医用超细晶TiNbZrTaFe复合材料的粉末冶金制备及其性能研究
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摘要
Ti合金由于具有生物相容性好、综合力学性能优异、耐腐蚀能力强等特点，被广泛应用于生物医用植入材料。目前采用铸造法制备的第三代β型Ti合金尽管综合力学性能和生物相容性较好，但还是存在高熔点金属带来的晶粒粗大、成分偏析较大、弹性模量较高、耐磨性较差等缺点。此外，细晶材料由于具有更好的生物相容性也成为目前的研究热点。本论文的研究目标是采用粉末冶金法（机械合金化和放电等离子烧结）制备高强度、低模量的超细晶医用钛合金，为制备生物相容性和综合力学性能优异的生物医用材料提供一种新的方法。因此，本课题的开展具有重要的学术和应用意义。
首先，在成分设计中，根据元素生物相容性初步筛选合金元素，通过“d电子理论”、“Inoue三原则”进一步筛选合金元素为Nb、Zr、Ta和Fe，选定合金成分为(Ti-35Nb-7Zr-5Ta，简称TNZT)100-xFex(x=0、2、6、10)。然后，采用“Miedema模型”分析计算了合金体系的非晶形成能力，并采用“团簇理论”对设计的合金成分的弹性模量大小进行预测，为后续采用非晶晶化法制备高强低模的医用钛合金提供充分的理论支持和指导。
在机械合金化过程中，研究了Fe含量对合金体系非晶形成能力、热稳定性和晶化方式的影响。结果表明：合金的非晶形成能力随Fe含量的增加而增强。只有当x=10时，球磨终态粉末为纯非晶结构；当x=0时，球磨终态粉末为纯纳米晶；x=2和6时，球磨终态粉末为非晶/纳米晶复合结构。所有合成的非晶/纳米晶粉末均具有宽的过冷液相区Tx，说明合成的非晶/纳米晶粉末具有较高的热稳定性。Fe含量影响合金体系晶化激活能大小，从而影响其热稳定性。当x=10时，合金的晶化激活能大于x=6的晶化激活能。Fe含量对球磨终态粉末的晶化方式也有显著影响。当x=6时，其Avrami指数n平均值为2.5，对应的晶化生长机制为体扩散控制的三维晶核生长。当x=10时，其Avrami指数n平均值为2.0，对应的晶化生长机制为典型的体扩散控制的二维形核生长。球磨终态粉末晶化生长机制的不同影响着晶化析出相的种类。当x=6时，其晶化析出相为bcc β-Ti和bcc FeTi相；当x=10时，其晶化析出相为α-Ti、bcc β-Ti和bcc FeTi相。
随后，采用放电等离子烧结法固结球磨粉末，制备了不同Fe含量的医用超细晶钛基复合材料。结果表明：Fe含量对制备的(TNZT)100-xFex(x=0、2、6、10)块体材料的力学性能产生了显著影响。仅当x=6时，块体材料具有显著塑性，当x=0、2、10时，块体材料无塑性。研究发现，力学性能的差异由块体材料的晶化析出相种类和微观结构所决定。当x=6时，合金显微结构为β-Ti基体包围FeTi的两相区，其断裂机理可以用“软硬模型”来解释。当烧结温度为1243K、烧结速率为290K/min、保温时间为5min时，超细晶(TNZT)94Fe6复合材料具有最好的综合力学性能，其屈服强度σy为2292MPa，断裂强度σmax为2531MPa，断裂应变εf为9.16%，其超声弹性模量E为53GPa，为目前文献报道的Ti-Nb-Zr合金体系中的极小值。
研究了制备的高强低模超细晶(TNZT)94Fe6合金的耐摩擦磨损性能，并与目前市场常用的两种医用钛合金Ti-6Al-4V (TAV)和Ti-13Nb-13Zr (TNZ)进行了比较。三种钛合金中，超细晶(TNZT)94Fe6合金具有最好的耐摩擦磨损性能，TNZ合金最差。并比较了晶粒尺寸对超细晶(TNZT)94Fe6合金耐摩擦磨损性能的影响，结果表明晶粒尺寸越小，(TNZT)94Fe6合金的耐摩擦磨损性能越优异。
研究了制备的高强低模超细晶(TNZT)94Fe6合金的耐腐蚀性能，并与目前市场常用的两种生物钛合金TAV和TNZ进行了比较。三种钛合金在模拟人体体液中的稳定性分别是(TNZT)94Fe6>TNZ>TAV。此外，晶粒尺寸也影响到超细晶(TNZT)94Fe6合金耐腐蚀性能，晶粒尺寸越大，其腐蚀倾向越大，腐蚀反应速度越慢。另外，对(TNZT)100-xFex(x=0、6、10)三种钛合金进行了细胞毒性实验，结果表明三种钛合金均为生物毒性I级，适合用作生物医用材料。
Because of their good biocompatibility, excellent mechanical properties and corrosionresistance, Ti alloys are widely used as biomedical materials. Though the third generation βtype Ti alloys prepared by casting method have good mechanical properties andbiocompatibility, they also possess shortcomings such as coarse grain, component segregationbrought by refractory metal, higher elastic modulus compared with human bone and poorwear resistance. Moreover, preparation of fine-grained biomaterials also becomes a researchfocus because of their better biocompatibility. The aim of the present study is to prepareultrafine-grained (UFG) biomedical titanium alloys with high strength and low modulus bypowder metallurgy (mechanical alloying (MA) and spark plasma sintering (SPS)). It canprovide a new method for preparation of biomedical materials. Therefore, this project hasimportant academic and application significance.
