钛合金应力诱导马氏体相变影响因素及力学性能研究
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摘要
钛及钛合金是继钢铁、铝合金之后又一种重要的结构金属材料。钛合金以其优异性能，广泛应用于航空航天、航海、石油化工、冶金、机械、能源、冶金及医疗卫生等领域。钛合金中相变和组织的多样化决定了其力学性能能在宽广范围内变化。如何通过组织最佳化获得综合性能良好的合金一直是研究工作者追求的目标。有研究表明应力诱导马氏体相变在提高材料强度的同时，塑性也能保持在一个较高的水平，其综合力学性能十分优异，应用前景十分广阔。
本文以一种商业钛合金Ti-10V-2Fe-3Al为初始研究对象，通过对其进行一系列的热处理和力学性能测试，运用X射线衍射、金相显微镜、扫描电子显微镜、透射电子显微镜、电子探针显微分析等先进表征技术，结合热力学理论计算软件Thermo-calc，对合金中的应力诱导马氏体相变等一系列相变进行了研究，并以此为理论基础，对合金的成分进行了调制，并对其进行系统的表征和研究。得到以下主要结论：
(1) Ti-10V-2Fe-3Al合金双态组织样品具有较高的塑性，经过(α+β)相区固溶处理后，针状α的消失导致合金塑性下降。相较于单一β相区固溶处理样品，经过β+(α+β)相区固溶处理后的样品塑性有所增加。球状α相的含量对应力诱导马氏体相变的临界诱发应力有较大影响，对普通样品的屈服强度影响不大，而在β+(α+β)相区固溶处理后析出的针状α相对临界诱发应力影响较小，对普通样品屈服强度影响较大。变形后α相中一直有{1011}<012>孪晶，而β相则随着稳定性的增加，变形机制由应力诱导马氏体相变逐渐变为{112}<111>孪晶。对于Ti-10V-2Fe-3Al合金来说，单级时效与双级时效所得的显微组织相似，都是由以相促进形核而生长的细小α相组成，时效时间虽然很短，但α相含量较高。它们的力学性能也相似。
(2)在Ti-10V-2Fe-3Al合金中，当α相的含量超过一定临界值时(约为50%)，应力诱导马氏体相变都将趋于消失。应力诱导马氏体相变行为主要受两个因素的影响：β相尺寸和β相稳定性。对于含球状α相的样品，由于其β相区域尺寸变化很小，因此其马氏体相变临界诱发应力主要受β相稳定性影响，随着α相含量的上升应力值也上升。对于含针状α相样品，其相变临界诱发应力同时受两个因素的影响，使得应力值随α相含量的上升变化不明显。应力诱导马氏体相变临界诱发应力值的大小可用一个线性叠加公式来进行计算：σ_(SIM)(Mo_(eq)=σ_(si)(d)|_(Mo_(eq0))+△σ_(st)(Mo_(eq)-Mo_(eq0))且应力诱导马氏体相变临界诱发应力值随β相区域尺寸的增加而增加。
(3)从Ti-10V-2Fe-3Al合金中得出的应力诱导马氏体相变临界诱发应力计算公式在一定条件下的Ti-10V-1Fe-3Al合金中仍然适用，但是对于Ti-10V-2Cr-3Al合金，计算应力值与实验应力值有一定的差距。在Ti-10V-2Cr-3Al合金中，由于Cr元素扩散速度较慢，在α相析出过程中容易在α/β相界面偏聚集，形成了马氏体无析出带，同时使得远离α/β相界面的β相容易产生淬火马氏体，对应力诱导马氏体相变产生了阻碍作用。当β相钼当量低于9时，合金会析出大量淬火马氏体；当钼当量在9与16之间时，能产生应力诱导马氏体相变；当钼当量高于16时，应力诱导马氏体相变消失。
(4) Ti-10V-2Cr-3Al合金与Ti-10V-1Fe-3Al合金经过β相区固溶处理后形成的淬火马氏体为六方α'相，不同应变速率压缩变形后(10~(-4)s~(-1)<ε<10~(-1)s~(-1))，都发生了应力诱导马氏体相变。Ti-10V-2Fe-3Al、Ti-10V-2Cr-3Al与Ti-10V-1Fe-3Al三种合金经过β相区固溶处理后，随着应变速率的增加，样品中应力诱导马氏体相变逐渐弱化，温度逐渐升高，三种合金的屈服应力(即临界诱发应力)增加；断裂应变上升，压缩强度先升高后降低。
(5)β+(α+β)相区固溶处理时，Ti-10V-2Cr-3Al合金中α相的析出速度比Ti-10V-1Fe-3Al合金慢；随着α相含量的增加，两合金的压缩强度逐渐下降，断裂应变保持稳定。经过单级时效后，Ti-10V-2Cr-3Al合金的组织比Ti-10V-1Fe-3Al合金细小，因此屈服应力与压缩强度较高，而断裂应变较低。经过双级时效后，Ti-10V-2Cr-3Al合金显微组织与力学性能变化不大，而Ti-10V-1Fe-3Al合金组织稍有细化，屈服强度与压缩强度有所提高，断裂应变降低。
Titanium and its alloys start to gain a unique position amongst other structuralmaterials, like Fe, Al-based alloy. Titanium alloys are attractive for a variety ofapplications such as aerospace, marine, petroleum, chemical, metallurgy, machinery,energy and health care due to their excellent properties. Titanium alloys offer manyopportunities to tailor the microstructure and the resulting deformation behavior andresulting application fields, because of their wide range of complex microstructuresand phase transformations. Phase transformation resulting from the deformation isintentiona lly used to improve properties. Previous studies sho wed that thestress-induced martensite (SIM) transformation starting from a metastable β phase canindeed result in an improved balance of strength and ductility and has a good potentialapplication.
