CN115478299A - 一种基于铁镍配位聚合物的电催化剂 - Google Patents
一种基于铁镍配位聚合物的电催化剂 Download PDFInfo
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Abstract
本发明公开一种通过制备电催化剂进行电化学测试并应用于锌空气电池。本发明设计了一种基于配合物的用于氧还原和氧析出反应的电催化剂。具体说是以FeNi配位聚合物(CP)作为前驱体,以氧化石墨烯(GO)作为模板,通过热解反应制备的电催化剂。该催化剂具有优异的电催化性能,并且应用在锌空电池上也显示出了其良好的稳定性和活性。
Description
技术领域
本发明属于涉及一种基于配合物的用于氧还原和氧析出反应的电催化剂;具体说是以FeNi配位聚合物(CP)作为前驱体,以氧化石墨烯(GO)作为模板,通过热解反应制备的电催化剂。
背景技术
由于全球能源需求的迅速上升和传统化石燃料造成的严重环境问题,先进储能和转换技术的发展变得越来越重要。其中,可充电锌空气电池(ZABs)因其具有高能量密度,低成本,环保和安全操作特性的巨大潜力而引起研究者们的极大兴趣。同时,由于它们可以通过增强动力学和还原过电位来确定电化学反应速率,因此用于析氧反应(OER)和氧还原反应(ORR)的催化剂在ZABs中起着至关重要的作用。目前,该领域多使用钌、铂等贵金属催化剂。然而,贵金属资源的稀缺性、有限寿命和高成本,严重限制了它们在大规模工业生产中的应用。因此,设计和制备低成本、高活性、长寿命的非贵金属催化剂,对于当前电化学催化领域具有重要意义;在本研究中,以镍离子掺杂的氰根桥联Fe(III)-Ni(II)CP为前驱体,GO为模板,通过简单沉淀和随后的退火处理,同时引入外部N源,制备了一种优良的双功能FeNi合金电催化剂(FeNi/N-GPCM),FeNi/N-GPCM与可逆氢电极(与RHE相比)相比,表现出0.883 V的优异ORR半波电位(E1/2),在10 mA cm-2下具有310 mV的OER过电势(η),均优于商用铂基(E1/2 = 0.84 V)和RuO2(η = 320 mV)催化剂。
发明内容
本发明的目的之一是基于配合物制备一种用于氧还原和氧析出反应的的电催化剂。
本发明的目的之二是将该材料用于电催化反应中活性和稳定性的检测。
本发明的技术方案如下:
一种以铁镍配位聚合物为前驱体,GO为模板的电催化剂制备如下:
(1)将5mL含有[Ni(L)(H2O)2][ClO4]2(以下称为2,6Ni,L=2,12-二甲基-3,7,11,17-四氮杂双环[11.3.1]七庚二环(17),2,11,13,15-五烯,(76.7mg,0.15mmol)的CH3CN溶液,加入到5mL K3[Fe(CN)6](32.9mg,0.10mmol)的水溶液中;
(2)将NiCl6·6H2O(0.04mmol,15.19mg)加入到上述悬浊液中,搅拌半小时,溶液陈化过夜,过滤得到沉淀(FeNi-CP),用乙腈洗涤,在空气中干燥;
(3)使用超声浴将30 mg氧化石墨烯(GO)在40mL乙醇中预处理2小时后,缓慢加入10mg FeNi-CP。混合液经超声处理3h,然后搅拌24h;
(4)将上述溶液置于空气中60°C条件下缓慢蒸发以获得粉末。最后,在三聚氰胺的保护下, 120~800°C的温度范围内,N2气氛下,在管式炉中热解得到FeNi/N-GPCM粉末。
本发明的有益效果为:
(1)以FeNi配合物为前驱体,由于配合物中包含较多的金属,在热解过程中可以生成FeNi合金,使活性位点增多,从而导致优异的电化学性能;
