CN108423717B - 一种自组装Ni3S2纳米片的合成方法 - Google Patents
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Abstract
一种自组装Ni3S2纳米片的合成方法,首先,将泡沫镍依次在丙酮和HCl溶液中超声清洗,然后分别用去离子水和无水乙醇洗涤干净室温晾干;其次,将晾干后的泡沫镍放入带聚四氟乙烯内衬的高温高压反应釜中,然后再向反应釜中加入硫脲溶液、聚乙烯吡咯烷酮形貌调控剂,将反应釜密封,置于烘箱中待反应结束后,自然冷却至室温后,取出泡沫镍,分别用水和无水乙醇反复冲洗;最后,将冲洗后的泡沫镍放入真空干燥箱室温干燥得到自组装Ni3S2纳米片阵列自支撑电极。本发明采用的溶剂热法具有工艺简单、制备周期短和反应条件容易控制的特性,可利用不同的温度来控制反应的进程和形貌大小,从而得到不同特殊的结构形貌。
Description
技术领域
本发明属于材料制备领域,具体涉及一种自组装Ni3S2纳米片的合成方法。
背景技术
目前具有良好金属性或导电性的非贵金属电催化剂的合成应该受到重视。Ni3S2是一种天然的黄镍铁矿。由于连续的Ni-Ni键网络贯穿于Ni3S2的整个结构,所以它具有本征的金属特性电导率高、廉价的Ni3S2在许多领域得到了应用,如氧还原、锂离子电池、染料敏化电池和储氢等。
电催化产氢产氧技术发展的核心问题就是提高HER电催化剂的活性。虽然已经开发了大量的廉价非贵金属产氢产氧电催化剂,但是与贵金属催化剂相比,其催化活性、催化稳定性以及使用范围等方面仍然存在着很大的差距。提高产氢产氧电催化剂性能的策略主要集中在材料的设计合成和后处理修饰方面。一般提高电催化产氢产氧性能的常用方法有:对电催化材料进行纳米构造、结构调控、掺杂和与导电基底(碳布、碳纤维纸、石墨烯、CNTs、泡沫镍和钛片等具有优异导电特性的物质)的复合。
发明内容
本发明的目的在于提供一种制备工艺简单,制备条件温和,成本低、制备周期短、工艺过程容易控制的自组装Ni3S2纳米片的合成方法。
为达到上述目的,本发明采用的技术方案是:
1)首先,将1cm×2cm的泡沫镍依次在丙酮和HCl溶液中超声清洗,然后分别用去离子水和无水乙醇洗涤干净室温晾干;
2)其次,将晾干后的泡沫镍放入50mL带聚四氟乙烯内衬的高温高压反应釜中,然后再向反应釜中加入5~15mL硫脲溶液,0.025~0.363g的聚乙烯吡咯烷酮形貌调控剂,将反应釜密封,置于烘箱中在130~180℃反应6~10h;
3)待反应结束后,自然冷却至室温后,取出泡沫镍,分别用水和无水乙醇反复冲洗;
4)最后,将冲洗后的泡沫镍放入真空干燥箱室温干燥得到自组装Ni3S2纳米片阵列自支撑电极。
所述步骤1)的超声清洗功率为70~80W,超声清洗时间为5~10min。
所述步骤1)HCl溶液的浓度为3mol/L。
所述步骤2)硫脲溶液的浓度为1.445mmol/L。
从制备方法上比较,本发明采用的溶剂热法具有工艺简单、制备周期短和反应条件容易控制的特性,可利用不同的温度来控制反应的进程和形貌大小,从而得到不同特殊的结构形貌。形貌结构的不同对材料的性能有较大的影响,另外,溶剂热法具有反应速率较快、反应充分彻底、等优势,它避免了传统方法的反应难以进行和难控制、能耗高、产率低和工艺复杂等缺点。层层堆叠的Ni3S2纳米片与基底泡沫镍(NF)紧密接触,这不仅提高了Ni3S2/NF的电催化稳定性,还有利于基底与催化活性物质界面之间电子的传输,暴露出高密度的催化位点活性,因此具有较快的电子转移速率,这有利于提高其电催化性能。其制备的Ni3S2纳米片紧密连接并形成了许多空隙,并且这些纳米片垂直生长在NF上。层层堆叠的纳米片阵列结构赋予该材料较大的活性面积,为催化反应提供了更多的活性位点,促使电子容易从电极传递到催化活性位,因此显示出高效、超稳定的电催化产氢和产氧活性。
附图说明
图1是本发明实施例1制备Ni3S2/NF纳米片阵列自支撑电极的XRD图。
图2是本发明实施例2制备的Ni3S2/NF纳米片阵列自支撑电极的Ni3S2的SEM 图。
具体实施方式
下面结合附图及实施例对本发明作进一步详细说明。
实施例1:
1)首先,将1cm×2cm的泡沫镍依次在丙酮和3mol/L的HCl溶液中以70W超声清洗8min,然后分别用去离子水和无水乙醇洗涤干净室温晾干;
2)其次,将晾干后的泡沫镍放入50mL带聚四氟乙烯内衬的高温高压反应釜中,再加入5mL浓度为1.445mmol/L硫脲溶液中,并加入0.275~0.363g聚乙烯吡咯烷酮 (PVP)形貌调控剂,将反应釜密封,置于烘箱中在130℃反应10h;
