CN110820010A - 一种自支撑Ni2P/Ni@C复合阴极析氢材料及其制备方法 - Google Patents
一种自支撑Ni2P/Ni@C复合阴极析氢材料及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种具有片状复合多孔结构的自支撑Ni2P/Ni@C电催化析氢阴极材料及其制备方法，该方法包含以下步骤：1.由粉末冶金法制得多孔Ni@C材料基底；2.在多孔Ni@C基底上水热原位生长Ni(OH)2前驱体；3.采用低温气相反应技术将Ni(OH)2/Ni@C进行磷化得到自支撑Ni2P/Ni@C材料。所得材料具有丰富连通的三维多孔结构，活性物质原位生长于自支撑多孔基底表面，完全不依赖第三方粘结助剂，避免粘结助剂对集流体转移电子的障碍，非常适用于电催化反应过程及电化学储能等应用领域。
Description
技术领域：
本发明涉及一种具有片状复合多孔结构的自支撑Ni2P/Ni@C电催化析氢阴极材料的制备方法，结合粉末冶金、水热合成及低温气相反应技术，原位合成复合多孔材料，用于电催化析氢反应。所得阴极材料具有丰富连通的三维多孔结构，活性物质原位生长于自支撑多孔基底表面，完全不依赖第三方粘结助剂，避免粘结助剂对集流体转移电子的障碍，为复合阴极的设计与制备提供新思路。此Ni2P/Ni@C复合自支撑材料非常适用于电催化过程及电化学储能等应用领域。
背景技术：
目前全世界范围内由于煤，石油，天然气等一次能源的过度开采和使用，导致了能源资源短缺和严重的环境问题。因此，寻找一种新型高效的能源来替代传统能源已经迫在眉睫。氢能作为一种清洁的可再生能源，具有燃烧热值高，燃烧产物是水，不会对环境造成破环。电解水制氢具有原料来源广，清洁无污染，可再生等优点，是未来氢能源能够大量生产和广泛应用的关键技术。
研究表明，一些廉价催化剂(过渡金属硫化物，碳化物以及磷化物)由于具有较高的电催化活性和稳定性，有望替代传统电解水阴极制氢材料，实现大规模氢生产。其中，磷化镍由于具有良好的金属导电性，具有类铂、钯贵金属的性质，且在酸碱介质中均具有良好的稳定性，被认为是一种具有很好前景的析氢电催化剂。传统的制备磷化镍方法主要是水热法合成粉体材料，再采用第三方粘结助剂将纳米粉体粘附于导电性良好的金属集流体表面，这个过程由于电子传输受到粘结助剂的阻碍，大大影响了磷化镍的真实应用表面活性。
本发明以多孔Ni@C复合自支撑材料为基底，通过水热原位生长和低温气相反应技术合成无粘接剂的Ni2P/Ni@C复合材料，避免了由于使用粘接剂而造成的材料电阻增大，过电位升高的情况，且基底的多孔结构增大了Ni2P的附着面积，大大提高了材料析氢活性。
发明内容:
为提高电解水的阴极析氢效率，降低能耗，本发明提供一种方法简便、成本低廉、析氢催化活性高、化学稳定性好的自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法。本发明主要采用水热原位生长技术和低温气相反应技术，合成了具有多维孔道结构且无粘接剂的自支撑Ni2P/Ni@C电催化析氢复合材料。
本发明采用以下技术方案进行制备：
(1)由粉末冶金法制得多孔Ni@C材料基底：采用高分子粘结剂与Ni粉混合，在乙醇分散作用下制成流变状态浆料，控制厚度在平板光洁面上覆膜，真空干燥后置于真空烧结炉，连续梯度升温烧结得多孔Ni@C材料基底；
(2)在多孔Ni@C基底上水热原位生长Ni(OH)2前驱体：以平均孔径低于30μm的多孔Ni@C材料为基底，经低温高压水热合成得到表面附着丰富片层氢氧化镍的Ni(OH)2/Ni@C复合结构；
(3)采用低温气相反应技术将Ni(OH)2/Ni@C进行磷化：NaH2PO2·H2O为磷源，将Ni(OH)2/Ni@C复合结构进行中温磷化反应得到多孔Ni2P/Ni@C复合材料。
附图说明：
图1是实施例采用的多孔Ni@C材料侧面形貌；
图2是实施例得到的多孔自支撑体Ni2P/Ni@C复合材料表面形貌；
图3是实施例得到的多孔自支撑体Ni2P/Ni@C复合材料的XRD谱图与标准卡片Ni2P(JCPDS No.03-0953)，单质Ni(JCPDS No.04-0850)的对比，横坐标为衍射角(单位：度)，纵坐标为衍射强度(单位：a.u.)；
