CN105753073A - 快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法 - Google Patents
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 73
- 229910052759 nickel Inorganic materials 0.000 claims description 35
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 31
- 229910052750 molybdenum Inorganic materials 0.000 claims description 31
- 239000011733 molybdenum Substances 0.000 claims description 31
- 238000005987 sulfurization reaction Methods 0.000 claims description 29
- 239000000376 reactant Substances 0.000 claims description 16
- 230000010355 oscillation Effects 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 229910019626 (NH4)6Mo7O24 Inorganic materials 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
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Abstract
本发明公开了一种快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法,该四硫化三镍/二硫化钼/石墨烯水凝胶复合物的制备方法包括以下步骤:将乙二醇加入到氧化石墨水溶液中,搅拌并超声振荡,得到均匀的分散液;步将Ni(NO3)2·6H2O和(NH4)6Mo7O24·4H2O的混合水溶液与分散液混合,搅拌形成均匀的悬浮液;将Na2S·9H2O加入到悬浮液中,搅拌形成反应液;将反应液在密闭反应釜中恒温反应、洗涤并冷冻干燥即得所述复合材料。本发明所述方法操作简单,测试方便,无需加入任何粘结剂和表面活性剂。
Description
技术领域
本发明涉及一种纳米复合材料的制备方法,特别是一种利用石墨烯水凝胶特性,快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法属于材料制备领域。
背景技术
四硫化三镍是一种立方尖晶石结构的物质,在大自然中以辉镍矿的形式存在。不管是作为锂离子电池的负极,超级电容器的电活性材料,加氢脱硫的催化剂,还是作为光催化制氢的助催化剂,四硫化三镍都表现出了优异的性能,所以,近年来引起了广大研究者的高度关注。
二硫化钼具有独特的物理、光学以及电性能,同时它具有很高的比表面积,这使得它在催化、纳米电子学、光电学、储氢、锂离子电池以及超级电容器等领域有着很好的应用。而由于其导电性高于氧化物,理论比电容高于石墨烯,二硫化钼近年来在超级电容器领域引起了很大的关注。
石墨烯是近年来发现的碳的新的同素异形体,是一种独特的二维纳米材料。由于其优异的导电性能、机械特性、良好的化学稳定性、大的长径比及较大的比表面积等,石墨烯在电子、复合材料、电池、传感器等领域具有潜在的应用前景。
采用氧化石墨烯为前驱物,利用其独特的水凝胶性质制备具有微观形貌的水凝胶纳米复合物材料,是一种新的探索。然而,关于利用石墨烯水凝胶特性制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的研究至今未见报道。
发明内容
本发明的目的在于,提出了一种利用石墨烯水凝胶性质制备了四硫化三镍/二硫化钼/石墨烯水凝胶纳米复合材料的方法。
实现本发明目的的技术解决方案为:一种快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法,包括以下步骤:
步骤一:将乙二醇加入到氧化石墨水溶液中,搅拌并超声振荡,得到均匀的分散液;
步骤二:将Ni(NO3)2·6H2O和(NH4)6Mo7O24·4H2O的混合水溶液与步骤一的分散液混合,搅拌形成均匀的悬浮液;
步骤三:将Na2S·9H2O加入到步骤二中的悬浮液中,搅拌形成反应液;
步骤四:将步骤三所得的反应液在密闭反应釜中恒温反应;
