摘要
碳纳米材料的制备及其功能化目前是一个热门课题。而水热碳化为碳纳米材料的制备及其功能化提供了一种便宜且有效的方法。前驱体决定着最终碳化产物的性能。生物质富含多样的功能基团如胺基,羟基和羧基等,因此水热碳化生物质为合成功能化碳纳米材料提供了多样的可能性。但是这些材料的制备往往涉及苛刻的合成条件和复杂后处理过程,制约其商业化。钯基电催化剂在一些电化学过程中如氧气还原反应和有机小分子氧化反应都表现出了高的电催化活性。在本论文中,论文以碳纳米材料的制备为背景,针对水热碳化为碳纳米的制备及功能化,开展深入研究,具有重要的实际应用价值,此外探索性研究了固体电解质界面和本征微孔聚合物中纳米钯的电催化。主要研究结论总结如下：
(1)以壳聚糖为前驱体,经过在不同温度(180°C/200°C/230°C)下12个小时不完全水热碳化制备了胺基功能化的碳纳米颗粒。拉曼光谱分析显示该碳纳米颗粒具有无定形的碳核,但是电化学测试显示该碳纳米颗粒是电绝缘体。在与另一种表面具有苯磺酸根碳纳米颗粒(Emperor2000)物理混合,进一步的电化学测试表明该颗粒的阴离子吸附容量的值70Cg(-1)。
(2)水热碳化制备了具有核壳结构的碳纳米材料。表面具有苯磺酸根的碳纳米颗粒(Emperor2000,卡博特公司)和在乙酸溶液中质子化壳聚糖超声分散,接着水热碳化处理,得到了具有pH响应的核壳碳纳米材料。用有最佳核壳比率(根据小角中子散射谱计算表明壳的平均厚度为4nnm)的碳纳米材料修饰电极显示该材料具有高pH响应的电阻,电容和法拉第电子转移响应(基于溶液体系中,共价配位和水热嵌入氧化还原探针)。为了解释观察到的pH开关效应,我们讨论了一种壳的“双层排斥”机理。
(3)基于碳纳米颗粒(Emperor2000,卡博特公司),在乙二酸溶液中质子化壳聚糖以及氯化钯,用水热碳化一步合成了一种钯-核壳碳纳米复合材料。该复合材料修饰电极不仅具有pH响应的电容电流和法拉第电流,而且具有对小分子的选择性电催化。我们还讨论了这种复合材料对小分子选择性电催化在燃料电池上的应用。
(4)研究了在固体盐电解质和加湿氮气条件下纳米钯颗粒的电化学催化性能。具体涉及到两种相关的氧化还原体系：(1)甲酸的氧化；(2)氢气的氧化。还研究了不同固体盐,甲酸的分压和加湿气体流速对纳米钯颗粒电催化的影响。观察到了一种显著的固体盐效应并讨论了“盐电池”在传感器的潜在应用。盐(其中硫酸铵最为有效),钯纳米颗粒和气相的三相接触界面即为电化学氧化过程进行的界面。膜电极被同时用作对电极和工作电极(用外部饱和甘汞电极),在于硫酸铵和加湿氮气接触条件下,研究了对苯二酚的氧化还原过程并得到了清晰的氧化还原响应。
(5)研究了两种本征微孔聚合物(PIMs)(i)二乙基葸(分子量为70kDa,BET比表面积为1027m~2,PIM-H)(ii)二甲基联苯基甲烷(分子量为100kDa,BET比表面积为47m~2,PIM-L)的吸附性能及其作为催化剂载体负载钯的电催化。用二价酸性靛蓝阴离子和二价PdCl42阴离子作为吸附物,电化学测试表明溶液类型显著影响在两种聚合物的结合位点和结合容量。研究了高比表面面积聚合物和低比表面积聚合物的薄膜厚度对纳米钯颗粒的甲酸氧化的影响。这个具有更规整和高表面积的本征微孔聚合物显示出“开孔”特征和在孔中钯颗粒可能具有高催化活动性。
Carbon nanomaterials preparation and their functionalization have currently become a hot topic. Hydrothermal carbonization synthesis based biomass offers a cost-effective method for preparation and functionalization of carbon nanomaterials due to cheap and environmentally friendly precursors. In addition, biomass rich in various functional moieties such as amino, hydroxyl and carboxyl also offers versatile possibility for carbon nanomaterials functionalization. Palladium-based electrocatalyst exhibits high catalytic activity in several electrochemical processes such as oxygen reduction reaction (ORR) and reduction of small organic molecules. In this thesis, the first part is concerned with Pd electrocatalysis in amino-functionalized hydrothermal carbon nanomaterials based chitosan. The second part concerns palladium electrocatalysis in non-conventional environments such as salt matrix and the pore of the polymers of intrinsic microporisity (PIMs). These conclusions are summarized as follows:
(1) The preparation of amino-functionalized carbon nanoparticles via partial hydrothermal carbonization from chitosan at180℃(or200℃,230℃) for12h. Raman analysis suggests amorphous carbon core but film electrodes show completely electrically insulating. Anion adsorption capability is exploited in conjuction with a second negatively charged carbon nanoparticles Emperor2000. The useful positive charge is maximized at a hydrothermal carbonization temperature of200℃with a specific anion binding capacity of70Cg-1
