Papers by Author: Masahiko Ikeda

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: Microstructure formation of CP-Ti and TiB reinforced titanium were in-situ observed during the thermal cycle simulated for Tungsten Inert Gas (TIG) welding, by using laser scanning confocal microscopy. Under the in-situ observation of TiB reinforced titanium, heterogeneous nucleation of α-phase at inclusion was clearly detected and plate growth was shown in high timeresolution. Furthermore, it was observed that grain boundary of β -phase was pinned by the inclusions. Microstructure difference between pure and TiB reinforced titanium was explained based on those in-situ observations.

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: To develop new shape memory and super-elastic alloys for medical applications, titanium alloys using non-toxic metallic elements, such as Ta and Nb, are being actively investigated. In this study, aimed at developing new shape memory Ti alloys, we investigate the effect of oxygen, a powerful alpha stabilizing interstitial element, on the heat treatment behavior of Ti-50mass%Ta-5mass%Zr through electrical resistivity and Vickers hardness measurements and shape-recovery tests. Ti-50Ta-5Zr-0.14Ox and 0.33Ox alloys, and the β and α” bi-phase was confirmed by XRD. Only the β phase was identified in the Ti-50Ta-5Zr-0.62Ox alloy. Upon isochronal heat treatment, the resistivity at LN and resistivity ratio of Zr-0.33 and 0.62Ox alloys decreased up to around 523 K. In the 5Zr-0.62Ox alloy, orthorhombic martensite and the α” and β phases were identified in the specimens heat-treated at 473 and 523 K. The decreases in resistivity at liquid nitrogen temperature and resistivity ratio are due to the formation of α” during isochronal heat treatment. The formation of α” was confirmed by X-ray diffraction in the 5Zr-0.62Ox alloy. The shape memory effect was observed in 5Zr-0.14 and 0.33Ox alloys and the shape recovery ratio of both alloys was about 40% at 673 K.

Abstract: It has been reported that scandium addition improved various properties of aluminum alloys. However, present authors can not find any reports about the addition of Sc to 6000 series alloys. In this study, Sc was added to 6061 alloy and various effects of the Sc addition on aging behavior were examined, comparing with Al-Sc binary alloy. In the STQ state, resistivity at 77K, ρD77, of 0.2%Sc added alloy (6061+Sc) was about 2.0n-m higher than the alloy of no addition (6061). The ρD77 increased in initial stage of isothermal aging up to 473K, then decreased. Though ρD77 of binary Al-0.176%Sc alloy began to decrease from 1.8Ms at 448K and 18ks at 523K, excess decrease in ρD77 of 6061+Sc corresponding to precipitation of Sc compounds was not clear. Peak value of the HV0.1 was decreased and peak aging time delayed by the Sc addition in aging up to 498K. However, softening by overaging was retarded by the Sc addition. These effects of the Sc addition are considered to come from vacancy trap by solute Sc atoms or interface between particles of Sc compound and matrix acting as vacancy sinks.

Abstract: In an attempt to optimize the shape recovery temperature, the effect of Zr addition on phase constitution and heat treatment behavior is investigated by electrical resistivity and Vickers hardness (HV) measurements, X-ray diffractometry (XRD) and shape recovery tests. Ti-25mass%Nb-0, 2, 7 and 12mass%Zr alloys (abbreviated as 0Zr, 2Zr, 7Zr and 12Zr, respectively) were prepared using an arc-furnace. Specimens were solution-treated at 1273 K for 3.6 ks and then quenched by iced water (STQ). STQed specimens were isochronally heat-treated. In 0Zr and 2Zr, only the orthorhombic martensite phase a” was identified by XRD, while the two-phase alloys a” and b were identified in 7Zr and 12Zr. In 7Zr, resistivity at liquid nitrogen and room temperature (rLN and rRT, respectively) and resistivity ratio (rLN/rRT) drastically increased at 523 K because of the reverse-transformation of a” into b phase. Thereafter, resistivity and resistivity ratio decreased with increasing heat treatment temperature due to isothermal w precipitation. Starting temperature of shape recovery is 623 K in 7Zr and 523 K in 12Zr. In 7Zr, shape recovery ratio is about 80% at 723 K, which is the maximum obtained in this study.

Abstract: In order to improve poor formability in magnesium alloy, grain refinement has been attempted on AZ91E alloy by a thermo-mechanical treatment. Specimens were firstly cold-rolled at 10 %, then solution heat treated at 673 K for 86.4 ks, and hot-rolled at 573 K with about 5 % for four passes, or hot-rolled at 20 % with one pass. The rolled specimens were finally heat treated at 473 to 673 K for 3.6 to 36 ks. Microstructures in the starting material characterized by grain boundary precipitates and aluminum rich regions with about 180 µm in grain size were changed into fine grained microstructures with about 10 to 30 µm in diameter, in which precipitates of Mg17Al12 were uniformly distributed. Although the specimen was prepared by rolling, the (0001) texture was not so remarkable.

Abstract: Using Ti-40mass%Ta-0, -4, -8 and -12mass%Sn alloys, the effect of Sn addition on phase constitution in the solution treated and quenched state and isochronal heat treatment behavior is studied by electrical resistivity and Vickers hardness measurements and X-ray diffactometry. To confirm shape memory effect of some of these alloys, shape-recovery test was also performed. Orthorhombic martensite,
” was identified in Ti-40Sn-0 to 8Sn alloy quenched from 1173K, while  phase was identified in STQed Ti-40Ta-12Sn alloy. On isochronal heat treatment, increases of resistivity at LN and resistivity ratio were observed in only 8Sn alloy, because these increases are due to reverse-transformation of
” to  phase. From result of shape recovery test, shape memory effect was observed in Ti-40Ta-4 and 8Sn alloys