步骤五:将所得到的产物洗涤并冷冻干燥即得四硫化三镍/二硫化钼/石墨烯水凝胶复合材料。
步骤一中,乙二醇与氧化水墨水溶液的体积比为1.5~3.5,氧化水墨水溶液中,氧化石墨的浓度为2.5~5mg/ml,超声振荡时间为10~30min;
步骤二中,混合水溶液中,Ni(NO3)2·6H2O浓度为10~30mg/ml,(NH4)6Mo7O24·4H2O浓度为12~18mg/ml,混合水溶液与步骤一中的分散液的体积比为0.7~1.2;
步骤三中,Na2S·9H2O的质量与Ni(NO3)2·6H2O的质量比为2~5;
步骤四中,反应温度为120℃~180℃,反应时间为12~24h。
与现有技术相比,本发明具有以下显著优点:1、操作简单,测试方便,无需加入任何粘结剂和表面活性剂,仅通过简单的石墨烯自身的水凝胶体系即可得到四硫化三镍/二硫化钼/石墨烯水凝胶纳米复合材料;2、较好地利用了石墨烯大比表面积的特点,所得材料继承了石墨烯良好的结构,所得四硫化三镍/二硫化钼/石墨烯水凝胶材料表现出了优异的电化学性能,表明其在电化学领域具有非常广阔的应用前景。
附图说明
图1为本发明利用石墨烯水凝胶特性制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物流程示意图。
图2为本发明制备的水凝胶复合物表征图,(a)X射线衍射图片,(b)X射线光电子能谱图片,(c)透射电镜图片,(d)恒电流充放电曲线。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步详细说明。
结合图1,本发明利用水凝胶体系快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法,其特征包括以下步骤:
步骤一:将乙二醇加入到氧化石墨水溶液中,搅拌并超声振荡,得到均匀的分散液,乙二醇的用量与氧化水墨水溶液的体积比为1.5~3.5,氧化石墨的浓度为2.5~5mg/ml,超声振荡时间为10~30min;
步骤二:将Ni(NO3)2·6H2O和(NH4)6Mo7O24·4H2O的混合水溶液与步骤一中的分散液混合,搅拌形成均匀的悬浮液,Ni(NO3)2·6H2O水溶液浓度为10~30mg/ml,(NH4)6Mo7O24·4H2O水溶液浓度为12~18mg/ml;
步骤三:将Na2S·9H2O加入到步骤二中的悬浮液中,搅拌形成反应液,Na2S·9H2O的质量与Ni(NO3)2·6H2O的质量比为2~5;
步骤四:将步骤三所得的反应液在密闭反应釜中恒温反应,反应温度为120℃~180℃,反应时间为12~24h;
步骤五:将所得到的产物洗涤并冷冻干燥即得四硫化三镍/二硫化钼/石墨烯水凝胶复合材料。
实施例1:
步骤一:将25ml乙二醇加入到10ml氧化石墨水溶液(5mg/ml)中,搅拌并超声振荡20min,得到均匀的分散液;
步骤二:将30mlNi(NO3)2·6H2O(30mg/ml)和(NH4)6Mo7O24·4H2O(12mg/ml)的混合水溶液与步骤一中的分散液混合,搅拌形成均匀的悬浮液;
步骤三:将1.8gNa2S·9H2O加入到步骤二中的悬浮液中,搅拌形成反应液;
步骤四:将步骤三所得的反应液在密闭反应釜中恒温反应,反应温度为180℃,反应时间为24h;
步骤五:将所得到的产物洗涤并冷冻干燥即得四硫化三镍/二硫化钼/石墨烯水凝胶复合材料。
由X射线衍射图片2(a)和X射线光电子能谱图片2(b),确定所制得的产物为四硫化三镍/二硫化钼/石墨烯水凝胶。如透射电镜2(c)所示,可以发现四硫化三镍和二硫化钼纳米粒子均匀地负载在石墨烯片层上。经恒电流充放电曲线2(d)计算,比电容为1121F/g,表明所得产物具有较好的电化学性能,暗示了其在超级电容器领域具有较好应用前景。
实施例2:
步骤一:将15ml乙二醇加入到10ml氧化石墨水溶液(5mg/ml)中,搅拌并超声振荡20min,得到均匀的分散液;
步骤二:将30mlNi(NO3)2·6H2O(20mg/ml)和(NH4)6Mo7O24·4H2O(15mg/ml)的混合水溶液与步骤一中的分散液混合,搅拌形成均匀的悬浮液;
步骤三:将1.5gNa2S·9H2O加入到步骤二中的悬浮液中,搅拌形成反应液;
步骤四:将步骤三所得的反应液在密闭反应釜中恒温反应,反应温度为150℃,反应时间为24h;
步骤五:将所得到的产物洗涤并冷冻干燥即得四硫化三镍/二硫化钼/石墨烯水凝胶复合材料。
由恒电流充放电曲线计算,该实例得到的四硫化三镍/二硫化钼/石墨烯水凝胶复合材料比电容为783F/g。
实施例3:
