HSLA铁素体钢中Cu析出强化和奥氏体韧化的原子探针层析技术研究
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摘要
以含有Cu和Ni的低合金高强度（HSLA）钢为材料，设计了奥氏体连续冷却（SCC）、马氏体回火（SQCT）和奥氏体-铁素体两相区淬火（SQIT）等三种热处理工艺，结合光学显微镜（OM）、扫描电子显微镜（SEM）和透射电子显微镜（TEM）等分析表征手段和方法，利用原子探针层析技术（APT），在原子尺度上研究了Cu析出和回转奥氏体（RA）的大小、形貌、数量等析出特点和形成过程，探讨了Cu析出强化和回转奥氏体韧化的机制，以及热处理工艺对Cu-Ni钢的室温拉伸、低温冲击和焊接性能的影响，得到以下结论：
在奥氏体连续冷却过程中，冷却速率通过影响合金元素在奥氏体和铁素体之间的动态扩散分配，决定了室温组织中多边形铁素体、针状铁素体、粒状铁素体、贝氏体、马氏体和残余奥氏体的组成比例，以及相变过程中Cu的析出过程和分布状态。在较慢冷速下，室温组织主要为多边形铁素体，并有少量贝氏体和残余奥氏体或马氏体。随着冷速的增加，多边形铁素体的形核和长大被抑制，体积分数逐渐减少，而粒状铁素体和针状铁素体不断增加，并存有少量未转变的残余奥氏体。在此过程中，Cu析出主要在多边形铁素体内通过相间沉淀的方式形成，分布不均匀，在一定程度上限制了其强化效果。
奥氏体相变产物中的微观结构（位错、碳化物（渗碳体）和奥氏体/铁素体界面）对Cu析出的形核、长大和粗化有不同的影响。APT研究表明，Cu析出和P偏聚的位错线没有明显的交互作用。在奥氏体-铁素体相变过程中，相对位错，奥氏体/铁素体界面更容易诱发Cu原子以相间沉淀的方式形核。在较慢的冷速下，渗碳体/基体界面成为Cu析出优先形核的部位，并促进其长大和粗化。溶质原子在铁素体和奥氏体之间的扩散、再分配和界面偏聚，促使Cu析出在奥氏体/铁素体界面形成。另外，Cu析出过程受到铁素体/奥氏体界面迁移速率的影响，即与奥氏体连续冷却速率有关。
经900℃固溶+淬火处理后，Cu-Ni钢为Cu原子过饱和固溶的板条马氏体组织。不同温度回火时，硬度曲线反映了马氏体组织软化，Cu析出强化和回转奥氏体的二次淬火等因素的共同作用效果。APT分析表明，随着回火温度的增加或时间的延长，Cu析出的数量密度逐渐减少，尺寸不断增加，同时形态从球型不断向椭球过渡。在形成早期，Cu析出中含有大量的Fe，以及一定量的Ni和Mn。随着Cu析出的长大和粗化，Ni和Mn倾向偏聚在Cu析出/基体界面处，而且Fe含量逐渐降低。高温（650℃）回火时，APT没有探测出Cu析出存在。
通过奥氏体-铁素体两相区回火，可以得到回转奥氏体弥散分布的板条状回火马氏体组织。Ni、Mn和Cu等奥氏体稳定性元素富集在回转奥氏体中，增加了回转奥氏体的热稳定性和力学稳定性，具有很强的低温韧化作用。APT分析表明，回转奥氏体附近存在有尺寸较大的Cu析出，证实了Cu原子向回转奥氏体中富集的倾向，而且在低温时伴随奥氏体的部分分解而析出。在铁素体基体中，存在大量细小的Cu析出，为后续常规回火时形成的，具有析出强化作用。
SCC反映了传统控轧、控冷工艺所涉及的物理冶金规律，此时Cu-Ni钢具有良好的室温拉伸性能，但在低温时普遍存在脆化倾向。SQCT反映了热处理工艺所涉及的物理冶金规律，此时Cu-Ni钢具有良好的拉伸性能，但屈强比较高，可靠性降低。SQIT工艺中，屈强比较低，拉伸性能优越，在-80℃时仍具有较高的冲击功，具有最佳的综合力学性能。SCC、SQCT和SQIT所获得的显观组织各异，拉伸和低温冲击等力学性能依次提高，但实际生产成本也逐渐增加。
Cu析出尺寸较小且与基体呈非共格时，位错切过机制起主导作用，其强化效应主要来源于化学强化、共格强化和模量强化等作用，三者的强化增量分别为3-6MPa，86MPa和139MPa，其中模量强化起主导作用；对于尺寸较大的非共格的FCC结构Cu析出，Orowan绕过机制起主导作用，强化增量约为18MPa。切过向绕过机制转变的临界半径约为2.9nm。
The copper precipitation and the formation of reverse austenite in Cu-andNi-containing high-strength low-alloy steelsare comprehensively studied by atomprobe tomography (APT) companying with optical microscopy (OM), scanningelectronic microscopy (SEM) and transmission electronic microscopy (TEM). Threedifferent heat treatment procedures including solution pluscontrolled cooling (SCC),solution and quenching plus conventional tempering (SQCT), and solution andquenching plus interstitial tempering plus conventional tempering (SQIT) aredesigned. The nature of Cu precipitation,and the effects of heat treatment on themicrostructural evolution and the final mechanical strength are discussed.
