大变形异步叠轧与热处理调控超细晶铜组织结构与性能研究
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摘要
本文通过大变形异步叠轧与热处理调控铜材组织,制备出具有均匀孪晶的超细晶铜材,通过大变形异步叠轧与热处理工艺探索、铜材不同工艺阶段组织结构分析、再结晶铜材晶界类型及孪晶分析与形成条件理论计算、铜材变形织构与再结晶织构计算、各工艺条件铜材性能测试等研究手段,围绕大变形异步叠轧铜材微观结构分析与晶粒细化机制、再结晶形成超细孪晶结构铜材组织演变与再结晶机制、变形与再结晶织构演变规律和孪晶取向形成机制、制备出超细孪晶铜材力学性能和导电性等内容开展了系统的实验分析与理论研究。研究获得以下结果：
1.研究了异步叠轧变形过程中铜材内部组织和晶界结构的变化规律,分析获得异步叠轧晶粒细化过程分为三个阶段：
异步叠轧等效应变ε≤1.6时,剪切应力作用下形成S带,S带中纵横交错的位错墙,将S带进一步细化为5-10μM的位错胞结构；晶界发生滑动、晶粒内部晶面发生滑移,大晶粒内部产生很多小角度晶界。
异步叠轧等效应变2.4≤ε≤4.0时,S带消失,大部分形变晶粒中都形成2～3个小亚晶；在相邻晶粒的塑性变形及位错胞壁的聚集作用下,亚晶最终被分裂成不同的两个大角晶粒,使晶粒进一步细化,亚晶胞尺寸在0.5μm以下；位错的塞积团聚分布不均匀。
异步叠轧等效应变ε=4.8时,显微组织结构有两种典型特征：一是部分大晶粒内包含几个由位错胞包裹的小晶粒；二是内部位错密度很高的区域,形状不规则,杂乱无序的分布在各个形变晶粒之间。
2.研究了异步叠轧(ε=4.8)制备超细晶铜材再结晶过程中组织结构和界面演变,并获得再结晶机制与孪晶形成机制：
异步叠轧(ε=4.8)铜材再结晶退火过程中首先发生回复,铜材内位错攀移,对消,并规则排列在亚晶界,形成规整锋锐的亚晶结构；随退火时间延长,发生再结晶形核,由于亚晶在回复过程中形成有效的取向梯度,以及大变形异步叠轧时晶界处位错的交滑移等因素的影响,产生亚晶聚合粗化形核；最后在亚晶粗化聚合后,小角度晶界比例减小,大角度晶界比重增加,大角晶界向位错密度高的区域弓出迁移,直到与相邻的再结晶晶粒相遇,再结晶完成。
240℃再结晶退火20分钟开始,形成在晶界处最初的退火孪晶形核,随退火时间的延长,这种由亚晶胞壁内萌生的部分位错在此亚晶胞结构内向前扫过时,孪晶形核的前端向晶粒内部生长,便产生不同的孪晶界,最终在退火35～40分钟时,形成大量超细孪晶。
异步叠轧变形过程中铜材的低Σ CSL晶界逐渐被剪切变形破碎；再结晶过程中,形成∑3再激发模型,随着再结晶形核和晶粒长大,大角晶界逐步迁移的过程,构成Σ3-Σ9-∑3的晶界连接网络,达到铜材再结晶过程GBDC优化效果。
3.研究了异步叠轧变形和再结晶过程铜材织构演变过程：
经过均匀化退火,铜材内形成退火织构,但在异步叠轧过程中退火织构组分消失,其他织构组分较为复杂,主要为剪切织构({001}<110>)组分,随着等效应变量的增大,剪切织构组分的取向密度随之增强,在道次间去应力退火处理后,会生成较弱的立方织构({001}<100>)组分。
再结晶退火铜材的织构组分变化较大,残余的变形织构只剩剪切织构组分,而且它的取向密度随退火时间延长而减弱,但再结晶完成时并不能完全消除剪切织构组分；而随着再结晶过程,逐渐形成新的织构组分,其中{221}<114>实质上是异步叠轧形成的剪切织构再结晶退火时沿{111}面的镜面反映,而形成的孪晶取向。
4.研究了不同等效应变异步叠轧变形铜材、再结晶不同阶段铜材的显微硬度、单向静拉伸、疲劳性能和导电性能,结合铜材组织研究对其性能变化进行分析：
异步叠轧过程中,随等效应变量的增大,变形铜材的强度随之增高,但延伸率降低；异步叠轧(ε=4.8)铜材在240℃进行再结晶退火处理40分钟后获得强度与塑性较好超细孪晶铜。
异步叠轧过程中,随等效应变量的增大,变形铜材的疲劳寿命先增后减,在三道次异步叠轧(ε=2.4)时达到极大值；240℃再结晶退火40分钟时,超细孪晶铜材疲劳寿命达到极大值,抗拉强度也为最大值,其综合性能是最好的。
铜材的电导率在异步叠轧变形过程中随等效应变量的增大而减小,再结晶退火过程中,随退火时间延长而逐渐增加,形成超细孪晶对导电性提高较大。
本论文通过大变形异步叠轧与热处理组合调控超细晶铜材组织、界面结构,制备出组织均匀、高强度、高塑性及良好导电性的超细孪晶铜材。通过大变形异步叠轧方法制备出超细孪晶铜材,为超细晶材料的组织控制提供新的研究内容,也为制备块体尺寸超细孪晶铜材提供新的方法。关于利用调控大变形异步叠轧和热处理方法制备含有均匀超细孪晶结构铜材,及对其组织结构、织构演变过程的研究工作具有特色与创新,并对晶粒细化机制、再结晶孪晶机制进行分析和讨论。
In present thesis, structure evolution process of copper was regulated by Asymmetrical Accumulative Rolling Bonding(AARB) and heat treatment. By means of AARB and heat treatment technology searching, analysis of copper microstructure in different conditions, analysis and theoretical calculation of the twins and grain boundaries, calculation of texture in deformed and recrystallized process, testing of copper in every process condition, the deformation and grain refinement mechanism of copper deformed by AARB, ultrafine twins and recrystallization mechanism of copper, evolution of deformed and recrystallized texture to twin orientation, mechanical properties and electrical conductivity of copper were researched by experimental and theoretical analysis. The mainly results could be concluded as follows.
