铁基纳米磷化物可控合成、结构调控及其电催化产氢性能的研究

发布时间：2018-03-08 16:26

  本文选题：三维有序大孔　切入点：FeP　出处：《内蒙古大学》2017年硕士论文　论文类型：学位论文

【摘要】：氢气由于其清洁无污染的性质,被认为是可以代替化石燃料的一种新型能源。电解水产氢被认为是可以实现工业化生产氢气的一种重要方式,但是电解水产氢的催化剂却成为了其实现工业化的一个难点。相对于其他过渡金属,Fe元素在地球上的含量最多,因此,利用Fe来做电化学产氢的催化剂是最为经济有效的。FeP以其优异的电催化析氢性能,受到研究人员广泛的关注,成为当前研究的热点。研究表明,通过提高FeP的电化学活性表面积或降低FeP的电阻、掺杂非金属阴离子或金属阳离子均可以有效的提高催化剂的产氢活性。基于此,本文构筑了三类具有特殊形貌和结构的3DOMFeP、3DOMSe掺杂FeP和中空FeCoP纳米电催化剂,通过结构、组成、尺寸和形貌、比表面积和表面特性的优化,极大地提升了这些催化剂的电催化产氢性能,获得了具有一定应用潜力的系列电催化产氢催化剂。本文具体研究内容如下:本文第一章对电催化产氢研究进展以及电催化产氢催化剂进行了综述,重点介绍了过渡金属磷化物电化学催化剂的研究进展。本文第二章本章以聚苯乙烯(PS)微球为模板,通过离心方法将其组装构筑了 PS微球交替晶体模板,随后以无水乙醇为溶剂,将Fe(NO3)3为前驱体溶液填充于PS微球交替晶体模板空隙,经600℃锻烧,获得具有规则三维有序大孔结构的3DOMFe2O3。以次磷酸钠为磷源,在不同温度下对3DOMFe2O3进行了磷化处理,获得了系列3DOM FeP,并通过XRD、SEM、TEM、STEM、BET和XPS等表征手段,对其相态、结构、尺寸、形貌、比表面与孔结构、表面元素组成与价态等进行了详细的分析,系统评价了 3DOM FeP催化剂的电催化析氢性能。本文第三章以3DOMFe20O为前驱体,以次磷酸钠为磷源,通过在磷化过程中添加Se粉和控制磷化温度,制备了系列3DOMSe掺杂FeP催化剂,通过调控Se粉与次磷酸钠的比例,成功将Se掺入FeP晶格。通过XRD、SEM、TEM和XPS等表征手段对所得3DOM Se掺杂FeP的相态、结构、尺寸和形貌、表面特性等进行了系统研究,并利用线性扫描伏安、循环伏安和交流阻抗等电化学测试方法对3DOM Se掺杂FeP催化剂的电催化析氢性能进行了研究。本文第四章以Cu2O为模板、NaS2O3为刻蚀剂,通过调整Co和Fe前驱体的比例,首先合成中空纳米盒形貌的FeCo(OH)2,再通过高温磷化方法合成系列中空盒装FeCoP催化剂。通过XRD、SEM、TEM和XPS等表征手段对所得3DOM Se掺杂中空FeCoP的相态、结构、尺寸和形貌、表面特性等进行了系统研究,并利用线性扫描伏安、循环伏安和交流阻抗等电化学测试方法对中空FeCoP催化剂的电催化析氢性能进行了研究。本文第五章对全文进行了总结,并对未尽研究工作和进一步探索进行了展望。
[Abstract]:Because of its clean and pollution-free nature, hydrogen is considered to be a new energy source that can replace fossil fuels. Electrolytic hydrogen in aquatic products is considered to be an important way to produce hydrogen in an industrial way. However, the catalyst for electrolytic hydrogen in aquatic products has become a difficult point in industrialization. Compared with other transition metals, Fe is the most abundant on earth, so, Using Fe as the catalyst for electrochemical hydrogen production is the most economical and effective catalyst for hydrogen evolution by electrocatalysis. It has been widely concerned by researchers and has become a hot research topic at present. By increasing the electrochemical active surface area of FeP or reducing the resistance of FeP, doping of nonmetallic anions or metal cations can effectively improve the hydrogen-producing activity of the catalyst. In this paper, three kinds of 3DOMFeP- 3DOMSe doped FeP and hollow FeCoP nanocrystalline electrocatalysts with special morphology and structure were constructed. The structure, composition, size and morphology, specific surface area and surface properties of the catalysts were optimized. This greatly improves the hydrogen production performance of these catalysts. A series of electrocatalytic catalysts for hydrogen production have been obtained with some potential applications. The main contents of this paper are as follows: in the first chapter, the research progress of electrocatalytic hydrogen production and the electrocatalytic hydrogen production catalysts are reviewed. In chapter 2, PS microspheres were used as templates, and PS microspheres were assembled by centrifugal method to form alternative crystal templates of PS microspheres. Then, with anhydrous ethanol as solvent, Fe(NO3)3 as precursor solution was filled in PS microspheres alternate crystal template voids. After calcined at 600 鈩，

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