CN103515109A - 碳包覆二氧化钛负载镍和氧化镍复合材料的超级电容器电极材料的制备方法 - Google Patents
碳包覆二氧化钛负载镍和氧化镍复合材料的超级电容器电极材料的制备方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000007772 electrode material Substances 0.000 title claims abstract description 17
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 13
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 12
- 239000002131 composite material Substances 0.000 title claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title abstract description 19
- 229910052759 nickel Inorganic materials 0.000 title abstract description 6
- 239000011248 coating agent Substances 0.000 title abstract 4
- 238000000576 coating method Methods 0.000 title abstract 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000004070 electrodeposition Methods 0.000 claims abstract description 5
- 239000010936 titanium Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 4
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 238000005253 cladding Methods 0.000 claims description 21
- 239000003990 capacitor Substances 0.000 claims description 13
- RDOUUDPRYOXGBF-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].[Ni+2] Chemical compound [O-2].[O-2].[Ti+4].[Ni+2] RDOUUDPRYOXGBF-UHFFFAOYSA-N 0.000 claims description 11
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract 2
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 abstract 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 abstract 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 16
- 239000002070 nanowire Substances 0.000 description 16
- 239000011159 matrix material Substances 0.000 description 10
- 229910044991 metal oxide Inorganic materials 0.000 description 6
- 150000004706 metal oxides Chemical class 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 239000011149 active material Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910003266 NiCo Inorganic materials 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
本发明提供的是一种碳包覆二氧化钛负载镍和氧化镍复合材料的超级电容器电极材料的制备方法。(1)将钛片,放入管式炉中,通入5%H2-N2气,在60℃下恒温两小时,再升温到800-1000℃,通入气体丙酮90min后冷却至室温得碳包覆二氧化钛纳米线阵列;(2)以碳包覆二氧化钛纳米线阵列为工作电极,铂电极为对电极,饱和甘汞电极为参比电极,以Ni(NO3)2和三乙醇胺为电解液,在电流为-0.005A cm-2至-2.5A cm-2的电流密度下电沉积5min至20min;(3)放入体积比为(95-70):(5-30)的乙醇和水为溶剂、0.1mol·L-1至1.0mol·L-1的草酸为溶质的溶液中进行原位生长1-2小时;(4)在200℃至300℃下煅烧3h至4h。采用本发明的方法制备出的超级电容器电极材料容量高、倍率性能大、循环性能好。
Description
技术领域
本发明涉及的是一种超级电容器电极材料的制备方法,具体地说是一种以原位合成的碳包覆二氧化钛负载镍和氧化镍复合材料的超级电容器电极材料的制备方法。
背景技术
