亚稳β型Ti-Nb-Ta-Zr-O合金的显微组织与性能
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摘要
2003年,斋藤等人研发出一组组分为Ti3(Ta+Nb+V) + (Zr、Hf) + O的新型多功能亚稳β钛合金。这组钛合金在室温下经过强变形后,不但同时具有高强度和低弹性模量,还具有超弹性、超塑性等诸多超级性能,是一种潜在的医用生物材料。斋藤等人认为这组亚稳β钛合金之所以具有这些优良性能,是因为它们具有一种特殊的塑性变形机制―无位错塑性变形机制。
本研究采用冷坩埚悬浮熔炼法制备了这组亚稳β钛合金的一种,其名义成分为Ti-23Nb-0.7Ta-2Zr-O (at.%, TNTZO),并系统研究了固溶态TNTZO合金在塑性变形后的显微组织及随后再结晶退火过程中的显微组织演变,分析了合金的变形机制,并考察了该合金的力学性能、物理性能和耐腐蚀性能。
研究结果表明:经过室温塑性变形后,TNTZO合金中β相保持稳定,没有应力诱发马氏体相变发生。经较大程度压缩变形后合金具有比较明显的<100>和<111>双织构。由于在冷旋锻过程中晶粒处于平面应变条件,因而经90%冷旋锻变形后, TNTZO合金的显微组织由大量平行于旋锻轴向的板条组织构成。这些板条扭曲并相互环绕,在垂直旋锻轴向的截面上形成由细小纤维状组织交织而成的大理石花纹状组织,同时合金中产生强烈的<110>丝织构。TEM观察结果表明变形后TNTZO合金中出现了高密度的位错聚集。因此,TNTZO合金仍然通过传统的位错滑移机制进行塑性变形,而不是通过所谓的无位错机制进行塑性变形。TNTZO合金的再结晶动力学曲线具有典型的“S”曲线特征,表明TNTZO合金
的再结晶是典型的形核长大过程。经90%冷旋锻变形的TNTZO合金的再结晶激活能约为180 kJ/mol。TEM观察结果表明TNTZO合金的回复通过多边形化机制进行,再结晶通过形核长大机制进行。随着退火时间的延长,TNTZO合金中小角晶界数量减少,CSL晶界和大角随机晶界数量增多,并出现退火孪晶界。由于再结晶晶粒不遵循定向长大机制,因而再结晶完成后合金中的晶粒取向趋向于随机分布,不存在明显的织构。TNTZO合金具有与普通金属相同的回复与再结晶机制,其回复与再结晶过程与位错的运动密切相关,这从另一个方面表明TNTZO合金通过传统的位错滑移机制进行塑性变形。
由于织构的存在,变形态TNTZO合金的弹性模量降低;而合金的弹性回复率升高,表现出超弹性行为。在820℃退火5分钟后,由于发生了再结晶,TNTZO合金的弹性模量恢复到固溶态合金的水平。冷旋锻态TNTZO合金在400℃以下具有很低的线膨胀系数,小于5×10-6 K-1,而在820℃再结晶退火5分钟后,合金的线膨胀系数急剧升高,达到约9×10-6 K-1。DSC曲线上吸热峰的出现表明合金在约400～480℃温度区间存在相变。在林格溶液中,TNTZO合金的钝化膜主要由Ti、Nb、Ta和Zr元素的氧化物组成。被Nb、Ta和Zr的氧化物改性的TiO2钝化膜比被Al和V的氧化物改性的TiO2钝化膜更稳定且具有更好的保护作用,因而TNTZO合金具有比Ti-6Al-4V合金更优异的耐蚀性。由于应变和织构的存在,塑性变形对TNTZO合金腐蚀性能的影响比较复杂。较小程度的变形引起TNTZO合金腐蚀性能的恶化,但是经过较大程度变形的合金样品反而具有与固溶态合金样品相近的耐蚀性。
In 2003, a group of metastableβ-type titanium alloys basically expressed as Ti3(Ta+Nb+V) + (Zr、Hf) + O were developed by Saito et. al.. These alloys were called as multifunctional alloys due to their many“super”properties, such as super elasticity, super plasticity, and Invar and Elinvar properties. Particularly, these are the alloys that combine the ultralow elastic modulus and ultrahigh strength, which breaks the norm that a metal can not have both simultaneously. Therefore, they can be expected to be very attractive materials in dental and orthopedic implants. In order to exhibit these properties, according to Saito et. al.,“each alloy system requires substantial cold working”. The unique properties of these alloys are attributed to a dislocation-free plastic deformation mechanism because no dislocation or twin crystal is observed after hard cold-working.
In this study, a multifunctional alloy with a typical chemical composition of Ti-23Nb-0.7Ta-2Zr-O (at.%, TNTZO) was prepared by cold crucible levitation melting (CCLM) technique. Then the microstructure of the TNTZO alloy after cold working and the microstructural evolution during recrystallization were investigated and the deformation mechanism was analyzed. Additionally, the mechanical, physical, and corrosion properties of this alloy were also studied.
