纳米多孔金属材料的设计、制备与催化性能研究
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摘要
本论文主要采用去合金化法制备了一系列纳米多孔的金属材料,分别从纳米多孔材料的制备、形成机理以及性质表征和应用研究几个方面进行了论述,主要内容包括电化学去合金化法制备小孔径的纳米多孔金及CO催化氧化性能研究,去合金化法与氧化还原置换法相结合制备纳米管道状介孔铂系合金纳米结构及其形成机理与电催化性能研究,去合金化三元合金制备纳米多孔的Pt/Au合金及其电催化性能研究。本论文旨在发展一种简便有效的方法来制备纳米多孔的金属材料,并探索这类材料的气相催化与电催化性能,探索它们在燃料电池和工业催化等方面的应用前景。
1.电化学去合金化法制备小孔径纳米多孔金及其CO催化氧化性能研究
在双电极体系中,以浓硝酸为电解质,铂片为阴极,25μm厚的Au/Ag合金(42:58,wt.%)片作为阳极,加阳极电压(电压范围0.6-1.0 V),在室温下腐蚀10-15 min制备了小孔径的纳米多孔金a-NPG。a-NPG具有三维双连续的海绵状结构,孔壁尺寸均匀分布在6 nm左右。根据多孔金形成的机理,银的溶解导致的表面粗糙化,与金原子的扩散导致的表面平滑化是相互竞争的,本文中改进了金银合金的去合金化方法,通过加一定的阳极电压,加快了银的溶解,抑制了金的扩散,缩短了去合金化的时间,制得了小尺寸的纳米多孔金。
基于a-NPG这种新的非负载型金催化体系,系统地研究了a-NPG对CO的一系列催化氧化性质,包括催化反应的活性物种、反应动力学、及反应温度、孔壁尺寸与空速对催化活性的影响。在没有金属氧化物衬底的情况下纳米多孔金对CO氧化显示了很高的低温催化活性。a-NPG中金属态的金是CO与O_2发生催化反应的活性位点。对于反应物浓度对反应速率的影响,通过实验观察到CO的浓度对催化反应的速率影响较大,而O_2的浓度只是轻微地影响了反应的速率,实验结果表明,在讨论的温度区间内CO在a-NPG催化剂表面的吸附可能是反应的速控步骤,CO在a-NPG上的催化氧化的反应速率方程式可以表示为R=K[CO]~(0.78)[O_2]~(0.25)。在233-273 K的温度区间内,CO氧化的反应速率随着温度的升高呈线性变化,在高温下,这种趋势逐渐减慢。利用Arrhenius行为分析估算出a-NPG上CO催化氧化的表观反应活化能大约是28.8 kJ/mol。从探讨纳米多孔金孔壁尺寸的影响中,较大尺寸的a-NPG也显示了一定的CO催化活性,表明了a-NPG高的活性不是量子尺寸效应的结果,可能与a-NPG孔壁尺寸较小时表面上存在的大量低配位金原子有关。电化学去合金化法制备a-NPG催化剂,制备方法简单、结构容易控制、产率高,该制备方法丰富了小尺寸纳米多孔金属材料的制备。基于a-NPG对CO催化氧化进行的一系列研究,通过彻底排除衬底的影响,所进行的一系列研究结果对金催化剂催化活性的起因提供了新的理解与认识。
2.去合金化法与氧化还原置换法相结合制备纳米管道状介孔铂系合金结构以及电催化性质研究
将简单的去合金化方法与氧化还原置换法相结合制备了一类以Pt系金属为基础的纳米管道状介孔合金材料。在NaOH溶液中选择性腐蚀50μm厚的Cu_(25)Al_(75)(at.%)合金片制备了纳米多孔铜(NPC)作为模板与还原剂。NPC显示了三维双连续的海绵状形态,其孔壁尺寸均匀分布在50 nm左右,去合金化方法制备NPC模板,简单有效,成本低,适合大量制备。通过透射电镜,扫描电镜及X-射线粉末衍射证明N-PC与H_2PtCl_6发生置换反应后得到了管状的纳米多孔Pt/Cu合金(NM-Pt/Cu),其中管道直径与孔壁的尺寸分别为60和10 nm左右。孔壁是由直径为～5 nm的纳米颗粒和孔径为～3 nm的小孔组成。与K_2PdCl_4溶液的反应产生了类似的纳米管道状介孔结构,其中管道直径和孔壁的尺寸大约为50和6 nm。