Impact of Microstructural and Surface Modifications on the Ti-45Nb Alloy’s Response to Bio-Environment

The Ti-45Nb (mass%) alloy’s corrosive and biocompatible response in simulated physiological conditions was investigated before and after its additional high-pressure torsion (HPT) and laser irradiation processing. The grain size reduction from 2.76 µm to ~ 200 nm and the appearance of laser-induced morphologically altered and highly oxidized surface led to the significant improvement of alloy corrosion resistance and cell–implant interaction. Moreover, an additional increase of the laser pulse energy from 5 to 15 mJ during the alloy irradiation in the air led to an increase in the surface oxygen content from 13.64 to 23.89% accompanied by an increase of excellent cell viability from 127.18 to 134.42%. As a result of the controlled alloy microstructural and surface modifications, the formation of protective bi-modal mixed Ti- and Nb-oxide external scale was enabled. The presence of this surface oxide scale enhanced the alloy’s resistance to corrosion deterioration and simultaneously boosted cell viability and proliferation.

Laser processing effects on Ti−45Nb alloy surface,corrosive and biocompatible properties

The Ti−45Nb(wt.%)alloy properties were investigated in relation to its potential biomedical use.Laser surface modification was utilized to improve its performance in biological systems.As a result of the laser treatment,(Ti,Nb)O scale was formed and various morphological features appeared on the alloy surface.The electrochemical behavior of Ti−45Nb alloy in simulated body conditions was evaluated and showed that the alloy was highly resistant to corrosion deterioration regardless of additional laser surface modification treatment.Nevertheless,the improved corrosion resistance after laser treatment was evident(the corrosion current density of the alloy before laser irradiation was 2.84×10^(−8)A/cm^(2),while that after laser treatment with 5 mJ was 0.65×10^(−8)A/cm^(2))and ascribed to the rapid formation of a complex and passivating bi-modal surface oxide layer.Alloy cytotoxicity and effects of the Ti−45Nb alloy laser surface modification on the MRC-5 cell viability,morphology,and proliferation were also investigated.The Ti−45Nb alloy showed no cytotoxic effect.Moreover,cells showed improved viability and adherence to the alloy surface after the laser irradiation treatment.The highest average cell viability of 115.37%was attained for the alloy laser-irradiated with 15 mJ.Results showed that the laser surface modification can be successfully utilized to significantly improve alloy performance in a biological environment.

Oxidation resistance of powder metallurgy Ti-45Al-10Nb alloy at high temperature

TiAl alloy with high Nb content,nominally Ti-45Al-10Nb,was prepared by powder metallurgy,and the oxidation resistance at 850,900,and 950℃was investigated.The high-temperature oxidation-resistance mechanism and oxidation dynamics were discussed following the oxide skin morphology and microstructural evolution analysis.The oxide skin structures were similar for 850 and 900℃,with TiO_(2)+Al_(2)O_(3)mixture covering TiO_(2)with dispersed Nb_(2)O_(5).At 950℃,the oxide skin was divided into four sublayers,from the outside to the parent metal:loose TiO_(2)+Al_(2)O_(3),dense Al_(2)O_(3),dense TiO_(2)+Nb_(2)O_(5),and TiO_(2)matrix with dispersed Nb_(2)O_(5).The Nb layer suppressed the outward diffusion of Ti atoms,hindering the growth of TiO_(2),and simultaneously promote the formation of a continuous Al_(2)O_(3)protective layer,providing the alloy with long-term high-temperature oxidation resistance.

DEFORMATION-INDUCED α2→γ TRANSFORMATION IN A HOT DEFORMED Ti-45A1-10Nb ALLOY

High-resolution transmission electron microscope (HRTEM) was employed to investigate the deformation-induced α2→γ phase transformation phenomenon in a hot deformed Ti-45Al-10Nb alloy. Such a tronsformation can be nucleated either at α2/γ interfaces or at stacking faults on the basal planes of the α2 phase. The growth of deformation-induced γplate is accomplished by the motion of α/6<100> Shockley partials on alternate basal planes (0001)α2, and the α/6<100> Shockley partials move in coordination rather than sweep on (0001)α2 plane one by one. It appears that no atom transportation is involved in this stress-induced α2→γ transfromation.