The results revealed that the TNTZO alloy is still composed of singleβphase and no transformation such as stress-inducedα" martensite andωphase occur after deformation. After severe cold swaging, the microstructure of the TNTZO alloy changed into characteristic“marble-like”structure because grains undergo plane-strain elongation. <100> and <111> compressed texture and <110> fiber texture, which are typical texture components of a bcc metal, are detected in the cold worked TNTZO alloy. Additionally, TEM results show that high density dislocations occur in the deformed TNTZO alloy. Therefore, the TNTZO alloy deforms by the traditional dislocation glide on slip systems, rather than by the dislocation-free mechanism.
The relationship of the recrystallized fraction versus annealing time for the TNTZO alloy can be described by a typically sigmoid curve, which indicates that the recrystallization process is a typical process of nucleation and growth of new grains. The activation energy of recrystallization was calculated to be 180 kJ/mol for the 90% cold swaged TNTZO alloy. TEM results show that recovery of the TNTZO alloy proceeds by polygonization mechanism, and recrystallization is achieved by the nucleation and growth of new grains at the expense of the deformed structure. Therefore, the number of low angle grain boundaries decreases, however, the number of the coincidence site lattice (CSL) and random boundaries increases with prolonging annealing time. Major texture components of the cold worked TNTZO alloy become diffused after complete recrystallization, thus no recrystallization texture forms. The TNTZO alloy has the same recovery and recrystallization mechanisms as the ordinary bcc metals, which also indicates that the TNTZO alloy deforms by the traditional dislocation glide on slip systems.
After cold working, Young's modulus of the TNTZO alloy decrease because of the occurrence of deformation texture. Additionally, the cold-worked TNTZO alloy exhibits super elastic property. After annealing at 820℃for 5 min, Young's modulus of the TNTZO alloy recovered to the level before cold working due to the recrystallization of the alloy. The thermal expansion coefficient of the cold swaged TNTZO alloy is extremely low, not exceeding 5×10-6 K-1 from room temperature to 400℃, however, it dramatically increases after annealing, is approximately 9×10-6 K-1. The endothermic peaks in DSC curves reveal that phase transformation occurs in the TNTZO alloy from about 400℃to 480℃.
The passive film of the TNTZO alloy is mainly composed of the oxides of Ti, Nb, Ta and Zr, and the film of the Ti-6Al-4V alloy consists of the oxides of Ti, Al and V. The passive TiO2 film modified by the oxides of Nb, Ta and Zr possesses higher stability and protective quality than the TiO2 film modified by the oxides of Al and V. Therefore the TNTZO alloy exhibits a better corrosion property than Ti-6Al-4V alloy in Ringer’s solution. Due to the existence of the strain and deformation texture, the effect of deformation on corrosion property of the TNTZO alloy is not monotonic. Small deformation causes the deterioration of the corrosion resistance, at high deformation level, however, the TNTZO alloy shows similar corrosion property to the as-soluted one.
本研究采用冷坩埚悬浮熔炼法制备了这组亚稳β钛合金的一种,其名义成分为Ti-23Nb-0.7Ta-2Zr-O (at.%, TNTZO),并系统研究了固溶态TNTZO合金在塑性变形后的显微组织及随后再结晶退火过程中的显微组织演变,分析了合金的变形机制,并考察了该合金的力学性能、物理性能和耐腐蚀性能。
研究结果表明:经过室温塑性变形后,TNTZO合金中β相保持稳定,没有应力诱发马氏体相变发生。经较大程度压缩变形后合金具有比较明显的<100>和<111>双织构。由于在冷旋锻过程中晶粒处于平面应变条件,因而经90%冷旋锻变形后, TNTZO合金的显微组织由大量平行于旋锻轴向的板条组织构成。这些板条扭曲并相互环绕,在垂直旋锻轴向的截面上形成由细小纤维状组织交织而成的大理石花纹状组织,同时合金中产生强烈的<110>丝织构。TEM观察结果表明变形后TNTZO合金中出现了高密度的位错聚集。因此,TNTZO合金仍然通过传统的位错滑移机制进行塑性变形,而不是通过所谓的无位错机制进行塑性变形。TNTZO合金的再结晶动力学曲线具有典型的“S”曲线特征,表明TNTZO合金
的再结晶是典型的形核长大过程。经90%冷旋锻变形的TNTZO合金的再结晶激活能约为180 kJ/mol。TEM观察结果表明TNTZO合金的回复通过多边形化机制进行,再结晶通过形核长大机制进行。随着退火时间的延长,TNTZO合金中小角晶界数量减少,CSL晶界和大角随机晶界数量增多,并出现退火孪晶界。由于再结晶晶粒不遵循定向长大机制,因而再结晶完成后合金中的晶粒取向趋向于随机分布,不存在明显的织构。TNTZO合金具有与普通金属相同的回复与再结晶机制,其回复与再结晶过程与位错的运动密切相关,这从另一个方面表明TNTZO合金通过传统的位错滑移机制进行塑性变形。
由于织构的存在,变形态TNTZO合金的弹性模量降低;而合金的弹性回复率升高,表现出超弹性行为。在820℃退火5分钟后,由于发生了再结晶,TNTZO合金的弹性模量恢复到固溶态合金的水平。冷旋锻态TNTZO合金在400℃以下具有很低的线膨胀系数,小于5×10-6 K-1,而在820℃再结晶退火5分钟后,合金的线膨胀系数急剧升高,达到约9×10-6 K-1。DSC曲线上吸热峰的出现表明合金在约400～480℃温度区间存在相变。在林格溶液中,TNTZO合金的钝化膜主要由Ti、Nb、Ta和Zr元素的氧化物组成。被Nb、Ta和Zr的氧化物改性的TiO2钝化膜比被Al和V的氧化物改性的TiO2钝化膜更稳定且具有更好的保护作用,因而TNTZO合金具有比Ti-6Al-4V合金更优异的耐蚀性。由于应变和织构的存在,塑性变形对TNTZO合金腐蚀性能的影响比较复杂。较小程度的变形引起TNTZO合金腐蚀性能的恶化,但是经过较大程度变形的合金样品反而具有与固溶态合金样品相近的耐蚀性。
