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Low-cost surface modification of a biomedical Zr-2.5Nb alloy fabricated by electron beam melting

Journal of Materials Science & Technology 2023年第12期143卷 178-188页

作者： Caixu Wang Xiaoli Zhao Shujun Li Lu Liu Deliang Zhang mitsuo niinomi School of Materials Science and Engineering Northeastern UniversityShenyang 110819China Shi-changxu Innovation Center for Advanced Materials Institute of Metal ResearchChinese Academy of SciencesShenyang 110016China Key Laboratory of Data Analytics and Optimization for Smart Industry(Ministry of Education) Northeastern UniversityShenyang 110819China Tianjin Key Laboratory of Bone Implants Interface Functionalization and Personalization Tianjin 300190China Institute for Materials Research Tohoku UniversitySendaiMiyagi 9808577Japan Division of Materials and Manufacturing Science Graduate School of EngineeringOsaka UniversityOsaka 565-0871Japan Department of Materials Science and Engineering Graduate School of Science and TechnologyMeijo UniversityNagoya 468-8502Japan Faculty of Chemistry Materials and BioengineeringKansai UniversityOsaka 564-860Japan

The Zr-2.5Nb alloy with a fine microstructure consisting ofαlaths was successfully prepared by electron beam melting(EBM).The thermal oxidation behaviors and kinetics of the as-built,and the EBM-built and hot isostatically pressed(HIPed)Zr-2.5Nb materials in a temperature range of 450-600°C were in-vestigated and compared with those of the alloy prepared by conventional casting and *** was found that the oxidation kinetics of the as-built and the forged materials followed the parabolic rate law during isothermal oxidation at 550°C,but the HIPed materials exhibited a parabolic-to-linear kinetic transition,suggesting that the larger grain sizes enhanced the *** oxide layers of all materials were composed of a large fraction of monoclinic zirconia phase(m-ZrO_(2))and a small fraction of tetrago-nal zirconia phase(t-ZrO_(2)),and transformed from t-ZrO_(2)to m-ZrO_(2)with increasing oxidation *** surface hardness of the as-built,the forged and the HIPed materials increased from 215,204,and 188 HV before oxidation to 902,1070,and 1137 HV after oxidation,*** cross-sections of the materi-als showed the presence of micropores and microcracks inside the oxide layers with thicknesses ranging from 4 to 8μ*** the oxidation temperature of 600°C and oxidation time duration of 3 h,a dense black m-ZrO_(2)oxide layer with smooth surface and 902 HV hardness was obtained on the EBM as-built Zr-2.5Nb materials.

关键词： Zr-2.5Nb alloy Electron beam melting Thermal oxidation Oxidation behaviors and kinetics Grain size

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New role of α phase in the fracture behavior and fracture toughness of a β-type bio-titanium alloy

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International Journal of Minerals,Metallurgy and Materials 2023年第9期30卷 1756-1763页

作者： Ran Wang Xiu Song Lei Wang Yang Liu mitsuo niinomi Deliang Zhang Jun Cheng Key Laboratory for Anisotropy and Texture of Materials(Ministry of Education)School of Materials Science and Engineering Northeastern UniversityShenyang 110819China Institute for Materials Research Tohoku University2-1-1 KatahiraAoba-kuSendai 980-8577Japan Meijo University 1-501 ShiogamaguchiTempaku-kuNagoya 468-8502Japan Nagoya University Furo-choChikusa-kuNagoya 464-8601Japan Shaanxi Key Laboratory of Biomedical Metal Materials Northwest Institute for Nonferrous Metal ResearchXi’an 710016China

