Ti-Ag基合金的组织结构与生物性能
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摘要
近年来,钛及钛合金由于其优异的抗腐蚀性与良好的生物安全性在医用领域得到了越来越广泛的应用,目前临床应用的主要有纯钛、Ti-6Al-4V合金、Ti-Ni合金等。但在临床使用中,钛及钛合金也暴露出一定的问题,例如纯钛的强度、耐磨性不足,Ti-6Al-4V合金含有元素Al、V,在植入人体后会持续溶出有毒的Al离子、V离子,对人体造成不利影响。同时,钛及钛合金暴露于含有氟离子的生理溶液中时,由于其表面钝化膜遭到破坏,抗腐蚀性下降明显。
针对以上问题,本论文用合金化的方法,选用Ag作为钛的第二组元来提高钛的强度、耐磨性与抗腐蚀性。此外,添加Fe、Ni等第三组元,进一步改善合金的各项生物学性能。采用光学组织观察、X射线衍射分析、透射电子显微观察、扫描电子显微观察、拉伸、压缩实验、摩擦实验、电化学实验、表面X射线光电子能谱分析、离子溶出测试、细胞毒性测试和溶血测试研究了Ti-Ag系合金、Ti-Ag-Fe系合金及Ti-Ni-Ag系合金的微观组织、相组成、力学性能、抗腐蚀性及生物相容性,主要考察合金元素(Ag、Fe、Ni)、处理工艺和使用环境对Ti-Ag基合金生物性能的影响规律。此外,还考察了Ti-Ni-Ag合金的抑菌性能。论文取得了如下研究成果：
设计并制备了Ti-Ag二元合金,通过固溶强化等机制提高了合金的强度与耐磨性；热-机械处理工艺对Ti-Ag合金的力学性能影响很大,950℃固溶处理的合金力学性能匹配最好,950℃固溶处理的Ti-20Ag合金拉伸屈服强度约620 MPa,延伸率10%。由于纯银较高的腐蚀电位,Ag的加入明显促进了钛的钝化,提高了合金的抗腐蚀性。同时,对Ti-Ag合金进行了进一步的热氧化处理,热氧化处理Ti-Ag合金的抗腐蚀性明显提高。
根据钛合金中合金元素对合金力学性能影响的规律,利用Fe元素生物安全性好、β稳定能力强等特点,在Ti-Ag二元合金的基础上,设计并制备了Ti-Ag-Fe三元合金。Fe元素能明显的稳定Ti-Ag合金的β相,当Fe元素含量达到5wt%时可以得到全β相的组织。Ti-5Ag-xFe合金在强度、耐磨性大幅度提高的同时,兼具良好的抗腐蚀性与生物安全性,Ti-5Ag-2.5Fe合金由于其合适的合金元素含量、双相组织结构,拉伸屈服强度约870MPa,延伸率约7%,强度与韧性的匹配最好,可能作为高强度牙科钛合金而得到应用。
采用铜坩埚冷却的真空非自耗熔炼炉制备了Ti-Ni-Ag块体合金,通过急冷制备工艺,解决了高Ag含量的Ti-Ni-Ag块体不易制备的问题,制备出的Ti-Ni-Ag块体合金中存在弥散分布的Ag单质颗粒。Ti-Ni-Ag合金的力学性能、抗腐蚀性、细胞毒性与Ti-Ni二元合金相当。对制备的Ti-Ni-Ag合金进行了抑菌性能评价,同Ti-Ni合金相比,Ti-Ni-Ag合金表现出了明显的抑制细菌黏附的能力。结合合金的微观组织结果、表面分析结果和离子溶出结果,可以认为在Ti-Ni-Ag合金与体液接触时,其中的金属Ag与体液反应,变为离子态的Ag进入体液。而Ag离子具有良好的广谱抗菌特性,在几微克/升的浓度下就能起到明显的抗菌特性,可以穿透细菌的细胞膜,同细菌的DNA起反应,从而导致细菌死亡。
Titanium and its alloys have been widely used as biomaterials due to its light weight, high corrosion resistance and excellent biocompatibility. Commercially pure Ti and Ti-6Al-4V alloy are most commonly used titanium materials for implant applications. However, the insufficient strength and poor wear resistance of unalloyed titanium was often complained. Furthermore, more and more concerns are raised due to the toxicity of aluminum and vanadium released from Ti-6A1-4V alloy. In addition, it has been reported that corrosion resistance of titanium and its alloys may be significantly reduced in environments containing fluoride ions, and fluoride ions often exist in oral environments.
In this study, the optical microsturcture, phase constitution, mechanical properties, corrosion resistance, and biocompatilbity of the three series of Ti-Ag, Ti-Ag-Fe, and Ti-Ni-Ag alloys are systematically investigated. The influence of the alloying elements and the heat treatment on these properties is revealed by optical microsope, X-ray diffrictation, scanning electron microscope (SEM), Transmission electron microscope (TEM), tensile and compression test, wear test, electrochemical measurments and biocompatibility evaluations. Moreover, the antibacterial activity of Ti-Ni-Ag alloys is investigated.
