CN107359330B - 一种石墨烯掺杂的二氧化铱基多孔电极及其制备方法 - Google Patents
一种石墨烯掺杂的二氧化铱基多孔电极及其制备方法 Download PDFInfo
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Abstract
本发明属于电极材料技术领域，具体涉及一种石墨烯掺杂的IrO2基多孔电极及其制备方法。本发明将氯铱酸与石墨烯进行负载，然后再将其与非贵金属氧化物复合，制得一种复合型电极材料。本发明通过结合石墨烯的高导电性、贵金属氧化物的导电性和活性以及非贵金属氧化物材料独特的外层电子结构，制备一种新型高比电容、高电解质选择性的多孔金属氧化物/石墨烯复合电极。
Description
技术领域
本发明属于电极材料技术领域，具体涉及一种石墨烯掺杂的IrO2基多孔电极及其制备方法。
背景技术
以IrO2和RuO2为代表的金属氧化物阳极因其具有良好的耐蚀性能、活性和电容性能倍受关注。添加非贵金属氧化物提高其电化学性能并降低成本是研究重点，几乎包含了所有的非贵金属氧化物。近些年，以活性炭、碳纳米管和石墨烯为代表的导电导热良好碳材料又成为电极材料的研究热点。然而，添加非贵金属氧化物可以有效提高以IrO2为基氧化物材料的电容性能，但是导电性较差，而且在充放电过程中体积膨胀严重，造成电极粉化和崩塌。单纯的碳材料电极活化困难，制备过程中容易发生团聚，往往得不到理想的电容性能。此外，电极材料的使用电解质不同，其电化学性能有很大差异。如以H2SO4为代表的酸性电解质通常选IrO2基氧化物材料，最典型的为IrO2-Ta2O5氧化物电极；以NaCl为代表的中性电解质首选RuO2基氧化物材料，最典型的为RuO2（摩尔分数30%）-TiO2氧化物电极；以KOH为代表的碱性电解质通常以泡沫镍为基体制备的镍钴复合氧化物（尖晶石型）电极材料。本发明意在结合石墨烯的高导电性、贵金属氧化物的导电性和活性以及非贵金属氧化物材料独特的外层电子结构，制备一种新型高比电容、高电解质选择性的多孔金属氧化物/石墨烯复合电极。
发明内容
本发明的目的在于提供一种石墨烯掺杂的IrO2基多孔电极及其制备方法。只要采用最简单的热分解法就可以获得高比电容、高电解质选择性的多孔金属氧化物/石墨烯复合电极。
常规IrO2基等电极常用作析氧电极，如IrO2-Ta2O5电极，当IrO2为 摩尔分数50%时可达到最好的电极性能。这些电极的表面微观形貌为龟裂状裂纹而非多孔。
所述石墨烯掺杂的IrO2基多孔电极的制备方法为：
（1）采用喷砂后的TA2钛板或泡沫Ni为基体，除油，刻蚀，用去离子水冲洗后，放入乙醇溶液中备用；
（2）按照铱的重量（载量）0.2-0.6mg/cm2取氯铱酸溶解于无水乙醇中超声震荡完全溶解；
（3）按照0.2-0.6g/cm2称取石墨烯并加入盐酸对石墨烯进行酸化处理，将酸化后的石墨烯混合到氯铱酸溶液，继续超声振荡；
（4）取非贵金属氧化物的前驱体溶解于无水乙醇/正丁醇等醇液中；
（5）将上述添加了石墨烯的氯铱酸溶液和非贵金属氧化物前驱体超声振荡混合直到完全溶解成为金属离子浓度为30wt%的涂液。将涂液涂刷到钛板或泡沫Ni上，红外灯下烘干，置于300℃的马弗炉中预氧化10min，空冷后重复上述涂覆过程，直到所有涂液用完，最后在300~380℃处理1~6h，可获得高比电容、高电解质选择性的多孔金属氧化物/石墨烯复合电极。
步骤（4）中的非贵金属氧化物的前驱体为CeCl3、TiCl3、SnCl2、SnCl4中的任意一种或几种。
步骤（4）非贵金属氧化物的前驱体与氯铱酸的金属离子摩尔比为4:1~1:4。
本发明的显著优点在于：贵金属含量可降低到0.2-0.6mg/cm2，涂层形貌为多孔结构，在酸、碱和盐溶液中都具有很好的电催化性能，电极可用于多种溶液。以泡沫Ni为基体时的比电容可高达3000F/g以上。
附图说明
图1 实施例1制得的多孔金属氧化物/石墨烯复合电极的不同放大倍数形貌。
图2-a为保温时间1h的多孔金属氧化物/石墨烯复合电极的吸脱附曲线和孔径分布图； 图2-b图为保温时间2h的多孔金属氧化物/石墨烯复合电极的吸脱附曲线和孔径分布图；图2-c为保温时间3h的多孔金属氧化物/石墨烯复合电极的吸脱附曲线和孔径分布图； 图2-d为保温时间4h的多孔金属氧化物/石墨烯复合电极的吸脱附曲线和孔径分布图；图2-e为保温时间5h的多孔金属氧化物/石墨烯复合电极的吸脱附曲线和孔径分布图；图2-f为保温时间6h的多孔金属氧化物/石墨烯复合电极的吸脱附曲线和孔径分布图。