The role of α precipitates formed during aging in the fracture toughness and fracture behavior of β-type bio-titanium alloy Ti–29Nb–13Ta–4.6Zr(TNTZ) was studied. Results showed that the fracture toughness of the TNTZ alloy aged at 723 K decreases to the minimum of 72.07–73.19 kJ·m^(-2)when the aging time is extended to 4–8 h and then gradually increases and reaches 144.89 kJ·m^(-2)after 72 h. The decrease in fracture toughness within the aging time of 4–8 h is caused by the large stress concentration at the tip of acicular α precipitates with a high aspect ratio and the preferential crack propagation along the inhomogeneous acicular α precipitates distributed in “V-shape” and “nearly perpendicular shape”. When the aging time is extended to 8–72 h, the precrack tip is uniformly blunted, and the crack is effectively deflected by α precipitates with multi long axis directions, more high homogeneity, low aspect ratio, and large number density. Analysis of the effect of αprecipitates on the fracture behavior suggested that the number of long axis directions of α precipitates is the key controlling factor for the fracture behavior and fracture toughness of the TNTZ alloy aged for different times.

关键词： fracture toughness Ti-29Nb-13Ta-4.6Zr alloy agedαphase crack tip blunting

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高强度和低弹性模量Ti−Nb−Fe−Zr合金的显微组织和力学性能

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Transactions of Nonferrous Metals Society of China 2022年第2期32卷 503-512页

作者：李强黄奇李俊杰何黔峰 Masaaki NAKAI 张柯 mitsuo niinomi Kenta YAMANAKA Akihiko CHIBA Takayoshi NAKANO 上海理工大学机械工程学院上海200093 中国科学院新疆理化技术研究所特殊环境功能材料与器件重点实验室乌鲁木齐830011 Division of Mechanical Engineering Faculty of Science and EngineeringKindai University3-4-1 KowakaeHigashiosakaOsaka 577-8502Japan 上海理工大学材料科学与工程学院上海200093 Institute for Materials Research Tohoku University2-1-1 KatahiraAoba-kuSendai 980-8577Japan Division of Materials and Manufacturing Science Graduate School of EngineeringOsaka University2-1 Yamada-OkaSuitaOsaka 565-0871Japan Department of Materials Science and Engineering Graduate School of Science and TechnologyMeijo University1-501 ShiogamaguchiTempaku-kuNagoya 468-8502Japan

将Zr添加到Ti−Nb−Fe合金中开发生物医用低模量、高强度β钛合金。采用电弧熔炼法制备Ti−12Nb−2Fe−(2,4,6,8,10)Zr(摩尔分数,%)铸锭,随后对其进行均匀化、冷轧和固溶处理。通过光学显微镜、X射线衍射和透射电子显微镜等技术分析合金的物... 详细信息

将Zr添加到Ti−Nb−Fe合金中开发生物医用低模量、高强度β钛合金。采用电弧熔炼法制备Ti−12Nb−2Fe−(2,4,6,8,10)Zr(摩尔分数,%)铸锭,随后对其进行均匀化、冷轧和固溶处理。通过光学显微镜、X射线衍射和透射电子显微镜等技术分析合金的物相和显微组织。采用拉伸试验测定力学性能。结果表明,Zr和Fe在合金中具有显著的固溶强化效果,因此,所有合金的屈服强度和抗拉强度分别高于510 MPa和730 MPa。Zr对变形机制的影响较小,孪晶出现在所有变形合金中,且对强度和塑性有益。具有亚稳β相的Ti−12Nb−2Fe−(8,10)Zr合金表现出低弹性模量、高抗拉强度和良好的塑性,是生物医学植入物的合适候选材料。

关键词：医用钛合金力学性能固溶强化加工硬化孪晶诱导塑性

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Corrosion Behavior of MgZnCa Bulk Amorphous Alloys Fabricated by Spark Plasma Sintering

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Acta Metallurgica Sinica(English Letters) 2016年第9期29卷 793-799页

作者： Feng-Xiang Qin Chuan Ji Zhen-Hua Dan Guo-Qiang Xie Hao Wang Shin-Ichi Yamaura mitsuo niinomi Yang-De Li School of Materials Science and Engineering Nanjing University of Science and Technology Institute for Materials Research Tohoku University College of Materials Science and Engineering Nanjing TECH University WPI-AIMR Tohoku University Dongguan Eontech Co. Ltd

