CN112246253B - 一种Co15Fe3S16纳米点状化合物及其制备方法 - Google Patents
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Abstract
本发明公开了一种Co15Fe3S16纳米点状化合物的制备方法，该方法为：称取原料和球磨处理；制备前驱体；液氨处理；水热法处理。本发明还公开一种Co15Fe3S16纳米点状化合物，其采用如上所述的方法制备而成。
Description
技术领域
本发明涉及一种制备Co15Fe3S16纳米点的方法及利用该方法制备的化合物。
背景技术
近年来，通过电催化的方法获得绿色能源氢能是当今世界的一个核心话题。析氧反应是限制电催化分解水反应速率的关键步骤。基于钴硫化合物的析氧电催化剂由于不含贵金属且地球储量丰富受到广泛的关注。目前已经报道的钴硫化合物电催化剂主要是通过水热的方法制备得到。由于水热法制备的样品颗粒较大，导致电化学活性面积有限。同时钴硫化合物本身催化活性仍未达到广泛应用的要求。因此，如何提高比表面积、增大电化学活性面积，并提高钴硫化合物电催化剂的催化析氧性能成为一个关键问题。
发明内容
本发明的目的在于公开一种具有优异电催化析氧活性的Co15Fe3S16纳米点状化合物。本发明还提供一种制备Co15Fe3S16纳米点状电催化剂的方法。
本发明的实现包括以下步骤：将钴粉、铁粉和硫粉按摩尔比5：1：6的比例称取，原料的总量为0.15摩尔，将称量好的原料密封在球磨罐中，球磨两小时使原料混合均匀；将混合好的原料转移到手套箱内，加入0.0375摩尔的钾块，密封在石英管内，并充入0.2个大气压，将石英管加热到900℃，在该温度下保持2天，将自然冷却后的样品重新研磨均匀，密封在石英管内，将石英管加热到950℃，在该温度下保持2天，石英管自然冷却后，将样品研磨均匀后即得到前驱体；将400毫克的前驱体置于石英管内，利用封管设备缓慢地将石英管抽成真空后，同时用液氮对石英管进行冷却，缓慢地将8毫升的液氨引入到石英管内，摇晃液氨使得样品与液氨充分混合均匀，反应10分钟后，将液氨缓慢抽干；将所得到的样品转移到水热釜内衬中，加入30毫升的氨水，10毫升的乙醇，混合均匀，将混合溶液转移至超声波清洗器中，超声12小时，离心清洗后得到Co15Fe3S16纳米点状化合物。
与现有技术相比，本发明所述的样品制备方法具有以下的优点：所制备的Co15Fe3S16化合物体积非常小，直径在3~5nm之间，具有纳米点形貌；所制备的Co15Fe3S16化合物电催化析氧性能优异，在10 mA/cm-2的电流密度下具有265 mV的过电位。
附图说明
图1为按照对比例和实施例的方法制备的Co15Fe3S16化合物的XRD图谱。
图2为按照对比例的方法制备的Co15Fe3S16化合物的SEM图谱。
图3为按照实施例的方法制备的Co15Fe3S16纳米点状化合物的TEM图谱。
图4为按照对比例和实施例的方法制备的Co15Fe3S16化合物的过电位曲线图。
具体实施方式
下面通过具体实施例对本发明做出进一步的具体说明，但本发明并不局限于下述实例。
实施例：将钴粉、铁粉和硫粉按摩尔比5：1：6的比例称取，原料的总量为0.15摩尔，将称量好的原料密封在球磨罐中，球磨两小时使原料混合均匀；将混合好的原料转移到手套箱内，加入0.0375摩尔的钾块，密封在石英管内，并充入0.2个大气压，将石英管加热到900℃，在该温度下保持2天，将自然冷却后的样品重新研磨均匀，密封在石英管内，将石英管加热到950℃，在该温度下保持2天，石英管自然冷却后，将样品研磨均匀后即得到前驱体；将400毫克的前驱体置于石英管内，利用封管设备缓慢地将石英管抽成真空后，同时用液氮对石英管进行冷却，缓慢地将8毫升的液氨引入到石英管内，摇晃液氨使得样品与液氨充分混合均匀，反应10分钟后，将液氨缓慢抽干；将所得到的样品转移到水热釜内衬中，加入30毫升的氨水，10毫升的乙醇，混合均匀，将混合溶液转移至超声波清洗器中，超声12小时，离心清洗后得到Co15Fe3S16纳米点状化合物。
