直接甲醇燃料电池膜电极的制备及电化学性能研究
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摘要
膜电极(MEA)是直接甲醇燃料电池(DMFC)的核心部件, MEA的性能较大程度地决定了DMFC的电池性能,因此制备高性能的MEA就显得非常重要。本论文针对主动式和自呼吸式DMFC的MEA进行了研究,包括MEA的制备方法和MEA催化层与扩散层组成与结构的优化,同时分析了MEA热压工艺的影响机制以及MEA的活化机制,并考察了主动式DMFC的工作条件。
系统研究了MEA热压工艺(热压温度、热压压力和热压时间)对电极结构与性能的影响,并利用电化学阻抗谱(EIS)分析了MEA热压工艺的影响机制。研究表明采用135℃热压温度,80 kg·cm-2热压压力,热压时间为90 s制备的MEA性能较好,在电池温度为80℃时,最大功率密度可达到46.0mW·cm-2,此MEA具有较小的欧姆电阻、电化学反应电阻和传质阻抗。
比较了不同的MEA催化层的制备工艺,SEM(Scanning electronmicroscopy)和AFM(Atomicforcemicroscopy)等分析结果表明,刮涂法制备的催化层表面裂纹较少,表面粗糙度较小,其MEA性能较好,并发现催化层表面形貌和表面粗糙度对MEA性能影响较小。同时优化了膜电极催化层中Nafion含量,发现阳极和阴极催化层中最佳的Nafion含量分别为34mass %和28 mass %,膜电极催化层中最佳的Nafion含量与催化层内催化剂的金属含量无关。
优化了MEA阳极扩散层的组成与结构,发现采用未浸渍聚四氟乙烯(PTFE)的碳纸作为阳极扩散层基底,碳粉与10 mass % Nafion混合物作为阳极微孔层的MEA性能最好。通过自制可视化单体电池,研究阳极产物CO2在不同阳极扩散层的析出和传质规律,发现憎水型阳极扩散层不利于阳极产物CO2的顺利排出。优化了MEA阴极扩散层的组成,发现阴极扩散层基底中较佳的PTFE含量为16 mass %。PTFE含量较少(20 mass %PTFE)的阴极微孔层有利于缓解阴极催化层的水淹,提高MEA的长时间放电性能。
考察了不同MEA活化方法对MEA的结构与性能的影响,通过EIS和电化学活性面积的测试并辅以SEM和XRD(X-ray diffraction)分析,对MEA活化机制进行研究,结果表明MEA中催化剂颗粒在活化过程中会发生长大,但活化过程可以打开电极的孔结构,提高电极的电化学活性面积。详细考察了主动式DMFC的工作条件,发现阳极甲醇水溶液的浓度更大程度地决定DMFC的性能,甲醇水溶液的流量对DMFC性能影响较小。对于主动式DMFC,不需要对阴极氧气进行加湿处理。
针对自呼吸式DMFC阴极存在较严重的水淹问题,设计了“内吸水”和“外吸水”两种自呼吸式MEA阴极结构。研究发现,在MEA阴极微孔层添加15 mass %的SiO2而构成“外吸水”式阴极结构,有利于提高MEA的性能,并可以提高阴极扩散层的亲水性及其排水能力,缓解阴极的水淹。另外,设计了一种“集流体内置型”自呼吸式DMFC的MEA新结构,把原本用作阴极集流体的薄金属网直接嵌入阴极催化层中。相比传统型MEA,此新型MEA具有更小的欧姆电阻、较好的氧气传输性和水管理能力,MEA的最大功率密度提高了10.3 %。
The membrane electrode assembly (MEA) was a key component of directmethanol fuel cell (DMFC), and the performance of the DMFC was greatly dependenton the performance of MEA. In this thesis, the MEAs of the active DMFC andair-breathing DMFC were investigated. The MEA fabrication methods were studied,and the compositions and the structures of the catalyst layers and gas diffusion layers(GDLs) of the MEAs were optimized. The mechanism of the effect of MEAhot-pressing technologies, and the mechanism of MEA activation were also analysed.Moreover, the operation parameters of active DMFC were studied.
The effects of the MEA hot-pressing technologies (hot-pressing temperatures,pressures and time) on the performances and structures of the MEA were detailedlyinvestigated. The mechanism analysis of the effects of MEAhot-pressing technologieswere revealed by electrochemical impedance spectroscopies (EIS). It was concludedthat the MEA which was hot pressed at 135℃under 80 kg cm-2 for 90 s showed thehighest power density (46.0 mW·cm-2 at cell temperature of 80℃), and the MEA hadthe lower cell resistance, electrochemical reaction resistance and diffusion resistance.
