贵金属纳米材料的合成及性能研究
摘要
贵金属纳米颗粒由于其具有催化、等离子体共振、光谱学等特有性质而成为无机纳米材料中研究最广泛的胶体体系之一。随着合成形貌可控的纳米材料技术的不断发展和更新,研究形貌(尺寸、形状、组分等)与纳米材料特有性质之间的关系已经受到人们广泛的关注。目前,大面积、精确地控制合成贵金属纳米材料,并研究其在催化、光学等领域的应用,依旧是当前纳米材料研究的热点和难点。
本论文基于晶种调制法,在水相中合成了分散性好、尺寸均一、形貌特殊的贵金属纳米材料,主要包括:Au多面体和涉及Au、Pd、Ag三种元素的核壳多面体复合结构,并进一步研究了上述不同纳米材料的光学和电化学性质,主要工作如下:
1.通过晶种调制法成功合成了尺寸均一、分散性良好的金六面体、八面体及菱形十二面体。并首次系统地研究了三种低指数面的单晶金多面体对葡萄糖的电催化行为。结果表明:葡萄糖的电催化氧化过程强烈地依赖于金多面体的不同晶面。相对于暴露{111}面的金八面体和{110}菱形十二面体而言,暴露{100}的金六面体表现出更高的催化活性,并且这些金多面体在催化过程中均具有较高稳定性。
2.通过晶种外延生长法制备了不同结构的Au-Pd、Pd-Au核-壳结构的多面体。首先,以椭球形Au纳米颗粒为晶核,H_2PdCl_4为钯源,抗坏血酸为还原剂,在十六烷基三甲基溴化铵溶液中通过反应条件的控制,合成了不同形貌的Au-Pd六面体、八面体、菱形十二面体。同样,通过晶种外延生长法以边长约为22 nm的Pd六面体纳米颗粒为晶核,HAuCl4为前驱体,抗坏血酸为还原剂,在十六烷基氯化吡啶溶液中合成了尺寸均一、分散性良好的Pd-Au六面体、八面体、菱形十二面体。同时研究了酸性条件下三种Au-Pd核-壳多面体对甲酸的电催化行为。结果表明:暴露{100}面的Au-Pd六面体相对于暴露{111}面的八面体和{110}面的菱形十二面体具有更高的催化电流密度。此外,较为系统地研究了不同厚度壳层的Au-Pd六面体的光学性质。结果表明:Au-Pd核-壳六面体表现出不同于椭球状Au纳米颗粒的光学活性,当Pd壳层的厚度小于5 nm时,Au-Pd核-壳结构的SPR在500-508 nm,当Pd壳层的厚度大于5 nm时,Au-Pd核壳六面体的SPR性质主要取决于外层Pd的光学性质。
Q3.通过晶种外延生长法以多面体Au-Pd和Pd-Au纳米颗粒为晶核,AgNO3为银源,抗坏血酸为还原剂,Br-为特定的吸附粒子,在十六烷基三甲基氯化铵溶液中合成了Au-Pd-Ag和Pd-Au-Ag三元核-壳结构的贵金属六面体。并比较了不同壳层厚度的Au-Pd-Ag和Pd-Au-Ag三元贵金属六面体的光学性质。对不同壳层厚度的Au-Pd-Ag和Pd-Au-Ag六面体,其光学性质主要由外层的Ag来决定,当晶种的大小不变,随着壳层厚度的减小,其光谱均发生蓝移。
In nano-science and nano-technology, colloidal metal nanoparticles are emerging as key materials for catalysis, plasmonics, and spectroscopy. With the development of synthesis method, it has been pay attention to study the relation between morphology (size, shape, composition) and physical and chemical properties. Nanomaterials with special morphology have been showed good properties and will been application in many field, meanwhile, precise control the morphology to tune special properties have been a hot topic.
