CN110394184B - 一种具有高HER和OER催化活性的CoP/Co2P复合催化剂的制备方法 - Google Patents
一种具有高HER和OER催化活性的CoP/Co2P复合催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有高HER和OER催化活性的CoP/Co2P复合催化剂的制备方法。将市售三氧化二钴和自制纳米黑磷按摩尔比为1:1～1:3加入到高能球磨罐中，原料与球的质量比为1:20‑25，密封，在10℃～50℃和球磨转速1200r/min的条件下球磨1～5h，制得CoP/Co2P复合催化剂。本方法仅需要一步高能球磨法便可快速制得CoP/Co2P复合催化剂，制备过程中无任何污染物排放且成本低廉可大规模生产，其电催化HER过电位低至69mV,电催化OER过电位低至266mV。
Description
本发明涉及电催化领域，具体说为一种CoP/Co2P复合催化剂的制备方法。
背景技术
面对当今日益增涨的全球能源消耗，化石燃料等传统能源的枯竭及它们对环境的负面影响，激发了人们对可再生能源储存和生产技术探索的紧迫感。随着燃料电池的不断发展，氢能成为一个极具潜力的选择，因为它具有已知的最高质量量能量密度(32.67kWhkg-1)，可以通过电化学水分裂以环保的方式生产，实现这一过程的关键是选择高效的催化剂。Pt/C和RuO2是目前公认的高效析氢和析氧催化剂，但是。由于贵金属Pt、Ru资源稀缺和成本高严重限制了它们在商业中的应用。
因此，在过去的几十年里，开发地球储量丰富、成本低、性能好的催化剂引起了科学界的广泛关注。研究发现，除碳基催化剂外，许多过渡金属、过渡金属化合物及其复合合物也具有优异的电催化性能。过渡金属磷化物(TMPs)由于其良好的热稳定性、导电性和高的催化活性，被广泛应用于加氢脱硫、脱氮、脱氧、脱氯等的研究。然而，近年来有研究证实TMPs对HER和OER也具有良好催化作用，因此受到电催化水裂解领域研究工作者的高度重视。目前，在碱性介质中，TMPs被列为性能最佳、最耐用的催化剂之一，尤其是在水和氯碱电解等能源密集型工艺中。许多新开发的催化材料在碱性介质中表现不佳或完全失效，迫使该行业直到今天都依赖于贵金属催化剂。因此，对TMP基催化材料的节能、环保合成方法提出了更高的要求。
目前，过渡金属磷化物的制备方法主要有：磷酸盐在氢气气氛中还原，金属有机化合物化学气相沉积，磷化氢或五氯化磷与过渡金属或金属盐直接还原，溶剂热，溶胶凝胶等方法。这些方法普遍存在原料成本高或工艺复杂、生产条件苛刻等缺陷，不利于金属磷化物的规模生产及广泛应用。
发明内容
本发明的目的在于克服现有过渡金属磷化物制备方法存在的不足及所制备的过渡金属磷化物电催化剂催化活性不够理想的问题，开发出一种制备工艺简单、对环境无污染、成本低廉、且可实现大规模生产的制备具有高HER和OER催化活性的CoP/Co2P 复合催化剂的方法。
本发明所采用的技术方案是：
将市售三氧化二钴和自制纳米黑磷按摩尔比为1:1～1:4加入到高能球磨罐中，按原料与磨料球的质量比为1:20加入磨料球，密封，在10℃～50℃和球磨转速为 1200r/min的条件下球磨1～5h，制得CoP/Co2P复合催化剂。
实施本发明的有益效果在于：
(1)相对于目前普遍采用的化学法，本方法仅需要一步高能球磨法便可制得所需产物，产物纯净无需后续处理，且其制备过程中无任何污染物排放。
(2)相比于其他的磷源，如如白磷，红磷等，本发明使用自制的黑磷成本低且可大量生产，具有更高的电化学稳定性和燃点，显著提高制备过程的安全性。
(3)本发明所制备的CoP/Co2P复合材料具有优异电催化HER、OER活性，是较为理想的双功能电催化剂。
附图说明
图1为实施例1制得的CoP/Co2P复合催化剂的XRD图；
图2为实施例1制得的CoP/Co2P复合催化剂的扫描电镜图；
图3为实施例1制得的CoP/Co2P复合催化剂的透射电镜图；
图4为实施例1制得的CoP/Co2P复合催化剂析氢反应的极化曲线图；
图5为实施例1制得的CoP/Co2P复合催化剂的析氢反应的稳定性图；
图6为实施例1和对比例1制得的CoP/Co2P复合催化剂析氧反应的极化曲线图；
图7为实施例1制得的CoP/Co2P复合催化剂的析氧反应的稳定性图；
图8为实施例1和对比例1制得的CoP/Co2P复合催化剂及其对比样品的全水分解图。
具体实施方式
以下，结合附图及具体实施例对本发明作进详细说明，但附图及具体实施例仅作为示例，不以任何方式限制本发明的范围。
在以下实施例中，三氧化二钴购于试剂商店，纳米黒磷以红磷为原料采用高能球磨法自制，高能球磨机选用的是德国莱驰高能球磨仪EMax
实施例1
分别称取2.5g的三氧化二钴粉末和1.0g自制黑磷于高能球磨罐中，加入质量为72g的不锈钢球，密封。设定低温25℃，高温为45℃，转速1200r/min，球磨2h，制得3.23gCoP/Co2P复合电催化剂。
取10mg所得CoP/Co2P复合电催化剂于样品管中，依次加入450μL异丙醇和 50μL的萘酚溶液，超声1h制备成悬浊液。将悬浊液滴涂到旋转圆盘电极(铂碳)上，以Ag/AgCl为参比电极，铂丝为对电极，测定其电催化HER。将悬浊液滴涂到石墨片上，一片为阴极，另一片为阳极，测定其催化全水分解性能。
对比例1
分别取10mg所得Pt/C和RuO2于样品管中，依次加入450μL异丙醇和50μL的萘酚溶液，超声1h制备成悬浊液。将两种悬浊液分别滴涂到两个石墨片上，其中滴涂 Pt/C的石墨片为阴极，另一片滴涂RuO2石墨片的为阳极，测定其催化全水分解性能。
图4为实施例1和对比例1制得的CoP/Co2P复合催化剂的析氢反应的极化曲线图；图5为实施例1制得的CoP/Co2P复合催化剂的析氢反应的稳定性图；图6为实施例1 制得的CoP/Co2P复合催化剂的析氧反应的极化曲线图；图7为实施例1制得的CoP/Co 2P复合催化剂的析氧反应的稳定性图；图8为实施例1和对比例1制得的CoP/Co2P复合催化剂及其对比样品Pt/C//RuO2的全水分解图。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (2)
1.一种具有高HER和OER催化活性的CoP/Co2P复合催化剂的制备方法，其特征在于：以市售三氧化二钴和纳米黑磷为原料，三氧化二钴与黑磷的摩尔比为1:1～1:3，采用高能球磨法，原料与球的质量比为1:20-25，球磨温度为25℃～50℃，球磨转速为1200r/min，球磨时间为1～3h。
2.根据权利要求1所述的一种具有高HER和OER催化活性的CoP/Co2P复合催化剂的制备方法，其特征在于：所制备出的CoP/Co2P复合催化剂电催化HER过电位低至69mV,电催化OER过电位低至266mV。
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| EP3170921A1 (en) * | 2015-11-20 | 2017-05-24 | INL - International Iberian Nanotechnology Laboratory | Electrode material |
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