Ti-Ta-Nb계 합금의 세포독성과 생체적합성의 평가

최득철,방몽숙,윤택림,Cui De-Zhe,Vang Mong-Sook,Yoon Taek-Rin 대한치과보철학회 2006 대한치과보철학회지 Vol.44 No.2

Statement of problem: Ti-alloy has been used widely since it was produced in the United States in 1947 because it has high biocompatibility and anticorrosive characteristics. Purpose: The pure titanium, however, was used limitedly due to insufficient mechanical charateristics and difficult manufacturing process. Our previous study was focused on the development of a new titanium alloy. In the previous study we found that the Ti-Ta-Nb alloy had better mechanical characteristics and similar anticorrosive characteristics to Ti-6Al-4V Material and methods: In this study, the cytotoxicity of the Ti-Ta-Nb alloy was evaluated by MTT assay using MSCs(Mesenchaimal stem cells) and L929 cells(fibroblast cell line). The biocompatibility of the Ti-Ta-Nb alloy was performed by inserting the alloy into the femur of the rabbits and observing the radiological and histological changes surrounding the alloy implant. Results: 1. In the cytotoxicity test using MSCs, the 60% survival rate was observed in pure titanium, 84% in Ti-6Al-4V alloy and 95% in Ti-10Ta-10Nb alloy. 2. In the animal study, the serial follow-up of the radiographs showed no separation or migration revealing gradual bone ingrowth surrounding the implants. Similar radiographic results were obtained among three implant groups pure titanium, Ti-6Al-4V alloy and Ti-10Ta-10Nb alloy. 3. In the histologic examination of the bone block containing the implants. the bone ingrowth was prominent around the implants with the lapse of time. There was no signs of any tissue rejection, degeneration, or inflammation. Active bone ingrowth was observed around the implants. In the comparison of the three groups, the rate of bone ingrowth was better in the Ti-10Ta-10Nb alloy group than those in pure titanium group or Ti-6Al-4V alloy group. In conclusion, Ti-10Ta-10Nb alloy revealed better biocompatibility in survival rate of the cells and bone ingrowth around the implants. Therefore we believe a newly developed Ti-10Ta-10Nb alloy can replace currently used Ti-6Al-4V alloy to increase biocompatibility and to decrease side effects. Conclusion: In conclusion, Ti-10Ta-10Nb alloy revealed better biocompatibility in survival rate of the cells and bone ingrowth around the implants. Therefore we believe a newly developed Ti-10Ta-10Nb alloy can replace currently used Ti-6Al-4V alloy to increase biocompatibility and to decrease side effects.

Ti-Cr-Mo계 및 Ti-Cr-V계 bcc 합금의 수소저장특성에 관한 연구

유정현,조성욱,박충년,최전 한국수소및신에너지학회 2005 한국수소 및 신에너지학회논문집 Vol.16 No.2

The characteristics of hydrogen storage have been investigated in the Ti-Cr-Mo and Ti-Cr-V ternary alloys with bcc structure. The alloys were melted by arc furnace and remelted 4-5 times for homogeneity. The lattice parameters, microstructures and phases of the alloys were examined by SEM, EDX and XRD, and the Pressure-Composition isotherms of the alloys were measured. From these data the relationship of the maximum and effective hydrogen storage capacities vs. chemical composition, lattice parameter and the radius of tetrahedral site were analyzed and discussed.The results showed that all of these alloy, in the range of the this study, had mainly bcc solid solutions with small amount of Ti segregation due to a lower melting point of Ti compared with other elements. Lattice parameters of the alloys were very near to the atomic average values of lattice parameters of the constituent elements. It was also found that maximum hydrogen storage capacities of the Ti-Cr-Mo alloys increased with increasing Ti content and the radius of tetrahedral site but the effective hydrogen storage capacities decreased after showing the maximum. The hydrogen storage capacities of the Ti-Cr-V alloys were almost same even though the V contens were quite different from alloy to alloy and this could be attributed to the almost same Ti/Cr ratio of the alloys. The maximum effective hydrogen storage capacity of the Ti-Cr-Mo alloys was revealed at Ti content of about 40∼50 at% and radius of tetrahedral site of 0.43∼0.45 nm. The Ti-Cr-V alloys showed the hydrogen storage capacities of 3.0 wt% and effective hydrogen storage capacities of 1.5 wt%.