As a first step, the alloying elements were selected preliminary according to elementsbiocompatibility. The chemical composition was selected as (Ti-35Nb-7Zr-5Ta)100-xFex(x=0、2、6、10) according to “d electronical theory”and “Inoue’s three principles”. Then,“MiedemaModel” was used to calculate glass forming ability (GFA) of designed alloys and “clustertheory” was used to predict chemical composition in order to find the alloy composition withlowest elastic modulus.
During MA, the effect of Fe content on GFA, thermal stability and crystallizationmechanism was investigated. The result shows that the GFA of the alloys increases with theincreasing of Fe content. With the increased Fe content, the synthesized alloy powders afterthe steady state milling transform from full nanocrystalline structure for x=0to fullamorphous structure for x=10. The synthesized amorphous/nanocrystalline alloy powderspossess high thermal stability because they all show wide supercooled liquid region Tx.Moreover, the crystallization activation energy E is affected by Fe content, and thus theirthermal stability is affected. The crystallization activation energy E for x=10is bigger thanthat for x=6. The crystallization mechanism of milled powder is also affected by Fe content.The average Avrami exponent n are2.5and2.0for x=6and10, respectively. Thecrystallization mechanisms are typical volume diffusion-controlled three and two-dimensionalgrowth of nuclei for x=6and10, respectively. The different crystallization mechanisms ofmilled powder affect the species of crystallization precipitation phase. For x=6, thecrystallization precipitation phases are composed of β-Ti and FeTi. For x=10, the crystallization precipitation phase contain α-Ti, β-Ti and FeTi.
Subsequently, biomedical UFG Ti-based composites with different Fe contents werefabricated by SPS method. The effect of Fe content on microstructure and mechanicalproperties of UFG bulk composites was investigated. The result shows Fe content affectsmechanical properties of consolidated bulk composites obviously. Only for x=6, the UFG bulkcomposites possess obvious plasticity. For x=0,2and10, the UFG bulk composites have noplasticity. The difference in mechanical properties of UFG bulk alloys is decided by species ofcrystallization precipitation phase and their microstructures. The microstructure is atwo-phase region consisting of FeTi phase surrounded by β-Ti matrix for x=6, and the fracturemechanism can be explained by the “soft-hard model”. The biomedical UFG (TNZT)94Fe6composite exhibits high strength and low modulus. The UFG bulk composite possessesexcellent mechanical properties fabricated by heating to1243K at290K/min and holding for5min. Its yield strength σy, fracture strength σmax, fracture strain and ultrasonic elasticmodulus are2292MPa,2531MPa,9.16%and53GPa, respectively. The value of elasticmodulus is relative small in the reported Ti-Nb-Zr alloy system.
The wear resistance of the fabricated UFG (TNZT)94Fe6composite was investigated bycompared with conventional biomedical Ti-6Al-4V (TAV) and Ti-13Nb-13Zr (TNZ) alloys.The result shows that the UFG (TNZT)94Fe6alloy possess the best wear resistance while theTNZ alloy possesses the worst. Besides, the effect of grain size on wear resistance of the UFG(TNZT)94Fe6composite was that the smaller the grain size, the better of its wear resistance.