(2) The preparation of hydrothermal core-shell nanocarbon. Carbon nanoparticles with phenylsulfonate negative surface functionality (Emperor2000, Cabot Corp.) are coated with positive chitosan followed by hydrothermal carbonization to give pH-responsive core shell nanocarbon composites. With optimised core-shell ratio (resulting in an average shell thickness of ca.4nm, estimated from SANS data) modified electrodes exhibit highly pH-sensitive resistance, capacitance and Faradaic electron transfer responses (solution based, covalently bound, or hydrothermally embedded). A shell "double layer exclusion" mechanism is discussed to explain the observed pH switching effects.
(3) A nanocomposite of carbon nanoparticles (Emperor2000TM), chitosan, and nano-palladium is synthesized in a one-step hydrothermal process with oxalate used as reducing agent. Nano-palladium composites show selective electrocatalysis toward small molecules as well as strong pH effects on capacitive and Faradaic current responses. Implications of selective electrocatalysis toward small molecules in fuel cell application are discussed.
(4) An alternative electrochemical system with the gas phase in closer contact to palladium nanoparticle catalyst is investigated based on a glassy carbon electrode and a solid salt electrolyte. Two relevant redox systems is under investigation:(i) the oxidation of formic acid and (ii) the oxidation of hydrogen. The effects of the type of salt, the partial pressure of formic acid, and the gas flow rate are investigated. A significant salt effect on the palladium catalyzed reaction is observed and potential future applications of "salt cells" in sensing are discussed. It is demonstrated that the reaction zone of salt (here (NH4)2SO4is most effective), palladium nanoparticle catalyst, and gas phase, is where the electrochemical oxidation process occurs. MEA is employed as both a counter electrode and working electrode (with an external SCE reference electrode) for oxidation of hydroquinone in contact with ammonium sulphate under humidified nitrogen gas. A well-defined redox response could be observed.
(5) Two intrinsically microporous polymers (PIMs)(i) ethanoanthracene TB-PIM (MW70kDa, BET surface area1027m2) and (ii) dimethyldiphenylmethane TB-PIM (MW100kDa, BET surface area47m2or PIM-L) are investigated as emerging novel membrane and catalyst support materials. Binding sites and binding ability/capacity in aqueous environments are compared in films deposited onto glassy carbon electrodes for (i) indigo carmine dianion immobilisation (weakly binding from water-ethanol) and (ii) PdCl42-immobilisation (strongly binding from acidic media). Electrocatalytic oxidation of formic acid (at pH6) is investigated for PIM-L and PIM-H as a function of film thickness. The more rigid high BET surface area material PIM-H exhibits "open-pore" characteristics with much more promising electrocatalytic activity at Pd within polymer pores.
引文
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