The fabrication methods for MEA catalyst layers were investigated. SEM andAFM analyses revealed that the scraping method was a little more profitable forimproving the cell performance due to the more flat and smooth (the surface roughnesswas lower) surface of the scraped catalyst layer. It was concluded that the surfacemorphology and roughness of the catalyst layer had less effect on the performance ofthe MEA. The optimum Nafion content in the catalyst layer was also investigated, andthe optimum Nafion content in the anode and cathode catalyst layer was 34 mass %and 28mass %, respectively. The optimum Nafion content in the catalyst layer was notrelated to the metal content of the catalyst.
The compositions and the structures of anode GDL were optimized. It wasrevealed that the MEA which consisted of the untreated carbon paper and hydrophilicanode micro-porous layer (comprised carbon black and 10mass% Nafion) showed thebest performance. The evolution and diffusion characteristics of anode CO2 gasbubbles on different anode GDLs were investigated using home-made transparentsingle cell. It was observed that the hydrophobic anode GDL was not helpful for improving the CO2 gas transport in the anode GDL. It was found that the optimumPTFE content in the cathode backing layerwas 16 mass%. The MEA with much lowerPTFE content (20mass % PTFE) in the cathode MPL was more beneficial for cathodewater releasing and the long-term operation.
The effects of MEA activation methods on the structures and performances of theMEAs were studied. And the MEA activation mechanism was investigated by EIStests, electrochemical surface areas tests, SEM and XRD analyses. Although theparticle sizes of the catalysts in the electrodes increased during the MEA activationprocess, the electrochemical surface areas of the catalysts were increased because thepores in the electrodes were opened after the activation. The influences of the celloperation parameters on the performances of active DMFC were also researched.Compared with anode flow rate of methanol solution, the concentration of methanolsolution was more influential on the performance of active DMFC. It was found thatthere was no need to humidify the cathode oxygen of the active DMFC.
In consideration of the water flooding in the cathode catalyst layer and cathodeGDL of air-breathing DMFC, two improved“Inner-water-absorption”and“Outer-water-absorption”cathode structures were proposed. It was revealed that the“Outer-water- absorption”cathode structure with 15 mass %SiO2 in the cathode MPLwas more suitable for the improvement of performance of MEA due to the increasingof hydrophilic water transport paths in the cathode MPL, thus the water floodings inthe cathode were alleviated. Moreover, a novel“current collector inside”air-breathingMEA was proposed, in which a thin metal mesh used as the cathode current collectorwas directly embedded in the cathode catalyst layer of this novel MEA cathode. Thenovel MEA showed better cell performance (increased 10.3 %) and long-termoperation performance than the conventional one because of the lower cell resistance,enhanced oxygen transport and increased water removal rate in such a novel MEAstructure.
系统研究了MEA热压工艺(热压温度、热压压力和热压时间)对电极结构与性能的影响,并利用电化学阻抗谱(EIS)分析了MEA热压工艺的影响机制。研究表明采用135℃热压温度,80 kg·cm-2热压压力,热压时间为90 s制备的MEA性能较好,在电池温度为80℃时,最大功率密度可达到46.0mW·cm-2,此MEA具有较小的欧姆电阻、电化学反应电阻和传质阻抗。
比较了不同的MEA催化层的制备工艺,SEM(Scanning electronmicroscopy)和AFM(Atomicforcemicroscopy)等分析结果表明,刮涂法制备的催化层表面裂纹较少,表面粗糙度较小,其MEA性能较好,并发现催化层表面形貌和表面粗糙度对MEA性能影响较小。同时优化了膜电极催化层中Nafion含量,发现阳极和阴极催化层中最佳的Nafion含量分别为34mass %和28 mass %,膜电极催化层中最佳的Nafion含量与催化层内催化剂的金属含量无关。
优化了MEA阳极扩散层的组成与结构,发现采用未浸渍聚四氟乙烯(PTFE)的碳纸作为阳极扩散层基底,碳粉与10 mass % Nafion混合物作为阳极微孔层的MEA性能最好。通过自制可视化单体电池,研究阳极产物CO2在不同阳极扩散层的析出和传质规律,发现憎水型阳极扩散层不利于阳极产物CO2的顺利排出。优化了MEA阴极扩散层的组成,发现阴极扩散层基底中较佳的PTFE含量为16 mass %。PTFE含量较少(20 mass %PTFE)的阴极微孔层有利于缓解阴极催化层的水淹,提高MEA的长时间放电性能。
考察了不同MEA活化方法对MEA的结构与性能的影响,通过EIS和电化学活性面积的测试并辅以SEM和XRD(X-ray diffraction)分析,对MEA活化机制进行研究,结果表明MEA中催化剂颗粒在活化过程中会发生长大,但活化过程可以打开电极的孔结构,提高电极的电化学活性面积。详细考察了主动式DMFC的工作条件,发现阳极甲醇水溶液的浓度更大程度地决定DMFC的性能,甲醇水溶液的流量对DMFC性能影响较小。对于主动式DMFC,不需要对阴极氧气进行加湿处理。
针对自呼吸式DMFC阴极存在较严重的水淹问题,设计了“内吸水”和“外吸水”两种自呼吸式MEA阴极结构。研究发现,在MEA阴极微孔层添加15 mass %的SiO2而构成“外吸水”式阴极结构,有利于提高MEA的性能,并可以提高阴极扩散层的亲水性及其排水能力,缓解阴极的水淹。另外,设计了一种“集流体内置型”自呼吸式DMFC的MEA新结构,把原本用作阴极集流体的薄金属网直接嵌入阴极催化层中。相比传统型MEA,此新型MEA具有更小的欧姆电阻、较好的氧气传输性和水管理能力,MEA的最大功率密度提高了10.3 %。