During continuously cooling of austenite, the solute elements of C, Ni, Mn andCu etc.are prone to diffuse into the untransformed austeniteand change the austenitedecomposition kinetics, leading to the formation of a variety of structural componentsof ferrite, bainite, martensite and/or retained austenite in the ambient microstructure.Besides, the Cu precipitation also greatly correlates with the austenite decomposition.The actual volume fractions of the final phases are as function of the cooling rates.The Cu phases are mostly formed by interphase precipitation in the polygonalferrite.But the Cu precipitation can also occur in polygonal ferrite after theaustenite-ferrite transformation is finished.The micro-constituents such as dislocations,carbides (cementite) and migrating austenite/ferrite heterophase interfaces duringaustenite decompositionhave an effect on the nucleation, growth and coarsening ofcopper precipitates. APT studies indicate that not all Cu precipitates are formed on thedislocations with P segregation, because the austenite/ferrite heterophase interfacesare more likely to induce the Cu nucleation compared to dislocation. The carbide/matrix interfaces are the preferential sites for Cu nucleation, and the formation ofcarbides will contribute to the growth and coarsening of Cu precipitates. Theinterphase precipitation of Cu phases is significantly impacted by migration rate ofaustenite/ferrite interfaces and the actual cooling rate. The structural andcompositional evolution is the same as that for the isothermal aging.
Thesolution-quench microstructure of the Cu-Ni steels mainly consists of lathmartensite with Cu in solution. Duringtempering, the micro-hardness evolution wellreflects the microstructuralevolutionresulting from the softening of martensite, Cuprecipitation strengthening and reverse austenite toughening. The number density ofCu precipitates decrease whereas the sizes increase with increasing of temperingintensity. At the same time, the morphology evolve form sphere to ellipse. At theinitial nucleation stage, the Cu precipitates contains considerable high Fe content aswell as a small amount of Ni and Mn, which are prone to segregate at the matrix/Cuprecipitate interface at the later growth and coarsening stages.
By additional interstitial tempering in QT procedure, a microstructure of lath-likemartensite with dispersed reverse austenite at lath boundary and prior austenite grainboundary is obtained.The mechanical and thermal stability of the reverseaustenitewhich is in direct proportion to the content of alloying elements especially Niplays an important role in toughening at low temperature. Copper can diffuse into andstabilize the reverse austenite and precipitate out companying with the partialdecomposition of reverse austenite during tempering. Copper still in solution duringinterstitial temperingis the contributor for the strengthening Cu precipitates formed insubsequent tempering.
