氰胶还原法制备Pt基催化剂及其在燃料电池中的应用
发布时间：2018-11-12 20:07
【摘要】：质子交换膜燃料电池(PEMFC)具有结构简单、比能量高、对环境友好等特点,可用于小型电站及便携式移动电源领域。然而,PEMFC阴阳极催化剂性能不佳,使其性能与商业化的要求仍有较大差距。因此,制备高性能阴阳极催化剂是PEMFC研究的一个重要课题。本文利用过渡金属氰胶作为前驱体,制备了具有三维网状结构的多孔Pt基电催化剂,并研究了它们对甲醇氧化、氧气还原的电催化性能。主要研究结果如下：1.双贵金属K2PdCl4/K2Pt(CN)4氰胶为具有三维骨架结构的深黄色果冻状,可以通过混合K2PdCl4和K2Pt(CN)4制备得到。利用K2PdCl4/K2Pt(CN)4氰胶作为反应前驱体,三维珊瑚状Pd-Pt合金纳米结构物可以通过简单的NaBH4还原法反应得到,而这种方法没有表面活性剂和模板剂。Pd-Pt合金纳米结构物的尺寸,形貌和表面组成通过扫描电子显微镜(SEM),透射电子显微镜(TEM),选区电子衍射(SAED),能量散射光谱(EDX),EDX面扫,X射线衍射(XRD),X射线光电子能谱(XPS)等表征进行研究。由于Pd-Pt合金纳米结构物独特的三维互联结构,电子效应和协同效应,与商业化Pt和Pd黑相比,它对乙醇氧化有着优异的电催化活性和稳定性。2.三元K2PtCl4/K3Co(CN)6-K2PdCl4/K3Co(CN)6混合氰胶可以通过混合K2PtCl4、K2PdCl4、K3Co(CN)6制备得到。直接以NaBH4为还原剂可以制备出高合金化程度的三维Pt-Pd-Co三元合金纳米网。三维Pt-Pd-Co三元合金纳米网的大小,形貌和表面成分通过扫描电子显微镜(SEM),透射电子显微镜(TEM),选区电子衍射(SAED),能量散射能谱(EDX),X射线衍射(XRD)和X射线光电子能谱(XPS)等表征进行研究。由于Pt-Pd-Co三元合金纳米网独特的三维结构,电子效应和协同效应,与商业化Pt黑相比,三维Pt-Pd-Co三元合金纳米网对氧还原反应显示出更高的电催化活性和稳定性。3. K2PdCl4/K2Ni(CN)4首先通过混合K2PdCl4和K2Ni(CN)4制备得到。直接用NaBH4作为还原剂制备出PdNi合金纳米网,再通过Galvanic取代反应合成富Pt的壳层以得到三维多孔PdNi@Pt核壳结构物。PdNi@Pt核壳结构物的尺寸,形貌和表面组成通过扫描电子显微镜(SEM),透射电子显微镜(TEM),选区电子衍射(SAED),能量散射光谱(EDX), EDX面扫,X射线衍射(XRD),X射线光电子能谱(XPS)等表征进行研究。由于PdNi@Pt核壳结构物独特的三维结构,电子效应,与商业化Pt黑相比,PdNi@Pt核壳结构物对甲醇氧化反应有极高的质量活性和稳定性。
[Abstract]:Proton exchange membrane fuel cell (PEMFC) has the advantages of simple structure, high specific energy and environmental friendliness. It can be used in the field of small power plants and portable mobile power sources. However, the performance of PEMFC cathode catalyst is not good enough to meet the requirements of commercialization. Therefore, the preparation of high performance cathode and cathode catalysts is an important subject of PEMFC research. In this paper, porous Pt based electrocatalysts with three-dimensional reticular structure were prepared by using transition metal cyanide as precursors, and their electrocatalytic properties for methanol oxidation and oxygen reduction were studied. The main results are as follows: 1. Double precious metal K2PdCl4/K2Pt (CN) 4 cyanide gum is a dark yellow jelly with three dimensional skeleton structure, which can be prepared by mixing K2PdCl4 and K2Pt (CN) 4. Using K2PdCl4/K2Pt (CN) _ 4 cyanide as the precursor of the reaction, the three-dimensional coral-like Pd-Pt alloy nanostructures can be obtained by simple NaBH4 reduction method. The size, morphology and surface composition of the nanostructures of Pd-Pt alloys were characterized by scanning electron microscopy (SEM), (SEM), transmission electron microscope (TEM), selective electron diffraction (SAED),). The energy scattering spectra were characterized by (EDX), EDX surface scan and X ray diffraction (XRD), X ray photoelectron spectroscopy (XPS). Because of the unique three-dimensional interconnecting structure, electronic effect and synergistic effect of Pd-Pt alloy nanostructures, it has excellent electrocatalytic activity and stability for ethanol oxidation compared with commercial Pt and Pd black. 2. Ternary K2PtCl4/K3Co (CN) 6-K2PdCl4/K3Co (CN) 6 mixed cyanide gum can be prepared by mixing K2PtCl4K2PdCl4K3Co (CN) 6. Three dimensional Pt-Pd-Co ternary alloy nanowires with high alloying degree can be prepared by using NaBH4 as reducing agent. The size, Morphology and Surface composition of Three-Dimensional Pt-Pd-Co Ternary Alloy Nanonets by scanning Electron microscope, (SEM), Transmission Electron microscope, (TEM), selective Electron diffraction (SAED), Energy scattering Spectroscopy (EDX), X-ray diffraction (XRD) (XRD) and X-ray photoelectron spectroscopy (XPS) were studied. Due to the unique three-dimensional structure, electronic effect and synergistic effect of Pt-Pd-Co ternary alloy nanowires, compared with commercial Pt black, Three-dimensional Pt-Pd-Co alloy nanowires showed higher electrocatalytic activity and stability for oxygen reduction. K2PdCl4/K2Ni (CN) _ 4 was first prepared by mixing K2PdCl4 and K2Ni (CN) _ 4. The PdNi alloy nanowires were prepared by using NaBH4 as reductant, and then the shell layer rich in Pt was synthesized by Galvanic substitution reaction to obtain the three-dimensional porous PdNi@Pt core-shell structure. The size of PdNi@Pt core-shell structure was obtained. Morphology and surface composition by scanning electron microscope, (SEM), transmission electron microscope, (TEM), selective electron diffraction, (SAED), energy scattering spectrum, (EDX), EDX surface scanning, X ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) was studied. Because of the unique three-dimensional structure and electronic effect of PdNi@Pt core-shell structure, compared with commercial Pt black, PdNi@Pt core-shell structure has high mass activity and stability for methanol oxidation.
