Papers by Author: Michiharu Ogawa

Abstract: If Mn could be partly substituted by Fe, Ti-Mn-Fe alloys would be less costly than Ti-Mn alloys. Furthermore, the use of iron as a beta-stabilizing element is more suitable than the use of manganese from a situation of an element strategy. In this study, 4.26 was admitted as the average ratio of valence electrons to atoms, e/a. The compositions of Mn and Fe were chosen under 4.26 as e/a. We investigated the influence Fe in selected Ti-Mn-Fe alloys by performing electrical resistivity, Vickers hardness, and X-ray diffraction measurements. In solution-treated and water-quenched 10Mn alloy, the beta and athermal omega phases were identified, while only the beta phase was identified in 8.7Mn-1Fe, 6.1Mn-3Fe, and 3.5Mn-5Fe alloys. In all alloys, equiaxial beta grains were observed by optical microscope. The resistivities at room and liquid-nitrogen temperatures and the Vickers hardness were relatively invariant across all Ti-Mn-Fe alloys, except for the Vickers hardness of the 5Fe alloy. During aging at 773 K, an isothermal omega phase precipitated in only the 3.5Mn-5Fe alloy, whereas only the alpha phase precipitated in the others.

Abstract: Hydroxyapatite (HAp), Ca10(PO4)6(OH)2, is known to precipitate on bioactive materials by soaking in simulated body fluid (SBF). The formation of HAp on TiO2 and CaTiO3 surfaces under continuous ultraviolet (UV) irradiation was investigated in this study. Pure Ti substrates were chemically treated with H2O2/ HNO3 solution at 353 K for 20 min to form a TiO2 gel layer. The samples were then hydrothermally treated with an aqueous NH3 or an aqueous Ca(OH)2 solution in an autoclave at 453 K for 12 h. An adhesive and sufficiently crystallized anatase-type TiO2 film or perovskite-type CaTiO3 film could be synthesized on the Ti surface, respectively. The samples were immersed in SBF in darkness or under UV irradiation. The UV irradiation promoted the formation of HAp, which may be due to the generation of functional Ti-OH or Ti-O groups on both surfaces. On the other hand, the UV light also produces electron-hole pairs in the product films. In TiO2, much photogenerated holes migrated to the surface and repelled the Ca2+ ions in the solution. As a consequence, the UV irradiation suppressed the formation of HAp thin film on the surface of TiO2.

Abstract: The combined chemical-hydrothermal synthesis of TiO2 and CaTiO3 films on pure Ti substrates was examined with a focus on film crystallinity and surface morphology. Pure Ti disks were chemically treated with H2O2/ HNO3 aqueous solutions at 353 K for 20 min in order to form a TiO2 gel layer on the surfaces. The samples were then hydrothermally treated in an autoclave at 453 K for 12 h or 24 h. Anatase-type TiO2 and perovskite-type CaTiO3 films with high crystallinity were obtained upon treatment with distilled water or aqueous NH3 and aqueous Ca(OH)2, respectively. Uniform, crack-free films were obtained. The surfaces showed excellent attachment of osteoblast-like MC3T3E1 cells in an incipient stage. Furthermore, the cells showed satisfactory proliferation, though at a slightly lower rate than on Ti. In addition, the samples were immersed in SBF (Simulated Body Fluid), adjusted to 310 K. A light hydroxyapatite (HAp) precipitate was observed on the unmodified Ti surface after 6 days of immersion. In contrast, precipitation was observed only after 2 to 4 days on the present oxide films. Thus, these oxide films are non-toxic and enhance the deposition of HAp.

