CN111185185A - 一种V-LaCoO3钙钛矿型电解水催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种V‑LaCoO3钙钛矿型电解水析氧催化剂及其制备方法与应用，其形貌为纳米棒。其制备方法包括：将硝酸镧、硝酸钴、氯化钒、氢氧化钾混合在一起制得混合反应液；将混合反应液通过水热法于180℃下反应10 h，制得前驱体；将前驱体置于石英舟中，通过煅烧法在250 ℃加热2 h，随后升温至650 ℃加热5 h，制得V掺杂LaCoO3钙钛矿型电解水析氧催化剂。本发明所述催化剂不仅具有显著的电解水析氧活性，而且稳定性好、原料丰富、成本低廉、制备工艺简单、快速高效，可实现低成本的规模化生产制备。
Description
技术领域
本发明涉及一种V-LaCoO3钙钛矿型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
随着能源需求的快速增长，能源危机变得越来越突出，设计高效，低成本的电化学能源转换催化剂以满足可再生能源的高要求变得非常迫切。氢气和氧气释放反应是许多可再生能源技术的关键步骤。然而，析氧反应由于涉及多步质子转移过程，需要很大的过电位才能达到理想的电流密度。IrO2、RuO2等贵金属氧化物被认为是最活跃的电解水析氧催化剂，但它们的稀有性和高成本在很大程度上阻碍了它们的进一步实际应用。因此，需要发展和设计性能优越并且廉价易得的电催化剂以降低电极反应的过电位，这对提高电解水制氢的效率具有关键性作用。
具有通式ABO3的钙钛矿氧化物因其可以容纳各种组分和结构可调性而受到越来越多的关注。到目前为止，高效钙钛矿型电解水催化剂的研究已经取得了重要的进展。除了结构和组分之外，钙钛矿的电子结构也是影响其催化活性高低的重要因素。催化剂的电子结构可以优化反应物的吸附能，从而改变催化活性，其中钙钛矿中的金属-氧桥键为其电子结构的调制提供了基础。但是具有受控结构并且性能良好的钙钛矿析氧电催化剂的设计仍然是一个挑战。V作为一种多价态金属，将它掺杂进入钙钛矿型电催化剂可以有效调节其中过渡金属的d电子轨道。因此，通过简便的方法将二者的优势结合起来，制备性能优异的电解水析氧催化剂尤为重要。因此，本发明发展了一种成本低廉、简便易行、低能耗的复合电解水催化剂的制备方法，进而制备了一种具有优异性能的V-LaCoO3钙钛矿型电解水催化剂。
发明内容
本发明的目的在于提供一种通过简便方法制备成本低廉、操作简单易行的V-LaCoO3钙钛矿型电解水催化剂。本发明提供的这种制备方法，工艺简单，成本低廉，且所制备的V掺杂LaCoO3具有优异的电解水析氧性能，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V-LaCoO3钙钛矿型电解水催化剂的制备方法，包括以下步骤：
1）称取0.3-0.5 mmol的La(NO3)2 .6H2O，0.04~0.05 mmol的Co(NO3)2 .6H2O以及0-0.01mmol的VCl3至烧杯中并加水溶解，保持搅拌；
2）配置浓度为1-3 mol/L的KOH水溶液；
3）将步骤2所得的KOH水溶液加入到步骤1所得混合溶液中，继续搅拌10-20 min后转移到反应釜中，150-200 ℃环境下反应8-12 h；
4）将步骤3所得的产物用去离子水和乙醇清洗，并在60-80 ℃环境下干燥；
5）将步骤4所得样品研磨成粉末后置于石英舟中在空气中煅烧，先在200-300 ℃环境下保温1-3 h再升温至600-700 ℃保温4-6 h，待自然冷却至室温后所得样品即V掺杂LaCoO3复合电解水析氧催化剂。
本发明的有益效果：
（1）本发明提供了一种新型V-LaCoO3钙钛矿型电解水催化剂的制备方法，即通过水热及煅烧法直接制备V掺杂LaCoO3电解水析氧催化剂。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V掺杂LaCoO3纳米棒，产物形貌尺寸均匀，可大规模制备易于利用；
（3）本发明制备的V掺杂LaCoO3钙钛矿型电解水析氧催化剂具有优异的析氧及良好的稳定性；
（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为本发明方法所制备的V掺杂LaCoO3钙钛矿型电解水析氧催化剂的前驱体用JEOL-1400透射电子显微镜观察后拍摄的透射电镜（TEM）照片；
图2为本发明方法所制备的V掺杂LaCoO3钙钛矿型电解水析氧催化剂用JEOL-1400透射电子显微镜观察后拍摄的透射电镜（TEM）照片；
图3为本发明方法所制备的V掺杂LaCoO3钙钛矿型电解水析氧催化剂的X射线衍射（XRD）图；
图4是本发明方法所制备的V掺杂LaCoO3钙钛矿型电解水析氧催化剂的电催化析氧性能图。
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0.0376 mmol La(NO3)2·6H2O和0.05 mmol Co(NO3)2·6H2O溶于9 mL超纯水中并搅拌，缓慢搅拌下加入浓度为1 mol/L的KOH溶液1 mL，继续搅拌15 min。搅拌结束后，将所得溶液用超纯水和乙醇分别洗涤后干燥处理并研磨成粉末。随后在空气中250 ℃煅烧2h随后升温至650 ℃继续煅烧5 h后得到制得的LaCoO3电解水析氧催化剂。
实施例2
首先将0.0376 mmol La(NO3)2·6H2O， 0.04 mmol Co(NO3)2·6H2O和0.01 mmol VCl3溶于9 mL超纯水中并搅拌，缓慢搅拌下加入浓度为1 mol/L的KOH溶液1 mL，继续搅拌20min。搅拌结束后，将所得溶液用超纯水和乙醇分别洗涤后干燥处理并研磨成粉末。随后在空气中250 ℃煅烧2 h随后升温至650 ℃继续煅烧5 h后得到V掺杂LaCoO3钙钛矿型电解水析氧催化剂。
实施例3
使用辰华660D电化学工作站对V掺杂LaCoO3钙钛矿型电解水析氧催化剂析氧活性进行测试。以碳棒为对电极，银/氯化银为参比电极，滴有V掺杂LaCoO3钙钛矿型电解水析氧催化剂的玻碳电极为工作电极，1 mol/L KOH水溶液为电解质溶液。在0 至1 V（相对于Ag/AgCl电极）电压范围内，以5 mV/s的扫速进行线性伏安扫描，即可得到其催化电解水产氧的极化曲线。
Claims (4)
1.一种V-LaCoO3钙钛矿型电解水催化剂，其特征在于该催化剂形貌为均匀的纳米棒状形貌。
2.一种制备V-LaCoO3钙钛矿型电解水催化剂的方法，其特征在于制备方法的步骤如下：
1）采用水热法，以硝酸镧、硝酸钴、氯化钒以及氢氧化钾为反应物制得前驱体；
2）将步骤1所得的前驱体进行干燥并研磨，通过煅烧法制得V-LaCoO3钙钛矿型电解水催化剂。
3.根据权利要求2所述的V-LaCoO3钙钛矿型电解水催化剂的制备方法，其特征在于，所述复合催化剂中V的掺杂量为0-0.01 mmol。
4.根据权利要求1所述的V-LaCoO3钙钛矿型电解水析氧催化剂的制备方法，其特征在于，所用溶剂为水溶液，无其他有机溶剂的使用，制备过程无毒无害。
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