Ti-Ag alloys consist of single a phase at room temperature. Ti-Ag alloys show slightly higer strength and hardness values than that of CP Ti. Moreover, the wear resistance of Ti-Ag could be largely improved. The lower corrosion current and higher open circuit potential indicate that Ti-Ag alloys have better corrosion resistance in artificial saliva solution with and without NaF. They are corrosion-resistant metal and exhibit very low ion release amount in 1% lactic acid solution and 0.1 mol/1 H2O2+0.9% NaCl+de-ionized water solution. In vitro cytotoxicity tests indicate that these alloys do not present any cytotoxic effect and exhibite as excellent biocompatibility as CP Ti. The homogeneous single-phase nature of the Ti-Ag alloys leads to the formation of a uniform passive film which is able to separate the bulk of the alloy from an aggressive environment and, hence, is responsible for the low ion release rate and excellent cellular response.
Ti-5Ag-xFe alloys are prepared andβphase could be retained by Fe addition. Ti-5Ag-xFe alloys show much larger compression strength and hardness values than that of CP Ti. Moreover, the wear resistance of Ti-5Ag-xFe could be largely improved by Fe addition. They also exhibit similar or improved corrosion resistance compared to that of CP Ti. The excellent corrosion resistance and low ion release rate can be mainly attributed to the TiO2 film on the surface. The cytocompatibility tests show that Ti-5Ag-xFe alloys indicate similar cell viability than that of CP Ti. Therefore, Ti-5Ag-xFe alloys may be good candidate as dental materials because of their superior mechanical properties, excellent corrosion resistance, low ion release rate and good biocompatibility.
Ti-Ni-Ag ternarys alloy are successfully fabricated with arc-melting method with water cooling Cu bath. The Ag particles precipitated within the Ti-Ni alloy matrix, with the size ranging from several tens of nanometers to several micrometers. The tensile tests show that Ti-Ni-Ag alloy has higher strength than that of Ti-Ni binary alloy. Compared with Ti-Ni alloy, Ti-Ni-Ag alloy possesses similar corrosion resistance and cyto-biocompatibility. Moreover, Ti-Ni-Ag alloy exhibits reduced bacteria adhesion when compared with Ti-Ni binary alloy. The antibacterial effect is attributed to the release of Ag ions from the tiny Ag precipitates. Therefore Ti-Ni-Ag alloy is believed to be a functional biomaterial which combines antibacterial activity and shape memory effect, and is likely to broaden the range of the biomedical application of Ti-Ni alloy system.
针对以上问题,本论文用合金化的方法,选用Ag作为钛的第二组元来提高钛的强度、耐磨性与抗腐蚀性。此外,添加Fe、Ni等第三组元,进一步改善合金的各项生物学性能。采用光学组织观察、X射线衍射分析、透射电子显微观察、扫描电子显微观察、拉伸、压缩实验、摩擦实验、电化学实验、表面X射线光电子能谱分析、离子溶出测试、细胞毒性测试和溶血测试研究了Ti-Ag系合金、Ti-Ag-Fe系合金及Ti-Ni-Ag系合金的微观组织、相组成、力学性能、抗腐蚀性及生物相容性,主要考察合金元素(Ag、Fe、Ni)、处理工艺和使用环境对Ti-Ag基合金生物性能的影响规律。此外,还考察了Ti-Ni-Ag合金的抑菌性能。论文取得了如下研究成果：
设计并制备了Ti-Ag二元合金,通过固溶强化等机制提高了合金的强度与耐磨性；热-机械处理工艺对Ti-Ag合金的力学性能影响很大,950℃固溶处理的合金力学性能匹配最好,950℃固溶处理的Ti-20Ag合金拉伸屈服强度约620 MPa,延伸率10%。由于纯银较高的腐蚀电位,Ag的加入明显促进了钛的钝化,提高了合金的抗腐蚀性。同时,对Ti-Ag合金进行了进一步的热氧化处理,热氧化处理Ti-Ag合金的抗腐蚀性明显提高。
根据钛合金中合金元素对合金力学性能影响的规律,利用Fe元素生物安全性好、β稳定能力强等特点,在Ti-Ag二元合金的基础上,设计并制备了Ti-Ag-Fe三元合金。Fe元素能明显的稳定Ti-Ag合金的β相,当Fe元素含量达到5wt%时可以得到全β相的组织。Ti-5Ag-xFe合金在强度、耐磨性大幅度提高的同时,兼具良好的抗腐蚀性与生物安全性,Ti-5Ag-2.5Fe合金由于其合适的合金元素含量、双相组织结构,拉伸屈服强度约870MPa,延伸率约7%,强度与韧性的匹配最好,可能作为高强度牙科钛合金而得到应用。
采用铜坩埚冷却的真空非自耗熔炼炉制备了Ti-Ni-Ag块体合金,通过急冷制备工艺,解决了高Ag含量的Ti-Ni-Ag块体不易制备的问题,制备出的Ti-Ni-Ag块体合金中存在弥散分布的Ag单质颗粒。Ti-Ni-Ag合金的力学性能、抗腐蚀性、细胞毒性与Ti-Ni二元合金相当。对制备的Ti-Ni-Ag合金进行了抑菌性能评价,同Ti-Ni合金相比,Ti-Ni-Ag合金表现出了明显的抑制细菌黏附的能力。结合合金的微观组织结果、表面分析结果和离子溶出结果,可以认为在Ti-Ni-Ag合金与体液接触时,其中的金属Ag与体液反应,变为离子态的Ag进入体液。而Ag离子具有良好的广谱抗菌特性,在几微克/升的浓度下就能起到明显的抗菌特性,可以穿透细菌的细胞膜,同细菌的DNA起反应,从而导致细菌死亡。