Centimeter-sized Mg65Zn30Ca5 bulk amorphous alloys were fabricated by the spark plasma sintering process from the amorphous powders with a size smaller than 5 la m prepared by ball-milling. The sintered Mg65Zn30Ca5 samples were in an amorphous state when the spark plasma sintering was performed at a temperature of 383 K under a pressure of 600 MPa. The data of polarization curves presented that the sintered Mg65Zn30Ca5 bulk amorphous alloys exhibited higher corrosion resistance than pure Mg and AZ31B alloy owing to high content of Zn and homogeneous structure. A calcium phosphate compound layer was formed on the sintered Mg65Zn30Ca5 bulk amorphous sample after immersion in Hanks＇ solution, which is effective in improving corrosion resistance and bioactivity. The sintered MgZnCa bulk amorphous alloys with large dimensions broaden the potential application of bulk amorphous alloys in the biomedical fields.

关键词： Mg Bulk amorphous alloys Spark plasma sintering Corrosion behavior Biomedical applications

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Using Cavitation Peening to Improve the Fatigue Life of Titanium Alloy Ti-6Al-4V Manufactured by Electron Beam Melting

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Materials Sciences and Applications 2016年第4期7卷 181-191页

作者： Mitsuru Sato Osamu Takakuwa Masaaki Nakai mitsuo niinomi Fumio Takeo Hitoshi Soyama Department of Nanomechanics Graduate School of Engineering Tohoku University Sendai Japan Institute for Materials Research Tohoku University Sendai Japan Department of Mechanical Engineering Hachinohe National College of Technology Hachinohe Japan

Although Electron Beam Melting (EBM) is an innovative technology, the fatigue properties of materials manufactured by EBM may be lower than those of casted and wrought materials due to defects and surface roughness. In order to enhance the fatigue life of components or structures manufactured by EBM, a mechanical surface treatment technology, e.g., peening, would be effective because peening introduces high compressive residual stress at the surface which can extend the fatigue life considerably. In the present study, specimens were manufactured by EBM using titanium alloy Ti-6Al-4V powder. Two types of specimens were prepared: as-built and as-machined specimens. Specimens of each type were treated by cavitation peening or shot peening. The fatigue lives of the specimens were evaluated by a plate bending fatigue tester. The residual stress and surface roughness were also evaluated. The results obtained showed that the fatigue strength of as-built specimens can be improved by 21% by cavitation peening or shot peening, and the fatigue life under particular applied stresses can also be extended by 178% by cavitation peening.

关键词： Component Electron Beam Melting Ti-6Al-4V Cavitaion Peening Residual Stress Fatigue

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Influence of Alloy Elements on the Osteoconductivity of Anodized Ti-29Nb-13Ta-4.6Zr Alloy

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Journal of Biomaterials and Nanobiotechnology 2013年第3期4卷 229-236页

作者： Dai Yamamoto Atsushi Waki Kensuke Kuroda Ryoichi Ichino Masazumi Okido Masato Ueda Masahiko Ikeda mitsuo niinomi Azusa Seki Department of Materials Science & Engineering Graduate School of Engineering Nagoya University Nagoya Japan EcoTopia Science Institute Nagoya University Nagoya Japan Faculty of Chemistry Materials and Bioengineering Kansai University Suita Japan Hamri Co. Ltd. Tokyo Japan Institute for Materials Research Tohoku University Sendai Japan

