基于MEMS技术的超级电容器三维微电极阵列制备及表征方法研究
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摘要
微型超级电容器是一种具有储能密度高、放电功率大、循环寿命长、体积小、充电速度快、可靠性好、污染小等特点的新型储能器件，是信息、电子、仪表、能源、交通和国防安全等领域重要的关键部件。论文针对如何解决微型超级电容器三维微电极加工及其表面功能薄膜制备关键技术难题，开展基于MEMS (MicroElectro Mechanical System)技术的超级电容器三维微电极阵列结构制备关键技术研究，具有重要的科学意义和实际应用价值。
本文针对微型超级电容器亟待解决的三维微电极加工及其表面功能薄膜制备技术难题，提出基于MEMS技术制备三维微电极阵列结构，在结构表面采用电化学方法沉积电极活性物质薄膜制备超级电容器三维微电极阵列的思路。分析了超级电容器电极性能与结构的关系，建立了三维微电极阵列电场分布模型；研究了基于硅基的SU-8胶和体硅三维微电极阵列结构设计与制备方法，采用恒电流、恒电压、脉冲等电化学沉积方法，在柱状、条状、梳齿、硅基井状等三维微电极阵列结构表面沉积氧化锰、氧化钌、聚苯胺薄膜等作为电极活性功能薄膜，成功研制出三维微电极阵列。采用扫描电镜、循环伏安、恒流充放电等多种表征方法对制备的电极进行了表征。基于聚焦离子束刻蚀方法，研究了导电薄膜电极分离技术，成功实现了超级电容器正电极和负电极的有效分离，研究了导电聚合物胶体电解质，突破了基于MEMS技术制备超级电容器的电极分离和封装关键技术，在硅基上成功研制出微型超级电容器原理样品。本文的研究主要工作：
①综述了超级电容器微型电极的研究现状与发展趋势，分析了现有各种微型电极制备方法存在的不足，提出了基于MEMS技术的微型超级电容器三维微电极阵列制备的整体思路；
②分析了超级电容器电极形貌、电极间距与性能的关系，采用有限元方法对三维微电极阵列的电场分布进行了分析，建立了电场有限元模型，研究了电极形状、电极尺寸、电极间距等因素对电场的影响，优化了三维微电极阵列结构参数；
③基于MEMS技术，提出了基于硅基SU-8胶和体硅三维微电极阵列结构设计与加工方法，使用电化学方法在三维微电极阵列结构表面沉积活性物质薄膜制备电极的方法。研究了SU-8胶微结构制备过程中的应力问题，解决了SU-8胶微电极阵列结构与基底结合力的关键问题；研究了体硅三维微电极阵列结构制备方法，解决了刻蚀过程中的“草地”和“黑硅”问题；
④研究了在三维微电极阵列结构表面沉积电极活性物质薄膜的制备方法和三维微电极阵列表面形貌表征及电化学性能表征；采用恒电压、恒电流方法沉积氧化锰薄膜，采用恒电压和循环伏安方法合成聚苯胺薄膜，以双电极方波脉冲方法制备氧化钌薄膜。采用扫描电镜、能谱仪和X射线衍射仪对三维微电极表面活性物质形貌及成分进行了表征，使用电化学工作站对电极进行循环伏安特性、交流阻抗特性、恒流充放电特性测试，完成了对微电极的测试与分析；
⑤研究了聚焦离子束刻蚀分离电极技术，成功分离了微型超级电容器的正、负电极；研制了导电聚合物胶体电解质等，解决了微型超级电容器电极分离、封装难题，在硅基上成功研制出基于MEMS技术的三维微电极阵列结构微型超级电容器，比容量可达33.05mF/cm2。
The micro-supercapacitor is a new type of energy storage device with high energystorage density, high-power discharge, long cycle life, small size, charge speed, goodreliability, little pollution and so on, it is key components of information, electronics,instrumentation, energy, transportation, aerospace and National defense and security.Based on MEMS technology, the thesis focuses on solving key technical problems ofthe three-dimensional micro-supercapacitor electrode processing and its surfacefunctional film preparation, carried out supercapacitor three-dimensional microelectrodearray structure fabrication technology research, which possess important scientificsignificance and practical value.