3)待反应结束后,自然冷却至室温后,取出泡沫镍,分别用水和无水乙醇反复冲洗;
4)最后,将冲洗后的泡沫镍放入真空干燥箱室温干燥得到自组装Ni3S2纳米片阵列自支撑电极。
由图1可以看出本实施例所制备样品为Ni3S2/NF的XRD谱图,该谱图中除了包括来自NF基体的衍射峰,还出现了六方相结构Ni3S2的衍射峰(JCPDS Card No. 44-1418)。
实施例2:
1)首先,将1cm×2cm的泡沫镍依次在丙酮和3mol/L的HCl溶液中以80W超声清洗5min,然后分别用去离子水和无水乙醇洗涤干净室温晾干;
2)其次,将晾干后的泡沫镍放入50mL带聚四氟乙烯内衬的高温高压反应釜中,再加入8mL浓度为1.445mmol/L硫脲溶液中,并加入0.2~0.264g聚乙烯吡咯烷酮(PVP) 形貌调控剂,将反应釜密封,置于烘箱中在140℃反应9h;
3)待反应结束后,自然冷却至室温后,取出泡沫镍,分别用水和无水乙醇反复冲洗;
4)最后,将冲洗后的泡沫镍放入真空干燥箱室温干燥得到自组装Ni3S2纳米片阵列自支撑电极。
图2可以看出本实施例所制备的一种自组装Ni3S2/NF纳米片阵列自支撑电极的Ni3S2纳米片层层堆叠紧密连接并形成了许多空隙。而且,这些纳米片垂直生长在NF 上,其厚度为10-15nm。
实施例3:
1)首先,将1cm×2cm的泡沫镍依次在丙酮和3mol/L的HCl溶液中以80W超声清洗10min,然后分别用去离子水和无水乙醇洗涤干净室温晾干;
2)其次,将晾干后的泡沫镍放入50mL带聚四氟乙烯内衬的高温高压反应釜中,再加入10mL浓度为1.445mmol/L硫脲溶液中,并加入0.15~0.198g聚乙烯吡咯烷酮 (PVP)形貌调控剂,将反应釜密封,置于烘箱中在150℃反应8h;
3)待反应结束后,自然冷却至室温后,取出泡沫镍,分别用水和无水乙醇反复冲洗;
4)最后,将冲洗后的泡沫镍放入真空干燥箱室温干燥得到自组装Ni3S2纳米片阵列自支撑电极。
实施例4:
1)首先,将1cm×2cm的泡沫镍依次在丙酮和3mol/L的HCl溶液中以70W超声清洗9min,然后分别用去离子水和无水乙醇洗涤干净室温晾干;
2)其次,将晾干后的泡沫镍放入50mL带聚四氟乙烯内衬的高温高压反应釜中,再加入12mL浓度为1.445mmol/L硫脲溶液中,并加入0.1~0.132g聚乙烯吡咯烷酮 (PVP)形貌调控剂,将反应釜密封,置于烘箱中在170℃反应7h;
3)待反应结束后,自然冷却至室温后,取出泡沫镍,分别用水和无水乙醇反复冲洗;
4)最后,将冲洗后的泡沫镍放入真空干燥箱室温干燥得到自组装Ni3S2纳米片阵列自支撑电极。
实施例5:
1)首先,将1cm×2cm的泡沫镍依次在丙酮和3mol/L的HCl溶液中以70W超声清洗7min,然后分别用去离子水和无水乙醇洗涤干净室温晾干;
2)其次,将晾干后的泡沫镍放入50mL带聚四氟乙烯内衬的高温高压反应釜中,再加入15mL浓度为1.445mmol/L硫脲溶液中,并加入0.025~0.033g聚乙烯吡咯烷酮 (PVP)形貌调控剂,将反应釜密封,置于烘箱中在180℃反应6h;
3)待反应结束后,自然冷却至室温后,取出泡沫镍,分别用水和无水乙醇反复冲洗;
4)最后,将冲洗后的泡沫镍放入真空干燥箱室温干燥得到自组装Ni3S2纳米片阵列自支撑电极。
Claims (3)
1.一种自组装Ni3S2纳米片的合成方法,其特征在于包括以下步骤:
1)首先,将1cm×2cm的泡沫镍依次在丙酮和HCl溶液中超声清洗,然后分别用去离子水和无水乙醇洗涤干净室温晾干;
2)其次,将晾干后的泡沫镍放入50mL带聚四氟乙烯内衬的高温高压反应釜中,然后再向反应釜中加入5~15mL硫脲溶液,0.025~0.363g的聚乙烯吡咯烷酮形貌调控剂,将反应釜密封,置于烘箱中在130~180℃反应6~10h;
3)待反应结束后,自然冷却至室温后,取出泡沫镍,分别用水和无水乙醇反复冲洗;
4)最后,将冲洗后的泡沫镍放入真空干燥箱室温干燥得到自组装Ni3S2纳米片阵列自支撑电极;
所述步骤2)硫脲溶液的浓度为1.445mmol/L。
2.根据权利要求1所述的自组装Ni3S2纳米片的合成方法,其特征在于:所述步骤1)的超声清洗功率为70~80W,超声清洗时间为5~10min。
3.根据权利要求1所述的自组装Ni3S2纳米片的合成方法,其特征在于:所述步骤1)HCl溶液的浓度为3mol/L。
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