• 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.

• Corrosion Science and Technology
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• v.8 no.4
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• pp.139-142
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• 2009

Recently, quaternary titanium alloys of the system Ti-Nb-Ta-Zr received considerable research interest as potential implant materials because of their excellent mechanical properties and biocompatibility. However, only few reported works were available on the corrosion behavior of such alloys. Hence, in the present work, electrochemical corrosion of Ti-35Nb-5Ta-7Zr alloy, which has been fabricated by arc melting and heat treatment, was studied in 0.9 wt% NaCl at $37\pm1^{\circ}C$, along with biomedical grade Ti-6Al-4V and CP-Ti. The phase and microstructure of the alloys were investigated employing XRD and SEM. The results of electrochemical studies indicated that the corrosion resistance of the quaternary alloy was inferior to that of Ti-6Al-4V and CP Ti.

• Korean Journal of Metals and Materials
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• v.50 no.1
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• pp.86-91
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• 2012

Ti-6Al-4V extra low interstitial (ELI) alloy has been widely used as an orthopedic implant material because of its excellent biocompatibility, corrosion resistance and mechanical properties. However, V-free titanium alloys such as Ti-6%Al-7%Nb and Ti-5%Al-2.5%Fe have recently been developed because of the toxicity of V. Hydroxyapatite (HA) is used as a coating material on Ti or Ti biomaterials due to its good biocompatibility. However, HA coated on Ti alloy causes a problem for tissue by peeling off during usage. Therefore, such peeling off during long time usage can be suppressed by adding HA in Ti or Ti alloy composites. The aim of this study was to manufacture an ultra fine grained (UFG) Ti-Nb-HA bulk alloy, which is usually difficult to fabricate using melting and casting technology, by rapid sintering process using high energy mechanical milled (HEMM) powder.

• The Journal of Korean Academy of Prosthodontics
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• v.49 no.1
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• pp.16-21
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• 2011

Purpose: The purpose of this study was to investigate the bioactivity of precalcified nanotubular $TiO_2$ layer on Ti-6Al-7Nb alloy. Materials and methods: Anodic oxidation was carried out at a potential of 20 V and current density of 20 mA/$cm^2$ for 1 hour. The glycerol solution containing 1 wt% $NH_4F$ and 20 wt% deionized water was used as an electrolyte. Precalcification treatment was obtained by soaking in $Na_2HPO_4$ solution at $80^{\circ}C$ for 30 minutes followed by soaking in saturated $Ca(OH)_2$ solution at $100^{\circ}C$ for 30 minutes, followed by heat treatment at $500^{\circ}C$ for 2 hours. To evaluate the activity of precalcified nanotubular $TiO_2$ layer, specimens were immersed in a simulated body fluid with pH 7.4 at $36.5^{\circ}C$ for 10 days. Results: 1. Nanotubular $TiO_2$ layer showed the highly ordered dense structure by interposing small diameter nanotubes between large ones, the shape of nanotubes was enlarged as going down. 2. The mean length of nanotubes was $517.0{\pm}23.2\;nm$ innm glycerol solution containing 1 wt% $NH_4F$ and 20 wt% $H_2O$ at 20 V for 1 hour. 3. The bioactivity of Ti-6Al-7Nb alloy was improved with formation of nanotubular $TiO_2$ layer and precalcification treatment in $80^{\circ}C$ 0.5 M $Na_2HPO_4$ and saturated $100^{\circ}C$ $Ca(OH)_2$ solution. Conclusion: Bioactivity of precalcified nanotubular $TiO_2$ layer on Ti-6Al-7Nb alloy was improved.

• 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.

• Korean Journal of Materials Research
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• v.15 no.5
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• pp.353-360
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• 2005

Surface treatment play an important role in nucleating calcium phosphate deposition on surgical Ti implant. Therefore, the purpose of this study is to examine whether the precipitation of apatite on cp-Ti and Ti alloys are affected by surface modification in HCl and $H_2O_2$ solution. Specimens were then chemically treated with a solution containing 0.1 M HCl and 8.8M $H_2O_2$ at $80^{\circ}C$ for 30 mins, and subsequently heat-treated at $400^{\circ}C$ for 1 hour. All specimens were immersed in the HBSS with pH 7.4 at $36.5^{\circ}C$ for 15 days, and the surface was examined with XRD, SEM, EDX ana XPS. Also, pure Ti, Ti-6Al-4V and Ti-6Al-7Nb alloy specimens with and without surface treatment were implanted in the abdominal connective tissue of mice for 4 weeks. All specimens chemically treated with HCl and $H_2O_2$ solution have the ability to form a apatite layer in the HBSS which has inorganic ion composition similar to human blood plasma. The average thickness of the fibrous capsule surrounding the specimens implanted in the connective tissue was $38.57\;{\mu}m,\;62.27\;{\mu}m\;and\;45.64\;{\mu}m$ in the cp-Ti, Ti-6Al-4V ana Ti-6Al-7Nb alloy specimens with the chemical treatment respectively, and $52.20\;{\mu}m,\;75.62\;{\mu}m\;and\;66.56\;{\mu}m$ in the commercial specimens of cp-Ti, Ti-6Al-4V and Ti-6Al-7Nb without any treatment respectively. The results of this evaluation indicate that the chemically treated cp-Ti, Ti-6Al-4V ana Ti-6Al-7Nb alloys have better bioactivity and biocompatibility compared to the other metals tested.

