CN111420682A - 一种具有光电集成解水制氢活性的纳米异质催化剂 - Google Patents
一种具有光电集成解水制氢活性的纳米异质催化剂 Download PDFInfo
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Abstract
本发明公开了一种具有光电集成解水制氢活性的纳米异质催化剂，该纳米异质催化剂为Ni3S2‑MoS2异质二维纳米片催化剂，采用水热法制备，步骤如下：将Na2MoO4和C2H5NS的混合溶液置于高压反应釜中，将泡沫镍浸入混合溶液中，升温至200℃，水热反应20小时，自然冷却至室温，清洗、真空干燥，获得所述的纳米异质催化剂。该催化剂通过耦联双重活性，集成可再生太阳能助推电解水，能够直接降低分解水制氢工艺成本，而且，双活性催化剂呈现了新颖的自然集成光电催化技术，区别于传统的光敏半导体和助催化剂复合集成的光电化学电极，基于该类催化剂的光电功能集成将革新水分解制氢技术，提高能量转化效率，降低工艺成本。
Description
技术领域
本发明涉及一种具有光电集成解水制氢活性的纳米异质催化剂，属于纳米能源功能材料领域。
背景技术
氢气具有能量密度高、可存储移动、便于重整转化、燃烧无污染等一系列优点，被认为是理想的绿色能源载体。在现行的制氢工艺中，依赖于活性催化剂的电解水技术是制取高纯度氢气的可行方案，贵金属基的铂（Pt）和氧化铱（IrO2）或氧化钌（RuO2）分别是当前最有效的析氢和析氧催化剂，然而它们的稀有性和高价格限制了电解水制氢技术的发展。所以，开发低成本、高效稳定的催化剂成为当前电解水制氢工业发展的先决条件。而且，将太阳能、风能等可再生能源集成驱动水电解反应路径，能够进一步降低制氢成本，具有显著的可持续发展能力。
发明内容
本发明的目的是提供一种具有光电催化双活性的纳米异质催化剂。
实现本发明目的的技术解决方案是：本发明所述的一种具有光电集成解水制氢活性的纳米异质催化剂，所述的纳米异质催化剂为Ni3S2-MoS2异质二维纳米片催化剂，采用水热法制备，步骤如下：
将Na2MoO4和C2H5NS的混合溶液置于高压反应釜中，将泡沫镍浸入混合溶液中，升温至200℃，水热反应20小时，自然冷却至室温，清洗、真空干燥，获得所述的纳米异质催化剂。
较佳的，混合溶液中，Na2MoO4与C2H5NS的摩尔比为2:9。
较佳的，泡沫镍的尺寸为1cm×3cm，经丙酮、3M盐酸、乙醇、去离子水各超声清洗10min去除氧化层。
较佳的，60℃下真空干燥。
上述纳米异质催化剂在二电极光电集成水解器中的应用，将两片生长有纳米异质催化剂的泡沫镍分别作为氧化和还原反应电极，构造二电极水解系统。
与现有技术相比，本发明的有益效果是：1、制备原料廉价、工艺简单，可工业化拓展，相对贵金属基催化剂而言，具有显著的成本优势；2、Ni3S2-MoS2异质催化剂具有优越的全解水活性；3、Ni3S2-MoS2异质催化剂具有独特的光电耦联效应，其构建的双电极解水器表现出优越的光电集成解水制氢反应活性和稳定性，可直接集成太阳能助推电解水效能；4、基于该类催化剂的光电功能集成将革新水分解制氢技术，提高能量转化效率，降低工艺成本。
附图说明
图1是本发明公开的纳米异质催化剂的X射线衍射图谱。
图2是本发明公开的纳米异质催化剂的透射电子显微镜照片。
图3是本发明设计的二电极光电集成水解器装置示意图。
图4是本发明设计的二电极光电集成水解器性能测试计时电流图。
具体实施方式
本发明公开一种过渡金属硫化物基纳米异质催化剂，其具有光电耦联效应即光电双重催化活性，可用于集成太阳能助推电解水效能，直接降低分解水制氢工艺成本。
下面的实施过程包括：（1）水热法制备纳米Ni3S2-MoS2异质二维纳米片催化剂；（2）设计二电极光电集成水解器，展现纳米异质Ni3S2-MoS2催化剂的光电耦合优势。