There are great difference in the final microstructure and thereby mechanicalproperties of the Cu-Ni steels. The disadvantages of SCC and SQCT processed steelsare lower temperature toughness and yield/tensile ratio, respectively, which can beoptimized by SQIT procedure. As to the shearable BCC coherent Cu precipitates, thestrength increments by the effects of chemical hardening, the coherency strain and themodulus strengthening are3-6,86and139MPa, respectively. For the incoherent,impenetrable FCC Cu precipitates, the strength increments by classical Orowanmechanism is18MPa. The critical transition size of Cu precipitates with differentstrengthening mechanism is calculated to be about2.9nm.
在奥氏体连续冷却过程中，冷却速率通过影响合金元素在奥氏体和铁素体之间的动态扩散分配，决定了室温组织中多边形铁素体、针状铁素体、粒状铁素体、贝氏体、马氏体和残余奥氏体的组成比例，以及相变过程中Cu的析出过程和分布状态。在较慢冷速下，室温组织主要为多边形铁素体，并有少量贝氏体和残余奥氏体或马氏体。随着冷速的增加，多边形铁素体的形核和长大被抑制，体积分数逐渐减少，而粒状铁素体和针状铁素体不断增加，并存有少量未转变的残余奥氏体。在此过程中，Cu析出主要在多边形铁素体内通过相间沉淀的方式形成，分布不均匀，在一定程度上限制了其强化效果。
奥氏体相变产物中的微观结构（位错、碳化物（渗碳体）和奥氏体/铁素体界面）对Cu析出的形核、长大和粗化有不同的影响。APT研究表明，Cu析出和P偏聚的位错线没有明显的交互作用。在奥氏体-铁素体相变过程中，相对位错，奥氏体/铁素体界面更容易诱发Cu原子以相间沉淀的方式形核。在较慢的冷速下，渗碳体/基体界面成为Cu析出优先形核的部位，并促进其长大和粗化。溶质原子在铁素体和奥氏体之间的扩散、再分配和界面偏聚，促使Cu析出在奥氏体/铁素体界面形成。另外，Cu析出过程受到铁素体/奥氏体界面迁移速率的影响，即与奥氏体连续冷却速率有关。
经900℃固溶+淬火处理后，Cu-Ni钢为Cu原子过饱和固溶的板条马氏体组织。不同温度回火时，硬度曲线反映了马氏体组织软化，Cu析出强化和回转奥氏体的二次淬火等因素的共同作用效果。APT分析表明，随着回火温度的增加或时间的延长，Cu析出的数量密度逐渐减少，尺寸不断增加，同时形态从球型不断向椭球过渡。在形成早期，Cu析出中含有大量的Fe，以及一定量的Ni和Mn。随着Cu析出的长大和粗化，Ni和Mn倾向偏聚在Cu析出/基体界面处，而且Fe含量逐渐降低。高温（650℃）回火时，APT没有探测出Cu析出存在。
通过奥氏体-铁素体两相区回火，可以得到回转奥氏体弥散分布的板条状回火马氏体组织。Ni、Mn和Cu等奥氏体稳定性元素富集在回转奥氏体中，增加了回转奥氏体的热稳定性和力学稳定性，具有很强的低温韧化作用。APT分析表明，回转奥氏体附近存在有尺寸较大的Cu析出，证实了Cu原子向回转奥氏体中富集的倾向，而且在低温时伴随奥氏体的部分分解而析出。在铁素体基体中，存在大量细小的Cu析出，为后续常规回火时形成的，具有析出强化作用。
SCC反映了传统控轧、控冷工艺所涉及的物理冶金规律，此时Cu-Ni钢具有良好的室温拉伸性能，但在低温时普遍存在脆化倾向。SQCT反映了热处理工艺所涉及的物理冶金规律，此时Cu-Ni钢具有良好的拉伸性能，但屈强比较高，可靠性降低。SQIT工艺中，屈强比较低，拉伸性能优越，在-80℃时仍具有较高的冲击功，具有最佳的综合力学性能。SCC、SQCT和SQIT所获得的显观组织各异，拉伸和低温冲击等力学性能依次提高，但实际生产成本也逐渐增加。
Cu析出尺寸较小且与基体呈非共格时，位错切过机制起主导作用，其强化效应主要来源于化学强化、共格强化和模量强化等作用，三者的强化增量分别为3-6MPa，86MPa和139MPa，其中模量强化起主导作用；对于尺寸较大的非共格的FCC结构Cu析出，Orowan绕过机制起主导作用，强化增量约为18MPa。切过向绕过机制转变的临界半径约为2.9nm。
The copper precipitation and the formation of reverse austenite in Cu-andNi-containing high-strength low-alloy steelsare comprehensively studied by atomprobe tomography (APT) companying with optical microscopy (OM), scanningelectronic microscopy (SEM) and transmission electronic microscopy (TEM). Threedifferent heat treatment procedures including solution pluscontrolled cooling (SCC),solution and quenching plus conventional tempering (SQCT), and solution andquenching plus interstitial tempering plus conventional tempering (SQIT) aredesigned. The nature of Cu precipitation,and the effects of heat treatment on themicrostructural evolution and the final mechanical strength are discussed.