(2)引入三聚氰胺作为外部氮源,可以进一步丰富热解产物中的氮元素含量;
(3)以GO为模板,由于GO的片状结构以及其耐高温的性质,使所制备的材料在热解过程中保持原来的形貌,增大了比表面积,从而增加了材料本身的活性,使得所制备材料具有优异的稳定性。
附图说明
图1 本发明材料FeNi/N-GPCM的制备过程示意图。
图2本发明材料FeNi/N-GPCM的电镜图。
图3 催化活性和稳定性测试图。
图4 锌空电池图。
具体实施方式
实施例1一种以铁镍配位聚合物为前驱体,GO为模板的电催化剂制备如下:
(1)将5mL含有[Ni(L)(H2O)2][ClO4]2(以下称为2,6Ni,L=2,12-二甲基-3,7,11,17-四氮杂双环[11.3.1]七庚二环(17),2,11,13,15-五烯,(76.7mg,0.15mmol)的CH3CN溶液,加入到5mL K3[Fe(CN)6](32.9mg,0.10mmol)的水溶液中;
(2)将NiCl6·6H2O(0.02mmol,7.59mg)加入到上述悬浊液中,搅拌半小时,溶液陈化过夜,过滤得到沉淀(FeNi-CP),用乙腈洗涤,在空气中干燥;
(3)使用超声浴将30 mg氧化石墨烯(GO)在40mL乙醇中预处理2小时后,缓慢加入10mg FeNi-CP。混合液经超声处理3h,然后搅拌24h;
(4)将上述溶液置于空气中60°C条件下缓慢蒸发以获得粉末。最后,在三聚氰胺的保护下, 120~800°C的温度范围内,N2气氛下,在管式炉中热解得到FeNi/N-CM粉末。
实施例2一种以铁镍配位聚合物为前驱体,GO为模板的电催化剂制备如下:
(1)将5mL含有2,6Ni(76.7mg,0.15mmol)的CH3CN溶液,加入到5mL K3[Fe(CN)6](32.9mg,0.10mmol)的水溶液中;
(2)将NiCl6·6H2O(0.08mmol,30.38mg)加入到上述悬浊液中,搅拌半小时,溶液陈化过夜,过滤得到沉淀(FeNi-CP),用乙腈洗涤,在空气中干燥;
(3)使用超声浴将30 mg氧化石墨烯(GO)在40mL乙醇中预处理2小时后,缓慢加入10mg FeNi-CP。混合液经超声处理3h,然后搅拌24h;
(4)将上述溶液置于空气中60°C条件下缓慢蒸发以获得粉末。最后,在三聚氰胺的保护下, 120~800°C的温度范围内,N2气氛下,在管式炉中热解得到FeNi/N-GPCM-1粉末。
实施例3一种以铁镍配合物为前驱体,GO为模板在700℃下制备的电催化剂;
(1)将5mL含有2,6Ni(76.7mg,0.15mmol)的CH3CN溶液,加入到5mL K3[Fe(CN)6](32.9mg,0.10mmol)的水溶液中;
(2)将NiCl6·6H2O(0.04mmol,15.19mg)加入到上述悬浊液中,搅拌半小时,溶液陈化过夜,过滤得到沉淀(FeNi-CP),用乙腈洗涤,在空气中干燥;
(3)使用超声浴将30 mg氧化石墨烯(GO)在40mL乙醇中预处理2小时,然后缓慢加入10mg FeNi-CP。混合液经超声处理3h,然后搅拌24h;
(4)将溶液进一步暴露在空气中的60°C缓慢蒸发以获得粉末。最后,在三聚氰胺的保护下,在120~700°C的温度范围内,在N2气氛下,在管式炉中热解得到FeNi/N-GPCM-700粉末。
实施例4一种以铁镍配合物为前驱体,GO为模板在900℃下制备的电催化剂;
(1)将5mL含有2,6Ni(76.7mg,0.15mmol)的CH3CN溶液,加入到5mL K3[Fe(CN)6](32.9mg,0.10mmol)的水溶液中;
(2)将NiCl6·6H2O(0.04mmol,15.19mg)加入到上述悬浊液中,搅拌半小时,溶液陈化过夜,过滤得到沉淀(FeNi-CP),用乙腈洗涤,在空气中干燥;
