• Journal of Dental Rehabilitation and Applied Science
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• v.21 no.1
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• pp.33-42
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• 2005

This study was performed to investigate the surface properties and in vitro biocompatibility of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1000 SiC paper, ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed using a regulated DC power supply. The applied voltages were given at 240, 280, 320, and 360 V and current density of $30mA/cm^2$. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. Samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ during 30 days. The results obtained were summarized as follows; 1. The oxide films were porous with pore size of $1{\sim}5{\mu}m$. The size of micropores increased with increasing the spark forming voltage. 2. The main crystal structure of the anodic oxide film was anatase type as analyzed with thin-film X-ray diffractometery. 3. Needle-like hydroxyapatite (HA) crystals were observed on anodic oxide films after hydrothermal treatment at $300^{\circ}C$ for 2 hours. The precipitation of HA crystals was accelerated with increasing the spark forming voltage. 4. The precipitation of the fine asperity-like HA crystals were observed after being immersed in Hanks' solution at $37^{\circ}C$. The precipitation of HA crystals was accelerated with increasing the spark forming voltage and the time of immersion in Hanks' solution. 5. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal as increasing the spark forming voltage and the time of immersion in Hanks' solution.

• Journal of Dental Rehabilitation and Applied Science
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• v.22 no.1
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• pp.101-110
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• 2006

This study was performed to investigate the surface properties and in vitro biocompatibility of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1000 SiC paper, ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed using a regulated DC power supply. The applied voltages were given at 240, 280, 320, and 360 V and current density of $30mA/cm^2$. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. Samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ during 30 days. The results obtained were summarized as follows; 1. The oxide films were porous with pore size of $1{\sim}5{\mu}m$. The size of micropores increased with increasing the spark forming voltage. 2. The main crystal structure of the anodic oxide film was anatase type as analyzed with thin-film X-ray diffractometery. 3. Needle-like hydroxyapatie (HA) crystals were observed on anodic oxide films after hydrothermal treatment at $300^{\circ}C$ for 2 hours. The precipitation of HA crystals was accelerated with increasing the spark forming voltage. 4. The precipitation of the fine asperity-like HA crystals were observed after being immersed in Hanks' solution at $37^{\circ}C$. The precipitation of HA crystals was accelerated with increasing the spark forming voltage and the time of immersion in Hanks' solution. 5. The Ca/P ration of the precipitated HA layer was equivalent to that of HA crystal as increasing the spark forming voltage and the time of immersion in Hanks' solution.

• Applied Chemistry for Engineering
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• v.10 no.4
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• pp.509-514
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• 1999

In Preparing $BaTiO_3$ powder under hydrothermal conditions, effects of reaction period feedstock concentration and mixing rate on crystallinity, mean size and size distribution of particles were studied. Experimental results showed that the particle size became smaller with its narrow distribution as the reaction period and mixing rate increased, but feedstock concentration decreased in contrast with the results based on the classical nucleation-growth model. From these results, $BaTiO_3$ particles seem to be prepared hydrothermally through a multiple reaction procedure that includes dissolution, precipitation, hydrolysis-condensation, aggregation, diffusion and transformation.

• 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.

• Journal of Powder Materials
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• v.14 no.5
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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 $2{\sim}7nm$.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 2000.06a
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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.

• Journal of the Korean Ceramic Society
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• v.24 no.4
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• pp.397-403
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• 1987

Pb(Zr0.52Ti0.48)O3 powders were prepared by hydrothermal synthesis. Using soluble salts such as Pb(NO3)2, TiCl4 and ZrOCl2$.$8H2O and oxide such as PbO and TiO2 as starting materials, PZT powder was hydrothermally synthesized at the temperature range between 150$^{\circ}C$ and 200$^{\circ}C$. The result showed that reactivity by alkali was decreased in the sequence of Pb(NO3)2, TiCl4, ZrOCl2, PbO, TiO2 and ZrO2. Using the first three soluble salts, PZT powder was synthesiged at 150$^{\circ}C$ for 1hr. In PbO-TiCl4-ZrOCl2 system, PZT powder was synthesized at 150$^{\circ}C$ for 8rs. In Pb(NO3)2-TiO2-ZrOCl2 system, PZT powder was synthesized at 150$^{\circ}C$ for 16hrs, in PbO-TiO2-ZrOCl2 system, the powder was synthesized at 200$^{\circ}C$ for 8hrs.

• Journal of the Korean Applied Science and Technology
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• v.26 no.4
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• pp.385-393
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• 2009

Different types magnesium hydroxide groups have been obtained using the hydrothermal precipitation technique from magnesium sulfate and calcium carbonate solution. The Mg atom coordinated around O atom of ${SO_4}^{2-}$ in another layer to form a multi-layer structure crystal. The influence of synthesis parameters on the morphological characteristics and size of magnesium hydroxide groups precipitated in aqueous were investigated such as different of additive and pH. Magnesium hydroxide groups were decomposed gradually and converted finally to MgO particles after heated in air temperature up to $1050^{\circ}C$. The particle size and it's distribution morphology, crystal phase and thermal behavior of the samples were characterized through XRD, SEM, EDS, and TG/DTA.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2006.06a
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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.

• The Journal of Korean Academy of Prosthodontics
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• v.43 no.5
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• pp.684-693
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• 2005

Statement of problem: Ti-6Al-7Nb alloy is used instead of Ti-6Al-4V alloy that was known to have toxicity. Purpose: This study was performed to investigate the effect of electrolyte concentration on the surface characteristics of anodized and hydrothermally-treated Ti-6Al-7Nb alloy Materials and methods: Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1,000 SiC paper ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed at current density $30mA/cm^2$ up to 300 V in electrolyte solutions containing $\beta-glycerophosphate$ disodium salt hydrate $(\beta-GP)$ and calcium acetate (CA). Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. All samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ for 30 days. Results and conclusion: The results obtained were summarized as follows: 1. After hydrothermal treatment, the precipitated HA crystals showed the dense fine needle shape. However, with increasing the concentration of electrolyte they showed the shape of thick and short rod. 2. When the dense fine needle shape crystals was appeared after hydrothermal treatment, the precipitation of HA crystals in Hanks' solution was highly accelerated. 3. The crystal structures of $TiO_2$ in anodic oxide film were composed of strong anatase peak and weak rutile peak as analyzed with thin-film X-ray diffractometery. 4. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal in Hanks' solution.