医用多孔钛基金属材料制备及性能研究
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摘要
采用粉末冶金法制备多孔钛、多孔Ti-Ag合金和多孔Ti-Si合金材料，重点研究多孔钛基金属材料的制备工艺，以及球磨工艺、Ag、Si元素对多孔钛基金属材料的微观结构、力学性能、磷灰石形成能力及细胞毒性的影响。通过行星球磨获得不同特性的钛粉末、Ti-Ag混合粉、Ti-Si混合粉，以尿素为造孔剂，在氩气气体保护气氛下高温烧结获得多孔钛、多孔Ti-Ag合金和多孔Ti-Si合金材料，并对其进行碱处理表面活化改性，通过模拟体液浸泡实验评价碱处理后多孔钛基金属材料的磷灰石形成能力。采用激光粒度分析仪、X射线衍射仪、扫描电子显微镜分析不同球磨工艺下制备的钛粉末的粒径、微观结构。采用压缩试验测试制备的多孔钛基金属材料的力学性能。采用X射线衍射仪、扫描电子显微镜、傅里叶变换红外光谱仪分析多孔钛基金属材料碱处理改性后的孔隙特征、微观结构，以及模拟体液浸泡后试样表面羟基磷灰石生长情况。采用MTT法评价多孔钛、多孔Ti-Ag合金和多孔Ti-Si合金材料的细胞毒性。
不同行星球磨时间（1h、5h、10h）制备的α-Ti钛粉末平均粒径29.25～1.84μm，体积比表面积0.24～3.90m~2/mm~3，钛粉末由α-Ti钛颗粒组成。球磨时间增加钛颗粒粒径减小，体积比表面积增加，钛晶粒逐渐细化；球磨时间5h时球磨工艺的细化效率最高。制备的多孔钛的孔隙大小350±150μm，孔隙率46.5～66.5%，制备的多孔钛物相结构为α-Ti+TiO，抗压强度15.7～61.9MPa，弹性模量0.9～1.9GPa。球磨时间增加，制备的多孔钛孔隙率下降，孔隙尺寸减小，压缩强度和弹性模量升高。球磨时间增加，多孔钛中TiO相量和多孔钛表面含氧量增加。
行星球磨5h制备不同Ag含量（1wt%、3wt%、5wt%）的Ti-Ag混合粉平均粒径2.08～2.13μm，体积比表面积3.37～3.46m~2/mm~3。添加少量（1～5wt%）Ag有利于细化混合钛粉粒径，但细化效果较弱。Ti-Ag混合粉末由α-Ti钛颗粒和均匀分布的单质Ag颗粒组成，球磨过程没有发生物相变化，仅形成片状的机械混合结构的Ti-Ag复合体。多孔Ti-Ag合金材料的孔隙大小350±150μm，孔隙率57.8～59.5%，物相组成为α-Ti和TiO，抗压强度27.9～32.8MPa，弹性模量1.2～1.5GPa。Ag含量增加，多孔Ti-Ag合金孔隙率下降，压缩强度和弹性模量升高。
行星球磨球磨5h制备不同Si含量（1wt%、3wt%、5wt%）Ti-Si混合粉，平均粒径1.94～2.11μm，体积比表面积3.40～3.69m~2/mm~3。添加少量（1～5wt%）Si有利于细化混合粉粒径，但细化效果较弱。Ti-Si混合粉末由α-Ti钛颗粒和均匀分布的单质Si颗粒组成，球磨过程没有发生物相变化，仅形成片状的机械混合结构的Ti-Si复合体。多孔Ti-Si合金材料的孔隙大小300±200μm，孔隙率46.2～55.8%，物相结构为α-Ti、Ti_3Si_5和TiO，抗压强度35.9～58.2MPa，弹性模量1.6～2.0GPa。Si含量增加，多孔Ti-Si合金孔隙率下降，压缩强度和弹性模量升高。
多孔钛由于孔隙的存在而降低了弹性模量，达到与骨组织弹性模量的匹配，但同时也造成了力学性能的显著下降。本文实验结果表明，增加钛粉球磨时间可以提高多孔钛的力学性能，满足人体骨替代材料的孔隙和力学性能要求，但由于钛颗粒表面能的增加，容易引入过多的杂质。合金元素Ag的引入可提升多孔钛基材料的力学性能，但易造成多孔钛基材料孔壁出现微孔，从而对多孔钛基材料力学性能改善作用有限。合金元素Si的引入可以显著提高多孔钛基材料的力学性能，通过与Ti发生强烈的扩散反应，可有效地促进钛粉的烧结过程。
碱处理后在多孔钛基材料表面获得微纳米网络结构的活化层，提高了多孔钛基材料磷灰石形成能力。模拟体液浸泡实验结果表明，钛粉末球磨时间增加，制备的多孔钛碱处理后表面羟基磷灰石形核能力升高。Ag含量增加，碱处理后多孔Ti-Ag合金材料表面羟基磷灰石形核能力降低。Si含量增加，碱处理后多孔Ti-Si合金材料表面羟基磷灰石形核能力增强。
细胞毒性实验结果表明：多孔钛、多孔Ti-Ag合金、多孔Ti-Si合金材料的细胞毒性评价均为1级。Ag和Si的加入没有恶化多孔钛的的细胞毒性。碱处理对多孔钛细胞毒性基本没有影响，对多孔Ti-Ag合金材料和多孔Ti-Si合金材料的细胞毒性产生的影响也很小。
Porous Ti-based metallic materials were fabricated by powder metallurgy. The effects ofpowder metallurgy process and addition of Ag, Si element on the microstructure, mechanicalproperties, biological activity, biological safety of the Ti-based metallic materials, weresystematically investigated. The powders of titanium, Ti-Ag mixed powder and Ti-Si mixedpowders were obtained by planet milling. With urea particles as the space-holder, the porousTi-based metallic materials were sintered at high temperature under Ar atmosphere. Alkalitreatment was introduced to modificate the surface activation of the porous Ti-based metallicmaterials. The apatite-inducing ability was evaluated by simulation body fluid (SBF)immersion test. The particle sizes, microstructure of powders were investigated by scanningelectron microscope (SEM), X-ray diffraction (XRD), laser particle size analyzer. Themechanical properties of porous Ti-based metallic materials were revealed by compressiontest. porosity characteristics, microstructure of prous Ti-based metallic materials before andafter alkali treatment, as well as the apatite growth after soaking in the SBF, were investigatedby scanning electron microscope (SEM), X-ray diffraction (XRD), X-ray photoelectronspectroscopy (XPS), Fourier transform infrared spectrum (FT-IR). The cytotoxicity of porousTi-based metallic materials was evaluated by the MTT method.
The average particale size and ratio of surface area to volume of the titanium powderswith different milling time (1h,5h,10h), varied respectively from29.25μm to1.84μm andfrom0.24m~2/mm~3to3.90m~2/mm~3. With the increase of the ball milling time, titaniumparticles were refined with less particle size and higher ratio of surface area, as well as thegrain size of titanium particle more finer. The efficiency of ball milling process would be thehighest for5hours’ balling time, and be lower with more ball milling time. Titanium powderswere consisted of α-Ti phase particles. The pore size, porosity, elastic modulus andcompressive strength of the porous titaniu materials fabricated by the different titaniumpowders, varied respectively from200μm to500μm, from46.5%to66.5%, from0.9GPa to1.9GPa, from15.7MPa to61.9MPa. With the increase of the ball milling time, the pore sizeand the porosity of the porous titanium mateials decrease, but the elastic modulus and thecompression strength increase. Porous titanium materials consist of α-Ti phase and TiO phase, with longer ball milling time of titanium powders more TiO formed and higher oxygencontent at the porous titanium surface.
The average particale size and ratio of surface area to volume of the Ti-Ag powders withdifferent Ag content (1wt%,3wt%,5wt%) after5hours’s milling time, variedrespectively2.08μm to2.13μm and from3.37m~2/mm~3to3.46m~2/mm~3. It was helpful torefining powder particle size that a small amount of Ag (1-5wt%) was added to the mixtureof titanium powders. The Ti-Ag powders were consisted of α-Ti phase particles and Agparticles with uniform distribution. No reaction happened during the balling milling process,but a lamellar complex mechanical mixing Ti-Ag structure was formed in the powders. Thepore size, porosity, elastic modulus and compressive strength of the porous Ti-Ag materialsfabricated by the different Ti-Ag powders, varied respectively from200μm to500μm, from57.8%to59.5%, from1.2GPa to1.5GPa, from27.9MPa to32.8MPa. Porous Ti-Agmaterials consist of α-Ti phase and TiO phase. With Ag content increasing, the pore size andthe porosity of the porous Ti-Ag materials decrease, but the elastic modulus and thecompression strength increase.
