CN107523845B - 一种碳布负载Ni-S-Se纳米片阵列的制备方法 - Google Patents

一种碳布负载Ni-S-Se纳米片阵列的制备方法 Download PDF

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CN107523845B
CN107523845B CN201710681126.3A CN201710681126A CN107523845B CN 107523845 B CN107523845 B CN 107523845B CN 201710681126 A CN201710681126 A CN 201710681126A CN 107523845 B CN107523845 B CN 107523845B
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徐波
陈志明
张哲�
杨贺
李村成
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Abstract

本发明涉及一种碳布负载Ni(S0.41Se0.59)2纳米片阵列及其制备方法，属于无机纳米材料制备技术领域。本发明以碳布负载的Ni(OH)2纳米片阵列为前驱体通过同时硫化‑硒化制备碳布负载Ni(S0.41Se0.59)2纳米片阵列。具体步骤如下：首先以硝酸镍、氟化铵和尿素为反应物通过水热法制得碳布负载的Ni(OH)2纳米片阵列为前驱体；进一步使用质量比1:3的硫粉和硒粉混合物对前驱体在氮气保护下进行同时的硫化和硒化制得碳布负载Ni(S0.41Se0.59)2纳米片阵列。

Description

一种碳布负载Ni-S-Se纳米片阵列的制备方法
技术领域
本发明涉及一种Ni-S-Se三组分纳米片阵列及其制备方法，属于无机纳米材料制备领域。
背景技术
随着全球能源危机及环境污染的加剧，可再生清洁能源受到了科学家越来越多的关注。其中氢能具有能量密度高、清洁无污染的优点，被认为是传统化石燃料的优异替代品。在催化剂存在下，利用太阳能或者电能分解水是制备氢气的重要方法。过渡金属硫属化合物（如：硫化钴、硒化镍、硫化钨、硫化钼等）具有优异的水分解催化性能，受到了广泛的关注。相关研究表明，此类催化剂的形貌、结构、组成等因素均对其催化活性具有重要的影响。比如纳米线等具有高比表面积的形貌结构有利于催化剂暴露更多的活性位点，从而提高其催化能力。利用化学手段调控催化剂的组分是另一种优化催化剂性能的重要方法。当前，金属离子掺杂被广泛应用于增强此类催化剂的催化性能。例如，X.P. Sun等人报道了Fe掺杂的NiSe纳米片，表现出优异的电催化分解水性能（Chem. Commun. 52 (2016) 4529-4532）；B. Liu等人报道了Mo掺杂的NiS，具有优良的分解水产氢性能（Adv. Mater. 29 (2017)1606521）。但是，尽管当前阳离子掺杂被广泛的应用于调控催化剂性能，采用阴离子掺杂的方式优化催化剂性能的相关报道仍然较少。
众所周知，硫化镍和硒化镍在分解水方面都具有良好的催化性能。而且硫的电负性（χ = 2.58）和硒的电负性（χ = 2.55）非常接近，有利于二者同时和镍化合。我们认为，基于镍、硫、硒三元素之间的协同效应，三组分的Ni-S-Se化合物的催化性能将会得到进一步的改善。同时，以具有多孔结构的碳布作为载体，有助于提高催化剂的比表面积，增强其催化性能。
发明内容
本发明的目的在于提供一种具有高比表面积的碳布负载Ni(S0.41Se0.59)2纳米片阵列的制备方法。本发明提供的这种制备方法，工艺简单，成本较低，所得碳布负载Ni(S0.41Se0.59)2纳米片阵列具有优异的电解水产氢催化性能，是一种优良的电催化剂。
本发明的目的是通过以下技术方案实现的，一种碳布负载Ni(S0.41Se0.59)2纳米片阵列的制备方法，包括以下步骤：
1）按照一定摩尔比分别称取Ni(NO3)2.6H2O, NH4F 和尿素并溶于去离子水中；
2）将步骤1所得混合溶液转移至聚四氟乙烯反应釜中，同时加入预先裁剪好的条状碳 布；
3）将反应釜放置到烘箱中加热后得到碳布负载的Ni(OH)2纳米片阵列；
4）将步骤3所得负载Ni(OH)2的放到石英舟一端，并在另一端加入一定摩尔比的硫粉和硒粉混合物；
5）将石英舟放入氮气保护的高温管式炉中，注意将盛放硫粉硒粉混合物的一端置于上气流方位，加热后即得到碳布负载Ni(S0.41Se0.59)2纳米片阵列；所述纳米片的长度为3-5微米，厚度为80-100纳米。
本发明的有益效果：
（1）本发明提供了一种新型碳布负载Ni(S0.41Se0.59)2纳米片阵列的制备方法，即首先以 水热法制备碳布负载的Ni(OH)2纳米片阵列，再同时对其进行硫化和硒化反应制得产物。制备方法简单易操作，成本低，具有潜在的大规模应用价值；
（2）本发明制备的产物为碳布负载Ni(S0.41Se0.59)2纳米片阵列，产物形貌尺寸均匀；
（3）本发明制备的碳布负载Ni(S0.41Se0.59)2纳米片阵列对于电催化分解水制备氢气具 有优异的催化性能；
（4）本发明的制备仅需实验室常用的普通设备，不需专用设备，工艺过程简便易行。
附图说明
图1为本发明方法所制备的碳布负载Ni(S0.41Se0.59)2纳米片阵列用美国FEIQUANTA FEG250扫描电子显微镜观察后拍摄的低倍扫描电镜（SEM）照片；
图2为本发明方法所制备的碳布负载Ni(S0.41Se0.59)2纳米片阵列用美国FEIQUANTA FEG250扫描电子显微镜观察后拍摄的高倍扫描电镜（SEM）照片；
图3是本发明方法所制备的碳布负载Ni(S0.41Se0.59)2纳米片阵列的X射线衍射（XRD）图；
图4是本发明方法所制备的碳布负载Ni(S0.41Se0.59)2纳米片阵列的X射线光电子能谱 图；
图5是本发明方法所制备的碳布负载Ni(S0.41Se0.59)2纳米片阵列用辰华660D电化学工 作站测试所得的析氢电流密度-电势图。
具体实施方式
下面通过具体实施实例并结合附图对本发明的内容作进一步详细说明，但这些实施例 并不限制本发明的保护范围。
实施例1
首先将浓度为0.05摩尔每升的硝酸镍，0.1摩尔每升的氟化铵和0.25摩尔每升的尿素 水溶液混合，然后转移至聚四氟乙烯反应釜中并加入预先裁剪好的1*4 cm的条状碳布。将 上述反应物在120摄氏度烘箱中反应6小时，自然降至室温后即得到碳布负载的Ni(OH)2纳 米片阵列。将上述碳布负载的Ni(OH)2纳米片阵列放置在石英舟的一端，并在另一端放上 80mg摩尔比1:3的硫粉和硒粉混合物。将石英舟放入放入氮气保护的高温管式炉中，注意将 盛放硫粉硒粉混合物的一端置于上气流方位，以10摄氏度每分钟的升温速率将管式炉温度 升至450摄氏度并保温反应1.5小时后自然降温至室温后即得到碳布负载Ni(S0.41Se0.59)2纳 米片阵列。
实施例2
首先将浓度为0.05摩尔每升的硝酸镍，0.1摩尔每升的氟化铵和0.25摩尔每升的尿素水溶液混合，然后转移至聚四氟乙烯反应釜中并加入预先裁剪好的1*4 cm的条状碳布。将 上述反应物在110摄氏度烘箱中反应10小时，自然降至室温后即得到碳布负载的Ni(OH)2纳 米片阵列。将上述碳布负载的Ni(OH)2纳米片阵列放置在石英舟的一端，并在另一端放上 100mg摩尔比1:3的硫粉和硒粉混合物。将石英舟放入放入氮气保护的高温管式炉中，注意 将盛放硫粉和硒粉混合物的一端置于上气流方位，以10摄氏度每分钟的升温速率将管式炉 温度升至450摄氏度并保温反应2小时后自然降温至室温后即得到碳布负载Ni(S0.41Se0.59)2 纳米片阵列。
实施例3
使用辰华660D电化学工作站对碳布负载Ni(S0.41Se0.59)2纳米片阵列的电解水催化活性 进行测试。以铂丝为对电极，银/氯化银为参比电极，碳布负载Ni(S0.41Se0.59)2纳米片阵列为工作电极，1.0摩尔每升KOH水溶液为电解质溶液。在-0.6 至0.2 V电压范围内，以5毫安每秒的扫速进行线性伏安扫描，即可得到碳布负载Ni(S0.41Se0.59)2纳米片阵列催化电解水产氢的极化曲线。

