镍钛合金表面银基复合镀层的制备与性能研究
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摘要
镍钛合金以其独特的形状记忆与超弹性、良好的生物相容性等成为独具特色的生物医用金属材料；而金属银具有很好的柔韧性和延展性，较好的化学稳定性，优异的导电性能，很强的杀菌能力。本论文的研究目的是在生物医用镍钛合金基体表面进行电镀银，以期改变镍钛合金在生物体内的医用功能，提高镍钛合金在生物体内的抗腐蚀能力；为推动镍钛合金在生物医学中的进一步应用，通过复合镀技术在其表面沉积Ag/PTFE复合镀层，提高了镀银层的耐腐蚀性能和耐磨性能；同时，采用该技术在镍钛合金表面制备Ag/TiO_2复合镀层，研究了复合镀层的耐腐蚀性能、血液相容性和抗菌性能。
本文首先优化了在镍钛合金表面电镀银的工艺，确定其电解液的基本组成及工艺条件为：磺基水杨酸120g/L，氢氧化钾10g/L，硝酸银30g/L，乙酸铵50g/L，氨水55ml/L，pH为9，搅拌速度为250r/min，镀液温度25°C，电流密度为0.4A/dm~2，电镀时间为1h。考察了电流密度和电镀时间对镀银层性能的影响。利用SEM、EDS、XRD等表征了镀层的表面形貌、组成及结构，同时采用开路电位-时间曲线、Tafel极化曲线、电化学交流阻抗法等手段对其耐腐蚀性能进行评价。镀银镍钛合金表面较平整，沉积速率较大，耐腐蚀性能较好。
在电镀银的基础上，往电解液中添加了表面活性剂包覆的PTFE粉末，制备了Ag/PTFE复合镀层。研究了三种类型表面活性剂及其复配制备的复合镀层的耐腐蚀性能，结果表明：添加非离子表面活性剂OP-10为1g/L时制备的复合镀层耐腐蚀性能最佳。在此基础上，研究电镀时间及PTFE的添加量对镀层性能的影响。结果表明：电镀时间为1h制备的镀层较均匀，镀液中PTFE含量的增加能使镀层结晶更加致密，晶粒细化，但PTFE含量过高，镀层中颗粒易聚集使晶粒粗大，镀层表面不均匀，镀液中PTFE的添加量为8g/L时获得的复合镀层的结晶最致密，在此条件下制备的复合镀层的耐腐蚀性能和耐磨性能均最佳。
为了提高镀银镍钛合金的耐腐蚀性能和生物相容性，采用表面活性剂包裹二氧化钛粉末加入、TiO_2粉末直接加入和TiO_2溶胶加入镀液三种方法，制备了Ag/TiO_2复合镀层。研究了表面活性剂种类及用量、TiO_2粉末的加入量、钛溶胶的加入量等因素对复合镀层的影响。采用表面活性剂包覆TiO_2粉末加入镀液的方法来制备Ag/TiO_2复合镀层，通过正交试验确定了较优的表面活性剂及TiO_2的添加量为：阴离子表面活性剂SDS含量为1g/L，TiO_2为30g/L，但Ag/TiO_2复合镀层的耐腐蚀性能不如银镀镍钛合金。采用直接加入TiO_2粉末法制备了Ag/TiO_2复合镀层，考察了镀液中TiO_2的添加量对镀层微观表面形貌和晶体组织结构的影响。随着镀液中TiO_2含量的增加镀层表面变得平坦，但TiO_2含量过高则出现大颗粒团聚，表面粗糙。镀液中TiO_2含量在50g/L时，复合镀层中TiO_2复合量最高、耐腐蚀性能最佳、Ag离子溶出量最少、血液相容性较好，镀层在Hank's溶液中的耐腐蚀性能较镀银镍钛合金好。采用TiO_2溶胶加入法制备Ag/TiO_2复合镀层，研究了溶胶加入量对镀层性能的影响，当TiO_2溶胶加入量为100ml/L、电镀时间为1h时，镀层表面最致密，镀层中TiO_2含量最大，大于直接加入法制备的镀层的复合量，同时复合镀层的耐腐蚀性能较直接加入法好。Ag/TiO_2复合镀层具有良好的抗菌性能。
Nickel-titanium alloy has become a very potential biomedical material for its uniqueshape memory, superelasticity and good biocompatibility. Metallic silver has a goodflexibility and scalability, good chemical stability, excellent electrical conductivity and astrong bactericidal capability. The purpose of this thesis is to electroplate silver on the surfaceof biomedical nickel-titanium alloy substrate, in order to change the biocompatibility ofnickel-titanium alloy in vivo and to improve the corrosion resistance of nickel-titanium alloy;to promote the further application of the nickel-titanium alloy in medicine, we improve thecorrosion resistance of Ag plating by composite depositing Ag/PTFE composite plating on thesurface of nickel-titanium alloy; meanwhile, to increase the corrosion property and frictionproperty of silver-plated layer by using the composite plating technology to deposit Ag/TiO_2composite plating on the surface of the nickel-titanium alloy, corrosion property, bloodcapatibility and antimicrobial property of Ag/TiO_2composite plating have been investigated.
