阳极铝箔工艺过程和立方织构的研究
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摘要
电解电容器是电子工业的三大基础元件之一，电容器用阳极铝箔是制造优质铝电解电容器的关键材料。为了实现阳极铝箔的国产化，替代进口产品并填补国产优质中、高压电解电容器阳极铝箔的空白，本文对阳极铝箔的立方织构形成及演变和工艺过程进行了较深入的研究。
本文首先对电解电容器用中、高压阳极铝箔的研究与生产现状进行综述，分析了国内外关于Fe、Si、Cu等化学成分对阳极铝箔性能影响，关于晶粒大小、位错密度、晶体取向等组织结构因素对阳极箔比电容影响的研究结果等文献。结合具体的工艺路线，分析研究了从均匀化退火、热轧温度、预备退火、附加退火、最终冷轧变形率到成品退火等的研究与工艺现状，及这些因素对铝箔最终退火立方织构比例影响规律和机制的国内外研究进展。在对热轧工艺的综述过程中，抓住了热轧工艺对原始取向的影响和Fe、Si杂质的存在状态两大研究线索。根据以上文献研究和生产工艺现状，设计了针对低铁硅和高铁硅原料分别进行试验的总体方案。
介绍了本文研究所用到的微织构分析试验，阐述了EBSD取向成像分析技术的原理，并就本文研究所用的LEO1530扫描电镜及所用软件，以及扫描电镜的新技术作了介绍。在对立方织构进行研究的过程中，为实现工业用快速织构检测，尤其是立方织构的快速定量分析，本文借鉴国外硅铁织构腐蚀坑形状分析的文献，发展了高纯铝箔快速织构检测方法，并总结了蚀坑法的理论依据和操作方法。
本文对乌铝(国产乌鲁木齐高纯铝)的工艺过程和立方织构进行了系统研究，重点研究了以低Fe、Si含量的高纯铝乌铝原料进行生产的工艺过程与立方织构的关系。通过对热终轧温度不同的热轧板进行预备退火、冷轧和成品退火试验及成品立方织构的定量检测，研究热终轧温度、预备退火温度、成品退火工艺对立方织构比例的影响规律。通过光学金相阳极复膜晶粒形态观察、扫描电镜组织形态观察、透射电镜析出物分布及高倍组织观察等实验手段，分析了乌铝立方织构演变的规律及影响成品立方织构比例的主要因素，提出低铁硅含量高纯铝阳极箔的成品退火织构中，立方织构的比例由原始(001)面晶粒比例、S织构强弱、析出物对再结晶的影响、铁硅的存在形式等共同决定。对乌铝立方织构的演变及影响因素进行了综合分析，为高纯铝阳极箔的生产工艺提供理论依据。
本文对较高Fe、Si含量的高纯铝——美铝(美国高纯铝)的工艺过程与立方织构的关系进行了比较研究。通过采用不同的预备退火温度、冷轧过程中附加的部分再结晶退火(即附加退火)不同的退火温度、附加退火后最终冷轧(即附加轧制)
重庆大学博士学位论文
不同的变形率、不同成品退火工艺等的组合试验及成品立方织构的定量检测，研究
预备退火温度、附加退火温度、附加轧制变形率及成品退火工艺对立方织构比例的
影响规律。优化出了适用于较高Fe、Si含量的高纯铝(美铝)的阳极铝箔生产工艺
参数，并对美铝工艺过程中立方织构的演变特点进行了分析。
在上述试验的基础上，本文针对乌铝和美铝中立方织构的演变及其它相关现象
作了研究分析。采用了扫描电镜微区取向成像技术进行微织构分析，研究高纯铝立
方织构演变及变形织构经多工艺环节向立方退火织构转变的规律，并结合热分析试
验结果及讨论，分析了生产过程的各种影响因素及作用机制。
通过本文的研究，确定了热轧和预备退火工艺参数的变化对立方织构的影响规
律及生产中应控制的范围，掌握了冷轧变形及附加退火工艺参数对成品箔立方织构
的影响规律。结合本文在热终轧温度、预备退火温度、附加轧制和附加退火温度的
关联性方面的重要研究进展，建立了优化阳极箔生产过程工艺参数和参数选择的依
据。研究成果已在工业生产中得到成功应用。
Electrolytic capacitor is one of the three basic electronic components, capacitor anode aluminum foil is the key material for high quality electrolytic capacitors. In order to develop domestic capacitor anode aluminum foil and to reduce the import of high voltage electrolytic capacitors, this thesis worked on the evolution of cube texture and making techniques of anode aluminum foil.