【学位授予单位】：南京师范大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O643.36;TM911.4
[Abstract]:Proton exchange membrane fuel cell (PEMFC) has the advantages of simple structure, high specific energy and environmental friendliness. It can be used in the field of small power plants and portable mobile power sources. However, the performance of PEMFC cathode catalyst is not good enough to meet the requirements of commercialization. Therefore, the preparation of high performance cathode and cathode catalysts is an important subject of PEMFC research. In this paper, porous Pt based electrocatalysts with three-dimensional reticular structure were prepared by using transition metal cyanide as precursors, and their electrocatalytic properties for methanol oxidation and oxygen reduction were studied. The main results are as follows: 1. Double precious metal K2PdCl4/K2Pt (CN) 4 cyanide gum is a dark yellow jelly with three dimensional skeleton structure, which can be prepared by mixing K2PdCl4 and K2Pt (CN) 4. Using K2PdCl4/K2Pt (CN) _ 4 cyanide as the precursor of the reaction, the three-dimensional coral-like Pd-Pt alloy nanostructures can be obtained by simple NaBH4 reduction method. The size, morphology and surface composition of the nanostructures of Pd-Pt alloys were characterized by scanning electron microscopy (SEM), (SEM), transmission electron microscope (TEM), selective electron diffraction (SAED),). The energy scattering spectra were characterized by (EDX), EDX surface scan and X ray diffraction (XRD), X ray photoelectron spectroscopy (XPS). Because of the unique three-dimensional interconnecting structure, electronic effect and synergistic effect of Pd-Pt alloy nanostructures, it has excellent electrocatalytic activity and stability for ethanol oxidation compared with commercial Pt and Pd black. 2. Ternary K2PtCl4/K3Co (CN) 6-K2PdCl4/K3Co (CN) 6 mixed cyanide gum can be prepared by mixing K2PtCl4K2PdCl4K3Co (CN) 6. Three dimensional Pt-Pd-Co ternary alloy nanowires with high alloying degree can be prepared by using NaBH4 as reducing agent. The size, Morphology and Surface composition of Three-Dimensional Pt-Pd-Co Ternary Alloy Nanonets by scanning Electron microscope, (SEM), Transmission Electron microscope, (TEM), selective Electron diffraction (SAED), Energy scattering Spectroscopy (EDX), X-ray diffraction (XRD) (XRD) and X-ray photoelectron spectroscopy (XPS) were studied. Due to the unique three-dimensional structure, electronic effect and synergistic effect of Pt-Pd-Co ternary alloy nanowires, compared with commercial Pt black, Three-dimensional Pt-Pd-Co alloy nanowires showed higher electrocatalytic activity and stability for oxygen reduction. K2PdCl4/K2Ni (CN) _ 4 was first prepared by mixing K2PdCl4 and K2Ni (CN) _ 4. The PdNi alloy nanowires were prepared by using NaBH4 as reductant, and then the shell layer rich in Pt was synthesized by Galvanic substitution reaction to obtain the three-dimensional porous PdNi@Pt core-shell structure. The size of PdNi@Pt core-shell structure was obtained. Morphology and surface composition by scanning electron microscope, (SEM), transmission electron microscope, (TEM), selective electron diffraction, (SAED), energy scattering spectrum, (EDX), EDX surface scanning, X ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) was studied. Because of the unique three-dimensional structure and electronic effect of PdNi@Pt core-shell structure, compared with commercial Pt black, PdNi@Pt core-shell structure has high mass activity and stability for methanol oxidation.
【学位授予单位】：南京师范大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O643.36;TM911.4
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