In this paper, we aiming at the urgent technology problem need to be solved formicro supercapacitor three dimensional micro electrode processing and surface functionfilm preparing, we proposed preparation of three-dimensional microelectrode arraystructure based on MEMS technology, and directly deposit the electrode activesubstance film on the three-dimensional microelectrode array structure surface by theelectrochemical method, then fabricated microelectrode array by this way. Analysisedthe relationship between morphology, spacing and the performance ofmicro-supercapacitor three-dimensional microelectrode array structure, and establishedthe electric field distribution model of three-dimensional micro-electrode array. Andstudied the design and preparation methods of SU–8photoresist and bulk siliconthree-dimensional microelectrode array structures. Galvanostatic, constant potential,pulse electrochemical deposition method were used to deposited manganese oxide,ruthenium oxide, polyaniline functional film as an electrode active substance on thesurface of the columnar, strip, comb, silicon based hole three-dimensionalmicro-electrode array structure. Three-dimensional micro-electrode array weresuccessfully prepared; Used scanning electron microscopy, cyclic voltammetry, constantcurrent charge-discharge method to characterize the electrodes character. Based on thefocused ion beam etching method, this paper studied the conductive film electrodeseparation technology, successfully separated the supercapacitor positive electrode andnegative electrode, researched and prepared the conductive polymer gel electrolyte,broke through the key techniques of supercapacitor electrode separation and packagebased on MEMS technology, and successfully fabricated a miniature super capacitor sample on the silicon. The main research works of this paper is listed as fellow:
①Reviewed the status and development trends of the supercapacitormicroelectrode research, and analysised the existing shortcomings of the microelectrodepreparation method. The idea of the preparation micro-supercapacitor three-dimensionalmicroelectrode array based on MEMS technology was proposed.
②Analysised the relationship between the micro supercapacitor three-dimensional microelectrode morphology, electrode distance and miniature supercapacitor performance, using finite element method analysis the distribution of theelectric field of the three-dimensional microelectrode array, the finite element model ofthe electric field of the three-dimensional micro-electrode array had been built, theinfluence of electric field of different electrode array morphology, size and distance hadbeen researched, the structure parameters of the three-dimensional microelectrode arrayhad been optimized.
③Based on MEMS technology, we proposed design and processing method ofthree-dimensional micro-electrode array structure using the SU-8photoresist and siliconmaterial, and used electrochemical methods to deposit the active material film on thesurface of three-dimensional microelectrode array structure for prepare electrode.Studied the stress problem of SU-8photoresist micro-structure during the preparationprocess, and solved the key issues of binding force of the SU-8photoresistmicroelectrode array structure and the silicon substrate; Studied the preparation methodof the three-dimensional microelectrode array structure using silicon as the material andresolved the problem of “grass "and" black silicon" in the etching process.
④Studied the preparation of electrode active material film in three-dimensionalmicroelectrode array structure surface, characterized surface morphology andelectrochemical properties of three-dimensional microelectrode array. Constant voltage,constant current method was used electro-deposition manganese oxide films, usingconstant voltage and cyclic voltammetry method to synthesize Polyaniline film,ruthenium oxide films had been prepared by dual-electrode square wave pulse. Theelectrode structure and the surface morphology and composition of the active materialfilm had been characterized by scanning electron microscopy, energy dispersivespectroscopy and X-ray diffraction. Electrochemical workstation was used to test themicroelectrode with cyclic voltammetry, AC impedance characteristics, constant currentcharge and discharge characteristics method, and completed the testing and analysis ofthe microelectrode.