Abstract: Although titanium is considered to be a ubiquitous element since it has the tenth highest Clarke number of all elements, it is classified as a rare metal because the current refinement process is more environmentally damaging than the processes used to refine iron and aluminum. Furthermore, the beta stabilizing elements of titanium alloys (e.g., V, Mo, Nb, and Ta) are very expensive due to their low crustal abundances. Manganese is also considered to be a ubiquitous element, since it has the 12th highest Clarke number of all elements. Therefore, manganese is a promising alloying element for titanium, especially as a beta-stabilizer. In order to develop beta titanium alloys as ubiquitous metallic materials, it is very important to investigate the properties of Ti-Mn alloys. In this study, the phase constitution of and the effect of heat treatment on Ti-3.3 to 8.7 mass% Mn alloys were investigated by electrical resistivity and Vickers hardness (HV) measurements and by X-ray diffraction (XRD) analysis and optical microscopy. In 3.3, 5.1, and 6.0 mass% Mn alloys quenched from 1173 K, ’ martensite and  phase were identified by XRD, whereas in the 8.7 mass% alloy, only the  phase was detected. The resistivities at both temperatures increased with increasing Mn content up to 6.0 mass% Mn and the positive temperature dependence of resistivity became negative at 6.0 mass% Mn. LN increased gradually with increasing Mn content up to 8.7 mass% Mn, whereasRT decreased considerably at a Mn content of 8.7 mass% Mn. HV increased with increasing Mn content up to 5.1 mass%, after which it began to decrease. In Ti-3.3 mass%Mn and 5.1 mass%Mn alloys, the resistivity and the resistivity ratio decreased with increasing temperature of isochronal heat treatment because of decomposition of ’ martensite. In 6.0Mn and 8.7Mn alloys, the resistivity and the resistivity ratio decreased, while Vickers hardness increased with increasing temperature of isochronal heat treatment because of isothermal  precipitation. Furthermore, the temperature for the onset of precipitation increased with higher Mn content.

Abstract: The effect of Al addition on the elastic modulus and aging behavior in Ti-10 Cr alloys was investigated by means of electrical resistivity, X-ray diffractometry and Vickers hardness measurements. All of the alloys used were formed from solutions treated at 1173 K for 3.6 ks and then quenched into ice water (STQ). Following STQ, all Al-containing specimens exhibited a  phase, with the athermal  appearing only for alloys with zero Al addition. The elastic modulus was found to decrease with addition of Al from approximately 80 to 70 GPa, due to the suppression of the athermal . The specimens following STQ were isothermally aged at 573 K, 673 K and 773 K. The addition of Al was found to retard the onset of precipitation of the isothermal  phase and decrease the upper limit temperature for precipitation of this phase. On the other hand, as the Al content was increased, precipitation of the  phase was accelerated in the presence of an existing isothermal  phase. By contrast, this precipitation was suppressed under single  phase conditions. Surface modification for osteointegration was also performed. When the modified specimens were immersed in simulated body fluid, the surface modification was found to promote the deposition of HAp.

Abstract: The surface of Ti-29Nb-13Ta-4.6Zr (TNTZ) subjected to gas nitriding at 1023–1223 K was investigated in comparison with the conventional biomedical titanium alloy, Ti-6Al-4V ELI (Ti64). After gas nitriding, the microstructures near the surface of these alloys were observed by optical microscopy, X-ray diffraction, Auger electron spectroscopy, and X-ray photoelectron spectroscopy. In both alloys, two titanium nitrides (TiN and Ti2N) are formed and the α phase precipitated by gas nitriding. Furthermore, oxygen impurity in the gas nitriding atmosphere reacts with the titanium nitrides; thus, TiO2 is formed at the outermost titanium nitride layer. The surface hardening was also evaluated by Vickers hardness measurement. The Vickers hardness near the surface of TNTZ and Ti64 increases significantly by gas nitriding.

Abstract: The tensile and plain fatigue properties of the β-type titanium alloy, Ti-29Nb-13Ta-4.6Zr alloy (TNTZ), which was subjected to various thermomechanical treatments, and cast TNTZ were investigated in order to judge its potential for biomedical and dental applications. The tensile strengths of TNTZ aged after solution treatment and that aged after cold rolling decrease with an increase in the aging temperature; however, their elongation exhibits an opposite trend. TNTZ composed of the ω phase or the ω and α phases in the β phase exhibits a tensile strength of about 1000 MPa or more. The tensile properties of the cast TNTZ with and without a surface reaction layer is are not significantly different, and are almost identcal to those of as-solutionized TNTZ. The plain fatigue strengths of TNTZ aged after solution treatment and those of TNTZ aged after cold rolling increase with the aging temperature. In particular, TNTZ aged at 723 K after cold rolling exhibits the highest fatigue strength in both the low- and high-cycle fatigue life regions. Further, the plain fatigue limit, which is about 770 MPa, is nearly equal to that of hot-rolled Ti-6Al-4V ELI alloy subjected to aging after solution treatment; Ti-6Al-4V ELI alloy is a representative α+β-type titanium alloy for biomedical applications. The plain fatigue strength of cast TNTZ with a surface reaction layer is considerably less than that of the as-cold-rolled and as-solutionized TNTZ. Consequently, in the low-fatigue life region, the fatigue crack easily occurs at the surface reaction layer, which is brittle, and in the high-fatigue life region, the fatigue crack occurs at the sites of casting defects (shrinkage). The fatigue limits range from 180 MPa to 200 MPa.