An initia l investigation on an existing commercial titanium alloy Ti-10V-2Fe-3Alwas conducted. A variety of different heat treatments and mechanical tests wereperformed. A series of phase transformations including stress-induced martensitictransformation were studied by X-ray diffraction, optical microscopy, scanningelectron microscopy, transmission electron microscopy, electron probe microanalysis,combined with the Thermo-calc software. Based on the theoretical foundation, twocertain kinds of new alloys were designed and manufactured; characterization andevaluation were also carried out. The obtained results are summarized as follows:
(1) In Ti-10V-2Fe-3Al alloy, the bi-modal microstructures possess a betterplasticity. After α+β phase field solution treatment, the failure strain was largelydecreased due to the disappearance of α laths in bi-modal microstructures. Comparewith β phase field solution treatment, samples under β+(α+β) conditions have higherfailure strain. Globular α phase has a great influence on triggering stress for SIMeffect, but does not show too much effect on mechanical properties for sampleswithout SIM. Acicular α phase has a weak influence on triggering stress for SIMtransformation, but shows some effect on samples without SIM. The deformationmechanism of α phase always contains {1011}<012> type twin. With increase the αphase volume fraction (both globular and acicular), the deformation mechanism of βphase varies from stress induced martensitic transformation to {112}<111> t ype twins.After single aging or dual aging treatments, alloys exhib it almost identical microstructures and thus similar mechanical properties, and age hardening is quiteeffective. The main deformation mode is slip.
(2) In Ti-10V-2Fe-3Al, no SIM was observed for specimens with the α volumefraction higher than a critical value (50%). The triggering stress of SIM in this alloy ismainly independently affected by these two factors: the β grain (or domain) size andthe stability (Moeq) of the β phase. For globular α samples, the β matrix stability has adominating effect on the triggering stress, but in samples containing acicular α, thesize of the retained β domains is also important. These two factors compete with eachother, and eventually decide the triggering stress. A linear super-position of the twoeffects was found to describe the data very well in the formula below:σ_(SIM)(Mo_(eq)=σ_(si)(d)|_(Mo_(eq0))+△σ_(st)(Mo_(eq)-Mo_(eq0))An increase in the β grain size linearly increases the triggering stress for SIM.