图3不同保温时间Ti/IrO2-CeO2-G电极的吸脱附曲线、孔径分布、总孔体积和BET。
图4不同涂覆载量制备的Ir-Ce-G电极比电容图。
具体实施方式
为进一步公开而不是限制本发明，以下结合实例对本发明作进一步的详细说明。
具体实施例1
采用喷砂后的TA2钛板为基体，除油，刻蚀，用去离子水冲洗后，放入乙醇溶液中备用。按照铱载量0.6mg/cm2取氯铱酸溶于无水乙醇中超声震荡完全溶解。按0.6g/cm2称取石墨烯加入到0.5ml/cm2浓盐酸中对石墨烯进行酸化处理，将酸化后的石墨烯混合到氯铱酸溶液，继续超声振荡。取非贵金属氧化物的前驱体CeCl3按氯铱酸：CeCl3的金属离子摩尔比3:1溶解于无水乙醇。将上述溶液超声振荡混合直到完全溶解成为金属离子浓度为30wt%的涂液。将涂液涂刷到钛板上，红外灯下烘干，置于300℃的马弗炉中预氧化10min，空冷后重复上述涂覆过程，直到所有涂液用完，最后在340℃热处理1~6h，可获得多孔金属氧化物/石墨烯复合电极。
将该电极分别在1.0M H2SO4、1 .0M Na2SO4和 1.0 M NaOH电解液中测试其比电容行为，比电容最高可分别达550.05F/g、390.84F/g和578 F/g，比退火1h的电极材料都有提高2倍以上。
Ti/IrO2-CeO2-G电极在1.0M H2SO4、1 .0 M Na2SO4和 1.0 M NaOH电解液中在500mV/s循环8000次后仍具有优良的循环稳定性。除了退火1h的电极比电容下降，其它电极的比电容均有所上升。
具体实施例2
采用喷砂后的TA2钛板为基体，除油，刻蚀，用去离子水冲洗后，放入乙醇溶液中备用。按每平方厘米钛上铱载量分别为0.2、0.4、0.6、0.8、1.0、1.2、1.4和1.6毫克溶于无水乙醇中超声震荡完全溶解。按0.4g/cm2称取石墨烯加入到0.5ml/cm2浓盐酸对石墨烯进行酸化处理，将酸化后的石墨烯混合到氯铱酸溶液，继续超声振荡。取非贵金属氧化物的前驱体CeCl3按氯铱酸：CeCl3的金属离子摩尔比3:1溶解于无水乙醇。将上述溶液超声振荡混合直到完全溶解为止成为涂液。将涂液涂刷到钛板上，红外灯下烘干然后放在红外光下干燥10min，接着在380℃箱式炉中热氧化10min后出炉空冷。该涂敷-烘干-烧结-冷却过程反复多次直到达到所需涂覆载量为止，最后一次在380℃恒温烧结5h。
将该电极分别在1.0M H2SO4电解液中测试其比电容行为，比电容最高可达507 F/g。如图4。
具体实施例3
按照铱载量0.4mg/cm2将氯铱酸和四氯化锡按金属离子摩尔比（7:3）溶于无水乙醇，超声混合均匀，静置得金属离子浓度为30wt%溶液。称取0.4g/cm2的石墨烯加到上述混合液中，超声混合均匀静置。取该溶液涂覆在泡沫Ni板上，然后放在红外光下烘烤至干燥，接着在380℃箱式炉中热氧化10min后出炉空冷。完全冷至室温后继续涂敷-烘干-烧结-冷却过程，反复多次直到达到所需涂覆铱载量0.4mg/cm2为止，最后一次在380℃恒温烧结5h。其比电容可高达3123.89F/g。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (2)
1.一种石墨烯掺杂的IrO2基多孔电极的制备方法，其特征在于：具体制备步骤为：
按照铱载量0.4mg/cm2将氯铱酸和四氯化锡按金属离子摩尔比7:3溶于无水乙醇，超声混合均匀，静置得金属离子浓度为30wt%溶液；称取0.4g/cm2的石墨烯加到上述混合液中，超声混合均匀静置；取该溶液涂覆在泡沫Ni板上，然后放在红外光下烘烤至干燥，接着在380℃箱式炉中热氧化10min后出炉空冷；完全冷至室温后继续涂敷-烘干-烧结-冷却过程，反复多次直到达到所需涂覆铱载量0.4mg/cm2为止，最后一次在380℃恒温烧结5h。
2.一种如权利要求1所述的方法制备的石墨烯掺杂的IrO2基多孔电极。
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