⑤Researched the separation electrode technology using focused ion beam etching,successfully separated the positive and negative electrodes of the micro-supercapacitor.Studied and prepared the conductive polymer gel electrolyte, and solve the problem ofthe micro-supercapacitor electrode separation and supercapacitor package based onMEMS technology, and successfully prepared a micro-supercapacitor withthree-dimensional micro array electrode structure on a silicon substrate based on MEMS,specific capacity can reach33.05mF/cm2.
本文针对微型超级电容器亟待解决的三维微电极加工及其表面功能薄膜制备技术难题，提出基于MEMS技术制备三维微电极阵列结构，在结构表面采用电化学方法沉积电极活性物质薄膜制备超级电容器三维微电极阵列的思路。分析了超级电容器电极性能与结构的关系，建立了三维微电极阵列电场分布模型；研究了基于硅基的SU-8胶和体硅三维微电极阵列结构设计与制备方法，采用恒电流、恒电压、脉冲等电化学沉积方法，在柱状、条状、梳齿、硅基井状等三维微电极阵列结构表面沉积氧化锰、氧化钌、聚苯胺薄膜等作为电极活性功能薄膜，成功研制出三维微电极阵列。采用扫描电镜、循环伏安、恒流充放电等多种表征方法对制备的电极进行了表征。基于聚焦离子束刻蚀方法，研究了导电薄膜电极分离技术，成功实现了超级电容器正电极和负电极的有效分离，研究了导电聚合物胶体电解质，突破了基于MEMS技术制备超级电容器的电极分离和封装关键技术，在硅基上成功研制出微型超级电容器原理样品。本文的研究主要工作：
①综述了超级电容器微型电极的研究现状与发展趋势，分析了现有各种微型电极制备方法存在的不足，提出了基于MEMS技术的微型超级电容器三维微电极阵列制备的整体思路；
②分析了超级电容器电极形貌、电极间距与性能的关系，采用有限元方法对三维微电极阵列的电场分布进行了分析，建立了电场有限元模型，研究了电极形状、电极尺寸、电极间距等因素对电场的影响，优化了三维微电极阵列结构参数；
③基于MEMS技术，提出了基于硅基SU-8胶和体硅三维微电极阵列结构设计与加工方法，使用电化学方法在三维微电极阵列结构表面沉积活性物质薄膜制备电极的方法。研究了SU-8胶微结构制备过程中的应力问题，解决了SU-8胶微电极阵列结构与基底结合力的关键问题；研究了体硅三维微电极阵列结构制备方法，解决了刻蚀过程中的“草地”和“黑硅”问题；
④研究了在三维微电极阵列结构表面沉积电极活性物质薄膜的制备方法和三维微电极阵列表面形貌表征及电化学性能表征；采用恒电压、恒电流方法沉积氧化锰薄膜，采用恒电压和循环伏安方法合成聚苯胺薄膜，以双电极方波脉冲方法制备氧化钌薄膜。采用扫描电镜、能谱仪和X射线衍射仪对三维微电极表面活性物质形貌及成分进行了表征，使用电化学工作站对电极进行循环伏安特性、交流阻抗特性、恒流充放电特性测试，完成了对微电极的测试与分析；
⑤研究了聚焦离子束刻蚀分离电极技术，成功分离了微型超级电容器的正、负电极；研制了导电聚合物胶体电解质等，解决了微型超级电容器电极分离、封装难题，在硅基上成功研制出基于MEMS技术的三维微电极阵列结构微型超级电容器，比容量可达33.05mF/cm2。
The micro-supercapacitor is a new type of energy storage device with high energystorage density, high-power discharge, long cycle life, small size, charge speed, goodreliability, little pollution and so on, it is key components of information, electronics,instrumentation, energy, transportation, aerospace and National defense and security.Based on MEMS technology, the thesis focuses on solving key technical problems ofthe three-dimensional micro-supercapacitor electrode processing and its surfacefunctional film preparation, carried out supercapacitor three-dimensional microelectrodearray structure fabrication technology research, which possess important scientificsignificance and practical value.
