• Bulletin of the Korean Chemical Society
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• v.29 no.4
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• pp.805-810
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• 2008

Using metallic Ti powder as raw materials and 1,2-diaminocyclohexane (DACH) as the trial template, two novel reduced titanophosphate open-structures were hydrothermally isolated by varying the $H_3PO_4/H_2O$ ratio to adjust the pH value. TiPO-1 crystallizes in orthorhombic Pbca space group with cell parameters a = 21.956(3) $\AA$, b = 8.6268(11) $\AA$, c = 7.2883(9) $\AA$, V = 1380.5(3) $\AA^3$, Z = 4. TiPO-2 crystallizes in triclinic space group P$\bar{1}$ with parameters a = 5.1620(10) $\AA$, b = 8.815(2) $\AA$, c = 10.655(3) $\AA$, $\alpha$ = $99.45^{\circ}$, $\beta$ = $102.94^{\circ}$, $\gamma$ = $91.06^{\circ}$, V = 465.34 $\AA^3$. TiPO-1 is constructed by infinite -Ti-O-Ti-O- linkage that is capped by $PO_4$ groups to form a chain structure with protonated DACH molecules occupying the interchain spaces. TiPO-2 represents a rare 3-D reduced titanophosphate with 12-MR channels. The structure of TiPO-2 is a neutral framework with water molecules located in the channels.

• Journal of Surface Science and Engineering
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• v.45 no.3
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• pp.97-105
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• 2012

The effects of pH, types of applied current, agitation method and time, additive on the amount of co-deposited $TiO_2$ particles in the matrix were investigated. The deposition rates increased with increasing pH values, while the volume fraction of $TiO_2$ particles and the size of agglomerated $TiO_2$ particles in the composite decreased. The volume fraction of $TiO_2$ particles in the composite decreased when pulsed current of 50% duty cycle was used. And the size of agglomerated $TiO_2$ particles in the nickel matrix of pulsed current was smaller than that of DC current specimen. The volume fraction of $TiO_2$ particles in the matrix decreased with longer time by air agitation, but in case of using magnetic bar, volume fraction in the same range of time was relatively constant. The volume fraction of the electrodeposited Ni-$TiO_2$ composite in the solution containing 0.01 M Dimethylamine borane (DMAB) increased slightly with increasing agitation time regardless of agitation methods. Thermal stability of the electrodeposited Ni-$TiO_2$ composite increased with lower pH at the temperature range of $200{\sim}800^{\circ}C$, and the results showed that the amount of co-deposited $TiO_2$ relies more on the deposition rate than zetapotential of $TiO_2$ particles.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 1999.10a
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• pp.3-4
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• 1999

