CN111111714A - 一种氟改性CoP纳米片全pH电解水催化剂的制备方法 - Google Patents
一种氟改性CoP纳米片全pH电解水催化剂的制备方法 Download PDFInfo
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Abstract
本发明涉及一种氟改性CoP纳米片全pH电解水催化剂及其制备方法，属于新型无机纳米功能材料制备技术领域。本发明以碳布负载的Co2(OH)2CO3纳米片阵列为前驱体在气体保护下通过低温磷化的方法制备F‑CoP/CFC复合催化剂。具体步骤如下：首先以硝酸钴和尿素为反应物通过水热法制得碳布负载的Co2(OH)2CO3为前驱体；进一步使用氟化铵对前驱体在气体保护下加热氟化制得碳布负载CoF2，再使用次磷酸钠对碳布负载的CoF2在气体保护下加热、磷化得到碳布负载的F‑CoP复合电解水催化剂。
Description
技术领域
本发明涉及一种氟改性CoP纳米片全pH电解水催化剂及其制备方法，属于新型无机纳米功能材料技术领域。
背景技术
传统化石燃料的过度利用以及环境污染的日益加剧引起了世界范围内的广泛关注，新型清洁能源的开发越来越引起人们的重视。电解水作为一种获取清洁能源的技术，因其具有简便易行的特点吸引了科学家的兴趣。但是，因为水分解的过程从化学热力学角度属于非自发反应，且其反应速率缓慢, 因而开发高效的电解水催化剂迫在眉睫。早期研究发现，Pt 基贵金属及其衍生物是目前最好的析氢催化剂，但是其高昂的价格严重制约了其大规模应用。然而，大多数报道的析氢催化剂仅适用于碱性电解槽，适应于酸性或中性介质的催化剂较少，但其对工业应用更有吸引力。因此，开发高效、稳定的全pH析氢催化剂势在必行。
对于低廉的金属磷化物作为析氢反应的催化剂所表现出的良好的性能已经吸引了越来越多的关注。但是，磷-氢键（P-Hads）很容易在金属磷化物表面形成，这会严重阻碍氢气析出反应（HER）的效率。研究表明，通过元素掺杂，实现氢吸附自由能优化，是提高其HER活性的有效方法。F元素由于具有最高的电负性，与水分子易于形成氢键。通过F元素表面改性，可以有效提高CoP催化剂表面水吸附自由能，进而提高催化活性。此外，使用粘结剂制备的催化剂增大了电阻，直接将催化剂生长在基底上面可以提高导电性，制备直接生长金属化合物纳米催化剂可以极大的提高电解水的效率。因此，本发明发展了一种成本低廉、简便易行、低能耗的碳布负载F改性CoP全pH电解水催化剂（F-CoP/CFC）的制备方法，进而制备了具有优异性能的F-CoP/CFC电解水催化剂，其在酸性、碱性、中性环境中都具有良好的催化性能。
发明内容
本发明发展了一种成本低廉、简便易行、低能耗的F改性CoP全pH电解水催化剂的制备方法。本发明提供的这种制备方法，工艺简单，成本低廉，且制备的F-CoP/CFC电解水催化剂在酸性、碱性、中性环境中都具有良好的催化性能，具有较高的实际应用价值。
本发明的目的是通过以下技术方案实现的，一种氟改性CoP纳米片全pH电解水催化剂的制备方法，包括以下步骤：
1）称取1-3 mmol的Co(NO3)2 .6H2O和5-8 mmol的尿素至聚四氟乙烯反应釜中并加水溶解；
2）在步骤1所得反应釜中加入预先裁剪好的1×4 cm的碳布并密封后放置到烘箱中加热后得到碳布负载的Co2(OH)2CO3纳米片阵列；
3）将步骤2所得的碳布负载的Co2(OH)2CO3纳米片阵列进行干燥，并称取150-250 mg的NH4F，将碳布负载的Co2(OH)2CO3和称取的NH4F一起置于石英舟中，并在N2的保护下加热得到碳布负载的CoF2纳米片阵列；
4）称取150-300 mg的NaH2PO2，将步骤3所得的碳布负载的CoF2和称取的NaH2PO2一起置于石英舟中，并在N2的保护下加热得到碳布负载的F-CoP纳米片阵列；
5）作为对比，将步骤2所得的碳布负载的Co2(OH)2CO3进行干燥，并称取150-250 mg的NaH2PO2，将碳布负载的Co2(OH)2CO3和称取的NaH2PO2一起置于石英舟中，并在N2的保护下加热得到碳布负载的CoP纳米片阵列。
本发明的有益效果：
（1）本发明提供了一种在全pH下都具有优异性能的 F-CoP/CFC电解水催化剂的制备方法，即首先通过简单的水热法制备碳布负载的Co2(OH)2CO3纳米片阵列，再继续在N2的保护下加热磷化得到碳布负载的F-CoP纳米片阵列。制备方法简单易操作，不需要特殊的设备，成本低廉且适于大规模制备，可以满足实际应用的需求；
（2）本发明制备的产物为碳布负载F-CoP纳米片阵列，产物形貌尺寸均匀，活性组份由碳布负载易于利用；