Current process and research status quo of anode aluminum foil for high voltage electrolytic capacitors was summarized firstly in this paper, including the influence of chemical composition such as Fe Si Cu on the properties of anode aluminum foil, the influence of microstructures such as grain size, dislocation density, crystal orientation on specific capacitance of anode aluminum foil. Relating to practical processes, the paper analyzed the technologic status quo of homogenizing, hot rolling, preparing anneal, additional anneal, additional rolling deformation and last anneal, and the rule and mechanism research development of their effects on cube texture ratio in aluminum foil after last anneal. From the summary of hot rolling processes, the effect of original orientation and status of Fe, Si impurities were taken as important research objects. According to above research and technologic status quo, the total project focused on aluminum foils with low Fe, Si impurity and high Fe, Si impurity respectively
The paper introduced the analysis experiment of micro-texture, stated the technological principle of EBSD orientation image, and introduced the LEO 1530 scanning electronic microscope and its software as well as some new techniques. In order to achieve quick test for industrial texture, and especially to measure cube texture quantitatively, by means of foreign references related to etch pit shape in silicon steel, the method of industrial texture quick test for high purity aluminum was developed by this paper. The test method and skill of etch pit experiments were also summarized.
The paper systematically researched the processing and the cube texture of Wu aluminum (high purity aluminum produced by Urumchi, China), emphasized the relationship between technological processes and cube texture of Wu aluminum containing low Fe, Si impurity. By tests of preparing anneal, cold rolling, last anneal and quantitative measurement of cube texture for finished product, the effect rule of hot finish rolling temperature, preparing anneal temperature, last anneal technique on the cube texture ratio was obtained. By observation of grain shape with positive electrode oxiding
film, microstructure under SEM, precipitation distribution and microstructure under TEM, as well as other test methods, the rules of cube texture development and the main factors effecting cube texture ratio in Wu aluminum were analyzed. It was suggested that the cube texture ratio in the finished product of high purity anode foil with low Fe, Si content depended on the following: the original ratio of (001) grains, amount of S orientation, the effect of precipitation on recrystallization, the status of Fe, Si in aluminum. The development of cube texture in Wu aluminum and its effecting factors were roundly analyzed, which could provide reference to the production of high purity anode aluminum foil.
The relationship between the processing and the cube texture of Mei aluminum (American high purity aluminum) containing high Fe, Si impurity was studied too in the paper. With quantitative measurement of cube texture in finished products, the effects of preparing anneal temperatures, additional partial recrystallization anneal temperatures, deformation rates of additional cold rolling and different processes for finished product anneal on the cube texture ratio were studied. The process variables were optimized to produce anode foil with high purity aluminum containing more Fe and Si content, and the development character of cube texture during technological process of Mei aluminum was analyzed and discussed.
On the basis of above experiments, the paper studied the developmen
本文首先对电解电容器用中、高压阳极铝箔的研究与生产现状进行综述，分析了国内外关于Fe、Si、Cu等化学成分对阳极铝箔性能影响，关于晶粒大小、位错密度、晶体取向等组织结构因素对阳极箔比电容影响的研究结果等文献。结合具体的工艺路线，分析研究了从均匀化退火、热轧温度、预备退火、附加退火、最终冷轧变形率到成品退火等的研究与工艺现状，及这些因素对铝箔最终退火立方织构比例影响规律和机制的国内外研究进展。在对热轧工艺的综述过程中，抓住了热轧工艺对原始取向的影响和Fe、Si杂质的存在状态两大研究线索。根据以上文献研究和生产工艺现状，设计了针对低铁硅和高铁硅原料分别进行试验的总体方案。
介绍了本文研究所用到的微织构分析试验，阐述了EBSD取向成像分析技术的原理，并就本文研究所用的LEO1530扫描电镜及所用软件，以及扫描电镜的新技术作了介绍。在对立方织构进行研究的过程中，为实现工业用快速织构检测，尤其是立方织构的快速定量分析，本文借鉴国外硅铁织构腐蚀坑形状分析的文献，发展了高纯铝箔快速织构检测方法，并总结了蚀坑法的理论依据和操作方法。
本文对乌铝(国产乌鲁木齐高纯铝)的工艺过程和立方织构进行了系统研究，重点研究了以低Fe、Si含量的高纯铝乌铝原料进行生产的工艺过程与立方织构的关系。通过对热终轧温度不同的热轧板进行预备退火、冷轧和成品退火试验及成品立方织构的定量检测，研究热终轧温度、预备退火温度、成品退火工艺对立方织构比例的影响规律。通过光学金相阳极复膜晶粒形态观察、扫描电镜组织形态观察、透射电镜析出物分布及高倍组织观察等实验手段，分析了乌铝立方织构演变的规律及影响成品立方织构比例的主要因素，提出低铁硅含量高纯铝阳极箔的成品退火织构中，立方织构的比例由原始(001)面晶粒比例、S织构强弱、析出物对再结晶的影响、铁硅的存在形式等共同决定。对乌铝立方织构的演变及影响因素进行了综合分析，为高纯铝阳极箔的生产工艺提供理论依据。
本文对较高Fe、Si含量的高纯铝——美铝(美国高纯铝)的工艺过程与立方织构的关系进行了比较研究。通过采用不同的预备退火温度、冷轧过程中附加的部分再结晶退火(即附加退火)不同的退火温度、附加退火后最终冷轧(即附加轧制)
