의 상동성을 가지고 있었다. Thermococcus 속의 미생물들이 일반적으로 이용할 수 없는 질산염과 산화철을 전자수용체로 첨가한 배양에서 관찰되었으나, 이는 환원제로 첨가한 $Na_2S$의 산화물을 이용하여 성장한 것으로 추정된다. Thermococcus 속에 속하는 고세균 외의 다양한 고세균의 배양을 위해서는 $Na_2S$ 대신 다른 환원제를 사용하는 배양조건의 이용이 요구된다.

• 한국전기전자재료학회:학술대회논문집
• /
• 한국전기전자재료학회 2009년도 추계학술대회 논문집
• /
• pp.238-238
• /
• 2009

In this work, we investigated the effect of the Zn complex concentration and growth temperature on the growth of ZnO nanorod by hydrothermal method. The ZnO nanorods were performed at condition of the various Zn complex concentration and growth temperature, 0.02 ~ 0.08 M and 60 ~ 80 $^{\circ}C$, respectably. We found from the SEM results that the diameter and length of ZnO nanorods were with increasing the growth temperature and Zn complex concentration. However, the growth condition in the two parameters wasmore than sensitive compared to Zn complex concentration on increasing the growth rate. From photoluminescence(PL) analysis, the strong band-edge emission for ZnO nanorod grown at 80 $^{\circ}C$ with 0.08 M indicated the fine crystallinity. Therefore, the diameter and length of ZnO nanorods have been able to control through the control of front growth parameters. Also, these ZnO nanorods grown low temperature will be available as building block for transparence flexible device applications.

• 한국세라믹학회:학술대회논문집
• /
• 한국세라믹학회 2003년도 추계총회 및 연구발표회 초록집
• /
• pp.28.2-28
• /
• 2003

• 한국세라믹학회:학술대회논문집
• /
• 한국세라믹학회 2003년도 추계총회 및 연구발표회 초록집
• /
• pp.91.2-91
• /
• 2003

• 공업화학
• /
• 제10권4호
• /
• pp.509-514
• /
• 1999

수열합성법을 이용한 $BaTiO_3$ 미세분말제조시 반응시간, 출발물질농도와 교반속도 등이 입자의 결정성, 평균입경과 입도분포에 미치는 영향을 조사하였다. 실험결과 기존의 핵생성-입자성장 모델과는 상이하게도 반응시간과 교반속도가 증가할수록 또는, 출발물질의 농도가 감소할수록 입자크기는 감소하였으며, 입도분포도 좁았다. 이로부터 $BaTiO_3$ 결정입자는 수열합성시 용해, 가수분해-축합반응, 침전, 응집, 확산, 전이 등의 복합적인 반응경로를 거치는 것으로 판단되었다.

• Bulletin of the Korean Chemical Society
• /
• 제25권9호
• /
• pp.1341-1345
• /
• 2004

We developed a novel synthesis strategy of titania nanowire arrays by employing simple hydrothermal reaction and ion-exchange reaction techniques. Hydrothermal reactions of metallic titanium powder with $H_2O_2$ in a 10 M NaOH solution produced a new sodium titanate compound, $Na_2Ti_6O_{13}{\cdot}xH_2O$ (x~4.2), as arrays of nanowires of lengths up to 1 mm. Acid-treatment followed by calcination of this material produced arrays of highly crystalline anatase nanowires as evidenced by x-ray diffraction, Raman spectroscopy, and transmission electron microscopy studies. In both cases of sodium titanate and anatase, the nanowires have exceptionally large aspect ratios of 10,000 or higher, and they form arrays over a large area of $1.5 {\times} 3 cm^2$. Observations on the reaction products with varied conditions indicate that the array formation requires simultaneously controlled formation and crystal growth rates of the $Na_2Ti_6O_{13}{\cdot}xH_2O$ phase.