1. The evolution of the structure and grain boundary structure of copper deformed by AARB were studied. The process of grain refinement was obtained.
The copper with big grains was obtained by AARB when the equivalent strain(ε) was less than1.6, bands shaped like "S" were formed with the action of shear stress. The crisscrossed dislocation walls in "S" band refined the "S" band to smaller dislocation cells. Based on the slipping of grain boundaries and the slipping of crystal in grains, low-angle boundaries were produced in most of the big grains.
As copper deformed by AARB with the equivalent strain(ε) within2.4and4.0,"S" bands can't be obtained, and about2-3subgrains were obtained in most of deformed grains. With the effect of plastic deformation and gathering of dislocation walls, one sub-grain was divided to two grains. Deformed grains were refined to0.5μm, and distribution of piling up of dislocations was uneven.
2. Ultrafine copper was treated by recrystallization annealing when ε was4.8, and the microstructure and twins was observed, the results were as follows:
Recovering of deformed grains was observed first of all in the recrystallization annealing of copper deformed by AARB with ε was4.8, in this stage, cliping and compensation of dislocations in deformed grains had happened. The dislocations were lined up in subgrain boundaries, and neat subgrain structure was obtained. Along with the recrystallization annealing time, nucleation and growth happened during recrystallization. Due to the orientation gradient in subgrains in recovering stage, the subgrains occured aggregation and coarsening to nucleation. At last, the grains grown to adjacent grain boundaries approached. In that stage, low-angle boundaries decreased and high-angle boundaries increased with which migrated to the dislocation area of high density.
The original annealing twin nucleation was observed at grain boundary when recrystallization annealing for20minutes. Along with the annealing time, when the partial dislocation inside the subgrain boundary swept forward in the very subgrain cell structure, the annealing twin nucleation grown to the grain inside, and two of twin boundaries were produced. Finally annealing for35～40minutes, a plenty of ultrafine twins were obtained.