Claims (2)

1.一种碳布负载Ni(S0.41Se0.59)2纳米片阵列，所述纳米片的长度为3-5微米，厚度为80-100纳米；
所述碳布负载Ni(S0.41Se0.59)2纳米片阵列的制备方法，步骤如下：
1）采用水热法，以硝酸镍、氟化铵和尿素为反应物制得碳布负载的Ni(OH)2纳米片阵列为前驱体；
2）将步骤1)所得碳布负载的Ni(OH)2纳米片阵列转移至石英舟中的一端，并在另一端放上摩尔比1:3的硫粉和硒粉混合物；将石英舟放入氮气保护的高温管式炉中，将盛放硫粉和硒粉混合物的一端置于上气流方位，以10摄氏度每分钟的升温速率将管式炉温度升至450摄氏度并保温反应后自然降温至室温即得到碳布负载Ni(S0.41Se0.59)2纳米片阵列。
2.一种碳布负载Ni(S0.41Se0.59)2纳米片阵列的制备方法，其特征在于制备方法的步骤如下：
1）采用水热法，以硝酸镍、氟化铵和尿素为反应物制得碳布负载的Ni(OH)2纳米片阵列为前驱体；
2）将步骤1)所得碳布负载的Ni(OH)2纳米片阵列转移至石英舟中的一端，并在另一端放上摩尔比1:3的硫粉和硒粉混合物；将石英舟放入氮气保护的高温管式炉中，将盛放硫粉和硒粉混合物的一端置于上气流方位，以10摄氏度每分钟的升温速率将管式炉温度升至450摄氏度并保温反应后自然降温至室温即得到碳布负载Ni(S0.41Se0.59)2纳米片阵列。
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