First, this paper optimized the process of silver electroplating on the surface ofnickel-titanium alloy, determines the basic composition and process conditions of our silverplating solution which are as follows: sulfosalicylic acid120g/L, potassium hydroxide10g/L,silver nitrate30g/L, ammonium acetate50g/L, and ammonia55ml/L；pH9, stirring speed250r/min, bath temperature25°C, current density0.4A/dm2, plating time1h. The effect ofplating time and current density on the coating properties is investigated. The morphology,composition and structure of coating surface are characterized by using SEM, EDS and XRD;while the open circuit potential-time curves, Tafel polarization curves and electrochemicalimpedance spectroscopy are used to evaluate corrosion resistance. The surface of Ag-coatedNiTi alloy is relatively smooth; the deposition rate is greater; the corrosion resistance is better.
Ag/PTFE composite plating is prepared by adding PTFE powder wrapped in surfactantsto the electrolyte on the basis of silver plating. The corrosion property of three types’surfactants and their mixed systems on the composite plating is studied, and the results showthat when added non-ionic surfactant OP-101g/L the corrosion resistance can be the best. Onthis basis, the effect of the PTFE addition and plating time on the properties of Ag/PTFEcomposite plating is investigated. The effect of the plating time and PTFE concentration onthe coating surface morphology and crystal structure is investigated. The results show thatwith1h plating time it can get a more uniform coating; the increases in PTFE concentrationcould make the crystalline grain of the coating refinement and more dense, but when the concentration of PTFE is too high, particles in the coating are easy to gather so that the grainswould be coarse, and coating surface is uneven. The most appropriate PTFE added in the bathis8g/L. The electrochemical and abrasive resistance tests show that the8g/L PTFEconcentration in the bath has the best coating corrosion resistance and abrasive resistance.
In order to improve the biocompatibility and corrosion property of the silver layer,Ag/TiO_2composite plating is prepared by using three methods which are adding TiO_2wrapped in the surfactant and then added to the bath, adding TiO_2powder directly and addingTiO_2sol to the plating solution. The effect of the adding amount of TiO_2powder, type andamount of surfactant, titanium sol dosage and other factors on the composite coatings hasbeen studied. Surfactant is used to coat TiO_2powder and then added to the bath to prepareAg/TiO_2composite coating. We design an orthogonal experiment to determine the optimumof the surfactant and TiO_2when adding TiO_2powder coated by surfactant to the bath toprepare Ag/TiO_2composite plating: anionic surfactant sodium dodecyl sulfate dose of1g/L,and TiO_230g/L. According to the analysis of the surface morphology and electrochemicalcorrosion results of prepared plating obtained by adding different surfactants in the bath, wefound the coating prepared with1g/L anionic surfactant in the bath has the best corrosionresistance. But the corrosion resistance of Ag/TiO_2composite plating is slightly bad. Theeffect of TiO_2addition in the bath on the micro-surface morphology and crystal organizationalstructure of the plating is studied, when added TiO_2powder directly to prepare nano Ag/TiO_2composite plating. As the TiO_2concentration in the bath increased, the plating surfaceflattened, however, when TiO_2concentration level is too high, large particles would aggregateand the surface would be rough. When the concentration of titanium dioxide particle inplating solution is50g/L, we can have the most abundant particles in the composite coatingand the corrosion resistance of the coating can be the best. Biological performance tests of thecomposite platings show that: resistance to ion release is the best when bath concentration is50g/L; all the prepared composite platings with different TiO_2concentration in the bath havegood blood compatibility. Ag/TiO_2composite coating is prepared by joining with TiO_2sol andthe effect of sol addition on the coating properties is studied. Coating surface is most dense;and TiO_2concentration in the coating is the largest when the amount TiO_2sol is100ml/L--theplating time is1hour--much larger than the composite amount in the plating prepared byadding directly. At the same time, the corrosion resistance of composite plating is better thanadded directly. The plating has good antimicrobial property.
