CN106920697A - 一种RGO和MoS2复合纳米纸、制备方法及其应用 - Google Patents
一种RGO和MoS2复合纳米纸、制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种RGO和MoS2复合纳米纸、制备方法及其应用,属于超级电容器电极材料制造技术领域,本发明采用超声剥离GO和MoS2纳米片,再将纳米片混合溶液进行抽滤,最后高温真空还原得到RGO和MoS2复合纳米纸,其表现出高体积比容量(在1A g‑1电流密度下体积比容量为787.1F cm‑3)。RGO和MoS2复合纳米纸组装的水系和有机系对称超级电容器,表现出较好的循环稳定性及较高的能量密度和功率密度,能量密度分别为7.6mWh cm‑3和25.8mWh cm‑3,功率密度分别为3.64W cm‑3和14.05W cm‑3,分别循环480000和270000次比容量均能保留100.0%。这些结果都证明RGO与MoS2复合纳米纸能成为超级电容器电极材料。
Description
技术领域
本发明属于超级电容器电极材料制造技术领域,具体涉及一种RGO和MoS2复合纳米纸、制备方法及其应用。
背景技术
二维石墨烯和类石墨烯材料由于大的比表面积,而有望成为超级电容器电极材料。在类石墨烯材料中,MoS2是一种典型二维层状过渡金属硫化物,具有大的层间距、高电化学活性和良好的化学稳定性。MoS2纳米片间大的层间距存在弱范德华力,有利于阳离子(H+、K+、Li+)的嵌入。通常,MoS2是2H相的半导体材料,它的导电性很差,在超级电容器电极充放电过程中表现出差的倍率性能和循环稳定性。目前,通过设计不同纳米结构和与其它导电性较好的材料进行复合来解决上述问题,例如和导电聚合、碳纳米管、无定型碳、碳纤维、石墨烯的复合。然而,在大的电流密度下,MoS2电极表现差的循环性能和倍率性能,且报道MoS2复合物超级电容器电极材料的工作也不多。二维多孔的RGO结构能增加MoS2电极的循环性能和倍率性能,主要是因为MoS2和RGO复合结构能形成三维的通道促进电解质离子的转移,而且多孔的RGO网能提供高导电性。
发明内容
为了克服现有机械剥离MoS2电极导电性差的问题,本发明采用超声剥离GO和MoS2纳米片,再将纳米片混合溶液进行抽滤薄膜,最后真空还原得到RGO和MoS2复合纳米纸,其表现出高体积比容量(在1Ag-1电流密度下体积比容量为787.1F cm-3)。RGO和MoS2复合纳米纸组装的水系和有机系对称超级电容器,能量密度分别为7.6mWh cm-3和25.8mWh cm-3,功率密度分别为3.64W cm-3和14.05W cm-3,分别循环480000和270000次比容量均能保留100.0%。这些结果都证明RGO与MoS2复合纳米纸能成为超级电容器电极材料。
本发明的上述目的通过以下技术方案实现:
一种RGO和MoS2复合纳米纸的制备方法,具体步骤如下:
S1.水热法制备MoS2纳米片:称取Na2MoO4·6H2O和CH3CSNH2加入到一定体积的去离子水中,混合均匀,再进行水热反应,然后冷却至室温并清洗样品,于60℃干燥24h,得到MoS2纳米片;其中,Na2MoO4·6H2O的质量为0.06~0.18g,CH3CSNH2的质量为0.18~0.36g;
S2.剥离MoS2纳米片:称取S1中的MoS2纳米片粉末加入到一定体积的去离子水中,探针超声,得到分散均匀的MoS2纳米片水溶液;其中,MoS2纳米片粉末的质量为0.01~0.08g,去离子水的体积为40~80mL;
S3.剥离GO纳米片:称取一定量的GO纳米片粉末加入到一定体积的去离子水中,探针超声,得到分散均匀的GO纳米片水溶液;其中,GO纳米片粉末的质量为0.03~0.09g,去离子水的体积为40~80mL;
S4.抽滤制备GO和MoS2复合纳米纸:将S2中MoS2纳米片水溶液和S3中GO纳米片水溶液按照体积比为1:1~1:10混合均匀,探针超声,真空抽滤GO和MoS2的混合溶液,自然干燥,剥下滤膜上的薄膜,得到GO和MoS2复合纳米纸;
S5.热还原制备RGO和MoS2复合纳米纸:将S4中的GO和MoS2复合纳米纸在真空下加热还原,得到RGO和MoS2复合纳米纸。
进一步地,步骤S1中所述去离子水体积为为30~60mL。
进一步地,步骤S1中所述水热反应温度为150~200℃,水热反应时间为18~36h。
进一步地,步骤S2、S3及S4中所述超声功率为500~1000W,超声时间为30~90min。
进一步地,步骤S4中所述干燥时间为24~72h。
进一步地,步骤S5所述加热温度为300~500℃,加热时间为3~9h。