• Korean Journal of Materials Research
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• v.22 no.3
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• pp.150-154
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• 2012

Ti-6Al-4V ELI (Extra Low Interstitial) alloy have been widely used as alternative to bone due to its excellent biocompatibility, although it still has many problems such as high elastic modulus and toxicity. Therefore, biomaterials with low elastic modulus and non toxic characteristics have to be developed. A novel ${\beta}$ Ti-35wt%Nb-7wt%Zr-Calcium pyrophosphate (CPP) composite that is a biocompatible alloy without elemental Al or V was fabricated by spark plasma sintering (SPS) at $1000^{\circ}C$ under 70 MPa using high energy mechanical milled (HEMM) powder. The microstructure and phases of the milled powders and the sintered specimens were studied using SEM, TEM, and XRD. Ti-35wt%Nb-7wt%Zr alloy was transformed from ${\alpha}$ phase to ${\beta}$ phase in the 4h-milled powder by sintering. The sintered specimen using the 4h-milled powder showed that all the elements were distributed very homogeneously and had higher density and hardness. ${\beta}$ Ti alloy-CPP composite, which has nanometer particles, was fabricated by SPS using HEMMed powder. During the sintering process, $CaTiO_3$, TixOy, and CaO were formed because of the reaction between Ti and CPP. The Vickers hardness of the composites increases with the increase of the milling time and the addition of CPP. The biocompatibility of the Ti-Nb-Zr alloys was improved by addition of CPP.

• Journal of Periodontal and Implant Science
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• v.36 no.4
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• pp.849-861
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• 2006

타이타늄은 기계적 특성이 우수하고 생체적합성이 뛰어나 의료용 장비의 주 재료로 사용되고 있으며 타이타늄 보다 기계적 특성이 더 우수한 타이타늄 합금들(주로 Ti-6Al-4V와 Ti-6Al-7Nb 합금)도 개발되어 치과와 의료용 임플란트로 사용되고 있다. 그러나 타이타늄 합금 성분들 중 알루미늄 (aluminum)과 바나디움(vanadium)은 인체에 노출되면 세포손상과 신경계에 문제를 일으킬 수 있다. 따라서 인체에 독성이 없으면서 기계적 성질과 생체적합성이 우수한 타이타늄 합금의 개발이 필요하다. 최근 인체에 독성이 없는 성분들이 함유된 새로운 ${\beta}$ - 형태의 타이타늄 합금들이 개발되고 있는데, ${\beta}$ - 타이타늄 합금은 그 기계적 성질이 기존의 ${\alpha}+{\beta}$ 타이타늄 합금에 비해 우수하다고 알려져 있다. 최근 새로운 ${\beta}$ - 타이타늄 합금이 전남대학교 부설 타이타늄 연구소에서 개발되었다. 이 연구는 새로 개발된 ${\beta}$ - 타이타늄 합금의 생채 적합성을 세포 증식도, 알카리 인산 분해 효소 활성과 유전자 증폭을 통해 알아보고자 하였다. 그 결과는 다음과 같다; 1. Titanium-6aluminum-4vanadium (Ti-6Al-4V) 합금 표면애서의 세포 증식율은 Titanium-Titanium8Tantalum-3Niobium (Ti-8Ta-3Nb) 합금과 순수 타이타늄 표면에 비해 유의하게 낮았다(p<0.00l). Ti-8Ta-3Nb 합금 표면에서의 증식도는 순수 타이타늄 표면과 유사하였다. 2. Ti-8Ta-3Nb 합금과 순수 타이타늄에서 배양된 세포이 알카리 인산 분해 효소의 활성도는 Ti-6Al-4V 합금에서의 것보다 유의하게 높았다 (p<0.001). 3. 유전자 증폭 분석 결과, Ti-8Ta-3Nb 합금과 순수 타이타늄에서 collagen type I과 bone sialoprotein mRNA 가 유사한 수준으로 발현되었다. 이상의 결과는 생체 적합성 측면에서 Ti-8Ta-3Nb 합금과 순수 타이타늄의 차이가 없음을 보여주며 따라서 Ti-8Ta-3Nb 합금이 의학 및 치의학 영역에서 새로운 임프란트 재료로 사용될 수 있음을 의미한다.

• Korean Journal of Materials Research
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• v.21 no.7
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• pp.384-390
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• 2011

Ti-6Al-4V ELI (Extra Low Interstitial) alloy has been widely used as an alternative to bone due to its excellent biocompatibility. However, it still has many problems, including a high elastic modulus and toxicity. Therefore, nontoxic biomaterials with a low elastic modulus should be developed. However, the fabrication of a uniform coating is challenging. Moreover, the coating layer on Ti and Ti alloy substrates can be peeled off after implantation. To overcome these problems, it is necessary to produce bulk Ti and Ti alloy with hydroxyapatite (HA) composites. In this study, Ti, Nb, and Zr powders, which are biocompatible elements, were milled in a mixing machine (24h) and by planetary mechanical ball milling (1h, 4h, and 6h), respectively. Ti-35%Nb-7%Zr and Ti-35%Nb-7%Zr-10%HA composites were fabricated by spark plasma sintering (SPS) at $1000^{\circ}C$ under 70MPa using mixed and milled powders. The effects of HA addition and milling time on the biocompatibility and physical and mechanical properties of the Ti-35%Nb-7%Zr-(10%HA) alloys have been investigated. $Ti_2O$, CaO, $CaTiO_3$, and $Ti_xP_y$ phases were formed by chemical reaction during sintering. Vickers hardness of the sintered composites increases with increased milling time and by the addition of HA. The biocompatibilty of the HA added Ti-Nb-Zr alloys was improved, but the sintering ability was decreased.