The low-Σ CSL grain boundries were broken crushed by AARB shearing deformation. According Σ3remotication model, the Σ3-Σ9-Σ3grain boundaries bonding formed with the growth of recrystallization nucleation and the migration of high-angle grain boundaries.
3. The evolution of texture of copper deformed by AARB with different s and recrystallization annealing for different times were observed, and the results showed as follows:
Annealing texture was obtained in copper after homogenizing annealing, and which disappeared in AARB deformation followed. The deformed texture was complex. But there was mainly shear texture ({001}<110>) whose density increased with the rise of ef fective strain s. The feeblish cube texture({001}<100>) was obtained after relief annealing in every twice passes.
Great changes had happened in copper during recrystallization. The shear texture was the only remained deformed texture, and whose density decreased with extension of annealing time. The new texture was obtained in recrystallization, in which texture {221}<114> was twin orientation, a mirror reflection of shear texture from AARB deformation along twinning plane{111}.
4. The micro hardness,tesile properties, fatigue properties and electrical conductivity of copper under different conditions were determined and the change of properties was analyzed.
During the course of AARB, the strength of copper increases with the rise ofε, but its elongation rate decreases. Ultrafine copper with good properties could be obtained when recrystallized annealing at240℃for40minutes.
During the course of AARB, the fatigue life of copper increases with the rise of ε; and it achieved the maximum at three passes deformed by AARB. Recrystallization annealing ultrafine copper achieved the maximum at240℃for40minutes, and its tensile strength got the maximum.
Electrical conductivity decreased with the rise of equivalent strain. During the recrystallization annealing, electrical conductivity of ultrafine copper increased with the annealing time extension. Ultral-fine annealing twins formed during recrystallization annealing increased the electrical conductivity of ultra-fine grain copper.
Ultra-fine grain copper possessing uniform structure, high strength and ductility, good electrical conductivity has been prepared by AARB and recrystallization annealing. Ultrafine-twin copper obtained by AARB was proposed firstly. This could provide new research contents to controling the stucture of ultrafine materials, and also provide a new method for preparing ultrafine-twin copper with block size. By means of regulating deformation by AARB and recrystallization annealing, preparation of ultrafine-twin copper and its structure and texture had not been reported yet, but this work was researched here, in the meantime, the mechanism of grain refinement and recrystallization twins formation were analyzed and discussed too.