随着全球经济的快速发展,化石燃料的耗尽以及越来越严重的环境问题,对于有效,清洁和可持续发展的清洁能源越来越为迫切。近年来,超级电容器(Supercapacitor)吸引了大量的关注,主要是由于他们的高功率密度大,生命周期长,能够弥补传统介电电容器(具有高功率输出)容量小和电池、燃料电池(具有高能量储存)功率密度低的缺点。传统的超级电容器电极的制备方法,是将活性物质粉末与粘结剂混合成糊状,然后涂覆在基体上(碳布、碳纸、泡沫镍),这种方法制备的电极由于粘结剂的存在会导致较低的导电性,而且部分活性物质不能与电解液接触从而成为“死面积”。为了解决这个问题,近年来,具有三维立体结构的纳米材料作为超级电容器的电极引起了广泛的研究。这种结构的电极可以使活性物质充分的接触电解液,并且一些特殊的纳米形貌也可以增加电极表面积,从而促进电荷的传递,利于能量的储存。一般来讲,超级电容器的电极材料主要包括金属氧化物、金属氢氧化物以及导电高分子聚合物等,可以发生大量的氧化还原反应。其中RuO2是引起广泛关注的超级电容器电极材料,然而由于其昂贵的价格和Ru元素的稀缺极大程度地阻碍了其大范围的应用。在这些可以应用的超级电容器电极材料中,金属氧化物(如Co3O4、MnO2、NiO、Fe3O4等)由于比传统的含碳材料具有较高的比电容得到了大量的研究。但是金属氧化物具有导电性差等弱点。可参阅C.Yuan,L.Yang,L.Hou,L.Shen,F.Zhang,D.Li,X.Zhang,Large-scale Co3O4nanoparticles growing on nickel sheets via a one-step strategy and their ultra-highly reversible redox reaction toward supercapacitors.Journal of Materials Chemistry,21(2011)18183-18185.以及L.Yu,G.Zhang,C.Yuan,X.W.Lou,Hierarchical NiCo2O4MnO2core–shell heterostructured nanowire arrays on Ni foam as high-performance supercapacitor electrodes,Chemical Communications,49(2013)137-139。
发明内容
本发明的目的在于提供一种能够制备出容量高、倍率性能大、循环性能好的超级电容器电极材料的碳包覆二氧化钛负载镍和氧化镍复合材料的超级电容器电极材料的制备方法。
本发明的目的是这样实现的:
(1)将1cm×10cm的钛片,放入管式炉中,通入5%H2-N2气,以升温速率为5-10℃/min,在60℃下恒温两小时,再升温到800-1000℃,通入气体丙酮90min后冷却至室温,以制备碳包覆二氧化钛(CTiO2)纳米线阵列;(2)以碳包覆二氧化钛纳米线阵列为工作电极,铂电极为对电极,饱和甘汞电极为参比电极,以0.05mol·L-1至0.5mol·L-1的Ni(NO3)2和0.1mol·L-1至2.0mol·L-1的三乙醇胺为电解液,在电流为-0.005A cm-2至-2.5A cm-2的电流密度下电沉积5min至20min;(3)将步骤(2)所的产物放入体积比为(95-70):(5-30)的乙醇和水为溶剂、0.1mol·L-1至1.0mol·L-1的草酸为溶质的溶液中进行原位生长1-2小时;(4)将步骤(3)所的产物在200℃至300℃下煅烧3h至4h,制得碳包覆二氧化钛负载镍和氧化镍(Ni-NiOCTiO2)复合材料的超级电容器电极材料。
本发明是以具有三维立体开放结构的碳包覆二氧化钛(CTiO2)纳米线阵列为基体,以Ni盐溶液为沉积母液,利用电沉积技术,将镍薄膜沉积在的基体上,然后将其放入生长溶液中进行原位生长一段时间,最后通过在空气中煅烧形成碳包覆二氧化钛负载镍和氧化镍(Ni-NiOCTiO2)复合电极材料。
本发明的实质是以原位合成的碳包覆二氧化钛负载镍和氧化镍(Ni-NiOCTiO2)复合材料取代RuO2等电极材料,以2-6M KOH为电解质,采用金属氧化物超级电容器的结构组成金属氧化物超级电容器。电极反应为:NiO+OH- NiOOH+e-。
本发明的优点是:Ti片载TiO2纳米阵列基体机械力学性能好,包覆碳后的碳包覆二氧化钛(CTiO2)纳米线阵列的导电性好,Ni-NiO纳米线通过原位技术再直接生长在CTiO2纳米线基体上,形成纳米线阵列上再长纳米线的独特结构。这种电极的结构是三维立体结构,不使用粘结剂和导电剂;可以使活性物质充分与电解液接触,有效地增加了电子/离子的传递。CTiO2纳米线阵列的C包覆层和Ni-NiO纳米线中的Ni的导电性好,克服了金属氧化物差的缺点,制备出容量高、倍率性能大、循环性能好的超级电容器电极。
具体实施方式
下面举例对本发明做更详细的描述。
(1)剪取1cm×10cm的钛片,放入管式炉中,通入5%H2-N2气,以升温速率为8℃/min,在60℃下恒温两小时,再升温到800-1000℃,通入气体丙酮90min后冷却至室温,以制备CTiO2纳米线阵列基体。(2)以CTiO2纳米线阵列为工作电极,铂电极为对电极,饱和甘汞电极为参比电极,以0.1mol·L-1的Ni(NO3)2和1.0mol·L-1的三乙醇胺为电解液,组成三电极体系。在电流为-1.0A cm-2的电流密度下电沉积5min至20min。(3)将沉积好的镍膜放 入体积比为(95-70):(5-30)的乙醇和水为溶剂,0.1mol·L-1至1.0mol·L-1的草酸为溶质的溶液中进行原位生长1-2小时。(4)最后将所制备的电极在200℃至300℃下煅烧3h至4h。即制备了原位合成的Ni-NiOCTiO2复合电极材料。
为了更好地说明本发明的效果,下面以具体应用实例加以说明。
应用实例1
将碳包覆二氧化钛(CTiO2)纳米线阵列作为基体在0.25mol·L-1NiSO4+70mL·L-1三乙醇胺沉积液中,恒定电流-0.010A·cm-2,沉积20min,得到金属Ni膜。在含有0.3mol L-1H2C2O4,5%H2O的混合溶液中浸泡3h,浸泡温度为45℃。然后将制备的样品放入马弗炉中,空气中煅烧1h,煅烧温度为300℃,得到最终的碳包覆二氧化钛负载镍和氧化镍(Ni-NiOCTiO2)电极。在2.0mol·L-1KOH中进行不同电流下的充放电测试。结果表明,在100A·g-1的充放电电流下,比容量高达811.1F·g-1。
应用实例2