Anodizing is expected to be an effective method to improve the osteoconductivity of the Ti-29Nb-13Ta-4.6Zr (TNTZ) alloy because the bioactivity of anodized Ti is good. However, it is not known how the alloy elements influence the surface roughness, composition, hydrophilicity, and osteoconductivity of the anodized film on the Ti alloy. In this study, we investigated the effects of anodizing on the surface properties and the osteoconductivity of the anodized TNTZ alloy, focusing on the functions of the individual alloy elements. The anodized oxides of the Nb, Ta, and Zr metals were hydrophobic at all the voltages applied, in contrast to the anodized oxide of Ti. As well as pure Ti, a TiO2-based oxide film formed on TNTZ after anodizing. However, the oxide film also contained large amounts of Nb species and the molar Nb/Ti ratio in the TNTZ alloy was high, which makes the surface more hydrophobic than the anodized oxide on Ti. In vivo tests showed that the osteoconductivity of the TNTZ alloy was sensitive to both its surface roughness and hydrophilicity. When the TNTZ alloy was anodized, the process increased either the surface hydrophobicity or the surface roughness at the voltage used in this study. These changes in the surface properties did not improve its osteoconductivity.

关键词： Ti-29Nb-13Ta-4.6Zr Anodizing Titanium Dioxide Alloy Element Hydrophilicity Osteoconductivity

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冷喷涂技术在生物医学领域中的应用及展望

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表面技术 2016年第9期45卷 25-31页

作者：刘奕所新坤黄晶新家光雄李华中国科学院宁波材料技术与工程研究所海洋新材料与应用技术重点实验室浙江省海洋与防护技术重点实验室浙江宁波315201 东北大学金属材料研究所生物材料科学实验室日本仙台980-8577

冷喷涂技术(cold spray technology)是一类赋予材料表面特殊性能的重要手段。概述了冷喷涂技术在制备温度敏感生物材料加工领域的优势,并重点综述了利用冷喷涂技术制备的典型生物材料。目前,冷喷涂沉积永久性植入金属材料,如Ti合金、Fe... 详细信息

冷喷涂技术(cold spray technology)是一类赋予材料表面特殊性能的重要手段。概述了冷喷涂技术在制备温度敏感生物材料加工领域的优势,并重点综述了利用冷喷涂技术制备的典型生物材料。目前,冷喷涂沉积永久性植入金属材料,如Ti合金、Fe基合金、Co-Cr合金和可降解金属材料Mg合金等技术相对成熟。近年来随着冷喷涂技术的发展,有效解决和拓展了用于医疗器械表面改性的涂层材料体系,如冷喷涂制备高分子材料超高分子量聚乙烯(UHMWPE)涂层,以及高密度聚乙烯(HDPE)和聚醚醚酮(PEEK)表面冷喷涂制备生物涂层。最值得关注的冷喷涂或真空冷喷涂技术制备陶瓷涂层,如羟基磷灰石(HA)、羟基磷灰石-石墨烯(HA-graphene)以及二氧化钛(Ti O2),在生物医学领域应用具有突破性进展。同时归纳了冷喷涂技术在生物医学领域的研究现状和问题,虽然在针对冷喷涂生物涂层的微观结构、力学行为、腐蚀抗力等方面取得了一定成果,在组织工程、抗菌材料等领域也取得了尝试性突破,但尚缺乏系统的冷喷涂涂层生物学性能表征,涂层与细胞/组织相互作用机理还不明确,相关的临床研究欠缺。最后,在此基础上,展望了未来生物材料朝功能化和个性化医疗方向的发展方向。冷喷涂技术在功能化载药涂层的低温制备和个性化医疗器械增材制造等领域将有更大的应用空间,并给新型生物材料的表面改性带来更多机遇和可能。

关键词：冷喷涂技术生物医疗生物材料生物学特性

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Ti-Nb-Ta-Zr合金组织研究

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金属学报 2002年第Z1期38卷 150-153页

作者：李述军郝玉琳杨锐崔玉友 M.niinomi 中国科学院金属研究所沈阳110016 Department of Production Systems Engineering Toyohashi University 1-1HibarigaokaTempaku-choToyohashi441-8580Japan

本文研究了时效处理对两种医用Ti-Nb-Ta-Zr合金组织的影响研究表明,在300-600℃之间对Ti-29Nb-13Ta-4.6Zr合金进行时效处理,α和ω相从β基体中析出Ti-39Nb-13Ta-4.6Zr合金比Ti-29Nb-13Ta-4.6Zr合金稳定,对其进行短期时效处理,未见α相... 详细信息

本文研究了时效处理对两种医用Ti-Nb-Ta-Zr合金组织的影响研究表明,在300-600℃之间对Ti-29Nb-13Ta-4.6Zr合金进行时效处理,α和ω相从β基体中析出Ti-39Nb-13Ta-4.6Zr合金比Ti-29Nb-13Ta-4.6Zr合金稳定,对其进行短期时效处理,未见α相和ω相析出.长期时效处理(12 d)后,才有可见α相出现.