Abstract: The effect of oxygen content on aging behavior and invar characteristics of Ti-29Nb-13Ta-4.6Zr (TNTZ) were investigated. The age hardening of TNTZ aged at 573 K and 723 K is enhanced with the oxygen content. The ω phase precipitates and grows from early stage of aging in TNTZ regardless of the oxygen content when aged at 573 K. The lath-like shape α phase precipitated in TNTZ aged at 723 K increases in size with the oxygen content. The elastic modulus increases with the oxygen content and aging. The ω phase increase the elastic modulus to a greater extent than the increase due to the α phase. The tensile strength increases with the oxygen content and aging, while the elongation decreases. TNTZ with oxygen content of 0.1 mass% exhibits invar-like characteristics through severe cold working. A higher oxygen content suppresses the invar-like characteristics of TNTZ.

Abstract: Phase constitution in the solution-treated and quenched state and the heat treatment behavior were investigated by electrical resistivity, hardness, and elastic modulus measurements, X-ray diffraction, and optical microscopy. Hexagonal martensite and the β phase were identified in the Zr-5mass%Nb alloy. β and ω phases were identified in the Zr-10 and 15mass%Nb alloys, and only the β phase was identified in the Ti-20Nb alloy. Resistivity at RT, Vickers hardness and elastic modulus increased up to 10Nb and then decreased dramatically at 15Nb. Above 15Nb, these values slightly decreased. The elastic moduli for 15Nb and 20Nb were 59.5 and 55.5 GPa, respectively. On isochronal heat treatment, the isothermal ω phase precipitated between 473 and 623 K and then the α phase precipitated in the 10Nb, 15Nb and 20Nb alloys.

Abstract: Plain and notch fatigue properties of a β-type titanium alloy, Ti-29Nb-13Ta-4.6Zr (TNTZ), which was subjected to various thermomechanical treatments, were investigated in order to judge its potential for biomedical applications. Microstructures of TNTZ aged at 723 K for 259.2 ks after cold rolling and those aged at 723 K for 259.2 ks after solution treatment are composed of a precipitated α phase in the β phase. However, microstructures of TNTZ aged at 598 and 673 K for 259.2 ks after cold rolling and aged at 598 K and 673 K for 259.2 ks after solution treatment are composed of a precipitated ω phase, and precipitated α and ω phases in the β phase, respectively. Futher, plain fatigue strengths of TNTZ aged after solution treatment and those of TNTZ aged after cold rolling increase with the aging temperature. In particular, TNTZ aged at 723 K after cold rolling exhibits the highest fatigue strength in both the low- and high-cycle fatigue life regions. Futher, the run-out, which is about 770 MPa, is nearly equal to that of hot-rolled Ti-6Al-4V ELI conducted with aging, which is one of the representative α+β-type titanium alloys for biomedical applications. The notch fatigue strengths of TNTZ aged at stress concentration factors of 2 and 6 decrease by 30% – 40% and 50% – 60%, respectively, as compared with the plain fatigue strengths in the low-cycle fatigue life region. Futher, the notch run-out range from 450 to 490 MPa and from 220 to 300 MPa, respecitvely; an exception to this is TNTZ aged at 598 K after cold rolling, which has a high volume fraction of the ω phase. Single- and multi- fatigue cracks initiate at the bottom of the notch at stress concentration factors of 2 and 6, respectively.