置换反应过程中这种管道状结构的形成机理如下:当NPC模板与铂系金属前驱体溶液混合以后,表面的Cu与前驱体溶液自发发生了置换反应,被还原生成的Pt或Pd原子沉积到NPC的表面上,随着反应的进行,越来越多的Cu原子从NPC结构内部滤出。同时,NPC结构里面的Cu逐渐向外扩散,溶液中沉积下来的Pt或Pd原子与未反应的Cu原子相互扩散形成合金,而暴露在溶液中的Cu逐渐被Pt或Pd置换并合金化,产物最终变为富Pt的Pt/Cu或富Pd的Pd/Cu合金,但是此时的Cu由于其周围大量Pt或Pd原子的存在而被钝化,导致置换反应终止,最终生成了管道状的纳米多孔合金结构。对于多孔的壳层表面,可能是Cu与金属前驱体溶液反应比较剧烈或高的表面能,使反应过程被还原的Pt或Pd原子聚集形成了纳米颗粒导致了多孔表面的形成。
在催化性能测试中发现NM-Pt/Cu与NM-Pd/Cu合金对甲醇电氧化,甲酸电氧化,氧还原等有机小分子的电催化具有高的活性,催化稳定性和强的抗中毒能力。这类纳米材料以其优异的催化性能、简便环保的制备方法、独特的结构为其在工业催化和燃料电池技术中的应用提供了明显的优势。
3.去合金化三元合金制备纳米多孔Pt/Au合金及其电催化性能研究
采用去合金化三元合金的方法制备了不同铂金组分的结构均匀的纳米多孔Pt/Au合金,其组分分别是Pt_4Au_1、Pt_1Au_1、Pt_1Au_4。纳米多孔的Pt/Au合金是通过电化学腐蚀法溶解Pt/Au/Cu合金的铜制得的。SEM与TEM研究证明选择性的去除三元合金中的铜简单有效地制备了三维双连续的纳米多孔Pt/Au合金。在同样的去合金化条件下,随着金含量的增加,孔径孔壁发生了粗化现象,其中Pt_4Au_1、Pt_1Au_1、Pt_1Au_4的孔径与孔壁尺寸分别是3、5、10 nm。XPS与XRD证明纳米多孔的Pt_4Au_1与Pt_1Au_1具有非常均匀的合金组分与相结构,而Pt_1Au_4发生了轻微的相分离,导致表面富金。这种纳米多孔的结构在金的含量较低时在酸性溶液中对Pt起了良好的结构稳定化作用。电催化性能测试表明,不同组分的Pt/Au合金对甲醇和甲酸的电催化氧化表现出了明显不同的性能。从甲醇催化来看,Pt_4Au_1与Pt_1Au_1具有较高的甲醇催化活性,而Pt_1Au_4却显示了最高的甲酸电催化性能由于采用直接脱氢的催化机理。实验证明通过炼合金时控制最初的Pt/Au双金属比例,可以获得不同的有机小分子电催化活性。去合金化法方法制备纳米多孔合金是一种简便有效的方法,整个过程贵金属基本没有损耗,适于大规模的合成。特别重要的是,去合金化是一个理想的“绿色”化学方法,其中没有任何有机物的参与和产生。这种方法作为一种有效常规的方法可以来合成其它的纳米多孔的合金催化剂。
This paper is focusing on designing and fabricating a novel class of nanoporous metallic materials and exploring their corresponding formation mechanism, catalytic and electrocatalytic properties.Investigations are based on several aspects mainly including:research on unsupported nanoporous gold(NPG) for CO oxidation,fabrication of multifunctional hierarchically hollow platinum-group bimetallic nanocomposites and their electrocatalytic activities, preparation of nanoporous Pt-based metals with controllable size and composition, and related characterization of their electrocatalytic performance.
