CN114590844A - 一种介孔Co3O4/CoO/CoP及其制备方法 - Google Patents
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- 238000002360 preparation method Methods 0.000 title abstract description 5
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Abstract
本发明公开了一种介孔Co3O4/CoO/CoP化合物，具有纳米管状形貌；本发明还公开了一种制备所述介孔Co3O4/CoO/CoP化合物的方法。本发明还公开了一种制备所述介孔Co3O4/CoO/CoP的方法，包括前驱体制备、水热反应、旋转蒸发处理、磷化处理等步骤。
Description
技术领域
本发明涉及电催化剂，具体涉及一种介孔Co3O4/CoO/CoP及其制备方法。
背景技术
随着自然资源的枯竭和环境污染，绿色可持续能源受到大家越来越多的关注。其中，氢能由于燃值比较高，燃烧产物是水，可重复利用，是一种重要的绿色可持续能源。而电解水产生氢是获得氢能的重要手段之一。为了更高效的产生氢能，往往需要电催化剂的辅助。目前，工业上电解水制氢最常用的电催化剂是贵金属铂。贵金属铂价格昂贵，且在地球上储量少，因此，开发可替代贵金属铂的电催化剂十分重要。
钴基电催化剂是一类重要的电催化剂，然而，钴基电催化剂还存在形貌结构普通，活性位点少，过电位高等问题，其催化活性可进一步提高，进而将其应用于工业领域。
发明内容
本发明的目的在于公开一种具有独特纳米管状形貌的介孔Co3O4/CoO/CoP，提高活性位点的负载量，调控Co3O4的能带结构，提高电催化析氢反应的催化活性。
本发明提出一种简单的制备所述的介孔Co3O4/CoO/CoP化合物的方法。
本发明提出的制备所述的介孔Co3O4/CoO/CoP化合物的方法，包括以下步骤：截取一块尺寸为3*3cm2的碳布，将切割好的碳布浸入浓盐酸中超声清洗十分钟，再浸入丙酮中超声五分钟，再浸入乙醇中超声清洗五分钟，将清洗之后的碳布放入真空干燥箱中干燥30分钟，温度为40摄氏度；称取或者量取2 g的P123，60 ml浓度为0.5 mol/L的盐酸放入烧杯中，用可控温的水浴锅将温度控制在40摄氏度下搅拌直至溶解，溶液呈现出均匀透明的颜色；向烧杯中加入6 ml的正硅酸乙酯,将其搅拌均匀；将上述的溶液倒入规格为100 mL的反应釜里将反应釜放入鼓风烘箱中，加热到100摄氏度，保温48小时；待温度降至室温后取出，用去离子水和乙醇离心清洗三遍；将所得到的白色固体粉末放入真空干烘箱中，温度设置65℃，保持12小时；将白色固体粉末放入马弗炉内进行650 ℃高温焙烧后，得到前驱体；称取0.3 g的六水硝酸钴，加入到2 ml的无水乙醇，加入0.05 g的前驱体，加入碳布，将其转移到旋转蒸发仪中，旋转蒸发后，将碳布放入马弗炉内进行450 ℃高温焙烧6小时；选用2mol/L的NaOH作为除模板剂，将碳布用去离子水和酒精超声清洗三遍；将碳布放于管式炉内，在氢氩混合气体的作用下，升温到250℃，保温半小时，冷却后取出；称取0.6 g的次亚磷酸钠，放于管式炉靠近进气口的位置，将碳布放进管式炉内，在氩气的作用下，设置1度每分钟的升温速度，加热到350摄氏度，保温2小时。
本发明的另一个目的在于提出的一种介孔Co3O4/CoO/CoP化合物，其特征在于，所述介孔Co3O4/CoO/CoP化合物具有纳米管状形貌，所述的纳米管的长度为100至700纳米，所述的纳米管外径为80至150纳米。
本发明提出的一种介孔Co3O4/CoO/CoP化合物，具有独特的纳米管状形貌，用于碱性条件下电催化析氢反应时，在交换电流密度为10 mA/cm2时，过电位为128 mV，明显优于未复合、形貌普通的Co3O4。
附图说明
为了更清楚地说明本发明实施的技术方案，下面将对实施例中所需要使用的附图作简单地介绍。
图1为按实施例的方法制备的样品的X射线粉末衍射谱。
图2为按实施例的方法制备的样品的扫描电子显微镜图。
图3为按实施例的方法制备的样品的电催化析氢过电位图。
具体实施方式