(3) The proposed relation between the occurrence of SIM formation upon roomtemperature compression of metastable titanium alloys derived for Ti-10V-2Fe-3Alwas found to apply also to the Ti-10V-1Fe-3Al, albeit that the actual triggering stresswas affected by the presence of thermal martensite already present prior to thecompression experiment. The formation of a martensite free zone‘around the α phasein the Ti-10V-2Cr-3Al due to a very limited diffusion distance for Cr atoms upon αformation during intercritical annealing, prevented the wider validation of theproposed relation between the chemical and microstructural β stability. However,based on the results obtained so far SIM martensite transformation is predicted tooccur for β phase fractions with a Mo equivalence between9and16. For Moequiva lences lower than9, thermal martensite may be present prior to deformation.For that higher than16, the β stability is such that even upon deformation the β phasefraction does not transform martensitically.
(4) α' martensite was observed in Ti-10V-2Cr-3Al alloy and Ti-10V-1Fe-3Alalloy after quenching from β phase fie ld. All heat treated samples researched showedstress-induced martensitic transformation for all strain rates (10~(-4)s~(-1)<ε<10~(-1)s~(-1))explored. The SIM triggering stress increases linearly with the logarithm of the strainrate. The rate of increase is the same as that for the yield stress of the grade notshowing SIM transformation. The failure strain increases linearly with the logarithmof the strain rate, irrespective of the occurrence of SIM transformation.
(5) After phase field solution treatment, the phase precipitation rateof Ti-10V-2Cr-3Al alloy is lower than Ti-10V-1Fe-3Al alloy. With increasing phase content, the compressive strength of both alloys decreased, but the fracture strainremained stable. After single aging, the microstructure of Ti-10V-2Cr-3Al alloy isfiner than Ti-10V-1Fe-3Al alloy, and results in a higher yield stress, a highercompressive strength and a lower fracture strain. After dual aging, the microstructuresand mechanical properties of Ti-10V-2Cr-3Al alloy change little, but forTi-10V-1Fe-3Al alloy, microstructures was slightly refined and thus increases in yie ldstrength and compressive strength, and reduces fracture strain.
本文以一种商业钛合金Ti-10V-2Fe-3Al为初始研究对象，通过对其进行一系列的热处理和力学性能测试，运用X射线衍射、金相显微镜、扫描电子显微镜、透射电子显微镜、电子探针显微分析等先进表征技术，结合热力学理论计算软件Thermo-calc，对合金中的应力诱导马氏体相变等一系列相变进行了研究，并以此为理论基础，对合金的成分进行了调制，并对其进行系统的表征和研究。得到以下主要结论：