In this paper, we aiming at the urgent technology problem need to be solved formicro supercapacitor three dimensional micro electrode processing and surface functionfilm preparing, we proposed preparation of three-dimensional microelectrode arraystructure based on MEMS technology, and directly deposit the electrode activesubstance film on the three-dimensional microelectrode array structure surface by theelectrochemical method, then fabricated microelectrode array by this way. Analysisedthe relationship between morphology, spacing and the performance ofmicro-supercapacitor three-dimensional microelectrode array structure, and establishedthe electric field distribution model of three-dimensional micro-electrode array. Andstudied the design and preparation methods of SU–8photoresist and bulk siliconthree-dimensional microelectrode array structures. Galvanostatic, constant potential,pulse electrochemical deposition method were used to deposited manganese oxide,ruthenium oxide, polyaniline functional film as an electrode active substance on thesurface of the columnar, strip, comb, silicon based hole three-dimensionalmicro-electrode array structure. Three-dimensional micro-electrode array weresuccessfully prepared; Used scanning electron microscopy, cyclic voltammetry, constantcurrent charge-discharge method to characterize the electrodes character. Based on thefocused ion beam etching method, this paper studied the conductive film electrodeseparation technology, successfully separated the supercapacitor positive electrode andnegative electrode, researched and prepared the conductive polymer gel electrolyte,broke through the key techniques of supercapacitor electrode separation and packagebased on MEMS technology, and successfully fabricated a miniature super capacitor sample on the silicon. The main research works of this paper is listed as fellow:
①Reviewed the status and development trends of the supercapacitormicroelectrode research, and analysised the existing shortcomings of the microelectrodepreparation method. The idea of the preparation micro-supercapacitor three-dimensionalmicroelectrode array based on MEMS technology was proposed.
②Analysised the relationship between the micro supercapacitor three-dimensional microelectrode morphology, electrode distance and miniature supercapacitor performance, using finite element method analysis the distribution of theelectric field of the three-dimensional microelectrode array, the finite element model ofthe electric field of the three-dimensional micro-electrode array had been built, theinfluence of electric field of different electrode array morphology, size and distance hadbeen researched, the structure parameters of the three-dimensional microelectrode arrayhad been optimized.
③Based on MEMS technology, we proposed design and processing method ofthree-dimensional micro-electrode array structure using the SU-8photoresist and siliconmaterial, and used electrochemical methods to deposit the active material film on thesurface of three-dimensional microelectrode array structure for prepare electrode.Studied the stress problem of SU-8photoresist micro-structure during the preparationprocess, and solved the key issues of binding force of the SU-8photoresistmicroelectrode array structure and the silicon substrate; Studied the preparation methodof the three-dimensional microelectrode array structure using silicon as the material andresolved the problem of “grass "and" black silicon" in the etching process.
④Studied the preparation of electrode active material film in three-dimensionalmicroelectrode array structure surface, characterized surface morphology andelectrochemical properties of three-dimensional microelectrode array. Constant voltage,constant current method was used electro-deposition manganese oxide films, usingconstant voltage and cyclic voltammetry method to synthesize Polyaniline film,ruthenium oxide films had been prepared by dual-electrode square wave pulse. Theelectrode structure and the surface morphology and composition of the active materialfilm had been characterized by scanning electron microscopy, energy dispersivespectroscopy and X-ray diffraction. Electrochemical workstation was used to test themicroelectrode with cyclic voltammetry, AC impedance characteristics, constant currentcharge and discharge characteristics method, and completed the testing and analysis ofthe microelectrode.
⑤Researched the separation electrode technology using focused ion beam etching,successfully separated the positive and negative electrodes of the micro-supercapacitor.Studied and prepared the conductive polymer gel electrolyte, and solve the problem ofthe micro-supercapacitor electrode separation and supercapacitor package based onMEMS technology, and successfully prepared a micro-supercapacitor withthree-dimensional micro array electrode structure on a silicon substrate based on MEMS,specific capacity can reach33.05mF/cm2.
引文
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