（3）本发明制备的F-CoP/CFC复合电解水催化剂在全pH环境下具有优异的电解水产氢性能及良好的稳定性；
（4）本发明的制备仅需实验室常用的普通设备，不需专用设备，工艺过程简便易行。
附图说明
图1 (a)为本发明步骤2所制得的碳布负载的Co2(OH)2CO3纳米片阵列用扫描电子显微镜观察后拍摄的扫描电镜（SEM）照片；
(b)为步骤3制得的碳布负载的CoF2纳米片阵列用扫描电子显微镜观察后拍摄的扫描电镜（SEM）照片；
(c)为步骤4最终制备的碳布负载的F-CoP纳米片阵列用扫描电子显微镜观察后拍摄的扫描电镜（SEM）照片；
(d)为步骤5制备的碳布负载的CoP纳米片阵列用扫描电子显微镜观察后拍摄的扫描电镜（SEM）照片。
图2 (a)为本发明步骤2所制得的碳布负载的Co2(OH)2CO3纳米片阵列的X射线衍射（XRD）图；
(b)为步骤3制得的碳布负载的CoF2纳米片阵列的X射线衍射（XRD）图；
(c)为步骤4最终制备的碳布负载的F-CoP纳米片阵列的X射线衍射（XRD）图；
(d)为步骤5制备的碳布负载的CoP纳米片阵列的X射线衍射（XRD）图。
图3为采用能量色散光谱仪对本发明最终制得的碳布负载的F-CoP纳米片阵列进行元素分析从而得到的能谱图。
图4为制备的碳布负载的F-CoP纳米片阵列作为电解水制氢反应的工作电极在(a)酸性、(b)碱性、(c)中性环境下进行电解水制氢实验，从而得到的极化曲线图。
具体实施方式
下面通过具体实施实例并结合附图对本发明的内容作进一步详细说明，但这些实施例并不限制本发明的保护范围。
实施例1
首先将物质的量为0.001摩尔的硝酸钴，0.005摩尔的尿素水溶液混合，然后转移至聚四氟乙烯反应釜中并加入预先裁剪好的1×4 cm的条状碳布。将上述反应物在120摄氏度烘箱中反应6小时，自然降至室温后即得到碳布负载的Co2(OH)2CO3纳米片。称取250 mg的NH4F，将碳布负载的Co2(OH)2CO3和称取的NH4F一起置于石英舟中，并在N2的保护下加热至350摄氏度1小时得到碳布负载的CoF2纳米片，再称取150mg的NaH2PO2，将所得的碳布负载的CoF2和称取的NaH2PO2一起置于石英舟中，并在N2的保护下加热至320摄氏度1小时得到碳布负载的F-CoP纳米片，自然降至室温后即得到碳布负载的F-CoP复合电解水催化剂。
实施例2
首先将浓度为0.001摩尔每升的硝酸钴，0.005摩尔每升的尿素水溶液混合，然后转移至聚四氟乙烯反应釜中并加入预先裁剪好的1×4 cm的条状碳布。将上述反应物在120摄氏度烘箱中反应6小时，自然降至室温后即得到碳布负载的Co2(OH)2CO3纳米片。称取250mg的NaH2PO2，将所得的碳布负载的Co2(OH)2CO3纳米片和称取的NaH2PO2一起置于石英舟中，并在N2的保护下加热至350摄氏度1.5小时得到碳布负载的CoP，自然降至室温后即得到碳布负载的CoP电解水催化剂。
实施例3
使用辰华760D电化学工作站对F-CoP/CFC复合电解水催化剂电解水产氢活性及稳定性进行测试。以铂丝为对电极，银/氯化银为参比电极，碳布负载的F-CoP为工作电极，1.0摩尔每升KOH水溶液、0.5摩尔每升H2SO4水溶液、1摩尔每升PBS水溶液为电解质溶液。在-0.8至-1.5V电压范围内，以5毫安每秒的扫速进行线性伏安扫描，即可得到其催化电解水产氢的极化曲线。
Claims (3)
1.一种氟改性CoP纳米片全pH电解水催化剂的制备方法，其特征在于制备方法步骤如下：
1）采用水热法，以硝酸钴和尿素为反应物制得碳布负载的Co2(OH)2CO3纳米片阵列为前驱体；
2）将步骤1所得的碳布负载的Co2(OH)2CO3进行干燥，并称取一定量的NH4F，将碳布负载的Co2(OH)2CO3和称取的NH4F一起置于石英舟中，并在保护气体的保护下加热得到碳布负载的CoF2纳米片阵列；
3）将步骤2所得的碳布负载的CoF2纳米片阵列进行干燥，并称取一定量的NaH2PO2，将碳布负载的CoF2纳米片阵列和称取的NaH2PO2一起置于石英舟中，并在保护气体的保护下加热得到碳布负载的F-CoP纳米片阵列。
2.根据权利要求1所述的碳布负载的F-CoP纳米片阵列复合电解水催化剂的制备方法，其特征在于，所述复合催化剂的前驱体的制备是通过水热反应进行的。
3.根据权利要求1所述的碳布负载的F-CoP纳米片阵列复合电解水催化剂的制备方法，其特征在于，所述产物皆是由前驱体在气体保护的无溶液的情况下合成的。
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