(1) Ti-10V-2Fe-3Al合金双态组织样品具有较高的塑性，经过(α+β)相区固溶处理后，针状α的消失导致合金塑性下降。相较于单一β相区固溶处理样品，经过β+(α+β)相区固溶处理后的样品塑性有所增加。球状α相的含量对应力诱导马氏体相变的临界诱发应力有较大影响，对普通样品的屈服强度影响不大，而在β+(α+β)相区固溶处理后析出的针状α相对临界诱发应力影响较小，对普通样品屈服强度影响较大。变形后α相中一直有{1011}<012>孪晶，而β相则随着稳定性的增加，变形机制由应力诱导马氏体相变逐渐变为{112}<111>孪晶。对于Ti-10V-2Fe-3Al合金来说，单级时效与双级时效所得的显微组织相似，都是由以相促进形核而生长的细小α相组成，时效时间虽然很短，但α相含量较高。它们的力学性能也相似。
(2)在Ti-10V-2Fe-3Al合金中，当α相的含量超过一定临界值时(约为50%)，应力诱导马氏体相变都将趋于消失。应力诱导马氏体相变行为主要受两个因素的影响：β相尺寸和β相稳定性。对于含球状α相的样品，由于其β相区域尺寸变化很小，因此其马氏体相变临界诱发应力主要受β相稳定性影响，随着α相含量的上升应力值也上升。对于含针状α相样品，其相变临界诱发应力同时受两个因素的影响，使得应力值随α相含量的上升变化不明显。应力诱导马氏体相变临界诱发应力值的大小可用一个线性叠加公式来进行计算：σ_(SIM)(Mo_(eq)=σ_(si)(d)|_(Mo_(eq0))+△σ_(st)(Mo_(eq)-Mo_(eq0))且应力诱导马氏体相变临界诱发应力值随β相区域尺寸的增加而增加。
(3)从Ti-10V-2Fe-3Al合金中得出的应力诱导马氏体相变临界诱发应力计算公式在一定条件下的Ti-10V-1Fe-3Al合金中仍然适用，但是对于Ti-10V-2Cr-3Al合金，计算应力值与实验应力值有一定的差距。在Ti-10V-2Cr-3Al合金中，由于Cr元素扩散速度较慢，在α相析出过程中容易在α/β相界面偏聚集，形成了马氏体无析出带，同时使得远离α/β相界面的β相容易产生淬火马氏体，对应力诱导马氏体相变产生了阻碍作用。当β相钼当量低于9时，合金会析出大量淬火马氏体；当钼当量在9与16之间时，能产生应力诱导马氏体相变；当钼当量高于16时，应力诱导马氏体相变消失。
(4) Ti-10V-2Cr-3Al合金与Ti-10V-1Fe-3Al合金经过β相区固溶处理后形成的淬火马氏体为六方α'相，不同应变速率压缩变形后(10~(-4)s~(-1)<ε<10~(-1)s~(-1))，都发生了应力诱导马氏体相变。Ti-10V-2Fe-3Al、Ti-10V-2Cr-3Al与Ti-10V-1Fe-3Al三种合金经过β相区固溶处理后，随着应变速率的增加，样品中应力诱导马氏体相变逐渐弱化，温度逐渐升高，三种合金的屈服应力(即临界诱发应力)增加；断裂应变上升，压缩强度先升高后降低。
(5)β+(α+β)相区固溶处理时，Ti-10V-2Cr-3Al合金中α相的析出速度比Ti-10V-1Fe-3Al合金慢；随着α相含量的增加，两合金的压缩强度逐渐下降，断裂应变保持稳定。经过单级时效后，Ti-10V-2Cr-3Al合金的组织比Ti-10V-1Fe-3Al合金细小，因此屈服应力与压缩强度较高，而断裂应变较低。经过双级时效后，Ti-10V-2Cr-3Al合金显微组织与力学性能变化不大，而Ti-10V-1Fe-3Al合金组织稍有细化，屈服强度与压缩强度有所提高，断裂应变降低。
Titanium and its alloys start to gain a unique position amongst other structuralmaterials, like Fe, Al-based alloy. Titanium alloys are attractive for a variety ofapplications such as aerospace, marine, petroleum, chemical, metallurgy, machinery,energy and health care due to their excellent properties. Titanium alloys offer manyopportunities to tailor the microstructure and the resulting deformation behavior andresulting application fields, because of their wide range of complex microstructuresand phase transformations. Phase transformation resulting from the deformation isintentiona lly used to improve properties. Previous studies sho wed that thestress-induced martensite (SIM) transformation starting from a metastable β phase canindeed result in an improved balance of strength and ductility and has a good potentialapplication.