1.Preparation of unsupported NPG with small length scale and research on their CO performance.
Typically,NPG sample with ligament size at～6 nm(a-NPG) was made by etching a piece of 25μm Ag/Au foil in a concentrated nitric acid for 10-15 min with an applied voltage of 0.6-1.0V.Platinum electrode was used as a cathode in a binary electrode system.Based on the dealloying principle,the evolution and formation of nanoporous structure is a competition between dissolution of Ag induced surface roughening and Au diffusion induced surface smoothing.By using the modified electrochemical dealloying method,the applied anode potential accelerates the dissolution of Ag and inhibits the diffusion of Au, resulting in the smaller length scale of NPG.
Based on the unsupported NPG catalysts,we discussed the catalytic activity of NPG as a function of space velocity,gas concentration,and reaction temperature etc.It was found that a-NPG shows unique catalytic activity towards low-temperature CO oxidation in the absence of metal oxide support.In kinetic studies,we found that the reaction rate of CO oxidation on unsupported NPG depends significantly on CO concentration but only slightly on O_2 concentration. It is considered that the CO adsorption onto the NPG surface may play a decisive role in the reaction as the rate-limiting step.CO oxidation rate on NPG was expressed by the following equation:RCO=K[CO]~(0.78)[O_2]~(0.25).With the increase in reaction temperature CO connversion rapidly increased between 235 and 273 K.At higher temperatures,the trend slowed,and CO reached near complete conversion.The analysis of Arrhenius behavior allows the extrapolation of the apparent activation energy to be 28.8 kJ/mol.Interestingly,we found that NPG with larger pore and ligament size also exhibited high CO catalytic activity.We think that the high catalytic activity of NPG originates form the high concentration of low-coordinated metallic Au atoms but not the quantum size effect.
The electrochemical dealloying method to prepare NPG is simple and convenient with absolute yield and controllable structure,which enriches the preparation of small-sized nanoporous metallic materials.A series of research on NPG towards CO oxidation provides new insights into gold catalysis by completely excluding the effect of support.
2.The preparation of nanotubular porous platinum-group bimetallic nanocomposites and research on their electrocatalytic performance.
In this research,a general approach is employed to large-scale synthesis of a novel class of nanotubular mesoporous platinum-group-metals(PGMs)-based nanostructures based on a simple room-temperature dealloying and galvanic replacement reaction.Dealloying was used to synthesize nanoporous metals to act as sacrificial templates,and followed by reacting with H_2PtCl_6 and K_2PdCl_4 solution precursors.The resulted NM-Pt/Cu and NM-Pd/Cu structures were confirmed by transmission electron spectroscopy(TEM) and scanning electron spectroscopy(SEM).NM-Pt/Cu shows a three-dimensional(3D) bicontinuous nanotubular mesoporous structure with tube diameter around 80 nm and shell thickness about 10 nm.Interestingly,the shell surfaces are not smooth and seamless but rather have many small pores and grains around 3 nm.The NM-Pd/Cu structure also exhibits hierarchical hollow structure with the tube diameter around 60 nm and shell thickness about 6 nm.X-ray diffraction(XRD) analysis confirmed that the resulted NM-Pt/Cu and NM-Pd/Cu have the single-phase alloy structure.The possible formation mechanism of such the hierarchically hollow structure was explained as follows:as Pt(or Pd) atoms are reduced and deposited onto the NPC substrate,Cu atoms are progressively leached away.At the same time,these deposited precious metal surface atoms will interdiffuse with Cu to form an alloy.As the reaction goes on,more Cu will be depleted;and accordingly,the surface was gradually passivated due to the further incorporation of more precious metal atoms.Eventually,a PGM-based bimetallic nanotubular mesoporous structure forms,which also marks the completion of the displacement reaction.