In 2003, a group of metastableβ-type titanium alloys basically expressed as Ti3(Ta+Nb+V) + (Zr、Hf) + O were developed by Saito et. al.. These alloys were called as multifunctional alloys due to their many“super”properties, such as super elasticity, super plasticity, and Invar and Elinvar properties. Particularly, these are the alloys that combine the ultralow elastic modulus and ultrahigh strength, which breaks the norm that a metal can not have both simultaneously. Therefore, they can be expected to be very attractive materials in dental and orthopedic implants. In order to exhibit these properties, according to Saito et. al.,“each alloy system requires substantial cold working”. The unique properties of these alloys are attributed to a dislocation-free plastic deformation mechanism because no dislocation or twin crystal is observed after hard cold-working.
In this study, a multifunctional alloy with a typical chemical composition of Ti-23Nb-0.7Ta-2Zr-O (at.%, TNTZO) was prepared by cold crucible levitation melting (CCLM) technique. Then the microstructure of the TNTZO alloy after cold working and the microstructural evolution during recrystallization were investigated and the deformation mechanism was analyzed. Additionally, the mechanical, physical, and corrosion properties of this alloy were also studied.
The results revealed that the TNTZO alloy is still composed of singleβphase and no transformation such as stress-inducedα" martensite andωphase occur after deformation. After severe cold swaging, the microstructure of the TNTZO alloy changed into characteristic“marble-like”structure because grains undergo plane-strain elongation. <100> and <111> compressed texture and <110> fiber texture, which are typical texture components of a bcc metal, are detected in the cold worked TNTZO alloy. Additionally, TEM results show that high density dislocations occur in the deformed TNTZO alloy. Therefore, the TNTZO alloy deforms by the traditional dislocation glide on slip systems, rather than by the dislocation-free mechanism.
The relationship of the recrystallized fraction versus annealing time for the TNTZO alloy can be described by a typically sigmoid curve, which indicates that the recrystallization process is a typical process of nucleation and growth of new grains. The activation energy of recrystallization was calculated to be 180 kJ/mol for the 90% cold swaged TNTZO alloy. TEM results show that recovery of the TNTZO alloy proceeds by polygonization mechanism, and recrystallization is achieved by the nucleation and growth of new grains at the expense of the deformed structure. Therefore, the number of low angle grain boundaries decreases, however, the number of the coincidence site lattice (CSL) and random boundaries increases with prolonging annealing time. Major texture components of the cold worked TNTZO alloy become diffused after complete recrystallization, thus no recrystallization texture forms. The TNTZO alloy has the same recovery and recrystallization mechanisms as the ordinary bcc metals, which also indicates that the TNTZO alloy deforms by the traditional dislocation glide on slip systems.
After cold working, Young's modulus of the TNTZO alloy decrease because of the occurrence of deformation texture. Additionally, the cold-worked TNTZO alloy exhibits super elastic property. After annealing at 820℃for 5 min, Young's modulus of the TNTZO alloy recovered to the level before cold working due to the recrystallization of the alloy. The thermal expansion coefficient of the cold swaged TNTZO alloy is extremely low, not exceeding 5×10-6 K-1 from room temperature to 400℃, however, it dramatically increases after annealing, is approximately 9×10-6 K-1. The endothermic peaks in DSC curves reveal that phase transformation occurs in the TNTZO alloy from about 400℃to 480℃.
The passive film of the TNTZO alloy is mainly composed of the oxides of Ti, Nb, Ta and Zr, and the film of the Ti-6Al-4V alloy consists of the oxides of Ti, Al and V. The passive TiO2 film modified by the oxides of Nb, Ta and Zr possesses higher stability and protective quality than the TiO2 film modified by the oxides of Al and V. Therefore the TNTZO alloy exhibits a better corrosion property than Ti-6Al-4V alloy in Ringer’s solution. Due to the existence of the strain and deformation texture, the effect of deformation on corrosion property of the TNTZO alloy is not monotonic. Small deformation causes the deterioration of the corrosion resistance, at high deformation level, however, the TNTZO alloy shows similar corrosion property to the as-soluted one.
引文
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