The corrosion resistance of the fabricated UFG (TNZT)94Fe6composite was investigatedby compared with conventional biomedical TAV and TNZ alloys. The result shows that thestability for three kinds of Ti alloys in corrosive media is (TNZT)94Fe6>TNZ>TAV. Moreover,the corrosion resistance of the UFG (TNZT)94Fe6alloy is affected by grain size. The smallerthe grain size, the greater its corrosion tendency, and the slower the speed of the corrosionreaction. The cytotoxicity test for UFG (TNZT)100-xFex(x=0,6and10) alloys shows thatbiological toxicity of three kinds of titanium alloy are all class one and suitable as
首先，在成分设计中，根据元素生物相容性初步筛选合金元素，通过“d电子理论”、“Inoue三原则”进一步筛选合金元素为Nb、Zr、Ta和Fe，选定合金成分为(Ti-35Nb-7Zr-5Ta，简称TNZT)100-xFex(x=0、2、6、10)。然后，采用“Miedema模型”分析计算了合金体系的非晶形成能力，并采用“团簇理论”对设计的合金成分的弹性模量大小进行预测，为后续采用非晶晶化法制备高强低模的医用钛合金提供充分的理论支持和指导。
在机械合金化过程中，研究了Fe含量对合金体系非晶形成能力、热稳定性和晶化方式的影响。结果表明：合金的非晶形成能力随Fe含量的增加而增强。只有当x=10时，球磨终态粉末为纯非晶结构；当x=0时，球磨终态粉末为纯纳米晶；x=2和6时，球磨终态粉末为非晶/纳米晶复合结构。所有合成的非晶/纳米晶粉末均具有宽的过冷液相区Tx，说明合成的非晶/纳米晶粉末具有较高的热稳定性。Fe含量影响合金体系晶化激活能大小，从而影响其热稳定性。当x=10时，合金的晶化激活能大于x=6的晶化激活能。Fe含量对球磨终态粉末的晶化方式也有显著影响。当x=6时，其Avrami指数n平均值为2.5，对应的晶化生长机制为体扩散控制的三维晶核生长。当x=10时，其Avrami指数n平均值为2.0，对应的晶化生长机制为典型的体扩散控制的二维形核生长。球磨终态粉末晶化生长机制的不同影响着晶化析出相的种类。当x=6时，其晶化析出相为bcc β-Ti和bcc FeTi相；当x=10时，其晶化析出相为α-Ti、bcc β-Ti和bcc FeTi相。
随后，采用放电等离子烧结法固结球磨粉末，制备了不同Fe含量的医用超细晶钛基复合材料。结果表明：Fe含量对制备的(TNZT)100-xFex(x=0、2、6、10)块体材料的力学性能产生了显著影响。仅当x=6时，块体材料具有显著塑性，当x=0、2、10时，块体材料无塑性。研究发现，力学性能的差异由块体材料的晶化析出相种类和微观结构所决定。当x=6时，合金显微结构为β-Ti基体包围FeTi的两相区，其断裂机理可以用“软硬模型”来解释。当烧结温度为1243K、烧结速率为290K/min、保温时间为5min时，超细晶(TNZT)94Fe6复合材料具有最好的综合力学性能，其屈服强度σy为2292MPa，断裂强度σmax为2531MPa，断裂应变εf为9.16%，其超声弹性模量E为53GPa，为目前文献报道的Ti-Nb-Zr合金体系中的极小值。
研究了制备的高强低模超细晶(TNZT)94Fe6合金的耐摩擦磨损性能，并与目前市场常用的两种医用钛合金Ti-6Al-4V (TAV)和Ti-13Nb-13Zr (TNZ)进行了比较。三种钛合金中，超细晶(TNZT)94Fe6合金具有最好的耐摩擦磨损性能，TNZ合金最差。并比较了晶粒尺寸对超细晶(TNZT)94Fe6合金耐摩擦磨损性能的影响，结果表明晶粒尺寸越小，(TNZT)94Fe6合金的耐摩擦磨损性能越优异。
研究了制备的高强低模超细晶(TNZT)94Fe6合金的耐腐蚀性能，并与目前市场常用的两种生物钛合金TAV和TNZ进行了比较。三种钛合金在模拟人体体液中的稳定性分别是(TNZT)94Fe6>TNZ>TAV。此外，晶粒尺寸也影响到超细晶(TNZT)94Fe6合金耐腐蚀性能，晶粒尺寸越大，其腐蚀倾向越大，腐蚀反应速度越慢。另外，对(TNZT)100-xFex(x=0、6、10)三种钛合金进行了细胞毒性实验，结果表明三种钛合金均为生物毒性I级，适合用作生物医用材料。
Because of their good biocompatibility, excellent mechanical properties and corrosionresistance, Ti alloys are widely used as biomedical materials. Though the third generation βtype Ti alloys prepared by casting method have good mechanical properties andbiocompatibility, they also possess shortcomings such as coarse grain, component segregationbrought by refractory metal, higher elastic modulus compared with human bone and poorwear resistance. Moreover, preparation of fine-grained biomaterials also becomes a researchfocus because of their better biocompatibility. The aim of the present study is to prepareultrafine-grained (UFG) biomedical titanium alloys with high strength and low modulus bypowder metallurgy (mechanical alloying (MA) and spark plasma sintering (SPS)). It canprovide a new method for preparation of biomedical materials. Therefore, this project hasimportant academic and application significance.