Mn-coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetron sputtering for dental applications

Park, Seon-Yeong,Choe, Han-Cheol Elsevier 2018 APPLIED SURFACE SCIENCE - Vol.432 No.2

<P><B>Abstract</B></P> <P>In this study, Mn-coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetrons sputtering for dental applications were studied using different experimental techniques. Mn coating films were formed on Ti-29Nb-xHf alloys by a radio frequency magnetron sputtering technique for 0, 1, 3, and 5min at 45W. The microstructure, composition, and phase structure of the coated alloys were examined by optical microscopy, field emission scanning electron microscopy, X-ray diffraction, and energy-dispersive X-ray spectroscopy. The microstructure of Ti-29Nb alloy showed α' phase in the needle-like structure and Ti-29Nb-15Hf alloy showed β phase in the equiaxed structure. As the sputtering time increased, the circular particles of Mn coatings on the Ti-29Nb alloy increased at inside and outside surfaces. As the sputtering time increased, [Mn+Ca/P] ratio of the plasma electrolytic oxidized films in Ti- 29Nb-xHf alloys increased. The corrosion potential (E<SUB>corr</SUB>) of Mn coatings on the Ti-29Nb alloy showed higher than that of Mn coatings on the Ti-29Nb-15Hf alloy. The passive current density (I<SUB>pass</SUB>) of the Mn coating on the Ti-29Nb alloy and Mn coatings on the Ti-29Nb-15Hf alloy was less noble than the non-Mn coated Ti-29Nb and Ti-29Nb-15Hf alloys surface.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Mn-coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetrons sputtering were studied. </LI> <LI> As the sputtering time increased, the circular particles of Mn on the Ti alloy increased at inside and outside surfaces. </LI> <LI> As the sputtering time increased, [Mn+Ca/P] ratio of the PEO films in Ti- 29Nb-xHf alloys increased. </LI> <LI> E<SUB>corr</SUB> of Mn coatings on the Ti-29Nb alloy showed higher than that of Mn coatings on the Ti-29Nb-15Hf alloy. </LI> <LI> Mn coatings on the Ti-29Nb-15Hf alloy were less noble than the non-coated Ti alloys. </LI> </UL> </P>

치과 임플란트용 순 Ti의 접촉부식 거동

김교한,허만수,김형일,황운석,高田 雄京,奧野 攻 대한치과기재학회 1999 대한치과재료학회지 Vol.26 No.4

One of the fields in which titanium(Ti) is becoming increasingly valuable is the field of biomaterials. Ti had shown its good corrosion resistance, high strength to weight ratio, and compatibility with human tissues. Such applications of Ti in this area involve replacing stainless steel and cobalt-chromium alloy implant which are used in skull, shoulder joint, spine, and dental implant. In dental field, titanium has been used as dental implant, so it becomes necessary to examine and estimate the anti-corrosion ability of Ti and its alloys at the severe conditions such as crevice corrosion and galvanic corrosion. The purposes of this study was to examine the corrosion mechanisms of the pure Ti showing good corrosion resistance under an oral corrosion environment when it is coupled with dental casting Type Ⅱ and Type Ⅳ gold alloys. These coupling corrosion mechanisms were studied in three conditions. First was by measuring the resting potential of pure Ti, when it was uncoupled and coupled with Type Ⅱ and Type Ⅳ alloys. Second was by measuring anode polarization behavior of pure Ti, Type Ⅱ and Type Ⅳ alloys, and third was by detecting dissolved ions from the pure Ti, uncoupled and coupled with Type Ⅱ and Type Ⅳ gold alloys which were immersed in 0.9% NaCl solution for 7 days. The resting potential showed a low potential value at the initial stage but increasing into a high value (to 0.18 V) with time elapse and reached a stable value. On the contrary, the potentials of Type Ⅱ and Type Ⅳ gold alloys were in their values at the initial stage of immersion, then decreased with the time and reached stable values, being higher than the value of pure Ti. When pure Ti coupled with Type Ⅱ and Type Ⅳ gold alloys, the resting potential of coupled one was between the values of each one. When Type Ⅱ and Type Ⅳ gold alloys were coupled with pure Ti, there was an increase in Ag, Cu, and Zn. Also, Zn ions released the high potential precious metal alloys, compared to the uncoupled case. Ti ion was not detected at any cases of pure Ti or coupled with gold alloys. It was thought that one of the causes of the increase in Ag, Zn, and Cu ions when Ti was coupled with dental gold alloys was that Ag, Zn, and Cu ions were selectively dissoluted from the Ag rich regions around grain boundary and the casting defects. In conclusions, the results of this study suggest that the pure Ti was very stable when coupled with the gold alloys in oral cavity.