本文首先优化了在镍钛合金表面电镀银的工艺，确定其电解液的基本组成及工艺条件为：磺基水杨酸120g/L，氢氧化钾10g/L，硝酸银30g/L，乙酸铵50g/L，氨水55ml/L，pH为9，搅拌速度为250r/min，镀液温度25°C，电流密度为0.4A/dm~2，电镀时间为1h。考察了电流密度和电镀时间对镀银层性能的影响。利用SEM、EDS、XRD等表征了镀层的表面形貌、组成及结构，同时采用开路电位-时间曲线、Tafel极化曲线、电化学交流阻抗法等手段对其耐腐蚀性能进行评价。镀银镍钛合金表面较平整，沉积速率较大，耐腐蚀性能较好。
在电镀银的基础上，往电解液中添加了表面活性剂包覆的PTFE粉末，制备了Ag/PTFE复合镀层。研究了三种类型表面活性剂及其复配制备的复合镀层的耐腐蚀性能，结果表明：添加非离子表面活性剂OP-10为1g/L时制备的复合镀层耐腐蚀性能最佳。在此基础上，研究电镀时间及PTFE的添加量对镀层性能的影响。结果表明：电镀时间为1h制备的镀层较均匀，镀液中PTFE含量的增加能使镀层结晶更加致密，晶粒细化，但PTFE含量过高，镀层中颗粒易聚集使晶粒粗大，镀层表面不均匀，镀液中PTFE的添加量为8g/L时获得的复合镀层的结晶最致密，在此条件下制备的复合镀层的耐腐蚀性能和耐磨性能均最佳。
为了提高镀银镍钛合金的耐腐蚀性能和生物相容性，采用表面活性剂包裹二氧化钛粉末加入、TiO_2粉末直接加入和TiO_2溶胶加入镀液三种方法，制备了Ag/TiO_2复合镀层。研究了表面活性剂种类及用量、TiO_2粉末的加入量、钛溶胶的加入量等因素对复合镀层的影响。采用表面活性剂包覆TiO_2粉末加入镀液的方法来制备Ag/TiO_2复合镀层，通过正交试验确定了较优的表面活性剂及TiO_2的添加量为：阴离子表面活性剂SDS含量为1g/L，TiO_2为30g/L，但Ag/TiO_2复合镀层的耐腐蚀性能不如银镀镍钛合金。采用直接加入TiO_2粉末法制备了Ag/TiO_2复合镀层，考察了镀液中TiO_2的添加量对镀层微观表面形貌和晶体组织结构的影响。随着镀液中TiO_2含量的增加镀层表面变得平坦，但TiO_2含量过高则出现大颗粒团聚，表面粗糙。镀液中TiO_2含量在50g/L时，复合镀层中TiO_2复合量最高、耐腐蚀性能最佳、Ag离子溶出量最少、血液相容性较好，镀层在Hank's溶液中的耐腐蚀性能较镀银镍钛合金好。采用TiO_2溶胶加入法制备Ag/TiO_2复合镀层，研究了溶胶加入量对镀层性能的影响，当TiO_2溶胶加入量为100ml/L、电镀时间为1h时，镀层表面最致密，镀层中TiO_2含量最大，大于直接加入法制备的镀层的复合量，同时复合镀层的耐腐蚀性能较直接加入法好。Ag/TiO_2复合镀层具有良好的抗菌性能。
Nickel-titanium alloy has become a very potential biomedical material for its uniqueshape memory, superelasticity and good biocompatibility. Metallic silver has a goodflexibility and scalability, good chemical stability, excellent electrical conductivity and astrong bactericidal capability. The purpose of this thesis is to electroplate silver on the surfaceof biomedical nickel-titanium alloy substrate, in order to change the biocompatibility ofnickel-titanium alloy in vivo and to improve the corrosion resistance of nickel-titanium alloy;to promote the further application of the nickel-titanium alloy in medicine, we improve thecorrosion resistance of Ag plating by composite depositing Ag/PTFE composite plating on thesurface of nickel-titanium alloy; meanwhile, to increase the corrosion property and frictionproperty of silver-plated layer by using the composite plating technology to deposit Ag/TiO_2composite plating on the surface of the nickel-titanium alloy, corrosion property, bloodcapatibility and antimicrobial property of Ag/TiO_2composite plating have been investigated.