(3)使用超声浴将30 mg氧化石墨烯(GO)在40mL乙醇中预处理2小时,然后缓慢加入10mg FeNi-CP。混合液经超声处理3h,然后搅拌24h;
(4)将溶液进一步暴露在空气中的60°C缓慢蒸发以获得粉末。最后,在三聚氰胺的保护下,在120~900°C的温度范围内,在N2气氛下,在管式炉中热解得到FeNi/N-GPCM-900粉末。
实施例5 活性测试
(1)在ORR和OER测试中,以表面积为0.196 cm2的玻碳(GC)电极作为工作电极,分别以石墨棒和饱和氯化银电极(饱和KCl溶液)作为对电极和参比电极;
(2)将O2流注入电解质30分钟以获得O2的饱和溶液;
(3)在室温下,在1.0 KOH的溶液中以5 mV s-1的扫描速率对材料进行LSV测试,并用电化学阻抗谱仪校正补偿电位;
(4)工作电极从400到2500rpm旋转,扫描速率为10mVs-1得到ORR测试曲线图。
实施例6 稳定性测试
(1) 将O2流注入电解质30分钟以获得O2的饱和溶液;
(2)通过电流(i-t)计时电流测量响应对ORR和OER进行了稳定性。
Claims (4)
1.一种以铁镍配合物为前驱体,GO为模板的电催化剂制备如下:
(1)将5mL含有[Ni(L)(H2O)2][ClO4]2(以下称为2,6Ni,L=2,12-二甲基-3,7,11,17-四氮杂双环[11.3.1]七庚二环(17),2,11,13,15-五烯,(76.7mg,0.15mmol)的CH3CN溶液,加入到5mL K3[Fe(CN)6](32.9mg,0.10mmol)的水溶液中;
(2)将NiCl6·6H2O(0.02mmol,7.59mg)加入到上述悬浊液中,搅拌半小时,溶液陈化过夜,过滤得到沉淀(FeNi-CP),用乙腈洗涤,在空气中干燥;
(3)使用超声浴将30 mg氧化石墨烯(GO)在40mL乙醇中预处理2小时后,缓慢加入10mgFeNi-CP,混合液经超声处理3h,然后搅拌24h;
(4)将上述溶液置于空气中60°C条件下缓慢蒸发以获得粉末,最后,在三聚氰胺的保护下, 120~800°C的温度范围内,N2气氛下,在管式炉中热解得到FeNi/N-GPCM粉末。
2.根据权利要求1所述的一种以铁镍配合物为前驱体,GO为模板的电催化剂,制备可充电锌空电池的步骤如下:
以抛光锌箔和6 M KOH + 0.2 M Zn(OAc)2的混合溶液分别作为阳极和电解质,将制备的催化剂涂覆在碳纸上,用于空气阴极,面积约为0.785 cm2,所制备的催化剂在碳纸上的总催化剂负载量均为2.0 mg cm-2。
3.使用Neware电池测试站系统(CT-3008)在10 mA cm-2的电流密度下,通过循环恒电流脉冲方法对Zn-空气电池进行恒电流充放电循环(充电20分钟,放电20分钟)。
4.根据权利要求1所述制备方法制备的电催化剂用于OER和ORR测试;
根据要求1所述的OER和ORR检测步骤如下:
(1)以表面积为0.196 cm2的玻碳(GC)电极作为工作电极,分别以石墨棒和饱和氯化银电极(饱和KCl溶液)作为对电极和参比电极;
(2)将O2流注入电解质30分钟以获得O2的饱和溶液;在室温下,在1.0 KOH的溶液中以5mV s-1的扫描速率对材料进行LSV测试,并用电化学阻抗谱仪校正补偿电位;
(3)工作电极从400到2500rpm旋转,扫描速率为10mVs-1得到ORR测试曲线图;通过电流(i-t)计时电流测量响应对ORR和OER进行了稳定性测试。
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