本发明的另一个目的是提供一种RGO和MoS2复合纳米纸在超级电容器电极方面的应用,具体如下:
在组装水系RGO/MoS2//RGO/MoS2对称型超级电容器方面的应用:在3MKOH溶液中以RGO和MoS2复合纳米纸贴泡沫镍上为电极及纤维素隔膜所组装成水系对称型超级电容器。其在3M KOH溶液中和1A g-1电流密度下表现高质量比容量378.1F g-1、体积比容量787.1Fcm-3,在电流密度0.5A g-1表现出高能量密度7.6mWh cm-3,在5A g-1电流密度下表现出高功率密度3.64W cm-3,在5A g-1电流密度下循环480000次比容量仍能保留100.0%。
在组装有机系RGO/MoS2//RGO/MoS2对称型超级电容器方面的应用:在1MMeEt3NBF4-AN溶液中以RGO和MoS2复合纳米纸贴在铝箔上为电极及纤维素隔膜所组装成有机系对称型超级电容器。其在电流密度0.5A g-1下得到高能量密度25.8mWh cm-3,在5A g-1电流密度下得到高功率密度14.05W cm-3,在5A g-1电流密度下循环270000次比容量仍能保留100.0%。
与现有技术相比,本发明的优点如下:
(1)选用RGO和MoS2作电极材料,资源丰富、电化学反应活性位多、极高比容量;
(2)选超声剥离和抽滤技术,工艺简单、操作简便;
(3)本发明的RGO和MoS2复合纳米纸在电流密度1A g-1下能得到高体积比容量787.1F cm-3、高质量比容量378.1F g-1;
(4)本发明的水系RGO/MoS2//RGO/MoS2对称型超级电容器的能量密度高达7.6mWhcm-3,功率密度高达3.64W cm-3,在5A g-1电流密度下循环480000次比容量仍能保留100.0%;
(5)本发明的有机系RGO/MoS2//RGO/MoS2对称型超级电容器能量密度高达25.8mWhcm-3,功率密度高达14.05W cm-3,在5A g-1电流密度下循环270000次比容量仍能保留100.0%。
附图说明
图1为实施例1及2步骤S2中MoS2纳米片的质量与RGO和MoS2复合纳米纸比容量关系图;
图2为实施例1中RGO和MoS2复合纳米纸的质量比容量和体积比容量与电流密度关系图;
图3为实施例1中水系RGO/MoS2//RGO/MoS2对称型超级电容器功率密度与能量密度关系图;
图4为实施例1中水系RGO/MoS2//RGO/MoS2对称型超级电容器在5A g-1电流密度下480000次循环寿命图;
图5为实施例1中有机系RGO/MoS2//RGO/MoS2对称型超级电容器功率密度与能量密度关系图;
图6为实施例1中有机系RGO/MoS2//RGO/MoS2对称型超级电容器在5Ag-1电流密度下270000次循环寿命图;
图7a为本发明实施例1中RGO和MoS2复合纳米纸的平面扫描电子扫描显像图,b为本发明实施例1中RGO和MoS2复合纳米纸的截面扫描电子扫描显像图。
具体实施方式
下面结合说明书附图和具体实施例对本发明作出进一步地详细阐述,但实施例并不对本发明做任何形式的限定。
实施例1
一种RGO和MoS2复合纳米纸制备方法及其应用,包含抽滤GO和MoS2复合纳米纸、组装水系RGO/MoS2//RGO/MoS2对称型超级电容器、组装有机系RGO/MoS2//RGO/MoS2对称型超级电容器,包括以下步骤:
S1.水热法制备MoS2纳米片:称取0.12gNa2MoO4·6H2O和0.24gCH3CSNH2加入到40mL的去离子水中,混合均匀,倒入反应釜内衬中,拧紧反应釜外的不锈钢瓶200℃水热反应24h,待反应釜冷却后清洗样品,并60℃干燥24h,得到MoS2纳米片;
S2.剥离MoS2纳米片:称取S1中的0.0125g MoS2纳米片粉末加入到一定75mL的去离子水中,800W探针超声60min,得到分散均匀的MoS2纳米片水溶液;
S3.剥离GO纳米片:称取常州第六元素材料科技股份有限公司的0.06g GO加入到一定75mL的去离子水中,800W探针超声60min,得到分散均匀的GO纳米片水溶液;
S4.抽滤制备GO和MoS2复合纳米纸:将S2中15mL MoS2纳米片水溶液和S3中15mL GO纳米片水溶液混合均匀,800W探针超声60min,在滤膜上真空抽滤GO和MoS2的混合溶液,自然干燥72h,轻轻剥下滤膜上的薄膜,得到GO和MoS2复合纳米纸;
S5.热还原制备RGO和MoS2复合纳米纸:将S4中的GO和MoS2复合纳米纸在真空下300℃加热5h还原,得到RGO和MoS2复合纳米纸;
一种RGO和MoS2复合纳米纸在超级电容器方面的应用,具体如下:
组装水系RGO/MoS2//RGO/MoS2对称型超级电容器:在3M KOH溶液中以RGO和MoS2复合纳米纸贴在泡沫镍上为电极及纤维素隔膜所组装成水系对称型超级电容器。
组装有机系RGO/MoS2//RGO/MoS2对称型超级电容器:在1MMeEt3NBF4-AN溶液中以RGO和MoS2复合纳米纸贴在铝箔上为电极及纤维素隔膜所组装成有机系对称型超级电容器。
实施例2
除了步骤S2中MoS2纳米片的质量分别为0.0250g、0.0375g、0.0500g、0.0625g及0.0000g之外,其他条件同实施例1;
所添加不同MoS2质量对RGO和MoS2复合纳米纸比容量的影响如图1所示;从图中可以看出,在电流密度5A g-1下,添加不同的MoS2质量0、0.0125、0.0250、0.0375、0.0500、0.0625g,分别得到RGO和MoS2复合纳米纸的比容量为155.0、232.1、145.0、101.4、82.1、55.7F g-1。说明过多的添加半导体MoS2质量,减弱了RGO和MoS2复合纳米纸导电性,阻碍了电子的转移,使电极的比容量降低。
实施例1中RGO和MoS2复合纳米纸的质量比容量和体积比容量与电流密度关系如图2所示,从图中可以看出,在不同的电流密度1、2、3、4、5A g-1下,质量比容量分别是378.1、248.6、227.6、217.7、212.1F g-1,体积比容量分别是787.1、517.4、473.7、453.2、441.6Fcm-3。在低的电流密度下,电极的欧姆电压降很低,这是因为电极材料中的活性位点能得到充分利用,有助于电极获得高比容量。
实施例1中水系RGO/MoS2//RGO/MoS2对称型超级电容器功率密度与能量密度如图3所示,从图中可以看出,水系RGO/MoS2//RGO/MoS2对称型超级电容器功率密度为0.36W cm-3、0.73W cm-3、1.46W cm-3、2.19W cm-3、2.91W cm-3、3.64W cm-3分别对应的能量密度为7.6mWh cm-3、6.9mWh cm-3、6.5mWh cm-3、6.3mWh cm-3、6.2mWh cm-3、6.2mWh cm-3。在相同功率密度下高于活性炭水系对称超级电容器(<4mWh cm-3)(Y.Tao,X.Xie,W.Lv,D.M.Tang,D.Kong,Z.Huang,H.Nishihara,T.Ishii,B.Li,D.Golberg,F.Kang,T.Kyotani,Q.H.Yang,Towards ultrahigh volumetric capacitance:graphene derived highly dense butporous carbons for supercapacitors,Scientific reports,2013,3:2975.)、CoO@PPy//AC水系非对称超级电容器(<3mWh cm-3)(C.Zhou,Y.Zhang,Y.Li,J.Liu,Construction ofhigh-capacitance 3D CoO@polypyrrole nanowire array electrode for aqueousasymmetric supercapacitor,Nano letters,2013,13(5):2078-2085.)、石墨烯水系对称超级电容器(<1mWh cm-3)(M.F.El-Kady,V.Strong,S.Dubin,R.B.Kaner,Laser scribingof high-performance and flexible graphene-based electrochemical capacitors,Science,2012,335(6074):1326-1330.)。
实施例1中水系RGO/MoS2//RGO/MoS2对称型超级电容器5A g-1电流密度下480000次循环寿命如图4所示,从图中可以看出,在5A g-1电流密度下循环480000次,比容量仍能保持100.0%,表现良好的循环稳定性;库伦效率一直接近100%,表明器件在整个循环过程中发生的电化学反应是可逆的。
