ECAP制备超细晶铜的组织演变、织构特征及力学性能研究
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摘要
基于大塑性纯剪切变形的ECAP技术能够有效的细化晶粒,在近年来受到了广泛的关注,但是人们对该变形过程及材料组织的变形机理尤其是织构的形成和转变过程尚缺乏全面的认识。本文系统的研究了多晶纯铜和定向凝固纯铜在ECAP中的变形过程、应变机理、织构特征和力学性能。首先用刚塑性弹性体模型对纯铜在ECAP中的模具结构、背压方式、流变行为以及温度变化和材料的应变及再结晶机理进行了模拟研究;然后用普通多晶纯铜和定向凝固纯铜分别进行了多路径、多道次的ECAP变形实验,制备出了超细晶材料;对比分析了各道次变形后试样的组织演变过程和不同原始组织纯铜在ECAP中的变形机理和XRD宏观取向特征。在此基础上,采用EBSD技术进一步对变形前几道次材料的织构特征进行了对比研究;最后,分别用2套模具对不同原始组织和不同模具结构下纯铜的力学性能进行了对比分析。主要结论如下:
1.通过有限元模拟发现,材料在进入ECAP剪切变形区后不同阶段处于不同的应力状态,试样内层为压应力,外层为压应力—拉应力—压应力的变化过程;在变形过程中纯铜的温度会发生显著变化,引起动态再结晶,变形结束后材料内部形成混晶结构;较小的模具内角和适当增加背压,能够有效提高变形后材料的组织均匀性;多道次ECAP变形能够有效地细化晶粒,但不同路径对晶粒细化的效果不同;普通多晶材料变形后的晶粒无明确的取向,但定向凝固组织用A路径细化后的亚晶具有定向排列特征,用Bc路径变形后的组织出现胞状结构。
2.多晶纯铜在ECAP中的变形过程为:晶界移动、晶粒转动、晶粒被拉长、晶粒被细化,晶粒内部发生了滑移和机械孪生并伴随着动态再结晶过程;多道次变形后,多晶铜的微观结构特征是含有高密度位错的大角度晶界等轴晶组织以及晶界上的非平衡结构;随着应变量增大,多晶组织位相差随剪切变形量的增加而增大;在大角度晶界数量增加的同时,晶粒更加趋于均匀化,使取向差分布的峰值不断向大角度晶界分布的中心移动。
3.定向凝固纯铜在ECAP变形过程中,塑性变形比多晶更容易发生;A路径和C路径变形时位错的定向运动导致亚晶排列具有明显的方向性,晶内形成了与基体组织取向差较大且延伸方向与压力轴方向基本一致的岛状结构,岛状结构的面积随着应变量增加而不断扩大,亚晶界逐渐向外扩展,在原始平直晶界上产生应变不对称性,引起柱状晶界破碎后的亚晶逐渐呈现出随机分布特征;Bc路径变形时晶粒内位错运动积聚后形成胞状结构,继续挤压后晶粒从胞壁处被分割,原始组织被不断细化。在小应变量下,晶粒内无孪晶出现,出现伪织构;晶内位错的分布特征与晶粒的应力状态密切相关,而且与基体存在明显的差异。
4.变形路径和模具结构对2种材料的力学性能影响不同,较小的模具角度下材料性能的变化较快;随着挤压道次的增加,材料逐渐从韧性断裂向脆性断裂方向发展,材料组织均匀化程度提高;多道次挤压后2种材料的硬度大幅度提高;ECAP后超细晶T2铜高周疲劳没有明显的疲劳极限。
5.原始组织对纯铜ECAP中的力学性能影响明显,挤压后晶粒的定向排列和单位体积内细晶数目增多两方面的原因促使定向凝固纯铜在多道次挤压中塑性稳步提高;而多晶铜在变形时位错在晶界附近积聚,在后续的挤压中晶粒的取向不会发生较大改变,晶粒被细化后晶界大幅度增加,变形抗力加大,其塑性变化出现波动。
分析认为,多晶铜在变形过程中各晶粒在变形中既相互阻碍,又相互促进,晶粒旋转方式的不同造成了多晶材料晶粒取向分布的差异性;塑性变形初期形成分布杂乱的位错缠结,变形量增加后形成胞状结构,胞壁位错纠结后不断凝集变为二维界面,形成小角度亚晶界或大角度晶界,从而实现组织的超细化。材料的细化机制概括为:剪切应变—位错分割—形变孪生强化—界面竞争消失(晶粒得到细化)。
原始晶粒的取向对形变结构具有重要影响。随着应变量增加,引起亚晶界的应变不对称性,并且进一步在柱状晶内部形成应变梯度,一部分亚晶界从小角度晶界向大角度晶界转变,逐渐形成混合分布特征。
塑性变形多晶材料的织构形成过程中晶粒从宏观“无序”向微观“有序”的转变,织构的演变又是从微观“有序”向宏观“有序”的转变,整个转变过程为:宏观“无序”微观“有序”宏观“有序”,存在“织构起伏”效应。“织构起伏”效应是材料组织在一定的温度和外力作用下的综合应变反映,其强度和方向与材料的应变状态密切相关,该过程连续作用的结果,将是材料组织均匀性不断提高的过程。材料内部新织构的产生与消失是晶群在受到外力作用后偏聚方向发生变化、内应力向相邻晶界传递的过程中,原来的聚集状态被破坏所致。
本研究将对原始组织影响织构形态、晶界特征在ECAP变形中的演变规律、织构与材料性能间的关系及加工过程中材料的均匀化过程有新的认识,尤其对塑性各向异性的变形响应及强度的不对称性变化过程具有重要的理论意义。
The equal channel angle pressing (ECAP) pure shear deformation that based on the super plastic deformation (SPD) technology can refinment the grains effectively, has received widespread concern in recent years, as yet, the research of the deformation process, especially the microstructure deformation mechanism and the texture changing process during the deformation process, lack of comprehensive understanding. This paper systematically studied the deformation process, strain mechanism, texture characteristic and mechanical property of polycrystalline pure copper and directional solidification pure copper during ECAP. First, use the plastic elastomer model, studied the die structure, backpressure, rheological behaviour, temperature changing and materials strain and recrystallization mechanism, then performed the experiments use polycrystalline and unidirectional solidification pure copper through multipath and multipass, respectively. Comparison and analysis of the deformation mechanism and XRD macro orientation characteristic of different original microstructure after ECAP, on the basis, using EBSD technology contrast studied the texture characteristics of the first few passes. Finally, analyzed the mechanical properties of pure copper that ECAPed by different mould structure, main conclusions are as follows:
1. Simulated by the finite element method, found that the sample was in different stress state at different stages in the ECAP shear deformation zone. The press stress was inside of the specimen, and the state of the surface was pressure stress–tensile stress - pressure stress. In the deformation process, temperature of the samples will have a significant changing. This will causing dynamic recrystallization. At the end of the deformation, mixed crystal structure formed inside of the material. Smaller inner-angle and appropriate increase the back pressure can improve the uniformity of the materials microstrusture during deformation. Many times ECAP deformation can effectively refinement the grain size, but different routes has different effects on the grain refinement. After deformation, the grains of the polycrystalline didn’t have a clear orientation, but the sub grains that deformated by route A of the solidification pure copper refined by route A, shows a obvious arrangement, and the microstructure that deformated by route Bc shows a cellular structure.
2. The deformation process of polycrystalline pure copper during ECAP is: crystal boundary migration, grain rotations, grain was elongated and then the grains were refined. Sliping and twinning accompaning with dynamic recrystallization in the grain interiors. After ECAPing, the microstructure of the polycrystalline copper is non-equilibrium structure at the grain boundaries and a high density dislocations and high angle grain boundaries (HAGBs). With the strain increasing, the oritation differecce of the microstrustrue of polycopper increasing with the strain, with the number of HAGBs increasing, the crystal grain become more uniform and the distribution peak of orientation kept moving to the center of HAGBs.
3. During the deformation of ECAP, the plastic deformation of directional solidification pure copper is more easily than polycrystalline copper. When deformated by route A and route C, dislocations moving within grains causing formed the island-like structure, continues to deformation, the area of the island-like structure is enlarged with the stain amount, causeing the ordernering transformation and the subgrain boundaries moving to the outsides, causing a strain unsymmetrical, the column grain refined and the subgrains shows a random distribution characteristic; when deformed by route Bc, the moving of dislocations resulted to cell structure. With the strains increasing, the original microstruture was refined. At small strains, there was no twins occurring in the grains but formed the fake texture.