NM-Pt/Cu catalyst exhibits high catalytic activity and CO-tolerance toward methanol oxidation.Meanwhile,NM-Pd/Cu shows a unique activity towards oxygen reduction reaction.This synthesis strategy is facile and efficient to fabricate similar ultra-high surface area nanocomposites in large scale with hierarchically hollow structures.These nanostructures have obvious structural advantages in terms of unique catalytic properties,simple and clean processing, and saving precious metals,which suggest their great potential for use in heterogeneous catalysis and fuel cell technologies.
3.Preparation of nanoporous Pt/Au alloys with controllable size and composition by dealloying ternary alloys and research on their electrocatalytic activity.
A simple and general dealloying method was employed to fabricate nanoporous Au/Pt alloys with pre-determined Au/Pt molar ratios.Structural characterization by electron microscopes confirms that selective etching of Cu from Au/Pt/Cu alloy precursors results in the formation of 3-dimensional bicontinuous porous network structures with uniform pores and ligaments.The as-made Pt_4Au_1,Pt_1Au_1,and Pt_1Au_4 samples are all resulted in the similar 3D bicontinuous network with ligament size at 3,5,and 10 nm,respectively.A careful inspection shows that under the same dealloying conditions,nanoporous alloys with high Pt content generally result in smaller feature sizes.X-ray photoelectron spectroscopy and X-ray diffraction demonstrate that Pt_4Au_1 and Pt_1Au_1 nanoporous alloys adopt a relatively uniform bimetallic alloy structure across the entire length scale,while Pt_4Au_1 sample shows slight phase segregation,leading to an Au-rich surface layer.These nanostructures show distinct surface structure sensitive electrocatalytic properties. For methanol electrooxidation,nanoporous Pt_4Au_1 and Pt_1Au_1 showed an obviously improved performance in structure stability and electrocatalytic activity with higher specific activity and lower peak potentials,as compared with the commercial nanoparticle-based catalysts.In sharp contrast,nanoporous Pt_1Au_4 exhibited the best activity for formic acid oxidation amongst all samples,which was characterized by a preferential dehydrogenation reaction process at lower potential. The resulted nanoporous alloys typically represent a class of macroscopic nanostructured materials with a three-dimensional bicontinuous spongy morphology, which are expected to have evident structural advantages as compared with zero-dimensional nanomaterials.Dealloying method is extremely simple and flexible,which is appropriate for large-scale synthesis.In addition,this method is a chemical "green" method,which offers new opportunities for the preparation of nanoporous Pt-M bimetallic catalysts with high surface area and high activities.