关键词： Ti-Nb-Ta-Zr合金,组织

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Ti-29Nb-13Ta-4.6Zr合金的磨损特性

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金属学报 2002年第Z1期38卷 282-285页

作者：李述军杨锐李曙郝玉琳崔玉友 M.niinomi 中国科学院金属研究所沈阳110016 Toyhashi University of Technology Toyohashi 441-8580Japan

利用环块式腐蚀磨损试验机研究了Ti-29Nb-13Ta-4.6Zrβ型医用钛合金的磨损特性,并与传统医用钛合金Ti-6Al-4V进行了比较.研究表明:在空气中干磨,Ti-29Nb-13Ta-4.6Zr合金及Ti-6Al-4V合金的抗磨能力主要取决于合金的硬度及抗拉强度等力学... 详细信息

利用环块式腐蚀磨损试验机研究了Ti-29Nb-13Ta-4.6Zrβ型医用钛合金的磨损特性,并与传统医用钛合金Ti-6Al-4V进行了比较.研究表明:在空气中干磨,Ti-29Nb-13Ta-4.6Zr合金及Ti-6Al-4V合金的抗磨能力主要取决于合金的硬度及抗拉强度等力学性能;在0.9%NaCl溶液中磨损,Ti-29Nb-13Ta-4.6Zr合金抗腐蚀磨损能力低于***含量的提高可以增强Ti-29Nb-13Ta-4.6Zr合金的抗腐蚀磨损能力.

关键词：新型医用β钛合金,干磨,腐蚀磨损

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α"马氏体相对Ti-29Nb-13Ta-4.6Zr医用钛合金杨氏模量和力学性能的影响

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金属学报 2002年第Z1期38卷 236-239页

作者：郝玉琳杨锐李述军崔玉友李东 M.niinomi 中国科学院金属研究所钛合金研究室沈阳110016 Deparement of Production Systems Engineering Toyhashi University of Technology1-1HibarigaokaTempaku-choToyohashi 441-8580Japan

研究了Ti-29Nb-13Ta-4.6Zr(质量分数,%)医用钛合金中α"马氏体相的形成及其对杨氏模量和力学性能的影响.对于β单相区固溶处理(1023,1123和1223 K分别热处理1.8,3.6,14.4和28.8 ks)并在冰水中淬火样品,X射线衍射和内耗测量表明:α"马氏... 详细信息

研究了Ti-29Nb-13Ta-4.6Zr(质量分数,%)医用钛合金中α"马氏体相的形成及其对杨氏模量和力学性能的影响.对于β单相区固溶处理(1023,1123和1223 K分别热处理1.8,3.6,14.4和28.8 ks)并在冰水中淬火样品,X射线衍射和内耗测量表明:α"马氏体相的体积含量随固溶温度和固溶时间变化.这主要归因于晶粒尺寸对β相的稳定性和马氏体起始转变温度(Ms)的影响:当晶粒小于临界尺寸(约40 μm)时,由于马氏体起始转变温度较低,导致相转变被抑制;当晶粒大于临界尺寸时,α"马氏体相的体积含量随晶粒尺寸的增加而迅速增加;随着晶粒进一步长大,α"马氏体相的体积含量反而减少.实验结果还表明:相对于β相,α"马氏体相具有高塑性、低强度、低硬度和相近的杨氏模量.

关键词： α"马氏体相,杨氏模量,力学性能

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