표면처리방법에 따른 강화된 치과용 임플란트의 개발 : Ⅰ.전자빔 진공증착법에 의한 치과용 임플란트의 내구성 개선 Ⅰ.Improvement of Endurance for Dental Implants by EB-PVD Coating Method

최한철,고영무 大韓齒科器材學會 2000 대한치과재료학회지 Vol.27 No.3

Ti-6Al-4V alloy has an excellent fatigue strength but it has a low corrosion resistance compared with pure titanium. To develop the alloys for the dental implant with better corrosion resistance, Ti, TiN and Ti/TiN were coated on Ti-6Al-4V alloy by electron-beam physical vapor deposition(EB-PVD) method. Ti-6Al-4V alloys were made under the condition of hydrogen and vacuum arc furnace and were quenched at 1,000℃ under high purity dried Ar gas atmosphere and were hold at 500℃ for 2hrs to achieve the fatigue strength(1140㎫) of alloys. Corrosion tests of three coated alloys were used to investigate the electrochemical corrosion behavior in 0.9% NaCl solution. The corrosion potential(+200㎷) of Ti-6Al-4V alloys coated with Ti/TiN is higher and lower active and passive current densities than that of alloys coated with Ti(-300㎷), TiN(-100㎷) and uncoated ones(-400㎷). Also uncoated alloys showed the decreasing of the pitting and repassivation potential in comparison with Ti, TiN and Ti/TiN coated alloys. The amount of Ti released was decreased in the order of Ti/TiN, TiN and Ti coated alloys. We conclude that coating Ti/TiN on Ti-6Al-4V is the most effective to improve of corrosion resistance of Ti-6Al-4V alloys with lower corrosion resistance to some extent by using Ti/TiN multilayer EB-PVD coating method.

Electrochemical Behaviors of a TiN-Coated/Nanotube-formed Ti-Zr Alloy

김원기,고영무,Han-Cheol Choe 한국물리학회 2009 THE JOURNAL OF THE KOREAN PHYSICAL SOCIETY Vol.54 No.3

Ti-Zr (10, 20, 30 and 40 wt%) alloys were prepared by arc melting, followed by homogenization for 24 hr at 1000℃ in an argon atmosphere. The formation of oxide nanotubes was achieved by anodizing a Ti-Zr alloy in H3PO4 electrolytes containing small amounts of fluoride ions at room temperature. Electrochemical experiments were carried out using a conventional three-electrode configuration with a platinum counter electrode and a saturated calomel reference electrode. The anodization treatments were carried out using a scanning potentiostat (EG&G Co., Model 362, USA). All the experiments were conducted at room temperature. The microstructures of the al- loys were examined by using optical microscopy (OM), field-emission scanning electron microscopy (FE-SEM) and X-ray diffractometry (XRD). A TiN coating was deposited on the anodized titanium- oxide layer by reactive RF magnetron sputtering using a Ti target (99.99 %). The corrosion prop- erties of the specimens were examined using potentiodynamic tests (potential range of -1500~2000 mV) in a 0.9 % NaCl solution by using potentiostat (EG&G Co, PARSTAT 2273. USA). The microstructural changes from the β phase to the α phase and the percentage of α phase increased with increasing Zr content. The composition of the alloys was found to have a significant influence on the two-size-scale structure. Moreover, a two-size-scale structure appeared as the Zr content was increased and small-sized nanotubes nucleated at the un-nucleated pore spacing areas. The anodic polarization behavior of the Ti-xZr alloys showed increasing corrosion resistance of the nanotube- formed alloy with increasing Zr content. In addition, the corrosion resistance of the TiN coating on the anodized Ti-xZr alloys was higher than that of the untreated Ti alloy, indicating a better protective effect. On the other hand, in the case of the nanotube-formed alloy, the polarization curves of the TiN-coated alloys were shifted to the right side at a high current density. Ti-Zr (10, 20, 30 and 40 wt%) alloys were prepared by arc melting, followed by homogenization for 24 hr at 1000℃ in an argon atmosphere. The formation of oxide nanotubes was achieved by anodizing a Ti-Zr alloy in H3PO4 electrolytes containing small amounts of fluoride ions at room temperature. Electrochemical experiments were carried out using a conventional three-electrode configuration with a platinum counter electrode and a saturated calomel reference electrode. The anodization treatments were carried out using a scanning potentiostat (EG&G Co., Model 362, USA). All the experiments were conducted at room temperature. The microstructures of the al- loys were examined by using optical microscopy (OM), field-emission scanning electron microscopy (FE-SEM) and X-ray diffractometry (XRD). A TiN coating was deposited on the anodized titanium- oxide layer by reactive RF magnetron sputtering using a Ti target (99.99 %). The corrosion prop- erties of the specimens were examined using potentiodynamic tests (potential range of -1500~2000 mV) in a 0.9 % NaCl solution by using potentiostat (EG&G Co, PARSTAT 2273. USA). The microstructural changes from the β phase to the α phase and the percentage of α phase increased with increasing Zr content. The composition of the alloys was found to have a significant influence on the two-size-scale structure. Moreover, a two-size-scale structure appeared as the Zr content was increased and small-sized nanotubes nucleated at the un-nucleated pore spacing areas. The anodic polarization behavior of the Ti-xZr alloys showed increasing corrosion resistance of the nanotube- formed alloy with increasing Zr content. In addition, the corrosion resistance of the TiN coating on the anodized Ti-xZr alloys was higher than that of the untreated Ti alloy, indicating a better protective effect. On the other hand, in the case of the nanotube-formed alloy, the polarization curves of the TiN-coated alloys were shifted to the right side at a high current density.