During continuously cooling of austenite, the solute elements of C, Ni, Mn andCu etc.are prone to diffuse into the untransformed austeniteand change the austenitedecomposition kinetics, leading to the formation of a variety of structural componentsof ferrite, bainite, martensite and/or retained austenite in the ambient microstructure.Besides, the Cu precipitation also greatly correlates with the austenite decomposition.The actual volume fractions of the final phases are as function of the cooling rates.The Cu phases are mostly formed by interphase precipitation in the polygonalferrite.But the Cu precipitation can also occur in polygonal ferrite after theaustenite-ferrite transformation is finished.The micro-constituents such as dislocations,carbides (cementite) and migrating austenite/ferrite heterophase interfaces duringaustenite decompositionhave an effect on the nucleation, growth and coarsening ofcopper precipitates. APT studies indicate that not all Cu precipitates are formed on thedislocations with P segregation, because the austenite/ferrite heterophase interfacesare more likely to induce the Cu nucleation compared to dislocation. The carbide/matrix interfaces are the preferential sites for Cu nucleation, and the formation ofcarbides will contribute to the growth and coarsening of Cu precipitates. Theinterphase precipitation of Cu phases is significantly impacted by migration rate ofaustenite/ferrite interfaces and the actual cooling rate. The structural andcompositional evolution is the same as that for the isothermal aging.
Thesolution-quench microstructure of the Cu-Ni steels mainly consists of lathmartensite with Cu in solution. Duringtempering, the micro-hardness evolution wellreflects the microstructuralevolutionresulting from the softening of martensite, Cuprecipitation strengthening and reverse austenite toughening. The number density ofCu precipitates decrease whereas the sizes increase with increasing of temperingintensity. At the same time, the morphology evolve form sphere to ellipse. At theinitial nucleation stage, the Cu precipitates contains considerable high Fe content aswell as a small amount of Ni and Mn, which are prone to segregate at the matrix/Cuprecipitate interface at the later growth and coarsening stages.
By additional interstitial tempering in QT procedure, a microstructure of lath-likemartensite with dispersed reverse austenite at lath boundary and prior austenite grainboundary is obtained.The mechanical and thermal stability of the reverseaustenitewhich is in direct proportion to the content of alloying elements especially Niplays an important role in toughening at low temperature. Copper can diffuse into andstabilize the reverse austenite and precipitate out companying with the partialdecomposition of reverse austenite during tempering. Copper still in solution duringinterstitial temperingis the contributor for the strengthening Cu precipitates formed insubsequent tempering.
There are great difference in the final microstructure and thereby mechanicalproperties of the Cu-Ni steels. The disadvantages of SCC and SQCT processed steelsare lower temperature toughness and yield/tensile ratio, respectively, which can beoptimized by SQIT procedure. As to the shearable BCC coherent Cu precipitates, thestrength increments by the effects of chemical hardening, the coherency strain and themodulus strengthening are3-6,86and139MPa, respectively. For the incoherent,impenetrable FCC Cu precipitates, the strength increments by classical Orowanmechanism is18MPa. The critical transition size of Cu precipitates with differentstrengthening mechanism is calculated to be about2.9nm.
引文
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