多孔Ti-24Nb-4Zr合金孔隙特征及性能的研究
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摘要
本文以设计和研究新型医用多孔钛合金为目标，通过Mo当量设计材料的元素比例，采用高真空烧结炉和氩气气氛管式炉烧结多孔Ti-24Nb-4Zr合金，通过金相显微镜、SEM、XRD、三点弯曲试验、压缩测试、电化学测试测定合金孔隙率，分析孔隙形貌和试样力学性能，以及多孔合金的电化学性能。
通过元素粉末冶金的方法制备的多孔Ti-24Nb-4Zr合金为亚稳定β型钛合金，并且随着造孔剂NH_4HCO_3添加量的增加，合金中α相所占比例增大。造孔剂碳酸氢铵的添加能有效改变烧结样品的孔隙率和孔径大小。孔隙率与造孔剂NH_4HCO_3添加量呈线性变化趋势，随着造孔剂添加量的增加，孔隙的平均孔径明显增大，但它对孔隙的圆度和最大孔径影响不是很大。试样孔隙内壁有明显的微孔，尺寸远小于普通孔隙尺寸，可见孔隙并不可能是完全封闭的。造孔剂NH_4HCO_3的添加能有效改变烧结产物的孔隙率和孔径大小，进而来影响其力学性能。随着孔隙率的升高，合金的杨氏模量、抗弯强度都明显下降，呈线性变化，因此可以通过设计添加不同的造孔剂来得到不同的力学性能要求的多孔钛合金。添加20wt.%NH_4HCO_3的多孔Ti-24Nb-4Zr合金弹性模量为3.3GPa，屈服强度为172MPa，基本符合医用植入材料的要求。多孔Ti-24Nb-4Zr合金的断裂为穿晶解理型的脆性断裂。由试样宏观断裂照片以及压缩试验中应力-应变曲线可以看出，试样表现出明显的斜45°方向的滑移失效，从应力应变曲线上看与一般的脆性断裂又不相同，因此多孔Ti-24Nb-4Zr合金的断裂机理是脆性断裂与塑性断裂相结合。
试样在不同的烧结温度、烧结时间、压制压力条件下，最终的烧结产物的物相组成没有明显区别，确定为亚稳定β相晶体结构。随着烧结温度的升高，试样的密度呈明显下降趋势，与之对应的开孔率显著上升，材料的孔隙特征中孔隙孔径下降，圆度上升，同时由于孔隙特征的变化，压缩力学性能出现明显对应变化，压缩弹性模量及抗压强度都呈增长趋势。随着烧结时间的延长，试样密度有一定的下降趋势，同时开孔率对应上升，材料的孔隙特征中孔隙孔径下降，圆度上升，压缩力性与孔隙特征对应变化，压缩弹性模量有一定增长趋势。压制压力对于试样的影响在实验中未出现明显影响，其规律不具有普遍性，表明在90MPa到130MPa的冷压环境下，压制压力对最后的制品影响不大。
四种材料具有相似的腐蚀电位，且制备的多孔钛合金所具有的腐蚀电位不高于其他三种材料，表明其具有较低的腐蚀倾向。多孔TNZ合金的阳极极化曲线中都伴随着钝化现象，在pH值为7.4的NaCl溶液中其维钝电流密度为3.4μA，击穿电位在1.2V左右，与参比材料相一致，在pH值为7.4的Hanks溶液中其维钝电流密度为4.4μA，击穿电位在0.6V左右，相比于参比材料较低，因此更容易产生过钝化。而且多孔TNZ合金并没有二次钝化现象，因此在较高的电压下其腐蚀速率较快。通过测试电化学阻抗谱及拟合分析表明多孔合金、纯Ti和Ti64合金的腐蚀体系的等效电路均为R(QR)模型。多孔合金的膜的阻抗在酸性环境中略低于其他三种材料。总之，通过相关的电化学测试，对制备的多孔钛合金进行耐蚀性评价，表明多孔合金具有较高的耐蚀性，能够满足生物医用的要求。
The purpose of this paper was to design and study biomedical porous titaniumalloy. The elements composition of this porous titanium alloy was designed by meansof Mo equivalent amount and it was prepared by high vacuum sintering furnace andargon t ube f urnace. The por osity, m orphology, m echanical pr operties a ndelectrochemical properties of this porous alloy were analyzed by optical microscope,SEM, XRD, tri-point bending test, compression test and electrochemical tests.
