多晶纯钴在动态塑性变形后的退火组织及变形孪晶研究
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摘要
本论文以具有密排六方结构(HCP)的纯钴样品为研究对象,首先利用X射线衍射(XRD)、电子背散射衍射(EBSD)和透射电子显微镜(TEM)对纯钴样品在动态塑性变形(DPD)后的退火组织进行了详细地表征和分析；用EBSD和高分辨透射电子显微镜(HRTEM)表征了在变形过程中产生的变形孪晶,并与准静态压缩变形(ND)形成的变形孪晶进行对比研究；利用位错分解的理论对DPD过程中产生的变形孪晶的形成机制进行了模拟研究。
对样品DPD后的退火组织进行研究发现：(1)钴从高温FCC相向低温HCP相转变时相变没有全部完成,室温下仍存在少量的FCC结构,约占8.5%。残留的FCC结构与HCP结构满足SN(Shoji-Nishiyama)的取向关系,即{111}FCC||{0001}HCP；<110>FCC||<1120>HCP。(2)残留的FCC结构的晶粒中发现存有∑3晶界,这种晶界是由于FCC结构的晶粒在退火过程中高角度随机自由晶界快速迁移导致。(3)873K温度下退火后,在HCP结构的晶粒中发现大量71.4°/<1120>特殊晶界,这种晶界的形成原因与FCC结构的晶粒中∑3晶界的形成原因不同,是由FCC→HCP马氏体相变导致,这种孪晶是相变孪晶。
对样品DPD后的微观组织随着变形量的增加产生的变化进行了研究,发现：(1)随着变形量增加,晶粒内部的层错附近出现锥面<1123>型位错,这些位错的产生会使样品在TEM测试时发生透射束和二次衍射束的相互干涉,从而形成莫尔条纹。同时,这种位错的出现表明,纯钴在DPD过程中启动了{1011}<1123>滑移系统,这种滑移系统的启动,能够更好地调节钴的塑性变形。(2)随着变形量的增大,各种变形孪晶界长度的相对百分含量发生变化。{1012}和{1121}两种拉伸孪晶的孪晶界长度相对百分含量随着变形量的增大急剧减少。{1122}、{1011}和{1013}三种压缩孪晶,其孪晶界长度的相对百分含量随着变形量的加大都有不同程度的增加。两种二次孪晶界长度的相对百分含量没有明显的变化。
对样品DPD后形成的孪晶形式及与ND后形成的孪晶形式对比研究发现：(1)钴在DPD和ND过程中都会产生七种变形孪晶,分别是两种拉伸孪晶{1012}、{1121},三种压缩孪晶{1122}、{1013}、{1011},和两种二次孪晶{1011}-{1012}、{1013}-{1012}。{1121}拉伸孪晶在DPD过程中更容易产生。(2)钴在DPD和ND过程中,同一个晶粒内部会产生多种变形孪晶,具体的孪晶形式与初始晶粒的取向有关。当初始晶粒的c轴与加载方向几乎垂直时,变形过程中此晶粒只产生拉伸孪晶。当初始晶粒的c轴与加载方向呈一定角度(如65。)时,晶粒在变形过程中会同时产生拉伸孪晶和压缩孪晶,甚至可能产生二次孪晶。(3)钴在DPD过程中产生的几种变形孪晶的孪晶界特征不同：其中{1012}变形孪晶的孪晶界呈现出曲折现象,这些曲折的地方是由于孪晶界出现的台阶导致,这些台阶的高度从一个原子层到十几个原子层不等,这些台阶造成了{1012}变形孪晶界的不连续性；钴在DPD过程中产生的{1121}孪晶界的形貌与{1012}孪晶界不同,没有出现台阶,而是一条连续笔直的晶界；{1011}变形孪晶在动态塑性变形过程中也会因为Zonal位错的原因产生台阶,而且,在{1011}孪晶界附近发现有<1123>位错,说明DPD可以使钴的{1011}<1123>滑移系统和{1011}<1012>孪生系统双重启动,从而更有利地在e轴方向发生塑性变形。
对纯钴在变形过程中产生的变形孪晶的形成机制模拟时发现,位错分解在变形孪晶的形成过程中起了重要作用。在加载应力下,全位错AB在{211ι}晶面和{101ι}晶面分解形成不同的孪生位错、不可滑移不全位错和可滑移的不全位错。其中,不可滑移不全位错会钉扎在两个孪生面之间,可滑移不全位错在加载应力下在(0002)面上滑移导致孪晶界的增长,孪生位错则可在加载应力下造成孪生剪切或者原子重组。在这三种不全位错的共同作用下,形成了钴在变形过程中形成的多种变形孪晶模式。
This thesis reports detailed investigations of the microstructure of polycrystalline cobalt during annealed process and room temperature dynamic plastic deformation (DPD), respectively. Microstructure observation of annealed cobalt was performed in an X-ray diffraction (XRD), in a scanning electron microscopy (SEM) with an electron backscatter diffracrion (EBSD) detector, and in a transmission electron microscopy (TEM) to investigate the annealing twins generated in polycrystalline cobalt containing face center cubic (FCC) and hexagonal close packed (HCP) phases during the annealed process. TEM and high-resolution TEM (HRTEM) were applied to characterize the multi-types of deformation twins of polycrystalline HCP cobalt during DPD. The relation of the dislocation dissociation and the formation of the deformation twins were discussed.
The investigation of annealed microstructure and annealing twins in FCC and HCP phases shows:(1) a small amount of high temperature (above690K) FCC phase is retained at room temperature, and there is a Shoji-Nishiyama orientation relationship between the low temperature HCP and the retained FCC phases of{111}FCC||{0001}HCP and<110>FCC||<1120> HCP-(2)∑3twin boundaries were observed in the retained FCC phase. These twins are produced during dissociation of fast moving random high-angle boundaries into a∑3boundary and another random high-angle boundary.(3) a high fraction of boundaries with twin misorientation of71.4°/<1120> is formed as a result of phase transformation from FCC to HCP following the Shoji-Nishiyama orientation relationship.