The membrane electrode assembly (MEA) was a key component of directmethanol fuel cell (DMFC), and the performance of the DMFC was greatly dependenton the performance of MEA. In this thesis, the MEAs of the active DMFC andair-breathing DMFC were investigated. The MEA fabrication methods were studied,and the compositions and the structures of the catalyst layers and gas diffusion layers(GDLs) of the MEAs were optimized. The mechanism of the effect of MEAhot-pressing technologies, and the mechanism of MEA activation were also analysed.Moreover, the operation parameters of active DMFC were studied.
The effects of the MEA hot-pressing technologies (hot-pressing temperatures,pressures and time) on the performances and structures of the MEA were detailedlyinvestigated. The mechanism analysis of the effects of MEAhot-pressing technologieswere revealed by electrochemical impedance spectroscopies (EIS). It was concludedthat the MEA which was hot pressed at 135℃under 80 kg cm-2 for 90 s showed thehighest power density (46.0 mW·cm-2 at cell temperature of 80℃), and the MEA hadthe lower cell resistance, electrochemical reaction resistance and diffusion resistance.
The fabrication methods for MEA catalyst layers were investigated. SEM andAFM analyses revealed that the scraping method was a little more profitable forimproving the cell performance due to the more flat and smooth (the surface roughnesswas lower) surface of the scraped catalyst layer. It was concluded that the surfacemorphology and roughness of the catalyst layer had less effect on the performance ofthe MEA. The optimum Nafion content in the catalyst layer was also investigated, andthe optimum Nafion content in the anode and cathode catalyst layer was 34 mass %and 28mass %, respectively. The optimum Nafion content in the catalyst layer was notrelated to the metal content of the catalyst.
The compositions and the structures of anode GDL were optimized. It wasrevealed that the MEA which consisted of the untreated carbon paper and hydrophilicanode micro-porous layer (comprised carbon black and 10mass% Nafion) showed thebest performance. The evolution and diffusion characteristics of anode CO2 gasbubbles on different anode GDLs were investigated using home-made transparentsingle cell. It was observed that the hydrophobic anode GDL was not helpful for improving the CO2 gas transport in the anode GDL. It was found that the optimumPTFE content in the cathode backing layerwas 16 mass%. The MEA with much lowerPTFE content (20mass % PTFE) in the cathode MPL was more beneficial for cathodewater releasing and the long-term operation.
The effects of MEA activation methods on the structures and performances of theMEAs were studied. And the MEA activation mechanism was investigated by EIStests, electrochemical surface areas tests, SEM and XRD analyses. Although theparticle sizes of the catalysts in the electrodes increased during the MEA activationprocess, the electrochemical surface areas of the catalysts were increased because thepores in the electrodes were opened after the activation. The influences of the celloperation parameters on the performances of active DMFC were also researched.Compared with anode flow rate of methanol solution, the concentration of methanolsolution was more influential on the performance of active DMFC. It was found thatthere was no need to humidify the cathode oxygen of the active DMFC.
In consideration of the water flooding in the cathode catalyst layer and cathodeGDL of air-breathing DMFC, two improved“Inner-water-absorption”and“Outer-water-absorption”cathode structures were proposed. It was revealed that the“Outer-water- absorption”cathode structure with 15 mass %SiO2 in the cathode MPLwas more suitable for the improvement of performance of MEA due to the increasingof hydrophilic water transport paths in the cathode MPL, thus the water floodings inthe cathode were alleviated. Moreover, a novel“current collector inside”air-breathingMEA was proposed, in which a thin metal mesh used as the cathode current collectorwas directly embedded in the cathode catalyst layer of this novel MEA cathode. Thenovel MEA showed better cell performance (increased 10.3 %) and long-termoperation performance than the conventional one because of the lower cell resistance,enhanced oxygen transport and increased water removal rate in such a novel MEAstructure.
引文
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