1.电化学去合金化法制备小孔径纳米多孔金及其CO催化氧化性能研究
在双电极体系中,以浓硝酸为电解质,铂片为阴极,25μm厚的Au/Ag合金(42:58,wt.%)片作为阳极,加阳极电压(电压范围0.6-1.0 V),在室温下腐蚀10-15 min制备了小孔径的纳米多孔金a-NPG。a-NPG具有三维双连续的海绵状结构,孔壁尺寸均匀分布在6 nm左右。根据多孔金形成的机理,银的溶解导致的表面粗糙化,与金原子的扩散导致的表面平滑化是相互竞争的,本文中改进了金银合金的去合金化方法,通过加一定的阳极电压,加快了银的溶解,抑制了金的扩散,缩短了去合金化的时间,制得了小尺寸的纳米多孔金。
基于a-NPG这种新的非负载型金催化体系,系统地研究了a-NPG对CO的一系列催化氧化性质,包括催化反应的活性物种、反应动力学、及反应温度、孔壁尺寸与空速对催化活性的影响。在没有金属氧化物衬底的情况下纳米多孔金对CO氧化显示了很高的低温催化活性。a-NPG中金属态的金是CO与O_2发生催化反应的活性位点。对于反应物浓度对反应速率的影响,通过实验观察到CO的浓度对催化反应的速率影响较大,而O_2的浓度只是轻微地影响了反应的速率,实验结果表明,在讨论的温度区间内CO在a-NPG催化剂表面的吸附可能是反应的速控步骤,CO在a-NPG上的催化氧化的反应速率方程式可以表示为R=K[CO]~(0.78)[O_2]~(0.25)。在233-273 K的温度区间内,CO氧化的反应速率随着温度的升高呈线性变化,在高温下,这种趋势逐渐减慢。利用Arrhenius行为分析估算出a-NPG上CO催化氧化的表观反应活化能大约是28.8 kJ/mol。从探讨纳米多孔金孔壁尺寸的影响中,较大尺寸的a-NPG也显示了一定的CO催化活性,表明了a-NPG高的活性不是量子尺寸效应的结果,可能与a-NPG孔壁尺寸较小时表面上存在的大量低配位金原子有关。电化学去合金化法制备a-NPG催化剂,制备方法简单、结构容易控制、产率高,该制备方法丰富了小尺寸纳米多孔金属材料的制备。基于a-NPG对CO催化氧化进行的一系列研究,通过彻底排除衬底的影响,所进行的一系列研究结果对金催化剂催化活性的起因提供了新的理解与认识。
2.去合金化法与氧化还原置换法相结合制备纳米管道状介孔铂系合金结构以及电催化性质研究
将简单的去合金化方法与氧化还原置换法相结合制备了一类以Pt系金属为基础的纳米管道状介孔合金材料。在NaOH溶液中选择性腐蚀50μm厚的Cu_(25)Al_(75)(at.%)合金片制备了纳米多孔铜(NPC)作为模板与还原剂。NPC显示了三维双连续的海绵状形态,其孔壁尺寸均匀分布在50 nm左右,去合金化方法制备NPC模板,简单有效,成本低,适合大量制备。通过透射电镜,扫描电镜及X-射线粉末衍射证明N-PC与H_2PtCl_6发生置换反应后得到了管状的纳米多孔Pt/Cu合金(NM-Pt/Cu),其中管道直径与孔壁的尺寸分别为60和10 nm左右。孔壁是由直径为～5 nm的纳米颗粒和孔径为～3 nm的小孔组成。与K_2PdCl_4溶液的反应产生了类似的纳米管道状介孔结构,其中管道直径和孔壁的尺寸大约为50和6 nm。置换反应过程中这种管道状结构的形成机理如下:当NPC模板与铂系金属前驱体溶液混合以后,表面的Cu与前驱体溶液自发发生了置换反应,被还原生成的Pt或Pd原子沉积到NPC的表面上,随着反应的进行,越来越多的Cu原子从NPC结构内部滤出。同时,NPC结构里面的Cu逐渐向外扩散,溶液中沉积下来的Pt或Pd原子与未反应的Cu原子相互扩散形成合金,而暴露在溶液中的Cu逐渐被Pt或Pd置换并合金化,产物最终变为富Pt的Pt/Cu或富Pd的Pd/Cu合金,但是此时的Cu由于其周围大量Pt或Pd原子的存在而被钝化,导致置换反应终止,最终生成了管道状的纳米多孔合金结构。对于多孔的壳层表面,可能是Cu与金属前驱体溶液反应比较剧烈或高的表面能,使反应过程被还原的Pt或Pd原子聚集形成了纳米颗粒导致了多孔表面的形成。
在催化性能测试中发现NM-Pt/Cu与NM-Pd/Cu合金对甲醇电氧化,甲酸电氧化,氧还原等有机小分子的电催化具有高的活性,催化稳定性和强的抗中毒能力。这类纳米材料以其优异的催化性能、简便环保的制备方法、独特的结构为其在工业催化和燃料电池技术中的应用提供了明显的优势。
3.去合金化三元合金制备纳米多孔Pt/Au合金及其电催化性能研究
采用去合金化三元合金的方法制备了不同铂金组分的结构均匀的纳米多孔Pt/Au合金,其组分分别是Pt_4Au_1、Pt_1Au_1、Pt_1Au_4。纳米多孔的Pt/Au合金是通过电化学腐蚀法溶解Pt/Au/Cu合金的铜制得的。SEM与TEM研究证明选择性的去除三元合金中的铜简单有效地制备了三维双连续的纳米多孔Pt/Au合金。在同样的去合金化条件下,随着金含量的增加,孔径孔壁发生了粗化现象,其中Pt_4Au_1、Pt_1Au_1、Pt_1Au_4的孔径与孔壁尺寸分别是3、5、10 nm。XPS与XRD证明纳米多孔的Pt_4Au_1与Pt_1Au_1具有非常均匀的合金组分与相结构,而Pt_1Au_4发生了轻微的相分离,导致表面富金。这种纳米多孔的结构在金的含量较低时在酸性溶液中对Pt起了良好的结构稳定化作用。电催化性能测试表明,不同组分的Pt/Au合金对甲醇和甲酸的电催化氧化表现出了明显不同的性能。从甲醇催化来看,Pt_4Au_1与Pt_1Au_1具有较高的甲醇催化活性,而Pt_1Au_4却显示了最高的甲酸电催化性能由于采用直接脱氢的催化机理。实验证明通过炼合金时控制最初的Pt/Au双金属比例,可以获得不同的有机小分子电催化活性。去合金化法方法制备纳米多孔合金是一种简便有效的方法,整个过程贵金属基本没有损耗,适于大规模的合成。特别重要的是,去合金化是一个理想的“绿色”化学方法,其中没有任何有机物的参与和产生。这种方法作为一种有效常规的方法可以来合成其它的纳米多孔的合金催化剂。
