CN110983374A - 一种用于电解酸性水的涂层电极及其制备方法 - Google Patents
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Abstract
本发明涉及的用于电解酸性水的涂层电极包括Ti基底、以及形成在Ti基底表面的(Mo,Ni)C/Si涂层，该涂层电极直接将(Mo,Ni)C/Si涂层制备在Ti基底电极上，相较于传统的采用粘合剂制备的涂覆型电极，该涂层电极结合力更好，具有更佳的稳定性，延长了电极的使用寿命；(Mo,Ni)C/Si涂层中金属碳化物与Si颗粒相结合使涂层具有良好的催化活性和导电性，提高了电解酸性水的工作效率。
Description
技术领域
本发明涉及一种用于电解酸性水的涂层电极及其制备方法。
背景技术
氢气(H2)因具有高能量密度和环境友好性，被视为有前途的清洁能源载体，可替代化石燃料。当前，通过电解水方法在阴极进行析氢反应(HER)，大规模生产高纯度氢气被认为是一种经济有效的方法。到目前为止，对于析氢反应具有高催化效率的催化剂仍限于贵金属材料(例如：铂)，但是高成本和低储量严重地限制了贵金属材料的工业应用。3d过渡金属由于具有特殊的电子结构，并且储量丰富，成本较低等成为非贵金属催化材料的研究热点。其中，过渡金属碳化物具有类似于铂等贵金属的良好催化活性，同时，过渡金属碳化物具有良好的稳定性和耐蚀性等机械性能。但是目前难以制备具有高比表面积的过渡金属碳化物。近期有研究发现，Si与析氢催化材料复合，在酸性水环境中可产生协同效应，促进析氢反应的快速进行。此外，大部分用于析氢反应的电极都是采用粘合剂将粉末状的催化材料涂覆在基底电极上，粘结剂会导致电极电阻增加、活性位点减少并掩蔽反应离子的扩散通道，极大地降低了阴极的析氢效率；并且粘合剂自身的附着力差，在电解过程中易脱落，从而降低电极的工作稳定。
发明内容
本发明的目的在于提供一种用于电解酸性水且具有良好催化活性、良好导电性以及稳定性高的涂层电极。
为达到上述目的，本发明提供如下技术方案：一种用于电解酸性水的涂层电极包括Ti基底、以及形成在所述Ti基底表面的(Mo,Ni)C/Si涂层。
进一步地，所述(Mo,Ni)C/Si涂层的厚度为2um-5um。
进一步地，所述(Mo,Ni)C/Si涂层包括(Mo,Ni)C层以及填充在(Mo,Ni)C层中的Si结构单元。
进一步地，所述(Mo,Ni)C/Si涂层中Si的原子百分比含量为10％-30％。
进一步地，所述(Mo,Ni)C层的厚度为2um-5um。
本发明还提供了一种用以制备所述用于电解酸性水的涂层电极的制备方法，所述制备方法如下：
S1、提供Ti基底，将所述Ti基底表面粗糙化；
S2、在所述Ti基底表面沉积(Mo,Ni)C层和Si结构单元；
进一步地，所述Ti基底表面使用硫酸使其粗糙化。
进一步地，所述(Mo,Ni)C层和所述Si结构单元由磁控溅射技术共沉积制备得到。
进一步地，在所述Ti基底表面沉积(Mo,Ni)C层之前，所述涂层电极制备方法还包括由离子轰击清洁所述Ti基底并活化所述Ti基底上的原子。
本发明的有益效果在于：本发明所提供的用于电解酸性水的涂层电极直接将(Mo,Ni)C/Si涂层形成在Ti基底电极上，相较于传统的采用粘合剂制备的涂覆型电极，该涂层电极结合力更好，具有更佳的稳定性，延长了电极的使用寿命；(Mo,Ni)C/Si涂层中金属碳化物与Si颗粒相结合使涂层具有良好的催化活性和导电性，提高了电解酸性水的工作效率。
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。
附图说明
图1为本发明一实施例中用于电解酸性水的涂层电极的结构示意图；
图2为图1中(Mo,Ni)C/Si涂层的部分结构示意图。
具体实施方式
下面将结合附图对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
在本发明的描述中，需要说明的是，术语“中心”、“上”、“下”、“左”、“右”、“竖直”、“水平”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的机构或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。此外，术语“第一”、“第二”、“第三”仅用于描述目的，而不能理解为指示或暗示相对重要性。
在本发明的描述中，需要说明的是，除非另有明确的规定和限定，术语“安装”、“相连”、“连接”应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或一体地连接；可以是机械连接，也可以是电连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通。对于本领域的普通技术人员而言，可以具体情况理解上述术语在本发明中的具体含义。
此外，下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
请参见图1和图2，本发明一实施例所示的用于电解酸性水的涂层电极，包括Ti基底1、以及形成在Ti基底1表面的(Mo,Ni)C/Si涂层2。(Mo,Ni)C/Si涂层2的厚度为2um-5um。(Mo,Ni)C/Si涂层2包括(Mo,Ni)C层21以及填充在(Mo,Ni)C层21中的Si结构单元22。(Mo,Ni)C/Si涂层2中Si的原子百分比含量为10％-30％，(Mo,Ni)C层21的厚度为2um-5um。