The average particale size and ratio of surface area to volume of the Ti-Si powders withdifferent Si content (1wt%,3wt%,5wt%) after5hours’s milling time, varied respectivelyfrom1.94μm to2.11μm and from3.40m~2/mm~3to3.69m~2/mm~3. It was helpful to refiningpowder particle size that a small amount of Si (1-5wt%) was added to the mixture oftitanium powders. The Ti-Si powders were consisted of α-Ti phase particles and Si particleswith uniform distribution. No reaction happened during the balling milling process, but alamellar complex mechanical mixing Ti-Si structure was formed in the powders. The poresize, porosity, elastic modulus and compressive strength of the porous Ti-Si materialsfabricated by the different Ti-Si powders, varied respectively from100μm to500μm, from46.2%to55.8%, from1.6GPa to2.0GPa, from35.9MPa to58.2MPa. Porous Ti-Simaterials consist of α-Ti phase, Ti3Si5phase and TiO phase. With Si content increasing, moreTi3Si5formed, the pore size and the porosity of the porous Ti-Si materials decrease, but theelastic modulus and the compression strength increase. Porous Ti-base material prepared inthis strudy, meet requirements of pore and mechanical performance from human body bonesubstitute materials.
The pores are intrudeced to reduce the elastic modulus of the porous Ti-based materials for matching with the elatic modulus of bone tissue, but also lead to significant reduction ofmechanical properties. There are large differences of porous Ti-based materials prepared bydiference methods and process parameters. The experiment results show that the mechanicalproperties of porous Ti-based materials prepared by the powders with longer milling timewould be better to meet requirements of mechanical performance from human body bonesubstitute materials, but more impurities brought to the porous Ti-based materials. Theaddition of Ag element could improve the mechanical properties of porous Ti-based materials,but it is limited for the presence of the microns wide hole in the cell wall. The addition of Sielement could improve significantly the mechanical properties of porous Ti-based materials,which effectively promoting the titanium powder sintering process through strong diffusionreaction.
After alkali treatment, activation layer of micro/nano network structure was formed onthe surface porous Ti-base materials which could improve the Ti-base materials biologicalactivity. It was indicated by the results of the simulated body fluids soaking experiment. Thenucleation ability of apatit on the porous titanium surface, fabricated by the titanium powderwith longer ball milling time, would be stronger. Thus, porous titanium fabricated by thetitanium powder with longer ball milling time would show better apatite-inducing ability.With Ag content increase, the nucleation ability of apatite on the porous Ti-Ag materialssurface would be weaker. Thus, addition of Ag would reduce the apatite-inducing ability ofporous Ti-based materials. With Si content increase, the nucleation ability of apatite on theporous Ti-Si materials surface would rise. Thus, addition of Si would increase theapatite-inducing ability of porous Ti-based materials.
The cytotoxicity experiment results show that the porous Ti-base materials prepared bypowder metallurgy have good biological safety. The cytotoxicity of porous titanium, porousTi-Ag and porous Ti-Si materials was below grade1. Alkali treatment has no evident effecton the porous titanium cytotoxicity, and a little negative effect on the Ti-Ag and porous Ti-Simaterials.
不同行星球磨时间（1h、5h、10h）制备的α-Ti钛粉末平均粒径29.25～1.84μm，体积比表面积0.24～3.90m~2/mm~3，钛粉末由α-Ti钛颗粒组成。球磨时间增加钛颗粒粒径减小，体积比表面积增加，钛晶粒逐渐细化；球磨时间5h时球磨工艺的细化效率最高。制备的多孔钛的孔隙大小350±150μm，孔隙率46.5～66.5%，制备的多孔钛物相结构为α-Ti+TiO，抗压强度15.7～61.9MPa，弹性模量0.9～1.9GPa。球磨时间增加，制备的多孔钛孔隙率下降，孔隙尺寸减小，压缩强度和弹性模量升高。球磨时间增加，多孔钛中TiO相量和多孔钛表面含氧量增加。