The investigation of variation of the microstructure of polycrystalline cobalt during DPD shows the results as following:(1) with the increasation of the strain, the<1123>-type dislocations have been observed in the vicinity of the stacking-faults, resulting in the fornation of moire fringes and activation of {1011}<1123> slip system.(2) with the increasation of the strain, the relative fractions of twin boundary length of various twins have been changed. Thereinto, the relative fractions of twin boundary length of tension twins have decreased acutely with the strain increasing. On the contrary, the relative fractions of twin boundary length of compression twins have increased with the strain increasing. The relative fractions of twin boundary length of double twins change unobviously with the strain increasing.
The detailed investigation of the characterization of deformation in polycrastalline cobalt during DPD shows the following results:(1) several deformation twinning modes including the tension twins of{1012} and{1121}, and compression twins of{1122},{1013} and{1011}, as well as double twins of{1011}-{1012} and{1013}-{1012} have been confirmed to take place during the deformations.(2) tension and compression twinning can take place in one grain. The c axes of most of the grains containing tension twins are nearly perpendicular to the compression direction, while the c axes of grains containing compounded twins are usually away from the compression direction. A similar twinning mode and microstructure of quasi-static compression have been found.(3) the twin boundaries of{1012} deformation twins can be regard as the step boundaries, which result in the unsuccessive characteristic. The height of the step contains the atomic player from one plater to more than ten players. The twin boundaries of{1121} deformation twins do not present step-like twin boundaries. The step-like twin boundaries are also observed in the {1011} deformation twin boundaries. In addition, a new slip system,{1011}<1123> is also activated, which can also provide strain in the c-axis direction. In other words, both the deformation twinning and the newly activated slip system can facilitate plastic strain in the c-axis direction in polycrystalline cobalt during DPD.
The discussion of the relation of the dislocation dissociation and the formation of the deformation twins shows that the dislocation dissociation has played an important role the nucleation of deformation twins of cobalt during deformation. The full dislocation of AB can dissociate different types of sessile partial dislocation, glissile partial dislocation and twinning partial dislocation in {211l} and{101l} panes under the applied stress. The sessile partial dislocations can pin at the intersection of the twinning planes, and the glissile partial dislocations glide to nucleate a twin on the (0002) planes, and the twinning partial dislocations can lead to the shear or the shuffle under the applied stress. The multi-types of deformation twins in polycrystalline cobalt can be generated by the reaction among the sessile partials, the glissile partialsand the twinning partials during deformation.