Deformation-induced α_2/γ Interfaces in a Hot-deformed Ti-45Al-10Nb Alloy

The structure change of α2/γ interface in a Ti-45Al-10Nb alloy induced by hot deformation was investigated by conventional and high-resolution transmission eIectron microscopy. Two types of hot deformation induced special α2/γ intedeces, coherent intedeces with high density of ledges and semi-coherent α2/γ intedeces were found to be due to the absorption of mobile dislocations into the α2/γ inteface. For the misoriented semi-coherent α2/γ interfaces, the densities of dislocation ledges increase with the misoriented angle between (111)γ and (0001)α2 planes, and 1/3[111] Frank partial dislocations were involved in the dislocation ledges. Formation mechanism of these deformation-induced α2/γ interfaces was discussed to be related to the role of α2/γ interface5 adjusting the deformation as a dislocation sink absorbing the slipping dislocations in the γ phase

紧固件用Ti-45Nb合金丝材的性能评价

研究不同规格的Ti-45Nb合金丝材的显微组织和力学性能。结果表明:随着Ti-45Nb合金丝材尺寸的增大,其抗拉强度不断降低,但屈服强度和剪切强度不断增加,而显微组织以及拉伸塑性的变化幅度不是很明显;经热暴露后的Ti-45Nb合金丝材,拉伸强度明显增加,但拉伸塑性的下降也比较明显;不同规格的Ti-45Nb合金丝材经过冷顶锻测试后的样品表面均没有宏观裂纹萌生,表明材料具有良好的冷成形性能。

Haemocompatibility of Ti-3Zr-2Sn-3Mo-25Nb biomedical alloy with surface heparinization using electrostatic self assembly technology

The haemocompatibility of Ti-3Zr-2Sn-3Mo-25Nb biomedical alloy was studied after surface heparinization. A layer of sol-gel TiO2 films was applied on the alloy samples followed by active treatment in the bio-functionalized solution for introducing the OH- and groups, and then the heparin was immobilized on the active TiO2 films through the electrostatic self assembly technology. It is shown that the heparinized films are mainly composed of anatase and rutile with smooth and dense surface. In vitro blood compatibility was evaluated by haemolysis test, clotting time and platelet adhesion behavior tests. The results show that the haemocompatibility of the alloy could be significantly improved by surface heparinization.

Preparation and osteoinduction of active micro-arc oxidation films on Ti-3Zr-2Sn-3Mo-25Nb alloy

A layer of porous film containing Ca and P was prepared by the micro-arc oxidation method on the surface of a novel near β biomedical Ti-3Zr-2Sn-3Mo-25Nb alloy, and then NH2- active group was introduced to the films by activation treatment. The phase composition, surface micro-topography and elemental characteristics of the micro-arc oxidation films were investigated with XRD, SEM, EDS and XPS, and the osteoinduction of the micro-arc oxidation films was tested using the simulated body fluid immersion, the in-vitro osteoblast cultivation test and animal experiment. The results show that the oxide layer is a kind of porous ceramic intermixture and contains Ca and P. The films in the simulated body fluid can induce apatite formation, resulting in excellent bioactivity. The cell test discovers that osteoblasts can grow well on the surface of micro-arc oxidation films. And the Ti-3Zr-2Sn-3Mo-25Nb biomedical alloy coated with active porous calcium-phosphate films shows better osteoinduction in vivo.

紧固件用Ti-45Nb合金热处理工艺研究

研究了真空退火热处理工艺对Ti-45Nb合金显微组织和力学性能的影响。结果表明:Ti-45Nb合金的β晶粒随退火温度的提高而长大;随着退火温度的提高,Ti-45Nb合金的拉伸性能以及剪切强度的变化不明显;当退火温度为810℃时,合金获得了较理想的显微组织以及拉伸强度与剪切强度的良好匹配。

Ti-45Al-10Nb合金的高温氧化行为

研究了Ti-45Al-10Nb(原子分数,％)合金在800～960℃在氧气和空气中的氧化行为。结果表明,该合金具有较好的高温抗氧化性能,其氧化增重速率与铁基耐热不锈钢相似或略优。与Ti-50Al合金相反,Ti-45Al-10Nb合金在空气中的氧化增重速率明显低于在纯氧中的氧化增重速率。X射线衍射与能谱分析表明,Ti-45Al-10Nb合金在氧气中的氧化产物主要有TiO_2和Al_2O_3,但在空气中的氧化产物中有TiN相。这是降低氧化速率的主要原因,同时,合金元素Nb稳定了氧化层中的TiN相,因而提高了合金在空气中的抗氧化性能。