图4为多孔自支撑体Ni2P/Ni@C复合材料作电解水阴极析氢活性测试结果，横坐标是过电位(单位：V)，纵坐标是电流密度(单位：mA·cm-2)，结果表明在10mA·cm-2的电流密度下，此阴极的析氢过电位为73mV，大大低于泡沫镍的过电位254mV。
具体实施例：
取面积大小为1×2cm2的多孔Ni@C材料，分别以去离子水和无水乙醇洗净表面。称取0.21g六水合硫酸镍(NiSO4·6H2O)，0.06g氟化铵(NH4F)和0.24g尿素[CO(NH2)2]溶解于20mL去离子水中，搅拌使之完全溶解后转入聚四氟乙烯高压釜中，将多孔Ni@C复合材料基底放入高压釜中，在140℃下恒温反应5h，冷却后将材料取出，以乙醇清洗后在50℃下真空干燥2h得到氢氧化镍的前驱体。最后将盛有前驱体的瓷舟放进管式炉中，通氮气做保护气，将0.2g NaH2PO2·H2O置于氮气流前端，在400℃下保温2h，冷却到室温后即可得到具有多维孔道形貌结构的Ni2P/Ni@C复合材料。
Claims (9)
1.一种自支撑Ni2P/Ni@C复合阴极析氢材料，其特征在于，自支撑多孔Ni@C上原位生长片层状Ni2P，形成复合多孔Ni2P/Ni@C材料，该复合材料用于电催化析氢反应，在10mA/cm-2电流密度下其过电位低于80mV。
2.一种自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法，其特征在于，结合粉末冶金、水热原位生长和低温气相反应技术进行连续制备。
3.一种自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法，其特征在于，包括以下步骤：
(1)由粉末冶金法制得多孔Ni@C材料基底；
(2)在多孔Ni@C基底上水热原位生长Ni(OH)2前驱体；
(3)采用低温气相反应技术将Ni(OH)2/Ni@C进行磷化。
4.根据权利要求3所述，一种自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法，其特征在于，所述步骤(1)由粉末冶金法制得多孔Ni@C材料基底，采用高分子粘结剂酚醛树脂、羧甲基纤维素钠、聚乙烯醇缩丁醛中的一种，与Ni粉混合后在乙醇分散作用下形成流变状态，控制厚度50～200μm，干燥后于500～950℃连续梯度升温烧结而成。
5.根据权利要求3所述，一种自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法，其特征在于，所述步骤(1)由粉末冶金法制得多孔Ni@C材料基底，平均孔径为5～30μm，连续梯度升温烧结在真空炉中进行，真空度低于10-3Pa，并于500℃保温4～7小时，700℃保温3～5小时，950℃保温3～6小时。
6.根据权利要求3所述，一种自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法，其特征在于，所述步骤(2)在多孔Ni@C基底上水热原位生长Ni(OH)2前驱体，水热反应溶液的组成分别为：NiSO4·6H2O(10～100mmol/L)、NH4F-(20～200mmol/L)和CO(NH2)2(50～500mmol/L)。
7.根据权利要求3所述，一种自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法，其特征在于，所述步骤(2)在多孔Ni@C基底上水热原位生长Ni(OH)2前驱体，水热反应温度为120℃～180℃，反应时间3～10小时。
8.根据权利要求3所述，一种自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法，其特征在于，所述步骤(3)采用低温气相反应技术将Ni(OH)2/Ni@C进行磷化，以NaH2PO2·H2O为磷源，用量为0.2～1.0g。
9.根据权利要求3所述，一种自支撑Ni2P/Ni@C复合阴极析氢材料的制备方法，其特征在于，所述步骤(3)采用低温气相反应技术将Ni(OH)2/Ni@C进行磷化，磷化过程由氩气保护，在管式炉中进行，升温速率为5℃/min，磷化温度300～500℃，恒温时间为1～3小时。
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