将碳包覆二氧化钛(CTiO2)纳米线阵列作为基体在0.25mol·L-1NiSO4+70mL·L-1三乙醇胺沉积液中,恒定电流-0.010A·cm-2,沉积10min,得到金属Ni膜。在含有0.3mol·L-1H2C2O4,5%H2O的混合溶液中浸泡3h,浸泡温度为45℃。然后将制备的样品放入马弗炉中,空气中煅烧1.5h,煅烧温度为250℃,得到最终的碳包覆二氧化钛负载镍和氧化镍(Ni-NiOCTiO2)电极。在2.0mol·L-1KOH中进行不同电流下的充放电测试。结果表明,在10A·g-1的充放电电流下,比容量高达1018.4F·g-1。
应用实例3
将碳包覆二氧化钛(CTiO2)纳米线阵列作为基体在0.25mol·L-1NiSO4+70mL·L-1三乙醇胺沉积液中,恒定电压-0.2V,沉积15min,得到金属Ni膜。在含有0.5mol·L-1H2C2O4,70%H2O的混合溶液中浸泡2h,浸泡温度为35℃。然后将制备的样品放入马弗炉中,空气中煅烧2h,煅烧温度为200℃,得到最终的Ni-NiOCTiO2电极。在2.0mol·L-1KOH中进行不同电流下的充放电测试。结果表明,在10A·g-1的充放电电流下,比容量高达1219F·g-1。
应用实例4
将碳包覆二氧化钛(CTiO2)纳米线阵列作为基体在0.25mol·L-1NiSO4+70mL·L-1三乙醇胺沉积液中,恒定电压-0.2V,沉积20min,得到金属Ni膜。在含有0.5mol·L-1H2C2O4,10%H2O的混合溶液中浸泡2.5h,浸泡温度为45℃。然后将制备的样品放入马弗炉中,空气中煅烧2h,煅烧温度为250℃,得到最终的碳包覆二氧化钛负载镍和氧化镍(Ni-NiOCTiO2)电极。在2.0mol·L-1KOH中进行不同电流下的充放电测试。结果表明,在20A·g-1的充放电电流下,比容量高达1021F·g-1。
Claims (1)
1.一种碳包覆二氧化钛负载镍和氧化镍复合材料的超级电容器电极材料的制备方法,其特征是:(1)将1cm×10cm的钛片,放入管式炉中,通入5%H2-N2气,以升温速率为5-10℃/min,在60℃下恒温两小时,再升温到800-1000℃,通入气体丙酮90min后冷却至室温,以制备碳包覆二氧化钛纳米线阵列;(2)以碳包覆二氧化钛纳米线阵列为工作电极,铂电极为对电极,饱和甘汞电极为参比电极,以0.05mol·L-1至0.5mol·L-1的Ni(NO3)2和0.1mol·L-1至2.0mol·L-1的三乙醇胺为电解液,在电流为-0.005A cm-2至-2.5A cm-2的电流密度下电沉积5min至20min;(3)将步骤(2)所的产物放入体积比为(95-70):(5-30)的乙醇和水为溶剂、0.1mol·L-1至1.0mol·L-1的草酸为溶质的溶液中进行原位生长1-2小时;(4)将步骤(3)所的产物在200℃至300℃下煅烧3h至4h,制得碳包覆二氧化钛负载镍和氧化镍复合材料的超级电容器电极材料。
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CN104383942A (zh) * | 2014-11-13 | 2015-03-04 | 三明学院 | 一种核壳结构的C@TiO2固体酸催化剂及其制备方法 |
CN104616910A (zh) * | 2015-01-09 | 2015-05-13 | 东南大学 | 碳包覆钛基纳米阵列材料及其制备方法和应用 |
CN105448536A (zh) * | 2015-11-26 | 2016-03-30 | 合肥工业大学 | 氧化镍/氧化钛纳米复合材料及其制备方法和储能应用 |
CN107895655A (zh) * | 2017-10-26 | 2018-04-10 | 燕山大学 | 一种超级电容器用多层结构二氧化钛电极及其制备方法 |
CN113380994A (zh) * | 2021-04-26 | 2021-09-10 | 厦门大学 | 一种无粘结剂、含氧缺陷的碳包覆氧化物电极及电池 |
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CN104201004A (zh) * | 2014-07-26 | 2014-12-10 | 渤海大学 | 柔性混合超级电容器电极的制备方法 |
CN104201004B (zh) * | 2014-07-26 | 2017-03-22 | 渤海大学 | 柔性混合超级电容器电极的制备方法 |
CN104383942A (zh) * | 2014-11-13 | 2015-03-04 | 三明学院 | 一种核壳结构的C@TiO2固体酸催化剂及其制备方法 |
CN104616910A (zh) * | 2015-01-09 | 2015-05-13 | 东南大学 | 碳包覆钛基纳米阵列材料及其制备方法和应用 |
CN105448536A (zh) * | 2015-11-26 | 2016-03-30 | 合肥工业大学 | 氧化镍/氧化钛纳米复合材料及其制备方法和储能应用 |
CN105448536B (zh) * | 2015-11-26 | 2018-05-25 | 合肥工业大学 | 氧化镍/氧化钛纳米复合材料及其制备方法和储能应用 |
CN107895655A (zh) * | 2017-10-26 | 2018-04-10 | 燕山大学 | 一种超级电容器用多层结构二氧化钛电极及其制备方法 |
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CN113380994A (zh) * | 2021-04-26 | 2021-09-10 | 厦门大学 | 一种无粘结剂、含氧缺陷的碳包覆氧化物电极及电池 |
CN113380994B (zh) * | 2021-04-26 | 2022-10-11 | 厦门大学 | 一种无粘结剂、含氧缺陷的碳包覆氧化物电极及电池 |
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