ICP-AES法测定Ti-45Nb合金中铁、硅、铬、镁和锰等杂质元素

介绍了采用电感耦合等离子体发射光谱法(ICP-AES)测定Ti-45Nb合金中杂质元素铁、硅、铬、镁、锰的方法,样品采用盐酸、氢氟酸加硝酸溶解,溶解温度控制在室温或水浴70℃以下。进行了仪器工作参数和待测元素分析线的选择试验,确定了仪器最佳工作条件,考察了合金基体钛和共存元素铌对待测元素的影响,确定了各待测元素分析线分别为Fe238.204nm,Si251.611nm,Cr205.560nm,Mg279.533nm,Mn260.568nm。通过基体匹配消除基体的影响,实现了用电感耦合等离子体原子发射光谱法测定钛铌合金中铁、硅、铬、镁、锰元素的含量。进行了加入回收试验,回收率在90~120%之间,方法的检出限是0.0006~0.008μg/mL,相对标准偏差小于10%。

钨对铸态Ti-45Al-8Cr-2Nb合金的高温性能影响

采用高温拉伸测试及显微组织观察,研究了微量钨对铸态Ti-45Al-8Cr-2Nb(原子百分比)合金的高温性能影响。结果表明,在基体合金中添加2%W,能使铸态合金的最大伸长率降低,而最大伸长率相应的温度向高温方向移动;高温变形过程中,晶粒滑动的协调过程由晶界扩散转化为体扩散;含钨的合金在800℃时的伸长率从0.62%提高到90%。

Effect of post-weld heat treatment on microstructure and properties of Ti-23Al-17Nb alloy laser beam welding joints

The mechanical properties of Ti-23Al-17Nb (mole fraction,%) laser beam welding alloy joint at room temperature are comparable to that of the base materials.However,the strength and ductility of the as-welded joint deteriorate seriously after high temperature circulation.The effect of post-welded heat treatment on the microstructure and mechanical properties of the joint was investigated.The heat treatment was taken at 980 ℃ for 1.5 h,then furnace cooling and air cooling were performed separately.The results indicate that proper post-welded heat treatment improves the ductility of the joint at high temperature.

Effect of heat treatment processing on microstructure and tensile properties of Ti-6Al-4V-10Nb alloy

Effects of heat treatment processing on the microstructure and mechanical properties of Ti-6Al-4V-10Nb alloy were investigated. The microstructures were investigated by SEM, TEM and XRD, and the mechanical properties were evaluated by tensile tests at room and elevated temperatures. The results indicate that the lath-like and globular primary α phase, secondary α phase and β phase are obtained after forging and heat treatment processing. The size of secondary α phase is much smaller than that of primary α phase. After heat treatment, the volume fraction of primary α phase is decreased, and that of secondary α phase is increased. With the increase of solution temperature, the volume fraction of primary α phase is gradually decreased, and that of secondary α phase is obviously increased. The yield strength and tensile strength of Ti-6Al-4V-10Nb alloy are significantly enhanced with the solution temperature increasing.

Accelerated fracture healing by osteogenic Ti45Nb implants through the PI3K–Akt signaling pathway

The key to managing fracture is to achieve stable internal fixation,and currently,biologically and mechanically appropriate internal fixation devices are urgently needed.With excellent biocompatibility and corrosion resistance,titanium–niobium alloys have the potential to become a new generation of internal fixation materials for fractures.However,the role and mechanism of titanium–niobium alloys on promoting fracture healing are still undefined.Therefore,in this study,we systematically evaluated the bone-enabling properties of Ti45Nb via in vivo and in vitro experiments.In vitro,we found that Ti45Nb has an excellent ability to promote MC3T3-E1 cell adhesion and proliferation without obvious cytotoxicity.Alkaline phosphatase(ALP)activity and alizarin red staining and semiquantitative analysis showed that Ti45Nb enhanced the osteogenic differentiation of MC3T3-E1 cells compared to the Ti6Al4V control.In the polymerase chain reaction experiment,the expression of osteogenic genes in the Ti45Nb group,such as ALP,osteopontin(OPN),osteocalcin(OCN),type 1 collagen(Col-1)and runt-related transcription factor-2(Runx2),was significantly higher than that in the control group.Meanwhile,in the western blot experiment,the expression of osteogenic-related proteins in the Ti45Nb group was significantly increased,and the expression of PI3K–Akt-related proteins was also higher,which indicated that Ti45Nb might promote fracture healing by activating the PI3K–Akt signaling pathway.In vivo,we found that Ti45Nb implants accelerated fracture healing compared to Ti6Al4V,and the biosafety of Ti45Nb was confirmed by histological evaluation.Furthermore,immunohistochemical staining confirmed that Ti45Nb may promote osteogenesis by upregulating the PI3K/Akt signaling pathway.Our study demonstrated that Ti45Nb exerts an excellent ability to promote fracture healing as well as enhance osteoblast differentiation by activating the PI3K/Akt signaling pathway,and its good biosafety has been confirmed,which indicates its clinical translation potential.