实施例
催化剂的制备：首先，准备一块1cm×3cm的泡沫镍，用丙酮、3M盐酸、乙醇、去离子水各超声清洗10min去除氧化层，把洗好的泡沫镍放到真空干燥箱里备用。然后，称取0.2mmol Na2MoO4·2H2O和0.9mmol C2H5NS分别溶解于10mL去离子水中，将两溶液混合搅拌30分钟，取一块准备好的干净泡沫镍放入混合溶液中，并注入到一个25mL的内衬聚四氟乙烯不锈钢高压反应釜中，封装后放入加热箱，升温至200℃，并保持20h。最后，将反应釜静止，自然冷却至室温，打开反应釜取出泡沫镍，用去离子水和乙醇分别反复冲洗，并放入真空干燥箱60℃干燥，获得泡沫镍上均一生长的纳米Ni3S2-MoS2异质催化剂。
催化剂的结构表征：首先，通过X射线衍射仪（XRD）对制得的样品进行微结构分析，如图1所示，样品的XRD图谱除了显示衬底Ni的衍射峰，还包含Ni3S2和MoS2特征衍射峰，证明了异质结构的形成。然后，利用透射电子显微镜（TEM）观察样品形貌，如图2所示，样品呈现为40~70nm大小的二维超薄纳米片，具有较大的比表面积，能够择优暴露表面催化位点。
催化剂的性能表征：利用两片生长有Ni3S2-MoS2异质催化剂的镍泡沫分别作为氧化和还原反应电极，构造二电极水解系统，结构如图3所示。图4显示了在电压1.62V下的计时电流曲线，在无光照射下（暗场）制备的Ni3S2-MoS2电极系统表现出优异的分解水活性。特别地，在模拟的太阳光（100mW/cm2）辐照下, 制备的Ni3S2-MoS2电极系统表现出显著且可重复的光电流，证实了稳定的光辅助催化效应。因此，制备的Ni3S2-MoS2电极系统不仅具有优越的本征电催化分解水活性，而且能够响应光辐照，为集成可再生太阳能助推电解水效能提供了方便、可行的途径。
Claims (7)
1.一种具有光电集成解水制氢活性的纳米异质催化剂的制备方法，其特征在于，采用水热法制备，步骤如下：
将Na2MoO4和C2H5NS的混合溶液置于高压反应釜中，将泡沫镍浸入混合溶液中，升温至200℃，水热反应20小时，自然冷却至室温，清洗、真空干燥，获得所述的纳米异质催化剂。
2.如权利要求1所述的方法，其特征在于，混合溶液中，Na2MoO4与C2H5NS的摩尔比为2:9。
3.如权利要求1所述的方法，其特征在于，泡沫镍的尺寸为1cm×3cm，经丙酮、3M盐酸、乙醇、去离子水各超声清洗10min去除氧化层。
4.如权利要求1所述的方法，其特征在于，60℃下真空干燥。
5.一种具有光电集成解水制氢活性的纳米异质催化剂，其特征在于，该纳米异质催化剂为Ni3S2-MoS2异质二维纳米片催化剂，采用如权利要求1-4任一所述的方法制备。
6.如权利要求5所述的纳米异质催化剂，其特征在于，该催化剂具有光电耦联效应。
7.如权利要求5所述的纳米异质催化剂在二电极光电集成水解器中的应用，其特征在于，将两片生长有纳米异质催化剂的泡沫镍分别作为氧化和还原反应电极，构造二电极水解系统。
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| CN109046383A (zh) * | 2018-07-31 | 2018-12-21 | 山东大学 | 一种MoS2/Ni3S2电极材料及其制备方法和应用 |
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| CN114635155A (zh) * | 2022-02-23 | 2022-06-17 | 哈尔滨工业大学 | 一种自支撑核壳结构催化剂及其制备方法和应用 |
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