Titanium and its alloys have been widely used as biomaterials due to its light weight, high corrosion resistance and excellent biocompatibility. Commercially pure Ti and Ti-6Al-4V alloy are most commonly used titanium materials for implant applications. However, the insufficient strength and poor wear resistance of unalloyed titanium was often complained. Furthermore, more and more concerns are raised due to the toxicity of aluminum and vanadium released from Ti-6A1-4V alloy. In addition, it has been reported that corrosion resistance of titanium and its alloys may be significantly reduced in environments containing fluoride ions, and fluoride ions often exist in oral environments.
In this study, the optical microsturcture, phase constitution, mechanical properties, corrosion resistance, and biocompatilbity of the three series of Ti-Ag, Ti-Ag-Fe, and Ti-Ni-Ag alloys are systematically investigated. The influence of the alloying elements and the heat treatment on these properties is revealed by optical microsope, X-ray diffrictation, scanning electron microscope (SEM), Transmission electron microscope (TEM), tensile and compression test, wear test, electrochemical measurments and biocompatibility evaluations. Moreover, the antibacterial activity of Ti-Ni-Ag alloys is investigated.
Ti-Ag alloys consist of single a phase at room temperature. Ti-Ag alloys show slightly higer strength and hardness values than that of CP Ti. Moreover, the wear resistance of Ti-Ag could be largely improved. The lower corrosion current and higher open circuit potential indicate that Ti-Ag alloys have better corrosion resistance in artificial saliva solution with and without NaF. They are corrosion-resistant metal and exhibit very low ion release amount in 1% lactic acid solution and 0.1 mol/1 H2O2+0.9% NaCl+de-ionized water solution. In vitro cytotoxicity tests indicate that these alloys do not present any cytotoxic effect and exhibite as excellent biocompatibility as CP Ti. The homogeneous single-phase nature of the Ti-Ag alloys leads to the formation of a uniform passive film which is able to separate the bulk of the alloy from an aggressive environment and, hence, is responsible for the low ion release rate and excellent cellular response.
Ti-5Ag-xFe alloys are prepared andβphase could be retained by Fe addition. Ti-5Ag-xFe alloys show much larger compression strength and hardness values than that of CP Ti. Moreover, the wear resistance of Ti-5Ag-xFe could be largely improved by Fe addition. They also exhibit similar or improved corrosion resistance compared to that of CP Ti. The excellent corrosion resistance and low ion release rate can be mainly attributed to the TiO2 film on the surface. The cytocompatibility tests show that Ti-5Ag-xFe alloys indicate similar cell viability than that of CP Ti. Therefore, Ti-5Ag-xFe alloys may be good candidate as dental materials because of their superior mechanical properties, excellent corrosion resistance, low ion release rate and good biocompatibility.
Ti-Ni-Ag ternarys alloy are successfully fabricated with arc-melting method with water cooling Cu bath. The Ag particles precipitated within the Ti-Ni alloy matrix, with the size ranging from several tens of nanometers to several micrometers. The tensile tests show that Ti-Ni-Ag alloy has higher strength than that of Ti-Ni binary alloy. Compared with Ti-Ni alloy, Ti-Ni-Ag alloy possesses similar corrosion resistance and cyto-biocompatibility. Moreover, Ti-Ni-Ag alloy exhibits reduced bacteria adhesion when compared with Ti-Ni binary alloy. The antibacterial effect is attributed to the release of Ag ions from the tiny Ag precipitates. Therefore Ti-Ni-Ag alloy is believed to be a functional biomaterial which combines antibacterial activity and shape memory effect, and is likely to broaden the range of the biomedical application of Ti-Ni alloy system.
引文
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