实施例1中有机系RGO/MoS2//RGO/MoS2对称型超级电容器功率密度与能量密度如图5所示,从图中可以看出,有机系RGO/MoS2//RGO/MoS2对称型超级电容器功率密度为1.41Wcm-3、2.81W cm-3、5.62W cm-3、8.43W cm-3、11.24W cm-3、14.05W cm-3分别对应的能量密度为25.8mWh cm-3、23.7mWh cm-3、20.3mWh cm-3、17.8mWh cm-3、15.9mWh cm-3、14.1mWh cm-3。在相同功率密度下高于锂薄膜电池(<9mWh cm-3)(Z.S.Wu,K,Parvez,X.Feng,K,Müllen,Graphene-based in-plane micro-supercapacitors with high power and energydensities,Nature communications,2013,4:2487.)、d-Ti3C2对称超级电容器(<1mWh cm-3)(M.R.Lukatskaya,O.Mashtalir,C.E.Ren,Y.Dall’Agnese,P.Rozier,Cationintercalation and high volumetric capacitance of two-dimensional titaniumcarbide,Science,2013,341(6153):1502-1505.)、石墨烯有机系对称超级电容器(<13mWhcm-3)(X.Yang,C.Cheng,Y.Wang,L.Qiu,D.Li,Liquid-mediated dense integration ofgraphene materials for compact capacitive energy storage,science,2013,341(6145):534-537.)。
实施例1中有机系RGO/MoS2//RGO/MoS2对称型超级电容器5A g-1电流密度下270000次循环寿命如图6所示,从图中可以看出,在5A g-1电流密度下循环270000次,比容量仍能保持100.0%,表现良好的循环稳定性;库伦效率一直接近100%,表明器件在整个循环过程中发生的电化学反应是可逆的。
实施例1中RGO和MoS2复合纳米纸的平面和截面扫描电子扫描显像图分别如图7a、b所示,从图7a中可以看出,RGO和MoS2复合纳米纸有很多突起的纳米片,能提供大的比表面积,促进电解质离子的进入。从图7b中可以看出,RGO和MoS2复合纳米纸的平均厚度约为1.74μm,且是叠层结构,能增加电极的循环稳定性。
Claims (8)
1.一种RGO和MoS2复合纳米纸的制备方法,其特征在于,具体步骤如下:
S1.水热法制备MoS2纳米片:称取Na2MoO4·6H2O和CH3CSNH2加入到一定体积的去离子水中,混合均匀,再进行水热反应,然后冷却至室温并清洗样品,于60℃干燥24h,得到MoS2纳米片;其中,Na2MoO4·6H2O的质量为0.06~0.18g,CH3CSNH2的质量为0.18~0.36g;
S2.剥离MoS2纳米片:称取S1中的MoS2纳米片粉末加入到一定体积的去离子水中,探针超声,得到分散均匀的MoS2纳米片水溶液;其中,MoS2纳米片粉末的质量为0.01~0.08g,去离子水的体积为40~80mL;
S3.剥离GO纳米片:称取一定量的GO纳米片粉末加入到一定体积的去离子水中,探针超声,得到分散均匀的GO纳米片水溶液;其中,GO纳米片粉末的质量为0.03~0.09g,去离子水的体积为40~80mL;
S4.抽滤制备GO和MoS2复合纳米纸:将S2中MoS2纳米片水溶液和S3中GO纳米片水溶液按照体积比为1:1~1:10混合均匀,探针超声,真空抽滤GO和MoS2的混合溶液,自然干燥,剥下滤膜上的薄膜,得到GO和MoS2复合纳米纸;
S5.热还原制备RGO和MoS2复合纳米纸:将S4中的GO和MoS2复合纳米纸在真空下加热还原,得到RGO和MoS2复合纳米纸。
2.如权利要求1所述一种RGO和MoS2复合纳米纸的制备方法,其特征在于,步骤S1中所述去离子水体积为30~60mL。
3.如权利要求1所述一种RGO和MoS2复合纳米纸的制备方法,其特征在于,步骤S1中所述水热反应温度为150~200℃,水热反应时间为18~36h。
4.如权利要求1所述一种RGO和MoS2复合纳米纸的制备方法,其特征在于,步骤S2、S3及S4中所述超声功率为500~1000W,超声时间为30~90min。
5.如权利要求1所述一种RGO和MoS2复合纳米纸的制备方法,其特征在于,步骤S4中所述干燥时间为24~72h。
6.如权利要求1所述一种RGO和MoS2复合纳米纸的制备方法,其特征在于,步骤S5所述加热温度为300~500℃,加热时间为3~9h。
7.一种RGO和MoS2复合纳米纸,其特征在于,由如权利要求1-6的任何一项方法制备得到。
8.权利要求7所述一种RGO和MoS2复合纳米纸在超级电容器电极方面的应用。
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