최근 산업이 고속도화, 고능률화 및 고정멸화의 추세로 발전함에 따라 우수한 내마모성, 인성, 고온 안정성 및 내구성을 갖는 공구 및 금형을 요구하게 되었다. 그러나 이와같은 성질들은 어떤 단일 재료에서는 얻을 수 없으며 적당한 기판공구나 금혈위에 내마모성 보호피막을 coating함으로 비교적 저렴하게 얻을 수 있다. 화학증착법으로 TiC, TiN등을 증착시킬때에는 $1000^{\circ}C$정도의 반응온도가 필요하며 이러한 증착온도는 모재가 초경합금일때는 문제가 안되나 강재일 경우 모재의 연화와 칫수변화의 문제를 야기시킨다. 최근에는 플라즈마를 사용하여 증착반응온도를 $550^{\circ}C$ 이하로 낮추는 플라즈마 화학 증착볍(PACVD)이 대두되고 있다. 그러나 이 방법어서 는 뚱착하려는 금속원소가 TiCl4의 형태로 공급되고 있으므로 생성된 층이 염소를 포함하고 있다. 이 층에 잔존하는 염소는 층의 기계적 성질을 저하시키고 층내의 stress를 유발시킨다. 또한 HCI개스의 생성으로 인하여 펌프 및 장비의 부식이 촉진 된다 이러한 결점을 극복하기 위하여 금속유기화합물 전구체(metallo-organic precursor)로 $TiCl_4$를 대체하고자 하는 연구가 활발하게 진행되고 있으며 본 연구실에서 이에 대하여 연구한 결과를 소개하고자 한다. diethylamino titanium을 전구체로 사용하여 $H_2,\;N_2,\;Ar$분위기하에서 pulsed d.c.를 사용하는 MO-PACVD에 의하여 $150~250^{\circ}C$의 저온에서 Al 2024 기판에 TiCN층 형 성을 하였다. 전구체 증발온도는 $74~78^{\circ}C$의 온도범위어야 하며 고경도의 코탱층은 54% duty, 14.2kHz, 450V의 조건에서 얻어졌으며 duty, 주파수, 전압이 증가함에 따라 경도는 저하되었다. 이때의 표면 morphology를 SEM으로 조사한바 dome structure가 크게 발달되었음을 알 수 있었다. 본 실험의 온도 범위내에서 얻은 TiCN 증착반응의 활성화에너지는 7.5Kcal/mol이었다. 증착된 TiCN층은 우수한 내마모섣을 나타내었으며 스크래치테스트 결과 17N의 엄계하중을 나타내었다. 본 연구에서 변화 시킨 duty, 주파수, 전압의 범위에서는 층의 밀착력은 크게 변화하지 않았다. titanium isopropoxide를 전구체로 사용하여 Hz, Nz 분위기하에서 d.c.를 사용하는 MO-PACVD에 의하여 Ti(NCO) 코팅층을 SKDll, SKD61, SKH9 공구강에 형성시키는 공정을 개발하였다. 최적의 Ti(NCO) 코탱층을 얻기 위해 유입전구체 부피%의 양은 향착압력의 5%를 넘지 않아야 되고 수소와 젤소 가스비가 1:1일 때 가장 높은 코팅층의 경도값을 나타내었다. 수소와 질소 가스비가 3:7일 때 TiFeCr(NCO)의 복화합물 코팅층이 형성됨을 알 수 있었고 500t의 증착온도에서 얻은 Ti(NCO) 코팅층이 높은 경도값과 좋은 내식성을 나타내었다. 또한 이와같은 Ti(NCO) 코팅공정과 본 실험실에서 개발한 확산층만 형성시키는 plsma nitriding 공정을 결합하여 복합코탱층을 형성하였는데 이 복합코팅층은 고경도와 우수한 내마모성, 내식성 뿐만 아니라 10)N 이상의 뛰어난 밀착력을 나타내었다. 현재 많이 사용되고 있는 PVD법은 step coverage가 좋지 않은 점과 cost intensive p process라는 단점이 있다. MO-PACVD법은 이러한 문제를 해결할 수 있는 방법으로서 앞으로 지속적인 도전이 요구되는 분야이다.

• Applied Chemistry for Engineering
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• v.19 no.5
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• pp.554-558
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• 2008

$(1-x)SiO_2-(x)TiO_2$ composite fibers with various compositions of $TiO_2$ were prepared by electrospinning their sol-gel precursors of titanium (IV) iso-propoxide (TiP), and tetraethyl orthosilicate (TEOS). The surface morphology and structure of sintered composite fibers were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), simultaneous thermogravimetric analysis-differential scanning calorimetry (TGA-DSC) and Fourier transform infrared spectroscopy (FT-IR). As the content of $TiO_2$ in $(1-x)SiO_2-(x)TiO_2$ system was increased the average diameter of composite fibers was proportionally increased. Also, the transformation of $TiO_2$ from anatase to rutile form was inhibited by the highly dispersed $TiO_2$ around $SiO_2$ particles up to $0.6SiO_2-0.4TiO_2$ composite fibers even after calcination at $1000^{\circ}C$. The photocatalytic activity of $SiO_2-TiO_2$ composite fibers was examined for the methylene blue (MB) decomposition which was confirmed using UV-vis/DRS spectra. The experiments demonstrated that the MB in aqueous solution was successfully photodegraded using $SiO_2-TiO_2$ composite nanofibers under UV-visible light irradiation.

• 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.