The porous Ti-24Nb-4Zr alloy prepared by metal powder metallurgy method wasmetastable β titanium alloy. With the addition of more NH_4HCO_3powder, the αpercentage increased a ccordingly. The a ddition of f orming a gent c ould effectivelyincrease the porosity and pore diameter. With the addition of more forming agent, theporosity increased linearly an d t he av erage p ore d iameter i ncreased su bstantiallywhile little influence was observed to pore roundness and maximum diameter. Theinner wall of pores possessed micro pores which were far smaller than average poreswhich means those pores were not completely close. The addition of NH_4HCO_3couldinfluence mechanical properties of the porous alloy by changing its porosity and porediameter. A s t he porosity increases, t he Y oung’s m odulus and be nding s trengthdecreases linearly. This means that porous titanium alloys with different mechanicalproperties could be prepared by addition of different amount of forming agent. PorousTi-24Nb-4Zr alloy was prepared by adding20wt.%NH_4HCO_3, and it possessed anelastic m odulus of3.3G Pa a nd a yi eld s trength of172M Pa w hich m eet t herequirements of bi omedical i mplant m aterials. T he f ractography of por ousTi-24Nb-4Zr a lloy exhibited b rittle f racture w ith tra nsgranular c leavagecharacteristics. Ju dging f rom t he m acro f ractography a nd s tress-strain c urve ofimpression test, the samples showed evidently slip failure with45°orientation and itwas different from ordinary brittle facture which means that the fracture mechanismwas a mixture of brittle fracture and plastic fracture.
The phase composition of final sintering products was metastable β phase whichshowed no distinct different when the samples were sintered with different sinteringtemperature and time as w ell as pressing pressure. When the sintering temperatureincreases, the density of samples and pore diameter decreases distinctively while theporosity and pore roundness increases sharply. Meanwhile as the pore characteristics changing, the c ompression m echanical p roperties c hange a ccordingly: t hecompression elastic modulus and compression strength increases. When the sinteringtime increases, the density of samples and pore diameter decreases slowly while theporosity and pore roundness increases, and the compression elastic modulus showsthe trend of increasing. Compression stress shows no obvious influence to the samples.The tests show that cold press with pressure of90M Pa to130M Pa exhibits littleinfluence to the final sintering samples.
The four materials exhibits similar corrosion potential and that of the poroustitanium a lloy w as lo wer th an th e o ther th ree m aterials which means t he p oroustitanium alloy possesses lower corrosion tendency. The anodic polarization curves ofporous TNZ alloys showed that passivation occurred during the tests. The passivecurrent density was3.4μA and breakdown potential was1.2V in NaCl solution withpH value of7.4which was t he same with r eference material; the passive currentdensity was4.4μA and breakdown potential was0.6V in Hanks solution with pHvalue of7.4which was lower than reference material and means it is easier to overdeactivated. H owever, por ous T NZ a lloy s howed no s econdary pa ssivation w hichmeans that the corrosion velocity under high voltage is much faster than referencematerial. According to electrochemical impedance spectroscopy and fitting analysis,the equivalent circuits of corrosion systems of porous TNZ alloy, pure Ti and TC4areall R(QR) types. The impedance of porous TNZ alloy oxidization film was a littlelower than the other three materials. In sum, corrosion resistant evaluation by relevantelectrochemical tests shows that porous TNZ alloy possesses high corrosion resistancewhich could meet the requirements of biomedical applications.
通过元素粉末冶金的方法制备的多孔Ti-24Nb-4Zr合金为亚稳定β型钛合金，并且随着造孔剂NH_4HCO_3添加量的增加，合金中α相所占比例增大。造孔剂碳酸氢铵的添加能有效改变烧结样品的孔隙率和孔径大小。孔隙率与造孔剂NH_4HCO_3添加量呈线性变化趋势，随着造孔剂添加量的增加，孔隙的平均孔径明显增大，但它对孔隙的圆度和最大孔径影响不是很大。试样孔隙内壁有明显的微孔，尺寸远小于普通孔隙尺寸，可见孔隙并不可能是完全封闭的。造孔剂NH_4HCO_3的添加能有效改变烧结产物的孔隙率和孔径大小，进而来影响其力学性能。随着孔隙率的升高，合金的杨氏模量、抗弯强度都明显下降，呈线性变化，因此可以通过设计添加不同的造孔剂来得到不同的力学性能要求的多孔钛合金。添加20wt.%NH_4HCO_3的多孔Ti-24Nb-4Zr合金弹性模量为3.3GPa，屈服强度为172MPa，基本符合医用植入材料的要求。多孔Ti-24Nb-4Zr合金的断裂为穿晶解理型的脆性断裂。由试样宏观断裂照片以及压缩试验中应力-应变曲线可以看出，试样表现出明显的斜45°方向的滑移失效，从应力应变曲线上看与一般的脆性断裂又不相同，因此多孔Ti-24Nb-4Zr合金的断裂机理是脆性断裂与塑性断裂相结合。
试样在不同的烧结温度、烧结时间、压制压力条件下，最终的烧结产物的物相组成没有明显区别，确定为亚稳定β相晶体结构。随着烧结温度的升高，试样的密度呈明显下降趋势，与之对应的开孔率显著上升，材料的孔隙特征中孔隙孔径下降，圆度上升，同时由于孔隙特征的变化，压缩力学性能出现明显对应变化，压缩弹性模量及抗压强度都呈增长趋势。随着烧结时间的延长，试样密度有一定的下降趋势，同时开孔率对应上升，材料的孔隙特征中孔隙孔径下降，圆度上升，压缩力性与孔隙特征对应变化，压缩弹性模量有一定增长趋势。压制压力对于试样的影响在实验中未出现明显影响，其规律不具有普遍性，表明在90MPa到130MPa的冷压环境下，压制压力对最后的制品影响不大。
