CN114150343B - 一种纳米茸状NiMoCu催化剂及其制备方法 - Google Patents
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Abstract
电解水制氢技术能在不消耗化石能源的基础上制取绿色氢气，采用高性能催化剂作为电极材料能够显著降低能量损耗、提高反应效率。本发明针对现有阴极催化剂的表面微观形貌匮乏、活性位点缺失的现状，提出了一种纳米茸状NiMoCu催化剂及制备方法，属于材料制备领域。本发明在含有Ni、Mo、Cu元素的电解液中引入具有形貌调节作用的添加剂，制得的纳米茸状NiMoCu催化剂表面分布有纳米尺度的不规则颗粒凸起，具有充足的反应表面积与催化位点，在1MKOH溶液中工作的塔菲尔斜率为70mV·dec‑1，电流密度为10mA·cm‑2时的过电位为45mV，电流密度为100mA·cm‑2时的过电位为147mV。
Description
技术领域
本发明属于新能源及电化学催化领域，具体涉及一种纳米茸状NiMoCu催化剂及其制备方法。
背景技术
氢气由其来源广泛、燃烧物无污染等特点被视为最有前景的能量载体。水电解制氢能克服可再生能源(如太阳能、风能)的间接性和扩散性，从而促进其持续使用和分配。而电解水系统中的两个半反应(即阳极的析氧反应，OER，和阴极的析氢反应，HER)缓慢的动力学严重阻碍了其广泛应用，需要采用高效的催化剂作为电极材料来促进其动力学性能。对于析氢反应而言，当前最好的非贵金属催化剂是基于NiMo体系的复合物。其中，掺杂了过渡金属Cu的NiMoCu催化剂具有优异的电导性和催化活性因而广受关注。电化学沉积技术是一种制备NiMoCu催化剂的常用方法，然而电沉积产物的微观形貌往往趋于平滑，反应活性面积有限，这对于电化学催化剂来说是一个劣势，因此可以通过改变该催化剂表面形貌来提升催化性能。
发明内容
本发明为克服电沉积技术所带来的不足，在含有Ni、Mo、Cu元素的电解液中引入添加剂对沉积物的表面微观形貌进行优化，制备了纳米茸状NiMoCu催化剂作为电解水反应的阴极材料。本发明所涉及的添加剂为乙二胺二盐酸(EDA)和对苯二酚(HQ)，它们分别代表了两种调节机理：EDA与电解液里的金属离子形成络合物，进而在基底附近产生离子浓度差，因离子局部集中而产生立体凸起。HQ上存在的两个对称羟基，一个吸附金属离子，另一个则吸附基底，起到中间桥梁作用，在HQ分子的位阻作用影响下离子的沉积更具有均一性和方向性，使沉积物表面更紧密。添加剂的加入使得沉积物的表面形成了纳米尺度的茸状颗粒凸起，改善了催化剂的反应面积及活性位点，有利于促进水分解反应的进行。
附图说明
图1为纳米茸状NiMoCu催化剂的扫描电镜图。
图2为纳米茸状NiMoCu催化剂的XRD图。
图3为纳米茸状NiMoCu催化剂在1M KOH中的HER线性扫描伏安曲线图。
图4为纳米茸状NiMoCu催化剂在1M KOH中的塔菲尔图。
图5为纳米茸状NiMoCu催化剂在1M KOH中的EIS图。
图6为纳米茸状NiMoCu催化剂经1000圈循环伏安测试前后的线性扫描伏安曲线图。
图7为纳米茸状NiMoCu催化剂在100mV过电位下工作12h的i-t图。
具体实施方式
裁剪面积为1×1cm2的钛片作为催化剂载体，先后在3M盐酸、无水乙醇和纯水中超声清洗10min，烘箱干燥后与电化学工作站连接，用作工作电极。将面积为2×3cm2的石墨片和Ag/AgCl电极与电化学工作站连接，分别用作对电极与参比电极。将1.314g六水硫酸镍、0.123g五水硫酸铜、0.121g钼酸钠、0.309g硼酸、2.941g二水合柠檬酸钠、0.067g乙二胺二盐酸和0.028g对苯二酚溶于50mL超纯水中作为电解液。在-25mA/cm2的电流密度下对钛片进行恒电流沉积，沉积时间为1800s，制得纳米茸状NiMoCu催化剂，最后在超纯水中冲洗材料若干次并在烘箱中干燥。
由图1可知，材料表面分布了大量纳米尺度的茸状颗粒。由图2的XRD花样与标准卡片对比可知，所得材料主要晶相为MoNi4、Cu、NiCu(JCPDF65-5480、JCPDF 65-9026、JCPDF65-9048)。
为测试催化剂的HER活性，采用纳米茸状NiMoCu催化剂为工作电极，金片为辅助电极，Ag/AgCl电极为参比电极，在1MKOH中进行LSV测试。测试结果如图3、图4。材料的塔菲尔斜率为70mV·dec-1，电流密度为10mA·cm-2时的过电位为45mV，电流密度为100mA·cm-2时的过电位为147mV。
由图5的EIS谱图可知，纳米茸状NiMoCu催化剂具有较小的电荷转移电阻。图6、图7为催化剂的稳定性测试。经过1000圈循环伏安测试后，催化剂的电流衰减很小，而经历12h的稳定性测试后，材料仍保持较大的工作电流，说明该催化剂具有良好稳定性。
Claims (2)
1.一种纳米茸状NiMoCu催化剂的制备方法，其特征在于，包括以下具体步骤：
裁剪面积为1×1cm2的钛片作为催化剂载体，先后在3M盐酸、无水乙醇和纯水中超声清洗10min，烘箱干燥后与电化学工作站连接，用作工作电极，将面积为2×3cm2的石墨片和Ag/AgCl电极与电化学工作站连接，分别用作对电极与参比电极，将1.314g六水硫酸镍、0.123g五水硫酸铜、0.121g钼酸钠、0.309g硼酸、2.941g二水合柠檬酸钠、0.067g乙二胺二盐酸和0.028g对苯二酚溶于50mL超纯水中作为电解液，在-25mA/cm2的电流密度下对钛片进行恒电流沉积，沉积时间为1800s，制得纳米茸状NiMoCu催化剂，最后在超纯水中冲洗材料若干次并在烘箱中干燥。
2.根据权利要求1所述的方法制备得到的纳米茸状NiMoCu催化剂。
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