4. The deformation routes and the die structure has different effect on the materials mechanical property, the mechanics changing rapid at the small die angles, with the deformation times increasing, the sample fracture developing from tough to brittle model, the homogeneity increasing, the hardness of the two kinds materials increasing and the high circle fatigue has no obvious fatigued limitation.
5. The original microstructure affected the mechanical properties of pure copper ECAP is obviously. The directional arrangement of grains and the increasing of fine-crystal grain in unit volume, causing the plasticity of directional solidification pure copper improved steadily after many times deformation, the dislocations accumulated to the grain boundaries (GBs) when the deformation occurred in polycrystalline copper, in the subsequent extrusion, grain orientations did not changing much, GBs increased greatly after be thinned, then the plastic shows a fluctuate charictristic.
Analysis that grains of polycrystalline copper affected each other during the deformation process. The different rotatation mode of the grains resulted the oritation difference in polycrystalline copper. In earlier of plastic deformation, formed the disorderly dislocation tangle, when increasing deformation times, formed the cellular structures, the dislocations tangled and accumulated to the two-dimensional boundaries at the cell boundaries, formed the low angle subgrain boundaries (LAGBs) and HAGBs, causing the refinement of the grains. The refining mechanism can be summed as: shear strain -- dislocations division -- deformated twins strengthen– GBs competition disappearance (the grains were refined).
The original grains orientation has an important influence on deformation structure. With the increasing of strain, causing the asymmetry of subgrain boundaries and formed the strain gradient in the internal of the columnar grains, then arosing the strain gradient, some GBs transferred from LAGBs to HAGBs, then gradually formed the mixed distribution characteristic.
During the course of plastic deformation of polycrystalline materials, the grains transformed from macroscopic "disorder" to microcosmic "order", the evolution of the texture is from microcosmic "order" to macroscopic "order", the whole changing process as follow: macro "disorder" micro "order" macro "order". Shows a " texture heave" effect.
The " texture heave" effect is the materials integrated strain reflect under certain temperature and external force. Its strength and direction are closely related to the materials strain state. The result of this continuously process will causing the uniformity improvement of the material microstructures. The arise and disappearance of new textures in materials is the original states of grains strain were damaged by external force in the processes of the change of partially gathered direction and inner-stresses were transferred to adjacent boundaries.
This study will be on influence of texture formation from original microstructure, the evolution rule of the grains during ECAP deformation, the relationship between the texture and the materials mechanical property and material uniformity during machining process. This study has important theoretical significance, especially for the deformation response of plastic anisotropic and the asymmetry changing process of the meteries intensity.
1.通过有限元模拟发现,材料在进入ECAP剪切变形区后不同阶段处于不同的应力状态,试样内层为压应力,外层为压应力—拉应力—压应力的变化过程;在变形过程中纯铜的温度会发生显著变化,引起动态再结晶,变形结束后材料内部形成混晶结构;较小的模具内角和适当增加背压,能够有效提高变形后材料的组织均匀性;多道次ECAP变形能够有效地细化晶粒,但不同路径对晶粒细化的效果不同;普通多晶材料变形后的晶粒无明确的取向,但定向凝固组织用A路径细化后的亚晶具有定向排列特征,用Bc路径变形后的组织出现胞状结构。
