CN115050588B - 一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料及其制备方法 - Google Patents
一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料及其制备方法 Download PDFInfo
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Abstract
一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料及其制备方法,属于超级电容器电极材料技术领域。利用钼酸铵、硫脲、醋酸镍、氧化石墨烯采用两步水热法在泡沫镍表面原位生长Ni3S2/NiS/MoS2/rGO纳米棒,所得电极材料具有良好的倍率性能和循环稳定性。在10A/g电流密度下,比电容可达1846.6F/g。在11A/g下,经过5000次充放电测试后,容量保持率为90.1%。该方法具有制备条件温和、环境友好、性能优良等优点,所制备的电极材料具备优良的电化学性能。
Description
技术领域
本发明属于超级电容器电极材料技术领域,具体涉及一种形貌可控的高性能Ni3S2/NiS/MoS2/rGO超级电容器电极材料及其制备方法。
背景技术
近年来,能源需求的提高和全球化石能源的消耗导致环境污染日益严峻,人们意识到传统不可再生能源存在污染大弊端的问题需要新能源材料的发展,其中新型储能装置成为研究者关注的热点问题。超级电容器因具有功率密度高、循环寿命长、工作温度范围宽、免维护、绿色环保等优点被认为是很有前途的储能器件,现已被广泛应用于电动公交车、航空、军事、电子设备等各个领域。NiS、CoNi2S4、Co3S4等过渡金属硫化物因具有良好的导电性、电化学活性、机械稳定性和更高的比电容成为超级电容器电极材料的研究热点。与单组分硫化物相比,由两种硫化物组成的复合材料能够发挥协同作用,使得氧化还原反应更加丰富,提高了电化学性能。专利CN103971953B通过溶剂热的方法制备的NiS/Co3S4呈现出球状结构并有明显的孔结构,有利于电荷的传递和扩散。当电流密度为1A/g时,比电容可达到775F/g,但其倍率性能不佳。专利CN110310835A首先采用水热法将NiCo2O4纳米线沉积在NiO纳米片骨架上,形成分层的异质纳米结构。然后,通过离子交换法得到纳米花NiS@NiCo2S4电极材料。当电流密度为1mA/cm2时,比电容可达15.51F/cm2,经过3500次充放电试验后电容保留率仅为79.8%。为进一步弥补以上不足,本研究引入了石墨烯和MoS2,利用石墨烯优良的导电性、高比表面积以及其与MoS2结合形成的片上杂化材料防止石墨烯和硫化镍的堆积,获得较大的比表面积,有利于镍硫化物的完全利用,提高比电容。
发明内容
本发明针对现有的技术缺陷,提出了一种形貌可控的高性能Ni3S2/NiS/MoS2/rGO超级电容器电极材料及其制备方法,该方法主要涉及以下步骤:
(1)将钼酸铵((NH4)6Mo7O24·4H2O)、硫脲(CH4N2S)和醋酸镍(Ni(OCOCH3)2·4H2O)加入氧化石墨烯(GO)分散液中,通过磁力搅拌形成均匀的前驱体溶液;
(2)将制备好的前驱体溶液转移至聚四氟乙烯内衬并密封于不锈钢的反应釜中,将预处理过的泡沫镍浸入其中,反应釜加热至150℃反应18h,待第一步反应完成后自然冷却至室温;
(3)在步骤(2)反应液中加入(NH4)6Mo7O24·4H2O和CH4N2S,在70℃~190℃温度下进行第二次水热反应,反应时间6h~18h;
(4)所得产物用乙醇和去离子水清洗,并置于70℃的真空烘箱干燥12h。
上述制备方法,所述步骤(1)中,所加的氧化石墨烯分散液浓度为1mg/mL,磁力搅拌时间为20min,(NH4)6Mo7O24·4H2O、CH4N2S和Ni(OCOCH3)2·4H2O在石墨烯分散液中的浓度分别为0.0007-0.0008mol/L、0.01mol/L和0.002mol/L。
上述制备方法,所述步骤(2)中,所述的泡沫镍作为复合材料的基底,并在使用前分别用丙酮、稀盐酸、乙醇和去离子水超声清洗5min。
上述制备方法,所述步骤(3)中,所加入的(NH4)6Mo7O24·4H2O和CH4N2S,使得溶液体系中(NH4)6Mo7O24·4H2O、CH4N2S的浓度为0.0007-0.0008mol/L、0.01mol/L。