An initia l investigation on an existing commercial titanium alloy Ti-10V-2Fe-3Alwas conducted. A variety of different heat treatments and mechanical tests wereperformed. A series of phase transformations including stress-induced martensitictransformation were studied by X-ray diffraction, optical microscopy, scanningelectron microscopy, transmission electron microscopy, electron probe microanalysis,combined with the Thermo-calc software. Based on the theoretical foundation, twocertain kinds of new alloys were designed and manufactured; characterization andevaluation were also carried out. The obtained results are summarized as follows:
(1) In Ti-10V-2Fe-3Al alloy, the bi-modal microstructures possess a betterplasticity. After α+β phase field solution treatment, the failure strain was largelydecreased due to the disappearance of α laths in bi-modal microstructures. Comparewith β phase field solution treatment, samples under β+(α+β) conditions have higherfailure strain. Globular α phase has a great influence on triggering stress for SIMeffect, but does not show too much effect on mechanical properties for sampleswithout SIM. Acicular α phase has a weak influence on triggering stress for SIMtransformation, but shows some effect on samples without SIM. The deformationmechanism of α phase always contains {1011}<012> type twin. With increase the αphase volume fraction (both globular and acicular), the deformation mechanism of βphase varies from stress induced martensitic transformation to {112}<111> t ype twins.After single aging or dual aging treatments, alloys exhib it almost identical microstructures and thus similar mechanical properties, and age hardening is quiteeffective. The main deformation mode is slip.
(2) In Ti-10V-2Fe-3Al, no SIM was observed for specimens with the α volumefraction higher than a critical value (50%). The triggering stress of SIM in this alloy ismainly independently affected by these two factors: the β grain (or domain) size andthe stability (Moeq) of the β phase. For globular α samples, the β matrix stability has adominating effect on the triggering stress, but in samples containing acicular α, thesize of the retained β domains is also important. These two factors compete with eachother, and eventually decide the triggering stress. A linear super-position of the twoeffects was found to describe the data very well in the formula below:σ_(SIM)(Mo_(eq)=σ_(si)(d)|_(Mo_(eq0))+△σ_(st)(Mo_(eq)-Mo_(eq0))An increase in the β grain size linearly increases the triggering stress for SIM.
(3) The proposed relation between the occurrence of SIM formation upon roomtemperature compression of metastable titanium alloys derived for Ti-10V-2Fe-3Alwas found to apply also to the Ti-10V-1Fe-3Al, albeit that the actual triggering stresswas affected by the presence of thermal martensite already present prior to thecompression experiment. The formation of a martensite free zone‘around the α phasein the Ti-10V-2Cr-3Al due to a very limited diffusion distance for Cr atoms upon αformation during intercritical annealing, prevented the wider validation of theproposed relation between the chemical and microstructural β stability. However,based on the results obtained so far SIM martensite transformation is predicted tooccur for β phase fractions with a Mo equivalence between9and16. For Moequiva lences lower than9, thermal martensite may be present prior to deformation.For that higher than16, the β stability is such that even upon deformation the β phasefraction does not transform martensitically.
(4) α' martensite was observed in Ti-10V-2Cr-3Al alloy and Ti-10V-1Fe-3Alalloy after quenching from β phase fie ld. All heat treated samples researched showedstress-induced martensitic transformation for all strain rates (10~(-4)s~(-1)<ε<10~(-1)s~(-1))explored. The SIM triggering stress increases linearly with the logarithm of the strainrate. The rate of increase is the same as that for the yield stress of the grade notshowing SIM transformation. The failure strain increases linearly with the logarithmof the strain rate, irrespective of the occurrence of SIM transformation.
(5) After phase field solution treatment, the phase precipitation rateof Ti-10V-2Cr-3Al alloy is lower than Ti-10V-1Fe-3Al alloy. With increasing phase content, the compressive strength of both alloys decreased, but the fracture strainremained stable. After single aging, the microstructure of Ti-10V-2Cr-3Al alloy isfiner than Ti-10V-1Fe-3Al alloy, and results in a higher yield stress, a highercompressive strength and a lower fracture strain. After dual aging, the microstructuresand mechanical properties of Ti-10V-2Cr-3Al alloy change little, but forTi-10V-1Fe-3Al alloy, microstructures was slightly refined and thus increases in yie ldstrength and compressive strength, and reduces fracture strain.
引文
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