First, this paper optimized the process of silver electroplating on the surface ofnickel-titanium alloy, determines the basic composition and process conditions of our silverplating solution which are as follows: sulfosalicylic acid120g/L, potassium hydroxide10g/L,silver nitrate30g/L, ammonium acetate50g/L, and ammonia55ml/L；pH9, stirring speed250r/min, bath temperature25°C, current density0.4A/dm2, plating time1h. The effect ofplating time and current density on the coating properties is investigated. The morphology,composition and structure of coating surface are characterized by using SEM, EDS and XRD;while the open circuit potential-time curves, Tafel polarization curves and electrochemicalimpedance spectroscopy are used to evaluate corrosion resistance. The surface of Ag-coatedNiTi alloy is relatively smooth; the deposition rate is greater; the corrosion resistance is better.
Ag/PTFE composite plating is prepared by adding PTFE powder wrapped in surfactantsto the electrolyte on the basis of silver plating. The corrosion property of three types’surfactants and their mixed systems on the composite plating is studied, and the results showthat when added non-ionic surfactant OP-101g/L the corrosion resistance can be the best. Onthis basis, the effect of the PTFE addition and plating time on the properties of Ag/PTFEcomposite plating is investigated. The effect of the plating time and PTFE concentration onthe coating surface morphology and crystal structure is investigated. The results show thatwith1h plating time it can get a more uniform coating; the increases in PTFE concentrationcould make the crystalline grain of the coating refinement and more dense, but when the concentration of PTFE is too high, particles in the coating are easy to gather so that the grainswould be coarse, and coating surface is uneven. The most appropriate PTFE added in the bathis8g/L. The electrochemical and abrasive resistance tests show that the8g/L PTFEconcentration in the bath has the best coating corrosion resistance and abrasive resistance.
In order to improve the biocompatibility and corrosion property of the silver layer,Ag/TiO_2composite plating is prepared by using three methods which are adding TiO_2wrapped in the surfactant and then added to the bath, adding TiO_2powder directly and addingTiO_2sol to the plating solution. The effect of the adding amount of TiO_2powder, type andamount of surfactant, titanium sol dosage and other factors on the composite coatings hasbeen studied. Surfactant is used to coat TiO_2powder and then added to the bath to prepareAg/TiO_2composite coating. We design an orthogonal experiment to determine the optimumof the surfactant and TiO_2when adding TiO_2powder coated by surfactant to the bath toprepare Ag/TiO_2composite plating: anionic surfactant sodium dodecyl sulfate dose of1g/L,and TiO_230g/L. According to the analysis of the surface morphology and electrochemicalcorrosion results of prepared plating obtained by adding different surfactants in the bath, wefound the coating prepared with1g/L anionic surfactant in the bath has the best corrosionresistance. But the corrosion resistance of Ag/TiO_2composite plating is slightly bad. Theeffect of TiO_2addition in the bath on the micro-surface morphology and crystal organizationalstructure of the plating is studied, when added TiO_2powder directly to prepare nano Ag/TiO_2composite plating. As the TiO_2concentration in the bath increased, the plating surfaceflattened, however, when TiO_2concentration level is too high, large particles would aggregateand the surface would be rough. When the concentration of titanium dioxide particle inplating solution is50g/L, we can have the most abundant particles in the composite coatingand the corrosion resistance of the coating can be the best. Biological performance tests of thecomposite platings show that: resistance to ion release is the best when bath concentration is50g/L; all the prepared composite platings with different TiO_2concentration in the bath havegood blood compatibility. Ag/TiO_2composite coating is prepared by joining with TiO_2sol andthe effect of sol addition on the coating properties is studied. Coating surface is most dense;and TiO_2concentration in the coating is the largest when the amount TiO_2sol is100ml/L--theplating time is1hour--much larger than the composite amount in the plating prepared byadding directly. At the same time, the corrosion resistance of composite plating is better thanadded directly. The plating has good antimicrobial property.
引文
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