2.多晶纯铜在ECAP中的变形过程为:晶界移动、晶粒转动、晶粒被拉长、晶粒被细化,晶粒内部发生了滑移和机械孪生并伴随着动态再结晶过程;多道次变形后,多晶铜的微观结构特征是含有高密度位错的大角度晶界等轴晶组织以及晶界上的非平衡结构;随着应变量增大,多晶组织位相差随剪切变形量的增加而增大;在大角度晶界数量增加的同时,晶粒更加趋于均匀化,使取向差分布的峰值不断向大角度晶界分布的中心移动。
3.定向凝固纯铜在ECAP变形过程中,塑性变形比多晶更容易发生;A路径和C路径变形时位错的定向运动导致亚晶排列具有明显的方向性,晶内形成了与基体组织取向差较大且延伸方向与压力轴方向基本一致的岛状结构,岛状结构的面积随着应变量增加而不断扩大,亚晶界逐渐向外扩展,在原始平直晶界上产生应变不对称性,引起柱状晶界破碎后的亚晶逐渐呈现出随机分布特征;Bc路径变形时晶粒内位错运动积聚后形成胞状结构,继续挤压后晶粒从胞壁处被分割,原始组织被不断细化。在小应变量下,晶粒内无孪晶出现,出现伪织构;晶内位错的分布特征与晶粒的应力状态密切相关,而且与基体存在明显的差异。
4.变形路径和模具结构对2种材料的力学性能影响不同,较小的模具角度下材料性能的变化较快;随着挤压道次的增加,材料逐渐从韧性断裂向脆性断裂方向发展,材料组织均匀化程度提高;多道次挤压后2种材料的硬度大幅度提高;ECAP后超细晶T2铜高周疲劳没有明显的疲劳极限。
5.原始组织对纯铜ECAP中的力学性能影响明显,挤压后晶粒的定向排列和单位体积内细晶数目增多两方面的原因促使定向凝固纯铜在多道次挤压中塑性稳步提高;而多晶铜在变形时位错在晶界附近积聚,在后续的挤压中晶粒的取向不会发生较大改变,晶粒被细化后晶界大幅度增加,变形抗力加大,其塑性变化出现波动。
分析认为,多晶铜在变形过程中各晶粒在变形中既相互阻碍,又相互促进,晶粒旋转方式的不同造成了多晶材料晶粒取向分布的差异性;塑性变形初期形成分布杂乱的位错缠结,变形量增加后形成胞状结构,胞壁位错纠结后不断凝集变为二维界面,形成小角度亚晶界或大角度晶界,从而实现组织的超细化。材料的细化机制概括为:剪切应变—位错分割—形变孪生强化—界面竞争消失(晶粒得到细化)。
原始晶粒的取向对形变结构具有重要影响。随着应变量增加,引起亚晶界的应变不对称性,并且进一步在柱状晶内部形成应变梯度,一部分亚晶界从小角度晶界向大角度晶界转变,逐渐形成混合分布特征。
塑性变形多晶材料的织构形成过程中晶粒从宏观“无序”向微观“有序”的转变,织构的演变又是从微观“有序”向宏观“有序”的转变,整个转变过程为:宏观“无序”微观“有序”宏观“有序”,存在“织构起伏”效应。“织构起伏”效应是材料组织在一定的温度和外力作用下的综合应变反映,其强度和方向与材料的应变状态密切相关,该过程连续作用的结果,将是材料组织均匀性不断提高的过程。材料内部新织构的产生与消失是晶群在受到外力作用后偏聚方向发生变化、内应力向相邻晶界传递的过程中,原来的聚集状态被破坏所致。
本研究将对原始组织影响织构形态、晶界特征在ECAP变形中的演变规律、织构与材料性能间的关系及加工过程中材料的均匀化过程有新的认识,尤其对塑性各向异性的变形响应及强度的不对称性变化过程具有重要的理论意义。
The equal channel angle pressing (ECAP) pure shear deformation that based on the super plastic deformation (SPD) technology can refinment the grains effectively, has received widespread concern in recent years, as yet, the research of the deformation process, especially the microstructure deformation mechanism and the texture changing process during the deformation process, lack of comprehensive understanding. This paper systematically studied the deformation process, strain mechanism, texture characteristic and mechanical property of polycrystalline pure copper and directional solidification pure copper during ECAP. First, use the plastic elastomer model, studied the die structure, backpressure, rheological behaviour, temperature changing and materials strain and recrystallization mechanism, then performed the experiments use polycrystalline and unidirectional solidification pure copper through multipath and multipass, respectively. Comparison and analysis of the deformation mechanism and XRD macro orientation characteristic of different original microstructure after ECAP, on the basis, using EBSD technology contrast studied the texture characteristics of the first few passes. Finally, analyzed the mechanical properties of pure copper that ECAPed by different mould structure, main conclusions are as follows:
1. Simulated by the finite element method, found that the sample was in different stress state at different stages in the ECAP shear deformation zone. The press stress was inside of the specimen, and the state of the surface was pressure stress–tensile stress - pressure stress. In the deformation process, temperature of the samples will have a significant changing. This will causing dynamic recrystallization. At the end of the deformation, mixed crystal structure formed inside of the material. Smaller inner-angle and appropriate increase the back pressure can improve the uniformity of the materials microstrusture during deformation. Many times ECAP deformation can effectively refinement the grain size, but different routes has different effects on the grain refinement. After deformation, the grains of the polycrystalline didn’t have a clear orientation, but the sub grains that deformated by route A of the solidification pure copper refined by route A, shows a obvious arrangement, and the microstructure that deformated by route Bc shows a cellular structure.