치과용 Ti-Xwt%Cu 합금의 연삭성

안재석,Ahn, Jae-Seok 대한치과기공학회 2009 대한치과기공학회지 Vol.31 No.4

This study evaluated the grindability of series of Ti-Cu alloys in order to develop a Ti alloy with better grindability than commercially pure titanium(CP Ti). Experimental Ti-Xwt%Cu alloys(X=2, 5, 10) were made in an argon-arc melting furnace. Slabs of experimental alloys were ground using a SiC abrasive wheel on an electric handpiece at circumferential speed(15000, 30000rpm) by applying a force(250, 300gr). Grindability was evaluated by measuring the amount of metal volume removed after grinding for 2 minutes. Data were compared to those for CP Ti and Ti-6wt%Al-4wt%V alloy. From results, It was observed that the grindability of Ti-Cu alloys increased with an increase in the Cu concentration compared to CP Ti, particularly the 10wt%Cu alloy exhibited the highest grindability at all speeds. By alloying with Cu, the Ti exhibited better grindability at high speed. The continuous precipitation of $Ti_2Cu$ among the ${\alpha}$-matrix grains made this material less ductile and facilitated more effective grinding because small segments more readily formed. The Ti-10wt%Cu alloy has a great potential for use as a dental machining alloy.

Study of the compression and wear-resistance properties of freeze-cast Ti and Ti‒5W alloy foams for biomedical applications

Choi, Hyelim,Shil'ko, Serge,Gubicza, Jenő,Choe, Heeman Elsevier 2017 Journal of the mechanical behavior of biomedical m Vol.72 No.-

<P><B>Abstract</B></P> <P>Ti and Ti‒5wt% W alloy foams were produced by freeze-casting process and their mechanical behaviors were compared. The Ti‒5W alloy foam showed a typical acicular Widmanstätten α/β structure with most of the W dissolved in the β phase. An electron-probe microanalysis revealed that approximately 2wt% W was uniformly dissolved in the Ti matrix of Ti‒5W alloy foam with few partially dissolved W particles. The compressive-yield strength of Ti‒5W alloy foam (~323MPa) was approximately 20% higher than that of the Ti foam (~256MPa) owing to the solid-solution-strengthening effect of W in the Ti matrix, which also resulted in a dramatic improvement in the wear resistance of Ti‒5W alloy foam. The compressive behaviors of the Ti and Ti‒5W alloy foams were predicted by analytical models and compared with the experimental values. Compared with the Gibson-Ashby and cellular-lattice-structure-in-square-orientation models of porous materials, the orientation-averaging method provided prediction results that are much more accurate in terms of both the Young's modulus and the yield strength of the Ti and Ti‒5W alloy foams.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Manufacturing of Ti and Ti-W alloy foams by freeze-casting method. </LI> <LI> Compressive test of Ti and Ti-W alloy foams. </LI> <LI> Evaluation of wear resistance of Ti and Ti-W alloy foams. </LI> <LI> Analytical prediction of the Young's moduli and yield strengths of Ti and Ti-5W alloy foams. </LI> </UL> </P> <P><B>Graphical abstract</B></P> <P>[DISPLAY OMISSION]</P>