行星球磨5h制备不同Ag含量（1wt%、3wt%、5wt%）的Ti-Ag混合粉平均粒径2.08～2.13μm，体积比表面积3.37～3.46m~2/mm~3。添加少量（1～5wt%）Ag有利于细化混合钛粉粒径，但细化效果较弱。Ti-Ag混合粉末由α-Ti钛颗粒和均匀分布的单质Ag颗粒组成，球磨过程没有发生物相变化，仅形成片状的机械混合结构的Ti-Ag复合体。多孔Ti-Ag合金材料的孔隙大小350±150μm，孔隙率57.8～59.5%，物相组成为α-Ti和TiO，抗压强度27.9～32.8MPa，弹性模量1.2～1.5GPa。Ag含量增加，多孔Ti-Ag合金孔隙率下降，压缩强度和弹性模量升高。
行星球磨球磨5h制备不同Si含量（1wt%、3wt%、5wt%）Ti-Si混合粉，平均粒径1.94～2.11μm，体积比表面积3.40～3.69m~2/mm~3。添加少量（1～5wt%）Si有利于细化混合粉粒径，但细化效果较弱。Ti-Si混合粉末由α-Ti钛颗粒和均匀分布的单质Si颗粒组成，球磨过程没有发生物相变化，仅形成片状的机械混合结构的Ti-Si复合体。多孔Ti-Si合金材料的孔隙大小300±200μm，孔隙率46.2～55.8%，物相结构为α-Ti、Ti_3Si_5和TiO，抗压强度35.9～58.2MPa，弹性模量1.6～2.0GPa。Si含量增加，多孔Ti-Si合金孔隙率下降，压缩强度和弹性模量升高。
多孔钛由于孔隙的存在而降低了弹性模量，达到与骨组织弹性模量的匹配，但同时也造成了力学性能的显著下降。本文实验结果表明，增加钛粉球磨时间可以提高多孔钛的力学性能，满足人体骨替代材料的孔隙和力学性能要求，但由于钛颗粒表面能的增加，容易引入过多的杂质。合金元素Ag的引入可提升多孔钛基材料的力学性能，但易造成多孔钛基材料孔壁出现微孔，从而对多孔钛基材料力学性能改善作用有限。合金元素Si的引入可以显著提高多孔钛基材料的力学性能，通过与Ti发生强烈的扩散反应，可有效地促进钛粉的烧结过程。
碱处理后在多孔钛基材料表面获得微纳米网络结构的活化层，提高了多孔钛基材料磷灰石形成能力。模拟体液浸泡实验结果表明，钛粉末球磨时间增加，制备的多孔钛碱处理后表面羟基磷灰石形核能力升高。Ag含量增加，碱处理后多孔Ti-Ag合金材料表面羟基磷灰石形核能力降低。Si含量增加，碱处理后多孔Ti-Si合金材料表面羟基磷灰石形核能力增强。
细胞毒性实验结果表明：多孔钛、多孔Ti-Ag合金、多孔Ti-Si合金材料的细胞毒性评价均为1级。Ag和Si的加入没有恶化多孔钛的的细胞毒性。碱处理对多孔钛细胞毒性基本没有影响，对多孔Ti-Ag合金材料和多孔Ti-Si合金材料的细胞毒性产生的影响也很小。
Porous Ti-based metallic materials were fabricated by powder metallurgy. The effects ofpowder metallurgy process and addition of Ag, Si element on the microstructure, mechanicalproperties, biological activity, biological safety of the Ti-based metallic materials, weresystematically investigated. The powders of titanium, Ti-Ag mixed powder and Ti-Si mixedpowders were obtained by planet milling. With urea particles as the space-holder, the porousTi-based metallic materials were sintered at high temperature under Ar atmosphere. Alkalitreatment was introduced to modificate the surface activation of the porous Ti-based metallicmaterials. The apatite-inducing ability was evaluated by simulation body fluid (SBF)immersion test. The particle sizes, microstructure of powders were investigated by scanningelectron microscope (SEM), X-ray diffraction (XRD), laser particle size analyzer. Themechanical properties of porous Ti-based metallic materials were revealed by compressiontest. porosity characteristics, microstructure of prous Ti-based metallic materials before andafter alkali treatment, as well as the apatite growth after soaking in the SBF, were investigatedby scanning electron microscope (SEM), X-ray diffraction (XRD), X-ray photoelectronspectroscopy (XPS), Fourier transform infrared spectrum (FT-IR). The cytotoxicity of porousTi-based metallic materials was evaluated by the MTT method.
The average particale size and ratio of surface area to volume of the titanium powderswith different milling time (1h,5h,10h), varied respectively from29.25μm to1.84μm andfrom0.24m~2/mm~3to3.90m~2/mm~3. With the increase of the ball milling time, titaniumparticles were refined with less particle size and higher ratio of surface area, as well as thegrain size of titanium particle more finer. The efficiency of ball milling process would be thehighest for5hours’ balling time, and be lower with more ball milling time. Titanium powderswere consisted of α-Ti phase particles. The pore size, porosity, elastic modulus andcompressive strength of the porous titaniu materials fabricated by the different titaniumpowders, varied respectively from200μm to500μm, from46.5%to66.5%, from0.9GPa to1.9GPa, from15.7MPa to61.9MPa. With the increase of the ball milling time, the pore sizeand the porosity of the porous titanium mateials decrease, but the elastic modulus and thecompression strength increase. Porous titanium materials consist of α-Ti phase and TiO phase, with longer ball milling time of titanium powders more TiO formed and higher oxygencontent at the porous titanium surface.