上述制备方法,所述步骤(4)中,所得产物分别用乙醇和去离子水清洗3次。所得产物用通式NMR-t-T表示,其中t、T分别为步骤(3)中的反应时间和温度。
本发明所得材料结构:泡沫镍表面原位生长Ni3S2/NiS/MoS2/rGO纳米棒,纳米棒相互交错,在纳米棒表面具有花状毛刺结构。
本发明的优点:
(1)本发明利用了原位生长法,即活性材料直接生长到载体泡沫镍上,更加简单高效。这里泡沫镍不仅提供了Ni3S2的镍源,也充当了氧化石墨烯的还原剂。
(2)多组分硫化物丰富了氧化还原反应,提高了电容性能。
(3)石墨烯及MoS2的引入使得该电极材料的倍率性能和循环稳定性大大提高。
(4)具有条件温和、环境友好、性能优良等优点。
附图说明
图1本发明实例4制备的NMR-18-150电极材料的X-射线衍射图。
图2本发明实例4制备的NMR-18-150电极材料的扫描电子显微镜图。
图3本发明实例4制备的NMR-18-150电极材料在不同扫速下的循环伏安曲线图。
图4本发明实例4制备的NMR-18-150电极材料在不同电流密度下的恒流充放电曲线图。
图5本发明实例4制备的NMR-18-150电极材料在不同电流密度下的比电容。
图6本发明实例制备4的NMR-18-150电极材料的循环稳定性。
以下结合具体实施方式对本发明作进一步说明,但本发明的保护范围不仅限于下述实施方式。
具体实施方式
实例1
本专利采用泡沫镍(1×1cm2)作为复合材料的基底。泡沫镍在后续处理前分别用丙酮、稀盐酸、乙醇和去离子水进行超声清洗各5min。
首先,将0.014mmol(NH4)6Mo7O24·4H2O、0.18mmol CH4N2S和0.036mmol Ni(OCOCH3)2·4H2O加入18ml氧化石墨烯(GO)分散液(1mg/mL)中,通过磁力搅拌20min形成均匀溶液。将制备好的前驱体溶液转移至25mL聚四氟乙烯内衬并密封于不锈钢的反应釜中,将预处理过的泡沫镍浸入其中。反应釜加热至150℃反应18h,待第一步反应完成后自然冷却至室温。然后在上述悬浮液中加入0.014mmol(NH4)6Mo7O24·4H2O和0.18mmol CH4N2S,在反应温度150℃下维持6h进行第二次水热反应。所得产物NMR-6-150用乙醇和去离子水分别洗涤三次,并置于70℃的真空烘箱干燥12h。
对上述制备的NMR-6-150电极材料在以KOH水溶液(2mol/L)为电解液的三电极体系中进行电化学性能测试。测试结果表明:在10A/g的电流密度下,比电容可达到1236.8F/g。
实例2
在实例1的基础上,将第二次水热反应时间调整为12h,反应温度为150℃,所得产物为NMR-12-150。
电化学性能测试结果表明:在10A/g的电流密度下,比电容可达到1101.8F/g。
实例3
在实例1的基础上,将第二次水热反应时间调整为15h,反应温度为150℃,所得产物为NMR-15-150。
电化学性能测试结果表明:在10A/g的电流密度下,比电容可达到927.6F/g。
实例4
在实例1的基础上,将第二次水热反应时间调整为18h,反应温度为150℃,所得产物为NMR-18-150。
电化学性能测试结果表明:在10A/g的电流密度下,比电容可达到1846.6F/g。
实例5
在实例1的基础上,将第二次水热反应时间调整为18h,反应温度为70℃,所得产物为NMR-18-70。
电化学性能测试结果表明:在10A/g的电流密度下,比电容可达到783.8F/g。
实例6
在实例1的基础上,将第二次水热反应时间调整为18h,反应温度为110℃,所得产物为NMR-18-110。
电化学性能测试结果表明:在10A/g的电流密度下,比电容可达到803F/g。
实例7
在实例1的基础上,将第二次水热反应时间调整为18h,反应温度为190℃,所得产物为NMR-18-190。
电化学性能测试结果表明:在10A/g的电流密度下,比电容可达到1791F/g。