Seed mediated method was employed to synthesize noble metal nanomaterials with special shape, including monodisperse Au single crystal polyhedra, core-shell polyhedra involving Au, Pd, and Ag. For special shape nanomaterials, SPR and electrochemical properties were studied. The following is the main result:
1. Using seed-mediated method to synthesize three types Au polyhedra including rhombic dodecahedra (RD), octahedra (Oct), and cubes, which were bounded with three low-index {110}, {111} and {100} facets, respectively. And then systematically explore the shape-dependent catalytic activities of gold nanoparticles toward glucose oxidation in alkaline electrolytes. Our findings clearly reveal that glucose oxidation is strongly dependent on the crystal facets of Au nanocrystals. The {100}-bounded cubic Au nanocrystals are significantly more active than the {110}-bounded rhombic dodecahedral and {111}-bounded octahedral Au nanocrystals. Furthermore, these Au nanocrystal catalysts exhibit remarkably high stability in the repetitive electrocatalytic oxidation process.
2. Au-Pd nano-polyhedral were synthesized through epitaxial growth method in aqueous solution. Ellipsoial Au were employed as the seeds, through reducing H2PdCl4 with L-ascorbic acid in cetyltrimethylammonium bromide (CTAB )solution,simply adjust―growth solution‖environment, Au-Pd core-shell rhombic dodecahedra (RD), octahedra (Oct), and cubes can synthesize. Pd-Au bimetallic nano-polyhedra were also synthesized using cubic Pd as seed, through reducing HAuCl4 with L-ascorbic acid in cetylpyridinium chloride (CPC) solution. The binary metal Au-Pd nanopolyhedra with uniform size were impolyed to study SPR and electrocatalytic. For electrocatalytic properties, the {100}-bounded cubic Au -Pd nanocrystals are significantly more active than the {110}-bounded RD and {111}-bounded octahedral Au-Pd nanocrystals. The study demonstrated for the Au-Pd core-shell nanocrystals, When Pd shells are smaller than 5nm, the SPR of Au-Pd core-shell was observed at 500-508nm. When shells are larger than 5nm, the SPR of Au-Pd are mainly determined by the exterior shell (Pd).
3. Au-Pd-Ag and Pd-Au-Ag nano-cubes were synthesized through epitaxial growth method in aqueous solution. Polyhedra Au-Pd and Pd-Au were employed as the seeds, Br- as special absorption ion, through reducing AgNO3 with L-ascorbic acid in cetyltrimethylammonium chloride ( CTAC ) solution. SPR of Au-Pd-Ag and Pd-Au-Ag with different thickness were also study. The SPR of Au-Pd-Ag and Pd-Au-Ag are mainly determined by the exterior shell (Ag) and with decreasing the size of trimetallic core-shell structure, the SPR are blue shift.
本论文基于晶种调制法,在水相中合成了分散性好、尺寸均一、形貌特殊的贵金属纳米材料,主要包括:Au多面体和涉及Au、Pd、Ag三种元素的核壳多面体复合结构,并进一步研究了上述不同纳米材料的光学和电化学性质,主要工作如下:
1.通过晶种调制法成功合成了尺寸均一、分散性良好的金六面体、八面体及菱形十二面体。并首次系统地研究了三种低指数面的单晶金多面体对葡萄糖的电催化行为。结果表明:葡萄糖的电催化氧化过程强烈地依赖于金多面体的不同晶面。相对于暴露{111}面的金八面体和{110}菱形十二面体而言,暴露{100}的金六面体表现出更高的催化活性,并且这些金多面体在催化过程中均具有较高稳定性。
2.通过晶种外延生长法制备了不同结构的Au-Pd、Pd-Au核-壳结构的多面体。首先,以椭球形Au纳米颗粒为晶核,H_2PdCl_4为钯源,抗坏血酸为还原剂,在十六烷基三甲基溴化铵溶液中通过反应条件的控制,合成了不同形貌的Au-Pd六面体、八面体、菱形十二面体。同样,通过晶种外延生长法以边长约为22 nm的Pd六面体纳米颗粒为晶核,HAuCl4为前驱体,抗坏血酸为还原剂,在十六烷基氯化吡啶溶液中合成了尺寸均一、分散性良好的Pd-Au六面体、八面体、菱形十二面体。同时研究了酸性条件下三种Au-Pd核-壳多面体对甲酸的电催化行为。结果表明:暴露{100}面的Au-Pd六面体相对于暴露{111}面的八面体和{110}面的菱形十二面体具有更高的催化电流密度。此外,较为系统地研究了不同厚度壳层的Au-Pd六面体的光学性质。结果表明:Au-Pd核-壳六面体表现出不同于椭球状Au纳米颗粒的光学活性,当Pd壳层的厚度小于5 nm时,Au-Pd核-壳结构的SPR在500-508 nm,当Pd壳层的厚度大于5 nm时,Au-Pd核壳六面体的SPR性质主要取决于外层Pd的光学性质。