1.研究了异步叠轧变形过程中铜材内部组织和晶界结构的变化规律,分析获得异步叠轧晶粒细化过程分为三个阶段：
异步叠轧等效应变ε≤1.6时,剪切应力作用下形成S带,S带中纵横交错的位错墙,将S带进一步细化为5-10μM的位错胞结构；晶界发生滑动、晶粒内部晶面发生滑移,大晶粒内部产生很多小角度晶界。
异步叠轧等效应变2.4≤ε≤4.0时,S带消失,大部分形变晶粒中都形成2～3个小亚晶；在相邻晶粒的塑性变形及位错胞壁的聚集作用下,亚晶最终被分裂成不同的两个大角晶粒,使晶粒进一步细化,亚晶胞尺寸在0.5μm以下；位错的塞积团聚分布不均匀。
异步叠轧等效应变ε=4.8时,显微组织结构有两种典型特征：一是部分大晶粒内包含几个由位错胞包裹的小晶粒；二是内部位错密度很高的区域,形状不规则,杂乱无序的分布在各个形变晶粒之间。
2.研究了异步叠轧(ε=4.8)制备超细晶铜材再结晶过程中组织结构和界面演变,并获得再结晶机制与孪晶形成机制：
异步叠轧(ε=4.8)铜材再结晶退火过程中首先发生回复,铜材内位错攀移,对消,并规则排列在亚晶界,形成规整锋锐的亚晶结构；随退火时间延长,发生再结晶形核,由于亚晶在回复过程中形成有效的取向梯度,以及大变形异步叠轧时晶界处位错的交滑移等因素的影响,产生亚晶聚合粗化形核；最后在亚晶粗化聚合后,小角度晶界比例减小,大角度晶界比重增加,大角晶界向位错密度高的区域弓出迁移,直到与相邻的再结晶晶粒相遇,再结晶完成。
240℃再结晶退火20分钟开始,形成在晶界处最初的退火孪晶形核,随退火时间的延长,这种由亚晶胞壁内萌生的部分位错在此亚晶胞结构内向前扫过时,孪晶形核的前端向晶粒内部生长,便产生不同的孪晶界,最终在退火35～40分钟时,形成大量超细孪晶。
异步叠轧变形过程中铜材的低Σ CSL晶界逐渐被剪切变形破碎；再结晶过程中,形成∑3再激发模型,随着再结晶形核和晶粒长大,大角晶界逐步迁移的过程,构成Σ3-Σ9-∑3的晶界连接网络,达到铜材再结晶过程GBDC优化效果。
3.研究了异步叠轧变形和再结晶过程铜材织构演变过程：
经过均匀化退火,铜材内形成退火织构,但在异步叠轧过程中退火织构组分消失,其他织构组分较为复杂,主要为剪切织构({001}<110>)组分,随着等效应变量的增大,剪切织构组分的取向密度随之增强,在道次间去应力退火处理后,会生成较弱的立方织构({001}<100>)组分。
再结晶退火铜材的织构组分变化较大,残余的变形织构只剩剪切织构组分,而且它的取向密度随退火时间延长而减弱,但再结晶完成时并不能完全消除剪切织构组分；而随着再结晶过程,逐渐形成新的织构组分,其中{221}<114>实质上是异步叠轧形成的剪切织构再结晶退火时沿{111}面的镜面反映,而形成的孪晶取向。
4.研究了不同等效应变异步叠轧变形铜材、再结晶不同阶段铜材的显微硬度、单向静拉伸、疲劳性能和导电性能,结合铜材组织研究对其性能变化进行分析：
异步叠轧过程中,随等效应变量的增大,变形铜材的强度随之增高,但延伸率降低；异步叠轧(ε=4.8)铜材在240℃进行再结晶退火处理40分钟后获得强度与塑性较好超细孪晶铜。
异步叠轧过程中,随等效应变量的增大,变形铜材的疲劳寿命先增后减,在三道次异步叠轧(ε=2.4)时达到极大值；240℃再结晶退火40分钟时,超细孪晶铜材疲劳寿命达到极大值,抗拉强度也为最大值,其综合性能是最好的。
铜材的电导率在异步叠轧变形过程中随等效应变量的增大而减小,再结晶退火过程中,随退火时间延长而逐渐增加,形成超细孪晶对导电性提高较大。
本论文通过大变形异步叠轧与热处理组合调控超细晶铜材组织、界面结构,制备出组织均匀、高强度、高塑性及良好导电性的超细孪晶铜材。通过大变形异步叠轧方法制备出超细孪晶铜材,为超细晶材料的组织控制提供新的研究内容,也为制备块体尺寸超细孪晶铜材提供新的方法。关于利用调控大变形异步叠轧和热处理方法制备含有均匀超细孪晶结构铜材,及对其组织结构、织构演变过程的研究工作具有特色与创新,并对晶粒细化机制、再结晶孪晶机制进行分析和讨论。
In present thesis, structure evolution process of copper was regulated by Asymmetrical Accumulative Rolling Bonding(AARB) and heat treatment. By means of AARB and heat treatment technology searching, analysis of copper microstructure in different conditions, analysis and theoretical calculation of the twins and grain boundaries, calculation of texture in deformed and recrystallized process, testing of copper in every process condition, the deformation and grain refinement mechanism of copper deformed by AARB, ultrafine twins and recrystallization mechanism of copper, evolution of deformed and recrystallized texture to twin orientation, mechanical properties and electrical conductivity of copper were researched by experimental and theoretical analysis. The mainly results could be concluded as follows.
1. The evolution of the structure and grain boundary structure of copper deformed by AARB were studied. The process of grain refinement was obtained.