2. The deformation process of polycrystalline pure copper during ECAP is: crystal boundary migration, grain rotations, grain was elongated and then the grains were refined. Sliping and twinning accompaning with dynamic recrystallization in the grain interiors. After ECAPing, the microstructure of the polycrystalline copper is non-equilibrium structure at the grain boundaries and a high density dislocations and high angle grain boundaries (HAGBs). With the strain increasing, the oritation differecce of the microstrustrue of polycopper increasing with the strain, with the number of HAGBs increasing, the crystal grain become more uniform and the distribution peak of orientation kept moving to the center of HAGBs.
3. During the deformation of ECAP, the plastic deformation of directional solidification pure copper is more easily than polycrystalline copper. When deformated by route A and route C, dislocations moving within grains causing formed the island-like structure, continues to deformation, the area of the island-like structure is enlarged with the stain amount, causeing the ordernering transformation and the subgrain boundaries moving to the outsides, causing a strain unsymmetrical, the column grain refined and the subgrains shows a random distribution characteristic; when deformed by route Bc, the moving of dislocations resulted to cell structure. With the strains increasing, the original microstruture was refined. At small strains, there was no twins occurring in the grains but formed the fake texture.
4. The deformation routes and the die structure has different effect on the materials mechanical property, the mechanics changing rapid at the small die angles, with the deformation times increasing, the sample fracture developing from tough to brittle model, the homogeneity increasing, the hardness of the two kinds materials increasing and the high circle fatigue has no obvious fatigued limitation.
5. The original microstructure affected the mechanical properties of pure copper ECAP is obviously. The directional arrangement of grains and the increasing of fine-crystal grain in unit volume, causing the plasticity of directional solidification pure copper improved steadily after many times deformation, the dislocations accumulated to the grain boundaries (GBs) when the deformation occurred in polycrystalline copper, in the subsequent extrusion, grain orientations did not changing much, GBs increased greatly after be thinned, then the plastic shows a fluctuate charictristic.
Analysis that grains of polycrystalline copper affected each other during the deformation process. The different rotatation mode of the grains resulted the oritation difference in polycrystalline copper. In earlier of plastic deformation, formed the disorderly dislocation tangle, when increasing deformation times, formed the cellular structures, the dislocations tangled and accumulated to the two-dimensional boundaries at the cell boundaries, formed the low angle subgrain boundaries (LAGBs) and HAGBs, causing the refinement of the grains. The refining mechanism can be summed as: shear strain -- dislocations division -- deformated twins strengthen– GBs competition disappearance (the grains were refined).
The original grains orientation has an important influence on deformation structure. With the increasing of strain, causing the asymmetry of subgrain boundaries and formed the strain gradient in the internal of the columnar grains, then arosing the strain gradient, some GBs transferred from LAGBs to HAGBs, then gradually formed the mixed distribution characteristic.
During the course of plastic deformation of polycrystalline materials, the grains transformed from macroscopic "disorder" to microcosmic "order", the evolution of the texture is from microcosmic "order" to macroscopic "order", the whole changing process as follow: macro "disorder" micro "order" macro "order". Shows a " texture heave" effect.
The " texture heave" effect is the materials integrated strain reflect under certain temperature and external force. Its strength and direction are closely related to the materials strain state. The result of this continuously process will causing the uniformity improvement of the material microstructures. The arise and disappearance of new textures in materials is the original states of grains strain were damaged by external force in the processes of the change of partially gathered direction and inner-stresses were transferred to adjacent boundaries.
This study will be on influence of texture formation from original microstructure, the evolution rule of the grains during ECAP deformation, the relationship between the texture and the materials mechanical property and material uniformity during machining process. This study has important theoretical significance, especially for the deformation response of plastic anisotropic and the asymmetry changing process of the meteries intensity.
引文
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