• Journal of the Korean Society for Heat Treatment
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• v.27 no.1
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• pp.1-9
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• 2014

For connector material applications, the influence alloying elements of Mn, Cr, Fe, and Ti and cold rolling reduction on the mechanical property, electrical conductivity and bendiability of Cu-Ni-Si-P alloy was investigated. The hot rolled plates were solution treated at $980^{\circ}C$ for 1.5 h, quenched into water, cold rolled by 10% and 30% reduction in thickness, and then aged at $440{\sim}500^{\circ}C$ for 3, 4, 5 times. respectively. Cu-Ni-Si-P-x alloys cold rolled by 10 reduction before heat treatment have a good bendability compare to cold rolled by 30 reduction. Cu-3.4Ni-0.8Si-0.03P-0.1Ti shows the peak strength value of 759 MPa, an electrical conductivity of 39%IACS, an elongation of 10% and a hardness of 256 Hv aged at $440^{\circ}C$ for 6 hrs. Thus it is suitable for lead frame and connector.

• Korean Journal of Materials Research
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• v.19 no.11
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• pp.613-618
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• 2009

We designed new compositions for lead free and low temperature sealing glass frit of $ZnO-V_2O_5-P_2O_5$ system, which can be used for PDP (Plasma Display Panel) or other electronic devices. The $ZnO-V_2O_5-P_2O_5$ system can be used as a sealing material at temperatures even lower than 430$^{\circ}C$. This system, however, showed lower bonding strength with glass substrate compared to commercialized Pb based sealing materials. So, we added $TiO_2$ as a promoter for bonding strength. We examined the effect of $TiO_2$ addition on sealing behaviors of $ZnO-V_2O_5-P_2O_5$ glasses with the data for flow button, wetting angle, temporary & permanent residual stress of glass substrate, EPMA analysis of interface between sealing materials and glass substrate, and bonding strength. As a result, sealing characteristics of $ZnO-V_2O_5-P_2O_5$ system glasses were improved with $TiO_2$ addition, but showed a maximum value at 5 mol% $TiO_2$ addition. The reason for improved bonding characteristics was considered to be the chemical interaction between glass substrate and sealing glass, and structural densification of sealing glass itself.

• Journal of Korean Society of Water and Wastewater
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• v.25 no.4
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• pp.527-534
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• 2011

In this research, the photocatalytic degradation of dibenzothiophene (DBT) in $TiO_2$ aqueous suspension has been studied. $TiO_2$ photocatalysts are prepared by a sol-gel method. The dominant anatase-structure on $TiO_2$ particles is observed after calcining the $TiO_2$ gel at $500^{\circ}C$ for 1hr. Photocatalysts with various transition metals (Nd, Pd and Pt) loading are tested to evaluate the effect of transition metal impurities on photodegradation. The photodegradation efficiencies with $TiO_2$ including Pt and Pd are higher than pure $TiO_2$ powder. Also we investigated the applicability of $H_2O_2$ to increase the efficiency of the $TiO_2$ photocatalytic degradation of dibenzothiophene. The degradation efficiency increases with increasing dosage of $H_2O_2$ in the range of 0.01M to 0.1M . The effect of pH is investigated; we obtained the maximum photodegradation efficiency at pH 5. In addition, the intermediate analysis found dihydroxyl -dibenzothiophene as a reaction intermediate of dibenzothiophene during the photodegradation.

• Journal of Korean Society of Water and Wastewater
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• v.25 no.4
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• pp.555-564
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• 2011

The photocatalytic degradation of trichloroethylene (TCE) in $TiO_2$ aqueous suspension has been studied. $TiO_2$ photocatalysts are prepared by a sol-gel method. The dominant anatase-structure on $TiO_2$ particles is observed after calcining the $TiO_2$ get at $500^{\circ}C$ for 1hr. The Langmuir-Hinshelwood model is applicable to describe the photodegradation, which indicates that adsorptionof the solute on the surface of $TiO_2$ particles plays an important role in photodegradation. Photocatalysts with various transition metals (Nd, Pd and Pt) loading are tested to evaluate the effect of transition metal impurities on photodegradation. The photodegradation efficiencies with $TiO_2$ including Pt, Pd and Nd are lower than pure $TiO_2$ powder. The effect of pH is investigated and the maximum photodegradation efficiency is obtained at pH 7. In addition, the intermediates such as dichloromethane, chloroform, and trichloroethane are detected during the photodegradation of TCE.