为了说明本实施例的技术效果，按照以下步骤制备样品作为本实施例的对比例：配置30毫升的0.033摩尔每升的六水硝酸钴溶液，加入1毫升的乙二胺，得到混合溶液；配置10毫升的0.1摩尔每升的硫脲溶液缓慢加入混合溶液中，搅拌30分钟；加入0.115克的铁粉，将溶液转移至高压反应釜的内衬中，在180 ℃下保持12小时后自然冷却，离心清洗后得到对比例的样品。
为了说明本实施例的技术效果，对按实施例和对比例的样品进行了表征。图1是按对比例和实施例的Co15Fe3S16化合物的XRD图谱，可以看到对比例的样品结晶性好，且衍射峰与Co9S8（PDF＃65-6801）的标准卡片的峰一一对应，没有杂相。实施例样品的衍射峰的强度明显变弱，只能观察到较强衍射峰，且衍射峰宽化，说明实施例样品的颗粒明显小于对比例样品。图2是按对比例的Co15Fe3S16化合物的SEM图谱，可以看到颗粒的长度均在微米级别。图3是按实施例的Co15Fe3S16纳米点状化合物的TEM图谱，可以看到样品是典型的纳米点形貌，体积非常小，直径在3~5 nm之间。图4是按对比例和实施例的Co15Fe3S16化合物的过电位曲线图，可以看到实施例的在10 mA/cm2电流密度下的过电位为265 mV，明显优于对比例的384mV的过电位。本发明还公开了一种Co15Fe3S16纳米点状电催化剂，其采用如实施例所述的方法制备而成。
需要声明的是，以上所述的仅是本发明的优选实施方式，本发明不限于以上实施例。可以理解，本领域技术人员在不脱离本发明的基本构思的前提下直接导出或联想到的其他改进和变化，均应认为包含在本发明的保护范围之内。
Claims (3)
1.一种制备Co15Fe3S16纳米点状化合物的方法，包括如下步骤：将钴粉、铁粉和硫粉按摩尔比5：1：6的比例称取，原料的总量为0.15摩尔，将称量好的原料密封在球磨罐中，球磨两小时使原料混合均匀；将混合好的原料转移到手套箱内，加入0.0375摩尔的钾块，密封在石英管内，并充入0.2个大气压，将石英管加热到900℃，在该温度下保持2天，将自然冷却后的样品重新研磨均匀，密封在石英管内，将石英管加热到950℃，在该温度下保持2天，石英管自然冷却后，将样品研磨均匀后即得到前驱体；将400毫克的前驱体置于石英管内，利用封管设备缓慢地将石英管抽成真空后，同时用液氮对石英管进行冷却，缓慢地将8毫升的液氨引入到石英管内，摇晃液氨使得样品与液氨充分混合均匀，反应10分钟后，将液氨缓慢抽干；将所得到的样品转移到水热釜内衬中，加入30毫升的氨水，10毫升的乙醇，混合均匀，将混合溶液转移至超声波清洗器中，超声12小时，离心清洗后得到Co15Fe3S16纳米点状化合物。
2.一种Co15Fe3S16纳米点状化合物，其特征在于，采用如权利要求1中的方法制备而成。
3.一种如权利要求2所述的Co15Fe3S16纳米点状化合物用于电催化析氧领域。
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| CN1094376A (zh) * | 1993-04-26 | 1994-11-02 | 中国石化齐鲁石油化工公司 | 钴-钼系一氧化碳变换催化剂的硫化方法 |
| CN105776353A (zh) * | 2016-03-29 | 2016-07-20 | 中国石油大学(北京) | 硫铁化合物及其制备方法 |
| CN107083501A (zh) * | 2017-05-19 | 2017-08-22 | 广东省钢铁研究所 | 一种铁镍钼合金粉体的制备方法 |
| CN109999865A (zh) * | 2019-05-15 | 2019-07-12 | 台州学院 | 一种镍磷硫硒电催化剂的制备方法 |
| CN111686735A (zh) * | 2020-06-30 | 2020-09-22 | 中国石油大学(华东) | 一种载体煤改性制备高分散型煤/重油加氢共炼催化剂 |
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