DEFORMATION STRUCTURES IN A Ti45Al 10Nb ALLOY AT ROOM TEMPERATURE

Dislocation structures in the γ phase grains of Ti 45Al 10Nb specimens have been characterized after tensile tests at room temperature. In addition to ordinary dislocations with b=1/2〈110], a certain density of superdislocations and faulted dipoles were observed, which are rarely present in the conventional two phase TiAl base alloys of normal impurity. This difference was attributed to the solution of high Nb in the γ phase, which may increase the CRSS for 〈110] ordinary slip.

Microstructure and mechanical properties of cast Ti-47Al-2Cr-2Nb alloy melted in various crucibles

The main factors limiting the mass production of TiAI-based components are the high reactivity of TiAl- based alloys with the crucible or mould at high temperature. In this work, various crucibles （e.g. CaO, Y203 ceramic crucibles and water-cooled copper crucible） were used to fabricate the Ti-47Al-2Cr-2Nb alloy in a vacuum induction furnace. The effects of crucible materials and melting parameters on the microstructure and mechanical properties of the alloy were analyzed by means of microstructure observation, chemical analysis, tensile test and fracture surface observation. The possibilities of melting TiAI alloys in crucibles made of CaO and Y2O3 refractory materials were also discussed.

Effect of hot deformation on α→β phase transformation in 47Zr-45Ti-5Al-3V alloy

The effect of strain rate and deformation temperature on theα→βphase transformation in 47Zr-45Ti-5Al-3V alloy with an initial widmanstattenαstructure was investigated.At the deformation temperature of 550°C,the volume fraction ofαphase decreased with increasing strain rate.At 600 and 650°C,the volume fraction ofαphase firstly increased to a maximum value with increasing strain rate from 1×10-3 to 1×10-2 s-1,and then decreased.At 700°C,the microstructure consisted of singleβphase.At a given strain rate,the volume fraction ofαphase decreased with increasing deformation temperature.With decreasing strain rate and increasing deformation temperature,the volume fraction and size of globularαphase increased.At 650°C and 1×10-3 s-1,the lamellarαphase was fully globularized.The variation in the volume fraction and morphology ofαphase with strain rate and deformation temperature significantly affected the hardness of 47Zr-45Ti-5Al-3V alloy.

国产与进口紧固件用Ti-45Nb合金丝材性能对比研究

对国产与进口紧固件用Ti-45Nb合金丝材的化学成分、拉伸性能和显微组织进行了对比分析。研究结果表明:国产材料在塑性指标方面优于进口材料,但在强度和显微组织方面存在一定程度的差距。为了改善国产Ti-45Nb材料的综合性能,应进一步调节化学成分,增加强度性能,细化晶粒改善显微组织。

Effects of solution time on microstructure and mechanical properties of Ti-22Al-24Nb alloy

In this research, the changing rules of billet forged Ti-22 Al-24 Nb alloy with various solution time were studied, and the mechanical properties of different microstructure were tested at the room temperature. The results indicate that the(α2+O+B2) three-phase microstructure with equiaxed grains was acquired by Ti-22 Al-24 Nb alloy billet forging, and the average size of the grains was about 300 μm. With the increase of solution time, the primary lath-shaped O phase began to dissolve, and then the equiaxial α2 phase started to dissolve, but the undissolved α2/O phase began to be equiaxial and grow. The grains of original B2 phase recrystallized and grew. After the 2 h solution treatment, the recrystallization of grains was completed basically and the average size of the grains was about 100 μm. After the 2.5 h solution treatment, the strength of the alloy decreased, and the plasticity increased. However, when the solution treatment increased to 3 h, the plasticity decreased but the strength increased. The optimal solution parameters of Ti-22 Al-24 Nb alloy were the holding time of 2 h, the solution temperature of 1 000 ?C, and water cooling. Excellent comprehensive mechanical properties can be accquired under these parameters. The tensile strength, the yield strength, the elasticity modulus, the elongation, and the section shrinkage were 950 MPa, 915 MPa, 90 GPa, 15.69% and 42.28%, respectively.