The copper with big grains was obtained by AARB when the equivalent strain(ε) was less than1.6, bands shaped like "S" were formed with the action of shear stress. The crisscrossed dislocation walls in "S" band refined the "S" band to smaller dislocation cells. Based on the slipping of grain boundaries and the slipping of crystal in grains, low-angle boundaries were produced in most of the big grains.
As copper deformed by AARB with the equivalent strain(ε) within2.4and4.0,"S" bands can't be obtained, and about2-3subgrains were obtained in most of deformed grains. With the effect of plastic deformation and gathering of dislocation walls, one sub-grain was divided to two grains. Deformed grains were refined to0.5μm, and distribution of piling up of dislocations was uneven.
2. Ultrafine copper was treated by recrystallization annealing when ε was4.8, and the microstructure and twins was observed, the results were as follows:
Recovering of deformed grains was observed first of all in the recrystallization annealing of copper deformed by AARB with ε was4.8, in this stage, cliping and compensation of dislocations in deformed grains had happened. The dislocations were lined up in subgrain boundaries, and neat subgrain structure was obtained. Along with the recrystallization annealing time, nucleation and growth happened during recrystallization. Due to the orientation gradient in subgrains in recovering stage, the subgrains occured aggregation and coarsening to nucleation. At last, the grains grown to adjacent grain boundaries approached. In that stage, low-angle boundaries decreased and high-angle boundaries increased with which migrated to the dislocation area of high density.
The original annealing twin nucleation was observed at grain boundary when recrystallization annealing for20minutes. Along with the annealing time, when the partial dislocation inside the subgrain boundary swept forward in the very subgrain cell structure, the annealing twin nucleation grown to the grain inside, and two of twin boundaries were produced. Finally annealing for35～40minutes, a plenty of ultrafine twins were obtained.
The low-Σ CSL grain boundries were broken crushed by AARB shearing deformation. According Σ3remotication model, the Σ3-Σ9-Σ3grain boundaries bonding formed with the growth of recrystallization nucleation and the migration of high-angle grain boundaries.
3. The evolution of texture of copper deformed by AARB with different s and recrystallization annealing for different times were observed, and the results showed as follows:
Annealing texture was obtained in copper after homogenizing annealing, and which disappeared in AARB deformation followed. The deformed texture was complex. But there was mainly shear texture ({001}<110>) whose density increased with the rise of ef fective strain s. The feeblish cube texture({001}<100>) was obtained after relief annealing in every twice passes.
Great changes had happened in copper during recrystallization. The shear texture was the only remained deformed texture, and whose density decreased with extension of annealing time. The new texture was obtained in recrystallization, in which texture {221}<114> was twin orientation, a mirror reflection of shear texture from AARB deformation along twinning plane{111}.
4. The micro hardness,tesile properties, fatigue properties and electrical conductivity of copper under different conditions were determined and the change of properties was analyzed.
During the course of AARB, the strength of copper increases with the rise ofε, but its elongation rate decreases. Ultrafine copper with good properties could be obtained when recrystallized annealing at240℃for40minutes.
During the course of AARB, the fatigue life of copper increases with the rise of ε; and it achieved the maximum at three passes deformed by AARB. Recrystallization annealing ultrafine copper achieved the maximum at240℃for40minutes, and its tensile strength got the maximum.
Electrical conductivity decreased with the rise of equivalent strain. During the recrystallization annealing, electrical conductivity of ultrafine copper increased with the annealing time extension. Ultral-fine annealing twins formed during recrystallization annealing increased the electrical conductivity of ultra-fine grain copper.
Ultra-fine grain copper possessing uniform structure, high strength and ductility, good electrical conductivity has been prepared by AARB and recrystallization annealing. Ultrafine-twin copper obtained by AARB was proposed firstly. This could provide new research contents to controling the stucture of ultrafine materials, and also provide a new method for preparing ultrafine-twin copper with block size. By means of regulating deformation by AARB and recrystallization annealing, preparation of ultrafine-twin copper and its structure and texture had not been reported yet, but this work was researched here, in the meantime, the mechanism of grain refinement and recrystallization twins formation were analyzed and discussed too.
引文
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