As a first step, the alloying elements were selected preliminary according to elementsbiocompatibility. The chemical composition was selected as (Ti-35Nb-7Zr-5Ta)100-xFex(x=0、2、6、10) according to “d electronical theory”and “Inoue’s three principles”. Then,“MiedemaModel” was used to calculate glass forming ability (GFA) of designed alloys and “clustertheory” was used to predict chemical composition in order to find the alloy composition withlowest elastic modulus.
During MA, the effect of Fe content on GFA, thermal stability and crystallizationmechanism was investigated. The result shows that the GFA of the alloys increases with theincreasing of Fe content. With the increased Fe content, the synthesized alloy powders afterthe steady state milling transform from full nanocrystalline structure for x=0to fullamorphous structure for x=10. The synthesized amorphous/nanocrystalline alloy powderspossess high thermal stability because they all show wide supercooled liquid region Tx.Moreover, the crystallization activation energy E is affected by Fe content, and thus theirthermal stability is affected. The crystallization activation energy E for x=10is bigger thanthat for x=6. The crystallization mechanism of milled powder is also affected by Fe content.The average Avrami exponent n are2.5and2.0for x=6and10, respectively. Thecrystallization mechanisms are typical volume diffusion-controlled three and two-dimensionalgrowth of nuclei for x=6and10, respectively. The different crystallization mechanisms ofmilled powder affect the species of crystallization precipitation phase. For x=6, thecrystallization precipitation phases are composed of β-Ti and FeTi. For x=10, the crystallization precipitation phase contain α-Ti, β-Ti and FeTi.
Subsequently, biomedical UFG Ti-based composites with different Fe contents werefabricated by SPS method. The effect of Fe content on microstructure and mechanicalproperties of UFG bulk composites was investigated. The result shows Fe content affectsmechanical properties of consolidated bulk composites obviously. Only for x=6, the UFG bulkcomposites possess obvious plasticity. For x=0,2and10, the UFG bulk composites have noplasticity. The difference in mechanical properties of UFG bulk alloys is decided by species ofcrystallization precipitation phase and their microstructures. The microstructure is atwo-phase region consisting of FeTi phase surrounded by β-Ti matrix for x=6, and the fracturemechanism can be explained by the “soft-hard model”. The biomedical UFG (TNZT)94Fe6composite exhibits high strength and low modulus. The UFG bulk composite possessesexcellent mechanical properties fabricated by heating to1243K at290K/min and holding for5min. Its yield strength σy, fracture strength σmax, fracture strain and ultrasonic elasticmodulus are2292MPa,2531MPa,9.16%and53GPa, respectively. The value of elasticmodulus is relative small in the reported Ti-Nb-Zr alloy system.
The wear resistance of the fabricated UFG (TNZT)94Fe6composite was investigated bycompared with conventional biomedical Ti-6Al-4V (TAV) and Ti-13Nb-13Zr (TNZ) alloys.The result shows that the UFG (TNZT)94Fe6alloy possess the best wear resistance while theTNZ alloy possesses the worst. Besides, the effect of grain size on wear resistance of the UFG(TNZT)94Fe6composite was that the smaller the grain size, the better of its wear resistance.
The corrosion resistance of the fabricated UFG (TNZT)94Fe6composite was investigatedby compared with conventional biomedical TAV and TNZ alloys. The result shows that thestability for three kinds of Ti alloys in corrosive media is (TNZT)94Fe6>TNZ>TAV. Moreover,the corrosion resistance of the UFG (TNZT)94Fe6alloy is affected by grain size. The smallerthe grain size, the greater its corrosion tendency, and the slower the speed of the corrosionreaction. The cytotoxicity test for UFG (TNZT)100-xFex(x=0,6and10) alloys shows thatbiological toxicity of three kinds of titanium alloy are all class one and suitable as
引文
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