Mo和Ni都是过渡金属，过渡金属碳化物(Mo,Ni)C层21具有类似于铂等贵金属的良好催化活性，可应用在催化析氢反应，同时，过渡金属碳化物(Mo,Ni)C层21具有良好的稳定性和耐蚀性等。Si与过渡金属碳化物(Mo,Ni)C层21复合，在酸性水环境中可产生协同效应，促进析氢反应的快速进行，由此(Mo,Ni)C/Si涂层2可做阴极来催化析氢反应。
本发明还提供了一种用以制备上述用于电解酸性水的涂层电极的制备方法，制备方法如下：
步骤1、提供Ti基底1，将Ti基底1表面粗糙化。具体的，将Ti基底1放入硫酸溶液中加热30min，对Ti基底1进行表面刻蚀。
步骤2、由离子轰击清洁Ti基底1并活化Ti基底1上的原子。具体的，将表面粗糙化的Ti基底1进行超声波清洗以及烘干，然后装进入磁控溅射仪的真空腔体内；抽真空、加热，待真空度到达1.0×10-3Pa以上，通入纯度为99.999％的氩气(Ar)，压力控制在1Pa-2Pa，开启电弧离子源对Ti基底1进行离子轰击，电流控制在40A-80A，偏压电压控制在100V-1000V，占空比控制在30％-50％，离子轰击时间为20min-40min。
步骤3、在Ti基底1表面沉积(Mo,Ni)C层21和Si结构单元22。具体的，(Mo,Ni)C层21和Si结构单元22由磁控溅射技术共沉积制备，抽真空到1.0x10-3Pa以上，采用C2H2作为反应气体，气体只从Mo靶和Ni靶表面进入，进入压力0.01MPa，真空室内分压力控制在0.1Pa-0.2Pa；与此同时，采用Ar作为辅助溅射气体，气体只从Si靶表面进入，进入压力0.1MPa，真空室分压力控制在0.5Pa-0.6Pa。衬底偏压控制在60V-100V。其中，通过改变Si靶的溅射功率来控制涂层中Si原子含量。Mo靶和Ni靶溅射功率分别设定在10KW，Si靶的溅射功率设定在0.5KW-3KW。镀膜时长控制在1h-3h，得到的(Mo,Ni)C/Si涂层2总厚度为2um-5um，(Mo,Ni)C层21的厚度为2um-5um，Si原子百分比含量为10％-30％。
本实施例在Ti基底1表面直接由磁控溅射技术共沉积制备得到(Mo,Ni)C/Si涂层2，相对采用粘合剂将涂层黏合到基底上，该方法得到的(Mo,Ni)C/Si涂层2在Ti基底1表面结合力更好，更牢固，形成的涂层电极更加稳定。
将制备所得的涂层电极作为阴极置于在0.5mol L-1硫酸溶液中，表现出良好的电解水催化活性能，在10mA cm-2的电流密度下过电位为60mV-80mV，Tafel斜率为50mV dec-1-60mV dec-1。
综上，本发明所提供的用于电解酸性水的涂层电极直接将(Mo,Ni)C/Si涂层制备在Ti基底电极上，相较于传统的采用粘合剂制备的涂覆型电极，该涂层电极结合力更好，具有更佳的稳定性，延长了电极的使用寿命；(Mo,Ni)C/Si涂层中金属碳化物与Si颗粒相结合使涂层具有良好的催化活性和导电性，提高了电解酸性水的工作效率。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (9)
1.一种用于电解酸性水的涂层电极，其特征在于，所述用于电解酸性水的涂层电极包括Ti基底、以及形成在所述Ti基底表面的(Mo,Ni)C/Si涂层。
2.如权利要求1所述的用于电解酸性水的涂层电极，其特征在于，所述(Mo,Ni)C/Si涂层的厚度为2um-5um。
3.如权利要求1所述的用于电解酸性水的涂层电极，其特征在于，所述(Mo,Ni)C/Si涂层包括(Mo,Ni)C层以及填充在(Mo,Ni)C层中的Si结构单元。
4.如权利要求3所述的用于电解酸性水的涂层电极，其特征在于，所述(Mo,Ni)C/Si涂层中Si的原子百分比含量为10％-30％。
5.如权利要求3所述的用于电解酸性水的涂层电极，其特征在于，所述(Mo,Ni)C层的厚度为2um-5um。
6.一种用以制备权利要求1至5项中任一项所述的用于电解酸性水的涂层电极的制备方法，其特征在于，所述制备方法如下：
S1、提供Ti基底，将所述Ti基底表面粗糙化；
S2、在所述Ti基底表面沉积(Mo,Ni)C层和Si结构单元。
7.如权利要求6所述的用于电解酸性水的涂层电极制备方法，其特征在于，所述Ti基底表面使用硫酸使其粗糙化。
8.如权利要求6所述的用于电解酸性水的涂层电极制备方法，其特征在于，所述(Mo,Ni)C层和所述Si结构单元由磁控溅射技术共沉积制备得到。
9.如权利要求6所述的用于电解酸性水的涂层电极制备方法，其特征在于，在所述Ti基底表面沉积(Mo,Ni)C层之前，所述涂层电极制备方法还包括由离子轰击清洁所述Ti基底并活化所述Ti基底上的原子。
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| CN109972159A (zh) * | 2019-04-08 | 2019-07-05 | 镁格氢动能源技术(苏州)有限公司 | 基于固体氢技术的水电储能系统 |
| CN110203904A (zh) * | 2019-06-06 | 2019-09-06 | 东北大学 | 用于制备纳米结构碳材料的前体材料及方法 |
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| CN109972159A (zh) * | 2019-04-08 | 2019-07-05 | 镁格氢动能源技术(苏州)有限公司 | 基于固体氢技术的水电储能系统 |
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