以下结合具体实施例对本发明的实现进行详细的描述。
本实施例的具体步骤如下：截取一块尺寸为3*3cm2的碳布，将切割好的碳布浸入浓盐酸中超声清洗十分钟，再浸入丙酮中超声五分钟，再浸入乙醇中超声清洗五分钟，将清洗之后的碳布放入真空干燥箱中干燥30分钟，温度为40摄氏度；称取或者量取2 g的P123，60 ml浓度为0.5 mol/L的盐酸放入烧杯中，用可控温的水浴锅将温度控制在40摄氏度下搅拌直至溶解，溶液呈现出均匀透明的颜色；向烧杯中加入6 ml的正硅酸乙酯,将其搅拌均匀；将上述的溶液倒入规格为100 mL的反应釜里将反应釜放入鼓风烘箱中，加热到100摄氏度，保温48小时；待温度降至室温后取出，用去离子水和乙醇离心清洗三遍；将所得到的白色固体粉末放入真空干烘箱中，温度设置65℃，保持12小时；将白色固体粉末放入马弗炉内进行650 ℃高温焙烧后，得到前驱体；称取0.3 g的六水硝酸钴，加入到2 ml的无水乙醇，加入0.05 g的前驱体，加入碳布，将其转移到旋转蒸发仪中，旋转蒸发后，将碳布放入马弗炉内进行450 ℃高温焙烧6小时；选用2 mol/L的NaOH作为除模板剂，将碳布用去离子水和酒精超声清洗三遍；将碳布放于管式炉内，在氢氩混合气体的作用下，升温到250℃，保温半小时，冷却后取出；称取0.6 g的次亚磷酸钠，放于管式炉靠近进气口的位置，将碳布放进管式炉内，在氩气的作用下，设置1度每分钟的升温速度，加热到350摄氏度，保温2小时。
下面结合附图，通过具体实施例，进一步阐述本发明。
图1为按实施例的方法制备的样品的X射线粉末衍射谱，从图谱中可以看到Co3O4，CoO和CoP各自对应的特征峰，表明按照实施例制备的样品的确为Co3O4/CoO/CoP化合物。对样品进行能谱测试表明，样品的原子比为C：Co：O：P =0.15：0.24：0.55：0.06，表明按照实施例制备的样品的确实现了Co3O4/CoO/CoP化合物的复合。图2为按实施例的方法制备的样品的扫描电子显微镜图，可以看到明显的管状形貌，所述的纳米管的长度为100至700纳米，所述的纳米管外径为80至150纳米。图3为按实施例的方法制备的样品的碱性条件下电催化析氢过电位图，在交换电流密度为10 mA/cm2时，过电位为128mV。
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 (2)
1.一种介孔Co3O4/CoO/CoP化合物的制备方法，其特征在于，包括以下步骤：截取一块尺寸为3*3cm2的碳布，将切割好的碳布浸入浓盐酸中超声清洗十分钟，再浸入丙酮中超声五分钟，再浸入乙醇中超声清洗五分钟，将清洗之后的碳布放入真空干燥箱中干燥30分钟，温度为40摄氏度；称取或者量取2 g的P123，60 ml浓度为0.5 mol/L的盐酸放入烧杯中，用可控温的水浴锅将温度控制在40摄氏度下搅拌直至溶解，溶液呈现出均匀透明的颜色；向烧杯中加入6 ml的正硅酸乙酯,将其搅拌均匀；将上述的溶液倒入规格为100 mL的反应釜里将反应釜放入鼓风烘箱中，加热到100摄氏度，保温48小时；待温度降至室温后取出，用去离子水和乙醇离心清洗三遍；将所得到的白色固体粉末放入真空干烘箱中，温度设置65℃，保持12小时；将白色固体粉末放入马弗炉内进行650 ℃高温焙烧后，得到前驱体；称取0.3 g的六水硝酸钴，加入到2 ml的无水乙醇，加入0.05 g的前驱体，加入碳布，将其转移到旋转蒸发仪中，旋转蒸发后，将碳布放入马弗炉内进行450 ℃高温焙烧6小时；选用2 mol/L的NaOH作为除模板剂，将碳布用去离子水和酒精超声清洗三遍；将碳布放于管式炉内，在氢氩混合气体的作用下，升温到250℃，保温半小时，冷却后取出；称取0.6 g的次亚磷酸钠，放于管式炉靠近进气口的位置，将碳布放进管式炉内，在氩气的作用下，设置1度每分钟的升温速度，加热到350摄氏度，保温2小时。
2.一种如权利要求1所述的方法制备的介孔Co3O4/CoO/CoP化合物，其特征在于，所述介孔Co3O4/CoO/CoP化合物具有纳米管状形貌；所述的纳米管的长度为100至700纳米；所述的纳米管外径为80至150纳米。
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