Characterization and colorization of microarc-oxidized layers of binary titanium alloys

Hwang, Moon-Jin,Choi, Hae-Rim,Song, Ho-Jun,Park, Yeong-Joon ELSEVIER SCIENCE 2018 JOURNAL OF ALLOYS AND COMPOUNDS Vol.732 No.-

<P><B>Abstract</B></P> <P>This study aimed to confer esthetic appearance on ash gray-colored titanium-based implant materials. Binary Ti alloys were prepared by arc-melting of titanium and one of the transition metals (Au, Cr, Cu, Mn, Mo, Nb, V, and Zr). Ti alloys containing 1, 2.5, 5 and 10 wt% alloying elements were microarc-oxidized in an electrolyte containing Ca and P ions under a constant current using a DC power supply. During the microarc oxidation (MAO) treatment, the potential <I>vs</I>. time curves were strongly affected by the alloying element type and content. The pore size, thickness, and crystallinity of the oxide layer increased as the final potential was increased. Colored oxide layers were obtained for the Ti alloys containing 3<I>d</I> (Cr, Cu, Mn, and V) and 5<I>d</I> (Au) transition metals. Their colors were dependent on the alloying metal type and content. In the L*a*b coordinate for color measurement adopted by the Commission Internationale d’Eclairage (CIE), the oxide layer of Ti-5Cr/MAO exhibited the highest average b* value of 19.81 (p < 0.05). The oxide layer of Ti-2.5Cu/MAO showed the next highest average b* value of 16.73. The oxidation state of 3<I>d</I> transition metals contributed to colorization of the microarc-oxidized Ti alloys. The characteristic colors of MAO-treated Ti alloys were rendered by the chemical binding state of alloying elements: yellow color for Cr<SUP>3+</SUP>, red color for Cu<SUP>+</SUP>, yellow color for Mn<SUP>4+</SUP> and yellow color for V<SUP>5+</SUP>. The purple color of the MAO-treated Ti-Au alloy surface originated from Au nanoparticles. The 4<I>d</I> transition metals (Zr, Nb, and Mo) did not affect color revelation of the MAO-treated Ti alloys.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Colored Ti alloys were prepared using MAO process in electrolyte with Ca and P ions. </LI> <LI> Color of the alloys varied depending upon the alloying element type and content. </LI> <LI> MAO-treated Ti-5Cr and Ti-2.5Cu exhibited a more yellowish color. </LI> <LI> MAO-treated Ti alloys with 3<I>d</I> metals could be used as esthetic implant materials. </LI> </UL> </P>

Hf가 첨가된 생체용 Ti-15Sn-4Nb 합금의 미세조직 및 내식성

이도재,이경구,조규종,윤택림,박효병,Lee, Doh-Jae,Lee, Kyung-Ku,Cho, Kyu-Zong,Yoon, Taek-Rim,Park, Hyo-Byung 대한치과기공학회 2001 대한치과기공학회지 Vol.23 No.1

This study is focusing on the improvement of problems of Ti-6Al-4V alloy. A new Ti based alloy, Ti-15Sn-4Nb, have designed to examine any possibility of improving the mechanical properties and biocompatibility. Specimens of Ti alloys were melted in vacuum arc furnace and homogenized at $100^{\circ}C$ for 24h. All specimens were solution treated at $812^{\circ}C$ and aged at $500^{\circ}C$ for 10h. The corrosion resistance of Ti alloys was evaluated by potentiodynamic polarization test and immersion test inl%Lactic acid solutions. Ti-15Sn-4Nb system alloys showed Widmanstatten microstructure after solution treatment which is typical microstructure of ${\alpha}+{\beta}$ type Ti alloys. Analysing the corrosion resistance of Ti alloys, it was concluded that the passive films of Ti-15Sn-4Nb system alloys are more stable than that of Ti-6Al-4V alloys. Also, the corrosion resistance of Ti-15Sn-4Nb system alloys was improved with adding elements, Hf. It was analysed that the passive film of the Ti-15Sn-4Nb alloy which was formed in air atmosphere was consisted of TiO2, SnO and NbO through X-ray photoelectron spectroscopy(XPS) analysis.