对样品DPD后的退火组织进行研究发现：(1)钴从高温FCC相向低温HCP相转变时相变没有全部完成,室温下仍存在少量的FCC结构,约占8.5%。残留的FCC结构与HCP结构满足SN(Shoji-Nishiyama)的取向关系,即{111}FCC||{0001}HCP；<110>FCC||<1120>HCP。(2)残留的FCC结构的晶粒中发现存有∑3晶界,这种晶界是由于FCC结构的晶粒在退火过程中高角度随机自由晶界快速迁移导致。(3)873K温度下退火后,在HCP结构的晶粒中发现大量71.4°/<1120>特殊晶界,这种晶界的形成原因与FCC结构的晶粒中∑3晶界的形成原因不同,是由FCC→HCP马氏体相变导致,这种孪晶是相变孪晶。
对样品DPD后的微观组织随着变形量的增加产生的变化进行了研究,发现：(1)随着变形量增加,晶粒内部的层错附近出现锥面<1123>型位错,这些位错的产生会使样品在TEM测试时发生透射束和二次衍射束的相互干涉,从而形成莫尔条纹。同时,这种位错的出现表明,纯钴在DPD过程中启动了{1011}<1123>滑移系统,这种滑移系统的启动,能够更好地调节钴的塑性变形。(2)随着变形量的增大,各种变形孪晶界长度的相对百分含量发生变化。{1012}和{1121}两种拉伸孪晶的孪晶界长度相对百分含量随着变形量的增大急剧减少。{1122}、{1011}和{1013}三种压缩孪晶,其孪晶界长度的相对百分含量随着变形量的加大都有不同程度的增加。两种二次孪晶界长度的相对百分含量没有明显的变化。
对样品DPD后形成的孪晶形式及与ND后形成的孪晶形式对比研究发现：(1)钴在DPD和ND过程中都会产生七种变形孪晶,分别是两种拉伸孪晶{1012}、{1121},三种压缩孪晶{1122}、{1013}、{1011},和两种二次孪晶{1011}-{1012}、{1013}-{1012}。{1121}拉伸孪晶在DPD过程中更容易产生。(2)钴在DPD和ND过程中,同一个晶粒内部会产生多种变形孪晶,具体的孪晶形式与初始晶粒的取向有关。当初始晶粒的c轴与加载方向几乎垂直时,变形过程中此晶粒只产生拉伸孪晶。当初始晶粒的c轴与加载方向呈一定角度(如65。)时,晶粒在变形过程中会同时产生拉伸孪晶和压缩孪晶,甚至可能产生二次孪晶。(3)钴在DPD过程中产生的几种变形孪晶的孪晶界特征不同：其中{1012}变形孪晶的孪晶界呈现出曲折现象,这些曲折的地方是由于孪晶界出现的台阶导致,这些台阶的高度从一个原子层到十几个原子层不等,这些台阶造成了{1012}变形孪晶界的不连续性；钴在DPD过程中产生的{1121}孪晶界的形貌与{1012}孪晶界不同,没有出现台阶,而是一条连续笔直的晶界；{1011}变形孪晶在动态塑性变形过程中也会因为Zonal位错的原因产生台阶,而且,在{1011}孪晶界附近发现有<1123>位错,说明DPD可以使钴的{1011}<1123>滑移系统和{1011}<1012>孪生系统双重启动,从而更有利地在e轴方向发生塑性变形。
对纯钴在变形过程中产生的变形孪晶的形成机制模拟时发现,位错分解在变形孪晶的形成过程中起了重要作用。在加载应力下,全位错AB在{211ι}晶面和{101ι}晶面分解形成不同的孪生位错、不可滑移不全位错和可滑移的不全位错。其中,不可滑移不全位错会钉扎在两个孪生面之间,可滑移不全位错在加载应力下在(0002)面上滑移导致孪晶界的增长,孪生位错则可在加载应力下造成孪生剪切或者原子重组。在这三种不全位错的共同作用下,形成了钴在变形过程中形成的多种变形孪晶模式。
This thesis reports detailed investigations of the microstructure of polycrystalline cobalt during annealed process and room temperature dynamic plastic deformation (DPD), respectively. Microstructure observation of annealed cobalt was performed in an X-ray diffraction (XRD), in a scanning electron microscopy (SEM) with an electron backscatter diffracrion (EBSD) detector, and in a transmission electron microscopy (TEM) to investigate the annealing twins generated in polycrystalline cobalt containing face center cubic (FCC) and hexagonal close packed (HCP) phases during the annealed process. TEM and high-resolution TEM (HRTEM) were applied to characterize the multi-types of deformation twins of polycrystalline HCP cobalt during DPD. The relation of the dislocation dissociation and the formation of the deformation twins were discussed.