重庆大学博士学位论文
不同的变形率、不同成品退火工艺等的组合试验及成品立方织构的定量检测，研究
预备退火温度、附加退火温度、附加轧制变形率及成品退火工艺对立方织构比例的
影响规律。优化出了适用于较高Fe、Si含量的高纯铝(美铝)的阳极铝箔生产工艺
参数，并对美铝工艺过程中立方织构的演变特点进行了分析。
在上述试验的基础上，本文针对乌铝和美铝中立方织构的演变及其它相关现象
作了研究分析。采用了扫描电镜微区取向成像技术进行微织构分析，研究高纯铝立
方织构演变及变形织构经多工艺环节向立方退火织构转变的规律，并结合热分析试
验结果及讨论，分析了生产过程的各种影响因素及作用机制。
通过本文的研究，确定了热轧和预备退火工艺参数的变化对立方织构的影响规
律及生产中应控制的范围，掌握了冷轧变形及附加退火工艺参数对成品箔立方织构
的影响规律。结合本文在热终轧温度、预备退火温度、附加轧制和附加退火温度的
关联性方面的重要研究进展，建立了优化阳极箔生产过程工艺参数和参数选择的依
据。研究成果已在工业生产中得到成功应用。
Electrolytic capacitor is one of the three basic electronic components, capacitor anode aluminum foil is the key material for high quality electrolytic capacitors. In order to develop domestic capacitor anode aluminum foil and to reduce the import of high voltage electrolytic capacitors, this thesis worked on the evolution of cube texture and making techniques of anode aluminum foil.
Current process and research status quo of anode aluminum foil for high voltage electrolytic capacitors was summarized firstly in this paper, including the influence of chemical composition such as Fe Si Cu on the properties of anode aluminum foil, the influence of microstructures such as grain size, dislocation density, crystal orientation on specific capacitance of anode aluminum foil. Relating to practical processes, the paper analyzed the technologic status quo of homogenizing, hot rolling, preparing anneal, additional anneal, additional rolling deformation and last anneal, and the rule and mechanism research development of their effects on cube texture ratio in aluminum foil after last anneal. From the summary of hot rolling processes, the effect of original orientation and status of Fe, Si impurities were taken as important research objects. According to above research and technologic status quo, the total project focused on aluminum foils with low Fe, Si impurity and high Fe, Si impurity respectively
The paper introduced the analysis experiment of micro-texture, stated the technological principle of EBSD orientation image, and introduced the LEO 1530 scanning electronic microscope and its software as well as some new techniques. In order to achieve quick test for industrial texture, and especially to measure cube texture quantitatively, by means of foreign references related to etch pit shape in silicon steel, the method of industrial texture quick test for high purity aluminum was developed by this paper. The test method and skill of etch pit experiments were also summarized.
The paper systematically researched the processing and the cube texture of Wu aluminum (high purity aluminum produced by Urumchi, China), emphasized the relationship between technological processes and cube texture of Wu aluminum containing low Fe, Si impurity. By tests of preparing anneal, cold rolling, last anneal and quantitative measurement of cube texture for finished product, the effect rule of hot finish rolling temperature, preparing anneal temperature, last anneal technique on the cube texture ratio was obtained. By observation of grain shape with positive electrode oxiding
film, microstructure under SEM, precipitation distribution and microstructure under TEM, as well as other test methods, the rules of cube texture development and the main factors effecting cube texture ratio in Wu aluminum were analyzed. It was suggested that the cube texture ratio in the finished product of high purity anode foil with low Fe, Si content depended on the following: the original ratio of (001) grains, amount of S orientation, the effect of precipitation on recrystallization, the status of Fe, Si in aluminum. The development of cube texture in Wu aluminum and its effecting factors were roundly analyzed, which could provide reference to the production of high purity anode aluminum foil.
The relationship between the processing and the cube texture of Mei aluminum (American high purity aluminum) containing high Fe, Si impurity was studied too in the paper. With quantitative measurement of cube texture in finished products, the effects of preparing anneal temperatures, additional partial recrystallization anneal temperatures, deformation rates of additional cold rolling and different processes for finished product anneal on the cube texture ratio were studied. The process variables were optimized to produce anode foil with high purity aluminum containing more Fe and Si content, and the development character of cube texture during technological process of Mei aluminum was analyzed and discussed.
On the basis of above experiments, the paper studied the developmen
引文
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