进一步地,对实例4中所得NMR-18-150电极材料进行表征。图1为NMR-18-150电极材料的X-射线衍射图,在21.66°、31.03°、37.60°和54.94°的特征峰对应的是Ni3S2(PDF#02-0772)的(101)、(012)、(003)和(104)晶面。在76.08°的衍射峰对应NiS(PDF#02-0693)的(431)晶面。在49.79°的衍射峰对应MoS2(PDF#06-0097)的(105)晶面。MoS2含量低,结晶性差,导致其没有主峰存在(~14.5°)。除此之外没有检测到其他衍射峰,表明复合材料中Ni3S2、NiS、MoS2的存在。图2为合成材料的扫描电子显微镜图,该复合材料的形貌呈现出表面附着了大量纳米花的棒状结构,该结构增大了比表面积,提供了大量活性位点,有利于电荷的快速转移,从而提高了电化学性能。图3为NMR-18-150电极材料在不同扫速下的循环伏安曲线图。可以看出,所有曲线均存在一对氧化还原峰,表明电极上存在氧化还原反应,根据曲线形状判断该电极为电池型材料。由于极化影响,随扫速的增加,还原峰向左偏移,氧化峰向右偏移,而曲线的形状没有明显变化,显示出良好的可逆性。该电极材料的恒流充放电测试如图4所示,所有曲线均呈现出明显的充放电平台,验证了该电极材料为电池型材料。在10A/g的电流密度下,充放电时间可以达到206s。图5为NMR-18-150在不同电流密度下的比电容,可以看到,在10A/g的电流密度下比电容高达1846.6F/g,当电流密度增加到15A/g时,比电容为1609.2F/g,容量保持率为87.14%,具有良好的倍率能力。该电极材料的循环稳定性如图6所示,在11A/g下,经过5000次充放电测试后,容量保持率为90.1%,表现出良好的稳定性。
Claims (8)
1.一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料的制备方法,其特征在于,包括以下步骤:
(1)将钼酸铵((NH4)6Mo7O24·4H2O)、硫脲(CH4N2S)和醋酸镍(Ni(OCOCH3)2·4H2O)加入氧化石墨烯(GO)分散液中,通过磁力搅拌形成均匀的前驱体溶液;
(2)将制备好的前驱体溶液转移至聚四氟乙烯内衬并密封于不锈钢的反应釜中,将预处理过的泡沫镍浸入其中,反应釜加热至150℃反应18h,待第一步反应完成后自然冷却至室温;
(3)在步骤(2)反应液中加入(NH4)6Mo7O24·4H2O和CH4N2S,在70℃~190℃温度下进行第二次水热反应,反应时间6h~18h;
(4)所得产物用乙醇和去离子水清洗,并置于70℃的真空烘箱干燥12h。
2.按照权利要求1所述的一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料的制备方法,其特征在于,所述步骤(1)中,所加的氧化石墨烯分散液浓度为1mg/mL。
3.按照权利要求1所述的一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料的制备方法,其特征在于,所述步骤(1)中,(NH4)6Mo7O24·4H2O、CH4N2S和Ni(OCOCH3)2·4H2O在石墨烯分散液中的浓度分别为0.0007-0.0008mol/L、0.01mol/L和0.002mol/L。
4.按照权利要求1所述的一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料的制备方法,其特征在于,所述步骤(2)中,所述的泡沫镍作为复合材料的基底,并在使用前分别用丙酮、稀盐酸、乙醇和去离子水超声清洗5min。
5.按照权利要求1所述的一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料的制备方法,其特征在于,所述步骤(3)中,所加入的(NH4)6Mo7O24·4H2O和CH4N2S,使得溶液体系中(NH4)6Mo7O24·4H2O、CH4N2S的浓度为0.0007-0.0008mol/L、0.01mol/L。
6.按照权利要求1所述的一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料的制备方法,其特征在于,所述步骤(4)中,所得产物分别用乙醇和去离子水清洗3次。
7.按照权利要求1所述的一种Ni3S2/NiS/MoS2/rGO超级电容器电极材料的制备方法,其特征在于,步骤(3)中第二次水热反应温度为150℃,反应时间为18h条件下,所得材料为:泡沫镍表面原位生长Ni3S2/NiS/MoS2/rGO纳米棒,纳米棒相互交错,在纳米棒表面具有花状毛刺结构。
8.按照权利要求1-7任一项所述的方法制备得到的一种材料的应用,作为超级电容器电极材料。
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