步骤一:将35ml乙二醇加入到10ml氧化石墨水溶液(2.5mg/ml)中,搅拌并超声振荡10min,得到均匀的分散液;
步骤二:将30mlNi(NO3)2·6H2O(30mg/ml)和(NH4)6Mo7O24·4H2O(18mg/ml)的混合水溶液与步骤一中的分散液混合,搅拌形成均匀的悬浮液;
步骤三:将1.8gNa2S·9H2O加入到步骤二中的悬浮液中,搅拌形成反应液;
步骤四:将步骤三所得的反应液在密闭反应釜中恒温反应,反应温度为180℃,反应时间为12h;
步骤五:将所得到的产物洗涤并冷冻干燥即得四硫化三镍/二硫化钼/石墨烯水凝胶复合材料。
由恒电流充放电曲线计算,该实例得到的四硫化三镍/二硫化钼/石墨烯水凝胶复合材料比电容为948F/g。
实施例4:
步骤一:将25ml乙二醇加入到10ml氧化石墨水溶液(2.5mg/ml)中,搅拌并超声振荡10min,得到均匀的分散液;
步骤二:将30mlNi(NO3)2·6H2O(10mg/ml)和(NH4)6Mo7O24·4H2O(15mg/ml)的混合水溶液与步骤一中的分散液混合,搅拌形成均匀的悬浮液;
步骤三:将1.5gNa2S·9H2O加入到步骤二中的悬浮液中,搅拌形成反应液;
步骤四:将步骤三所得的反应液在密闭反应釜中恒温反应,反应温度为120℃,反应时间为12h;
步骤五:将所得到的产物洗涤并冷冻干燥即得四硫化三镍/二硫化钼/石墨烯水凝胶复合材料。
由恒电流充放电曲线计算,该实例得到的四硫化三镍/二硫化钼/石墨烯水凝胶复合材料比电容为975F/g。
实施例5:
步骤一:将25ml乙二醇加入到10ml氧化石墨水溶液(5mg/ml)中,搅拌并超声振荡10min,得到均匀的分散液;
步骤二:将30mlNi(NO3)2·6H2O(20mg/ml)和(NH4)6Mo7O24·4H2O(12mg/ml)的混合水溶液与步骤一中的分散液混合,搅拌形成均匀的悬浮液;
步骤三:将1.5gNa2S·9H2O加入到步骤二中的悬浮液中,搅拌形成反应液;
步骤四:将步骤三所得的反应液在密闭反应釜中恒温反应,反应温度为180℃,反应时间为18h;
步骤五:将所得到的产物洗涤并冷冻干燥即得四硫化三镍/二硫化钼/石墨烯水凝胶复合材料。
由恒电流充放电曲线计算,该实例得到的四硫化三镍/二硫化钼/石墨烯水凝胶复合材料比电容为896F/g。
本发明制备的水凝胶复合物具有优异的电化学性能和离子传输能力,且四硫化三镍与二硫化钼具有较高的变电容。该复合物有望在超级电容器领域具有良好的应用。通过简单的水凝胶体系制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物,有望使材料的性能得到进一步的提升。
Claims (5)
1.一种快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法,其特征在于,包括以下步骤:
步骤一:将乙二醇加入到氧化石墨水溶液中,搅拌并超声振荡,得到均匀的分散液;
步骤二:将Ni(NO3)2·6H2O和(NH4)6Mo7O24·4H2O的混合水溶液与步骤一的分散液混合,搅拌形成均匀的悬浮液;
步骤三:将Na2S·9H2O加入到步骤二中的悬浮液中,搅拌形成反应液;
步骤四:将步骤三所得的反应液在密闭反应釜中恒温反应;
步骤五:将所得到的产物洗涤并冷冻干燥即得四硫化三镍/二硫化钼/石墨烯水凝胶复合材料。
2.如权利要求1所述的快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法,其特征在于,步骤一中,乙二醇与氧化水墨水溶液的体积比为1.5~3.5,氧化水墨水溶液中,氧化石墨的浓度为2.5~5mg/ml,超声振荡时间为10~30min。
3.如权利要求1所述的快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法,其特征在于,步骤二中,混合水溶液中,Ni(NO3)2·6H2O浓度为10~30mg/ml,(NH4)6Mo7O24·4H2O浓度为12~18mg/ml,混合水溶液与步骤一中的分散液的体积比为0.7~1.2。
4.如权利要求1所述的快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法,其特征在于,步骤三中,Na2S·9H2O的质量与Ni(NO3)2·6H2O的质量比为2~5。
5.如权利要求1所述的快速制备四硫化三镍/二硫化钼/石墨烯水凝胶复合物的方法,其特征在于,步骤四中,反应温度为120℃~180℃,反应时间为12~24h。
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