四种材料具有相似的腐蚀电位，且制备的多孔钛合金所具有的腐蚀电位不高于其他三种材料，表明其具有较低的腐蚀倾向。多孔TNZ合金的阳极极化曲线中都伴随着钝化现象，在pH值为7.4的NaCl溶液中其维钝电流密度为3.4μA，击穿电位在1.2V左右，与参比材料相一致，在pH值为7.4的Hanks溶液中其维钝电流密度为4.4μA，击穿电位在0.6V左右，相比于参比材料较低，因此更容易产生过钝化。而且多孔TNZ合金并没有二次钝化现象，因此在较高的电压下其腐蚀速率较快。通过测试电化学阻抗谱及拟合分析表明多孔合金、纯Ti和Ti64合金的腐蚀体系的等效电路均为R(QR)模型。多孔合金的膜的阻抗在酸性环境中略低于其他三种材料。总之，通过相关的电化学测试，对制备的多孔钛合金进行耐蚀性评价，表明多孔合金具有较高的耐蚀性，能够满足生物医用的要求。
The purpose of this paper was to design and study biomedical porous titaniumalloy. The elements composition of this porous titanium alloy was designed by meansof Mo equivalent amount and it was prepared by high vacuum sintering furnace andargon t ube f urnace. The por osity, m orphology, m echanical pr operties a ndelectrochemical properties of this porous alloy were analyzed by optical microscope,SEM, XRD, tri-point bending test, compression test and electrochemical tests.
The porous Ti-24Nb-4Zr alloy prepared by metal powder metallurgy method wasmetastable β titanium alloy. With the addition of more NH_4HCO_3powder, the αpercentage increased a ccordingly. The a ddition of f orming a gent c ould effectivelyincrease the porosity and pore diameter. With the addition of more forming agent, theporosity increased linearly an d t he av erage p ore d iameter i ncreased su bstantiallywhile little influence was observed to pore roundness and maximum diameter. Theinner wall of pores possessed micro pores which were far smaller than average poreswhich means those pores were not completely close. The addition of NH_4HCO_3couldinfluence mechanical properties of the porous alloy by changing its porosity and porediameter. A s t he porosity increases, t he Y oung’s m odulus and be nding s trengthdecreases linearly. This means that porous titanium alloys with different mechanicalproperties could be prepared by addition of different amount of forming agent. PorousTi-24Nb-4Zr alloy was prepared by adding20wt.%NH_4HCO_3, and it possessed anelastic m odulus of3.3G Pa a nd a yi eld s trength of172M Pa w hich m eet t herequirements of bi omedical i mplant m aterials. T he f ractography of por ousTi-24Nb-4Zr a lloy exhibited b rittle f racture w ith tra nsgranular c leavagecharacteristics. Ju dging f rom t he m acro f ractography a nd s tress-strain c urve ofimpression test, the samples showed evidently slip failure with45°orientation and itwas different from ordinary brittle facture which means that the fracture mechanismwas a mixture of brittle fracture and plastic fracture.
The phase composition of final sintering products was metastable β phase whichshowed no distinct different when the samples were sintered with different sinteringtemperature and time as w ell as pressing pressure. When the sintering temperatureincreases, the density of samples and pore diameter decreases distinctively while theporosity and pore roundness increases sharply. Meanwhile as the pore characteristics changing, the c ompression m echanical p roperties c hange a ccordingly: t hecompression elastic modulus and compression strength increases. When the sinteringtime increases, the density of samples and pore diameter decreases slowly while theporosity and pore roundness increases, and the compression elastic modulus showsthe trend of increasing. Compression stress shows no obvious influence to the samples.The tests show that cold press with pressure of90M Pa to130M Pa exhibits littleinfluence to the final sintering samples.
The four materials exhibits similar corrosion potential and that of the poroustitanium a lloy w as lo wer th an th e o ther th ree m aterials which means t he p oroustitanium alloy possesses lower corrosion tendency. The anodic polarization curves ofporous TNZ alloys showed that passivation occurred during the tests. The passivecurrent density was3.4μA and breakdown potential was1.2V in NaCl solution withpH value of7.4which was t he same with r eference material; the passive currentdensity was4.4μA and breakdown potential was0.6V in Hanks solution with pHvalue of7.4which was lower than reference material and means it is easier to overdeactivated. H owever, por ous T NZ a lloy s howed no s econdary pa ssivation w hichmeans that the corrosion velocity under high voltage is much faster than referencematerial. According to electrochemical impedance spectroscopy and fitting analysis,the equivalent circuits of corrosion systems of porous TNZ alloy, pure Ti and TC4areall R(QR) types. The impedance of porous TNZ alloy oxidization film was a littlelower than the other three materials. In sum, corrosion resistant evaluation by relevantelectrochemical tests shows that porous TNZ alloy possesses high corrosion resistancewhich could meet the requirements of biomedical applications.
引文
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