This paper is focusing on designing and fabricating a novel class of nanoporous metallic materials and exploring their corresponding formation mechanism, catalytic and electrocatalytic properties.Investigations are based on several aspects mainly including:research on unsupported nanoporous gold(NPG) for CO oxidation,fabrication of multifunctional hierarchically hollow platinum-group bimetallic nanocomposites and their electrocatalytic activities, preparation of nanoporous Pt-based metals with controllable size and composition, and related characterization of their electrocatalytic performance.
1.Preparation of unsupported NPG with small length scale and research on their CO performance.
Typically,NPG sample with ligament size at～6 nm(a-NPG) was made by etching a piece of 25μm Ag/Au foil in a concentrated nitric acid for 10-15 min with an applied voltage of 0.6-1.0V.Platinum electrode was used as a cathode in a binary electrode system.Based on the dealloying principle,the evolution and formation of nanoporous structure is a competition between dissolution of Ag induced surface roughening and Au diffusion induced surface smoothing.By using the modified electrochemical dealloying method,the applied anode potential accelerates the dissolution of Ag and inhibits the diffusion of Au, resulting in the smaller length scale of NPG.
Based on the unsupported NPG catalysts,we discussed the catalytic activity of NPG as a function of space velocity,gas concentration,and reaction temperature etc.It was found that a-NPG shows unique catalytic activity towards low-temperature CO oxidation in the absence of metal oxide support.In kinetic studies,we found that the reaction rate of CO oxidation on unsupported NPG depends significantly on CO concentration but only slightly on O_2 concentration. It is considered that the CO adsorption onto the NPG surface may play a decisive role in the reaction as the rate-limiting step.CO oxidation rate on NPG was expressed by the following equation:RCO=K[CO]~(0.78)[O_2]~(0.25).With the increase in reaction temperature CO connversion rapidly increased between 235 and 273 K.At higher temperatures,the trend slowed,and CO reached near complete conversion.The analysis of Arrhenius behavior allows the extrapolation of the apparent activation energy to be 28.8 kJ/mol.Interestingly,we found that NPG with larger pore and ligament size also exhibited high CO catalytic activity.We think that the high catalytic activity of NPG originates form the high concentration of low-coordinated metallic Au atoms but not the quantum size effect.
The electrochemical dealloying method to prepare NPG is simple and convenient with absolute yield and controllable structure,which enriches the preparation of small-sized nanoporous metallic materials.A series of research on NPG towards CO oxidation provides new insights into gold catalysis by completely excluding the effect of support.
2.The preparation of nanotubular porous platinum-group bimetallic nanocomposites and research on their electrocatalytic performance.
