摘要：在能源危机日益加剧的21世纪，氢气作为一种高效、清洁绿色的能源，电化学电解水为其最理想的制备方法。在过渡金属氧化物中，Nb2O5作为一种非贵金属材料，具有高比表面积、高化学稳定性和耐腐蚀性等优点，使其在作为催化剂、传感器材料等方面得到了广泛应用。本文通过阳极氧化法在电解液为1 wt% HF 加 1 M H3PO4 的混合溶液中60 V电压下反应30 min，制备出了厚度约为500 nm的高度有序的多孔纳米氧化铌。在这篇文章中，我们通过改变阳极氧化电位和氧化时间及 HF 浓度对多孔氧化铌制备过程中的影响，探究能够制备出稳定的高度有序多孔氧化铌结构和形貌的最优条件，并通过SEM、XPS和XRD等对其形貌和结构进行表征。并且在最优条件下通过高温退火方法向氧化铌中掺入氮或磷元素进一步对其进行改性，用电化学工作站测试其电化学性能。结果表明，当电流密度都为10 mA cm-2时，Nb2O5，Nb2N 和Nb2O5/P的过电位分别为693、489和149 mV。由析氢曲线图可知，经过过氩气退火后的氧化铌具有一定的电催化性能，但性能不如Nb2N，掺磷后的氧化铌析氢效果最好。

关键词  阳极氧化 纳米多孔膜 电催化产氢  

毕业设计说明书外文摘要

Title   Preparation of porous Nb2O5 thin films by anodic oxidation and explore    their electrocatalytic hydrogen production                                                          

Abstract ：With the energy crisis is expangding in the 21st century，hydrogen as an efficient, clean green energy, the electrochemical electrolysis has been thought as it’s the most ideal way of preparation.In transition metal oxides, Nb2O5 as a kind of non-precious metal material, has high specific surface area,excellent chemical stability and corrosion resistance which make it has been widely used as a catalyst,sensor material and so on. In this paper, ordered porous niobium oxide with the thickness of 500 nm is prepared by anodization of niobium foils at 60V in the mixture of 1 wt% HF and 1M H3PO4 for 30 min, we investigated the effects of anodic oxidation potential and oxidation time and HF concentration on the preparation of porous niobium oxide, and explored the optimum conditions for the preparation of stable highly ordered porous niobium oxide structures and morphology and the morphology and structure were characterized by SEM, XPS and XRD. Under the optimum conditions, the nitrogen or phosphorus elements were doped with niobium oxide by annealing method, and the electrochemical performance was also tested with electrochemical workstation. According to the result that shows the overpotential of the annealing Nb2O5, Nb2N and Nb2O5 / P are 693, 489 and 149 mV, respectively, when the current density is 10 mA cm-2. From the hydrogen evolution curve, it can be seen that the niobium oxide after argon annealing has a certain electrocatalytic performance, but it is not as good as Nb2N, and the hydrogen evolution of niobium oxide after phosphorus removal is the best.

Keywords  Anodized   Nano-porous oxide flim   Electrocatalytic hydrogen production

目次

1  引言 1

1.1 选题背景及意义 1

1.2 电化学催化介绍 2

1.2.1 电化学催化析氢原理 2

1.2.2 电催化在实际工程中的应用 3

1.3 阳极氧化法介绍 4

   1.3.1 阳极氧化机理介绍 4

   1.3.2 阳极氧化法的应用 5

2 实验部分 6

2.1 阳极氧化实验过程 6

2.2 多孔氧化铌改性实验过程 6

3 实验结果与讨论 8

3.1 多孔有序氧化铌的形貌表征 8

3.2 多孔氧化铌的成分分析 12

3.3 电催化性能表征 13

3.3.1 氧化铌电催化性能表征 13