The average particale size and ratio of surface area to volume of the Ti-Ag powders withdifferent Ag content (1wt%,3wt%,5wt%) after5hours’s milling time, variedrespectively2.08μm to2.13μm and from3.37m~2/mm~3to3.46m~2/mm~3. It was helpful torefining powder particle size that a small amount of Ag (1-5wt%) was added to the mixtureof titanium powders. The Ti-Ag powders were consisted of α-Ti phase particles and Agparticles with uniform distribution. No reaction happened during the balling milling process,but a lamellar complex mechanical mixing Ti-Ag structure was formed in the powders. Thepore size, porosity, elastic modulus and compressive strength of the porous Ti-Ag materialsfabricated by the different Ti-Ag powders, varied respectively from200μm to500μm, from57.8%to59.5%, from1.2GPa to1.5GPa, from27.9MPa to32.8MPa. Porous Ti-Agmaterials consist of α-Ti phase and TiO phase. With Ag content increasing, the pore size andthe porosity of the porous Ti-Ag materials decrease, but the elastic modulus and thecompression strength increase.
The average particale size and ratio of surface area to volume of the Ti-Si powders withdifferent Si content (1wt%,3wt%,5wt%) after5hours’s milling time, varied respectivelyfrom1.94μm to2.11μm and from3.40m~2/mm~3to3.69m~2/mm~3. It was helpful to refiningpowder particle size that a small amount of Si (1-5wt%) was added to the mixture oftitanium powders. The Ti-Si powders were consisted of α-Ti phase particles and Si particleswith uniform distribution. No reaction happened during the balling milling process, but alamellar complex mechanical mixing Ti-Si structure was formed in the powders. The poresize, porosity, elastic modulus and compressive strength of the porous Ti-Si materialsfabricated by the different Ti-Si powders, varied respectively from100μm to500μm, from46.2%to55.8%, from1.6GPa to2.0GPa, from35.9MPa to58.2MPa. Porous Ti-Simaterials consist of α-Ti phase, Ti3Si5phase and TiO phase. With Si content increasing, moreTi3Si5formed, the pore size and the porosity of the porous Ti-Si materials decrease, but theelastic modulus and the compression strength increase. Porous Ti-base material prepared inthis strudy, meet requirements of pore and mechanical performance from human body bonesubstitute materials.
The pores are intrudeced to reduce the elastic modulus of the porous Ti-based materials for matching with the elatic modulus of bone tissue, but also lead to significant reduction ofmechanical properties. There are large differences of porous Ti-based materials prepared bydiference methods and process parameters. The experiment results show that the mechanicalproperties of porous Ti-based materials prepared by the powders with longer milling timewould be better to meet requirements of mechanical performance from human body bonesubstitute materials, but more impurities brought to the porous Ti-based materials. Theaddition of Ag element could improve the mechanical properties of porous Ti-based materials,but it is limited for the presence of the microns wide hole in the cell wall. The addition of Sielement could improve significantly the mechanical properties of porous Ti-based materials,which effectively promoting the titanium powder sintering process through strong diffusionreaction.
After alkali treatment, activation layer of micro/nano network structure was formed onthe surface porous Ti-base materials which could improve the Ti-base materials biologicalactivity. It was indicated by the results of the simulated body fluids soaking experiment. Thenucleation ability of apatit on the porous titanium surface, fabricated by the titanium powderwith longer ball milling time, would be stronger. Thus, porous titanium fabricated by thetitanium powder with longer ball milling time would show better apatite-inducing ability.With Ag content increase, the nucleation ability of apatite on the porous Ti-Ag materialssurface would be weaker. Thus, addition of Ag would reduce the apatite-inducing ability ofporous Ti-based materials. With Si content increase, the nucleation ability of apatite on theporous Ti-Si materials surface would rise. Thus, addition of Si would increase theapatite-inducing ability of porous Ti-based materials.
The cytotoxicity experiment results show that the porous Ti-base materials prepared bypowder metallurgy have good biological safety. The cytotoxicity of porous titanium, porousTi-Ag and porous Ti-Si materials was below grade1. Alkali treatment has no evident effecton the porous titanium cytotoxicity, and a little negative effect on the Ti-Ag and porous Ti-Simaterials.
引文
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