In this research,a general approach is employed to large-scale synthesis of a novel class of nanotubular mesoporous platinum-group-metals(PGMs)-based nanostructures based on a simple room-temperature dealloying and galvanic replacement reaction.Dealloying was used to synthesize nanoporous metals to act as sacrificial templates,and followed by reacting with H_2PtCl_6 and K_2PdCl_4 solution precursors.The resulted NM-Pt/Cu and NM-Pd/Cu structures were confirmed by transmission electron spectroscopy(TEM) and scanning electron spectroscopy(SEM).NM-Pt/Cu shows a three-dimensional(3D) bicontinuous nanotubular mesoporous structure with tube diameter around 80 nm and shell thickness about 10 nm.Interestingly,the shell surfaces are not smooth and seamless but rather have many small pores and grains around 3 nm.The NM-Pd/Cu structure also exhibits hierarchical hollow structure with the tube diameter around 60 nm and shell thickness about 6 nm.X-ray diffraction(XRD) analysis confirmed that the resulted NM-Pt/Cu and NM-Pd/Cu have the single-phase alloy structure.The possible formation mechanism of such the hierarchically hollow structure was explained as follows:as Pt(or Pd) atoms are reduced and deposited onto the NPC substrate,Cu atoms are progressively leached away.At the same time,these deposited precious metal surface atoms will interdiffuse with Cu to form an alloy.As the reaction goes on,more Cu will be depleted;and accordingly,the surface was gradually passivated due to the further incorporation of more precious metal atoms.Eventually,a PGM-based bimetallic nanotubular mesoporous structure forms,which also marks the completion of the displacement reaction.
NM-Pt/Cu catalyst exhibits high catalytic activity and CO-tolerance toward methanol oxidation.Meanwhile,NM-Pd/Cu shows a unique activity towards oxygen reduction reaction.This synthesis strategy is facile and efficient to fabricate similar ultra-high surface area nanocomposites in large scale with hierarchically hollow structures.These nanostructures have obvious structural advantages in terms of unique catalytic properties,simple and clean processing, and saving precious metals,which suggest their great potential for use in heterogeneous catalysis and fuel cell technologies.
3.Preparation of nanoporous Pt/Au alloys with controllable size and composition by dealloying ternary alloys and research on their electrocatalytic activity.
A simple and general dealloying method was employed to fabricate nanoporous Au/Pt alloys with pre-determined Au/Pt molar ratios.Structural characterization by electron microscopes confirms that selective etching of Cu from Au/Pt/Cu alloy precursors results in the formation of 3-dimensional bicontinuous porous network structures with uniform pores and ligaments.The as-made Pt_4Au_1,Pt_1Au_1,and Pt_1Au_4 samples are all resulted in the similar 3D bicontinuous network with ligament size at 3,5,and 10 nm,respectively.A careful inspection shows that under the same dealloying conditions,nanoporous alloys with high Pt content generally result in smaller feature sizes.X-ray photoelectron spectroscopy and X-ray diffraction demonstrate that Pt_4Au_1 and Pt_1Au_1 nanoporous alloys adopt a relatively uniform bimetallic alloy structure across the entire length scale,while Pt_4Au_1 sample shows slight phase segregation,leading to an Au-rich surface layer.These nanostructures show distinct surface structure sensitive electrocatalytic properties. For methanol electrooxidation,nanoporous Pt_4Au_1 and Pt_1Au_1 showed an obviously improved performance in structure stability and electrocatalytic activity with higher specific activity and lower peak potentials,as compared with the commercial nanoparticle-based catalysts.In sharp contrast,nanoporous Pt_1Au_4 exhibited the best activity for formic acid oxidation amongst all samples,which was characterized by a preferential dehydrogenation reaction process at lower potential. The resulted nanoporous alloys typically represent a class of macroscopic nanostructured materials with a three-dimensional bicontinuous spongy morphology, which are expected to have evident structural advantages as compared with zero-dimensional nanomaterials.Dealloying method is extremely simple and flexible,which is appropriate for large-scale synthesis.In addition,this method is a chemical "green" method,which offers new opportunities for the preparation of nanoporous Pt-M bimetallic catalysts with high surface area and high activities.
引文
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