The investigation of annealed microstructure and annealing twins in FCC and HCP phases shows:(1) a small amount of high temperature (above690K) FCC phase is retained at room temperature, and there is a Shoji-Nishiyama orientation relationship between the low temperature HCP and the retained FCC phases of{111}FCC||{0001}HCP and<110>FCC||<1120> HCP-(2)∑3twin boundaries were observed in the retained FCC phase. These twins are produced during dissociation of fast moving random high-angle boundaries into a∑3boundary and another random high-angle boundary.(3) a high fraction of boundaries with twin misorientation of71.4°/<1120> is formed as a result of phase transformation from FCC to HCP following the Shoji-Nishiyama orientation relationship.
The investigation of variation of the microstructure of polycrystalline cobalt during DPD shows the results as following:(1) with the increasation of the strain, the<1123>-type dislocations have been observed in the vicinity of the stacking-faults, resulting in the fornation of moire fringes and activation of {1011}<1123> slip system.(2) with the increasation of the strain, the relative fractions of twin boundary length of various twins have been changed. Thereinto, the relative fractions of twin boundary length of tension twins have decreased acutely with the strain increasing. On the contrary, the relative fractions of twin boundary length of compression twins have increased with the strain increasing. The relative fractions of twin boundary length of double twins change unobviously with the strain increasing.
The detailed investigation of the characterization of deformation in polycrastalline cobalt during DPD shows the following results:(1) several deformation twinning modes including the tension twins of{1012} and{1121}, and compression twins of{1122},{1013} and{1011}, as well as double twins of{1011}-{1012} and{1013}-{1012} have been confirmed to take place during the deformations.(2) tension and compression twinning can take place in one grain. The c axes of most of the grains containing tension twins are nearly perpendicular to the compression direction, while the c axes of grains containing compounded twins are usually away from the compression direction. A similar twinning mode and microstructure of quasi-static compression have been found.(3) the twin boundaries of{1012} deformation twins can be regard as the step boundaries, which result in the unsuccessive characteristic. The height of the step contains the atomic player from one plater to more than ten players. The twin boundaries of{1121} deformation twins do not present step-like twin boundaries. The step-like twin boundaries are also observed in the {1011} deformation twin boundaries. In addition, a new slip system,{1011}<1123> is also activated, which can also provide strain in the c-axis direction. In other words, both the deformation twinning and the newly activated slip system can facilitate plastic strain in the c-axis direction in polycrystalline cobalt during DPD.
The discussion of the relation of the dislocation dissociation and the formation of the deformation twins shows that the dislocation dissociation has played an important role the nucleation of deformation twins of cobalt during deformation. The full dislocation of AB can dissociate different types of sessile partial dislocation, glissile partial dislocation and twinning partial dislocation in {211l} and{101l} panes under the applied stress. The sessile partial dislocations can pin at the intersection of the twinning planes, and the glissile partial dislocations glide to nucleate a twin on the (0002) planes, and the twinning partial dislocations can lead to the shear or the shuffle under the applied stress. The multi-types of deformation twins in polycrystalline cobalt can be generated by the reaction among the sessile partials, the glissile partialsand the twinning partials during deformation.
引文
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