Q3.通过晶种外延生长法以多面体Au-Pd和Pd-Au纳米颗粒为晶核,AgNO3为银源,抗坏血酸为还原剂,Br-为特定的吸附粒子,在十六烷基三甲基氯化铵溶液中合成了Au-Pd-Ag和Pd-Au-Ag三元核-壳结构的贵金属六面体。并比较了不同壳层厚度的Au-Pd-Ag和Pd-Au-Ag三元贵金属六面体的光学性质。对不同壳层厚度的Au-Pd-Ag和Pd-Au-Ag六面体,其光学性质主要由外层的Ag来决定,当晶种的大小不变,随着壳层厚度的减小,其光谱均发生蓝移。
In nano-science and nano-technology, colloidal metal nanoparticles are emerging as key materials for catalysis, plasmonics, and spectroscopy. With the development of synthesis method, it has been pay attention to study the relation between morphology (size, shape, composition) and physical and chemical properties. Nanomaterials with special morphology have been showed good properties and will been application in many field, meanwhile, precise control the morphology to tune special properties have been a hot topic.
Seed mediated method was employed to synthesize noble metal nanomaterials with special shape, including monodisperse Au single crystal polyhedra, core-shell polyhedra involving Au, Pd, and Ag. For special shape nanomaterials, SPR and electrochemical properties were studied. The following is the main result:
1. Using seed-mediated method to synthesize three types Au polyhedra including rhombic dodecahedra (RD), octahedra (Oct), and cubes, which were bounded with three low-index {110}, {111} and {100} facets, respectively. And then systematically explore the shape-dependent catalytic activities of gold nanoparticles toward glucose oxidation in alkaline electrolytes. Our findings clearly reveal that glucose oxidation is strongly dependent on the crystal facets of Au nanocrystals. The {100}-bounded cubic Au nanocrystals are significantly more active than the {110}-bounded rhombic dodecahedral and {111}-bounded octahedral Au nanocrystals. Furthermore, these Au nanocrystal catalysts exhibit remarkably high stability in the repetitive electrocatalytic oxidation process.
2. Au-Pd nano-polyhedral were synthesized through epitaxial growth method in aqueous solution. Ellipsoial Au were employed as the seeds, through reducing H2PdCl4 with L-ascorbic acid in cetyltrimethylammonium bromide (CTAB )solution,simply adjust―growth solution‖environment, Au-Pd core-shell rhombic dodecahedra (RD), octahedra (Oct), and cubes can synthesize. Pd-Au bimetallic nano-polyhedra were also synthesized using cubic Pd as seed, through reducing HAuCl4 with L-ascorbic acid in cetylpyridinium chloride (CPC) solution. The binary metal Au-Pd nanopolyhedra with uniform size were impolyed to study SPR and electrocatalytic. For electrocatalytic properties, the {100}-bounded cubic Au -Pd nanocrystals are significantly more active than the {110}-bounded RD and {111}-bounded octahedral Au-Pd nanocrystals. The study demonstrated for the Au-Pd core-shell nanocrystals, When Pd shells are smaller than 5nm, the SPR of Au-Pd core-shell was observed at 500-508nm. When shells are larger than 5nm, the SPR of Au-Pd are mainly determined by the exterior shell (Pd).
3. Au-Pd-Ag and Pd-Au-Ag nano-cubes were synthesized through epitaxial growth method in aqueous solution. Polyhedra Au-Pd and Pd-Au were employed as the seeds, Br- as special absorption ion, through reducing AgNO3 with L-ascorbic acid in cetyltrimethylammonium chloride ( CTAC ) solution. SPR of Au-Pd-Ag and Pd-Au-Ag with different thickness were also study. The SPR of Au-Pd-Ag and Pd-Au-Ag are mainly determined by the exterior shell (Ag) and with decreasing the size of trimetallic core-shell structure, the SPR are blue shift.
引文
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