CN108479791B - 一种Co/Ni-MoO2复合电解水催化剂的制备方法 - Google Patents
一种Co/Ni-MoO2复合电解水催化剂的制备方法 Download PDFInfo
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Abstract
本发明涉及一种Co/Ni‑MoO2复合电解水制氢催化剂及其制备方法，属于无机纳米材料制备技术领域。本发明以硝酸钴、硝酸镍、钼酸铵和F127四种物质为前驱体通过研磨混合后加热的方法制备Co/Ni‑MoO2催化剂。具体步骤如下：首先以硝酸钴、硝酸镍、钼酸铵和F127为反应物通过混合研磨的方法制备面团状前驱体；进一步分别先后在70摄氏度和300摄氏度下加热制得Co/Ni‑MoO2复合催化剂。
Description
技术领域
本发明涉及一种Co/Ni-MoO2复合电解水制氢催化剂及其制备方法，属于无机纳米材料技术领域。
背景技术
随着传统化石燃料的不断消耗以及环境污染的日益加剧，再生清洁能源受到了越来越广泛的关注。氢能具有能量密度高、清洁环保等特点，被认为是优异的化石燃料替代品。通过电解水的方法可以方便的制备氢气，满足实际应用需求。但是，由于水裂解反应为非自发反应，其吉布斯自由能变高达237kJ/mol，使得电解水过程中的电能消耗较大。铂族金属常被用作电解水的催化剂以降低水裂解过程中的电能消耗，但是其价格过于昂贵，无法广泛使用。因而，开发价格便宜的电解水催化剂，对于减少电解水过程中的能源消耗，减少铂等贵金属的用量，降低电解水的成本具有重要的意义。
MoO2具有接近金属的良好导电性，且化学稳定性高、价格便宜，有望成为一类重要的电解水催化剂。但是在电解水过程中，MoO2会和氢自由基之间形成键能很强的金属氢化物，从而降低了反应速率。将过渡金属修饰到MoO2基体中，制备过渡金属-MoO2复合催化剂是解决这一问题的常见方法。例如，L.J. Yang等人通过将Co掺杂到MoO2纳米线中的方法提高了催化性能（Nano Energy 41 (2017) 772-779）；B.W. Ren等人报道了Ni掺杂的MoO2纳米线，具有良好的电解水产氢性能及稳定性（J. Mater. Chem. A 5 (2017) 24453-24461）。但是，尽管当前已有多篇通过掺杂过渡金属到MoO2中制备具有优良性能的电解水催化剂的报道，但是相关催化剂制备方法往往比较复杂、催化剂产量往往较低。开发一种成本低廉、简便易行、适于大规模应用的过渡金属-MoO2复合催化剂的制备方法具有重要的意义。
发明内容
本发明的目的在于提供一种成本低廉、简便易行的Co/Ni-MoO2复合电解水制氢催化剂的制备方法。本发明提供的这种制备方法，工艺简单，成本低廉，且所制备的Co/Ni-MoO2具有优异的电解水产氢催化性能，具有较高的实际应用价值。
本发明的目的是通过以下技术方案实现的，一种Co/Ni-MoO2复合电解水制氢催化剂的制备方法，包括以下步骤：
1）按照一定摩尔比分别称取Co(NO3)2 .6H2O, Ni(NO3)2 .6H2O，(NH4)2MoO4和(EO)106(PO)70(EO)106三嵌段聚合物(Pluronic F127)至研钵中；
2）将步骤1所得混合物在室温下研磨20分钟，得到面团状固体；
3）将步骤2所得面团状固体转移到石英舟中，并放置于马弗炉中加热后即得到Co/Ni-MoO2复合电解水制氢催化剂。
本发明的有益效果：
（1）本发明提供了一种新型Co/Ni-MoO2复合电解水制氢催化剂的制备方法，即首先通过简单混合研磨的方法制备面团状的前驱体混合物，再对其进行加热反应即可制得产物。制备方法简单易操作，不需要特殊的设备，成本低廉且适于大规模制备，可以满足实际应用的需求；
（2）本发明制备的Co/Ni-MoO2复合催化剂具有优异的电解水制氢催化性能及良好的稳定性。
附图说明
图1为本发明方法所制备的Co/Ni-MoO2复合电解水制氢催化剂用美国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Co/Ni-MoO2复合电解水制氢催化剂用美国FEI QUANTAFEG250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Co/Ni-MoO2复合电解水制氢催化剂的X射线衍射（XRD）图；
图4是本发明方法所制备的Co/Ni-MoO2复合电解水制氢催化剂的X射线光电子能谱图；
图5是本发明方法所制备的Co/Ni-MoO2复合电解水制氢催化剂用辰华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
首先分别称取硝酸钴、硝酸镍、钼酸铵和F127各2.0毫摩尔于研钵中，室温下混合研磨20分钟制得面团状前驱体。将上述前驱体转移至马弗炉中，在空气气氛下，先在70摄氏度下加热5小时，然后将温度升高至300摄氏度加热1小时后自然降温至室温，即得到Co/Ni-MoO2复合电解水制氢催化剂。
实施例2
首先分别称取硝酸钴、硝酸镍、钼酸铵和F127各2.0毫摩尔于研钵中，室温下混合研磨20分钟制得面团状前驱体。将上述前驱体转移至马弗炉中，在空气气氛下，先在80摄氏度下加热8小时，然后将温度升高至300摄氏度加热1小时后自然降温至室温，即得到Co/Ni-MoO2复合电解水制氢催化剂。
实施例3
首先分别称取硝酸钴、硝酸镍、钼酸铵和F127各3.0毫摩尔于研钵中，室温下混合研磨20分钟制得面团状前驱体。将上述前驱体转移至马弗炉中，在空气气氛下，先在70摄氏度下加热8小时，然后将温度升高至300摄氏度加热1小时后自然降温至室温，即得到Co/Ni-MoO2复合电解水制氢催化剂。
实施例4
将Co/Ni-MoO2复合电解水制氢催化剂负载到商业泡沫镍片上，使用辰华660D电化学工作站对其电解水催化活性及稳定性进行测试。以铂丝为对电极，银/氯化银为参比电极，泡沫镍负载Co/Ni-MoO2为工作电极，1.0摩尔每升KOH水溶液为电解质溶液。在-0.5 至0.1 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Co/Ni-MoO2复合催化剂催化电解水产氢的极化曲线。
Claims (2)
1.一种Co/Ni-MoO2复合电解水制氢催化剂的制备方法，其特征在于制备方法的步骤如下：
1）通过混合研磨的方法以硝酸钴、硝酸镍、钼酸铵和F127为反应物制得面团状的前驱体混合物；
2）将步骤1）所得面团状的前驱体混合物置于马弗炉中，先在70摄氏度下加热5小时，然后将温度升高至300摄氏度加热1小时后自然降温至室温即得到Co/Ni-MoO2复合电解水制氢催化剂。
2.根据权利要求1所述的Co/Ni-MoO2复合电解水制氢催化剂的制备方法，其特征在于，所述前驱体混合物中硝酸钴、硝酸镍、钼酸铵和F127四种物质的摩尔比为1:1:1:1。
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| CN112563522A (zh) * | 2020-12-11 | 2021-03-26 | 西北大学 | 一种钴掺杂二氧化钼电催化剂的制备方法及其应用 |
| CN114774970A (zh) * | 2022-03-22 | 2022-07-22 | 杭州师范大学 | MoO2/Co—NC纳米复合电催化剂及其制备方法和应用 |
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