CN108269694A - 聚苯胺/氢氧化钴超级电容器复合电极材料的制备方法 - Google Patents
聚苯胺/氢氧化钴超级电容器复合电极材料的制备方法 Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 28
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 28
- 239000003990 capacitor Substances 0.000 title claims abstract description 27
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 title claims abstract description 25
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000178 monomer Substances 0.000 claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 27
- 239000003792 electrolyte Substances 0.000 claims abstract description 24
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 19
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000002500 ions Chemical class 0.000 claims abstract description 9
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 5
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 22
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 22
- 229940011182 cobalt acetate Drugs 0.000 description 18
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 18
- 239000000203 mixture Substances 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910020630 Co Ni Inorganic materials 0.000 description 1
- 229910002440 Co–Ni Inorganic materials 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
本发明公开了一种聚苯胺/氢氧化钴超级电容器复合电极材料的制备方法。在钴离子的浓度为0.1~2M的水溶液中加入苯胺单体,室温搅拌2h直至苯胺单体完全溶解,制得电解液,取50mL电解液置入电解槽,以压实碳纸或者石墨烯纸为工作电极和对电极,饱和甘汞电极为参比电极,配置三电极体系,以5~2000mV/s的扫描速率在‑1V~1V之间对体系进行循环伏安扫描100~10000圈,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,最后在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。本发明方法制备过程简单、环保、可靠,原料来源广泛、成本低廉,适合工业化生产,且所得的电极材料兼具高电导率和高的电容量,是一种理想的超级电容器电极材料。
Description
技术领域
本发明涉及一种用电化学沉积制备聚苯胺/氢氧化钴超级电容器复合电极材料的办法,具体的来说,涉及一种聚苯胺/氢氧化钴超级电容器复合电极材料的制备方法。
背景技术
聚苯胺作为一种常见的导电聚合物,由于其制备简单,成本低廉,以及具有良好的环境稳定性和独特的物理和化学性质,常常被用于超级电容器、电池、传感器以及防腐领域,得到了世界各国科研工作者的大力关注。特别是具有纳米结构的导电聚苯胺,由于其粒径极小、比表面积大、极快的电子转移速率等性质,赋予了纳米导电聚苯胺材料具有传统块体所不具备的许多独特性能。
氢氧化钴作为一种超级电容器的电极材料,因为能够提供赝电容,在碱性电解质中特定容量高、稳定性好等特点,成为碱性超级电容器电极材料的研究热点。层状的双氢氧化物(Layered Double Hydroxide,简称 LDHs),有着独特的层状结构,在化学传感器、电催化、超级电容器中,都有广泛的应用研究。((a) Chen, J.; Xu, J.; Zhou, S.; Zhao, N.;Wong, C. P., Amorphous nanostructured FeOOH and Co–Ni double hydroxides forhigh-performance aqueous asymmetric supercapacitors. Nano Energy 2016, 21,145-153; (b) Wang, L.; Feng, X.; Ren, L.; Piao, Q.; Zhong, J.; Wang, Y.; Li,H.; Chen, Y.; Wang, B., Flexible Solid-State Supercapacitor Based on a Metal-Organic Framework Interwoven by Electrochemically-Deposited PANI. Journal ofthe American Chemical Society 2015, 137 (15).)
虽然氢氧化钴作为超级电容器电极在容量上虽然比较有优势,但是一般电化学窗口比较窄和导电性较差。聚苯胺在复合电极之中可以起到拓宽电化学窗口和增强导电性的作用。本发明以苯胺单体和钴盐水溶液为电解液,通过循环伏安的办法在同一电极上同时进行阳极沉积聚苯胺和阴极沉积氢氧化钴,是一种简单且环保的制备方法,所得复合材料结构规整且具有良好的电化学性能,是一种理想的超级电容器电极材料,尤其是适合工业化生产。
发明内容
本发明的目的是提供一种聚苯胺/氢氧化钴超级电容器复合电极材料的制备方法。
具体步骤为:
(1)在钴离子的浓度为0.1~2M的水溶液中加入苯胺单体,室温搅拌2h直至苯胺单体完全溶解,制得电解液。
(2)取50mL步骤(1)制得的电解液置入电解槽,以压实碳纸或者石墨烯纸为工作电极和对电极,饱和甘汞电极为参比电极,配置三电极体系,以5~2000mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描100~10000圈。
(3)反应结束后,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,最后在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
所述苯胺单体与钴离子的物质的量之比为0.1~5:1。
本发明方法制备过程简单、环保、可靠,原料来源广泛、成本低廉,适合工业化生产。所制得的聚苯胺/氢氧化钴超级电容器复合电极材料兼具高电导率和高的电容量,有着更大的电化学窗口、更高的比电容,是一种理想的超级电容器电极材料。
附图说明
图1是本发明实施例5中制备过程的电沉积曲线。
图2是本发明实施例5中制得的聚苯胺/氢氧化钴超级电容器复合电极材料的扫描电镜图。
图3是本发明实施例5中制得的聚苯胺/氢氧化钴超级电容器复合电极材料在氢氧化钾溶液中的循环伏安图。
图4是本发明实施例5中制得的聚苯胺/氢氧化钴超级电容器复合电极材料在氢氧化钾溶液中的恒电流充放电图。
具体实施方式
实施例1:
(1)配置100ml 0.2M的硝酸钴水溶液,加入苯胺单体至苯胺单体浓度为0.02M。室温搅拌2h直至苯胺单体完全溶解,制得电解液。
(2)取50ml步骤(1)制得的电解液置入电解槽,以1×4cm2压实碳纸为工作电极和对电极。饱和甘汞电极为参比电极,配置三电极体系,以100mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描150圈。
(3)反应结束后,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
实施例2:
(1)配置100ml 0.2M的硝酸钴水溶液,加入苯胺单体至苯胺单体浓度为0.04M。室温搅拌2h直至苯胺单体完全溶解,制得电解液。
(2)取50ml步骤(1)制得的电解液置入电解槽,以1×4cm2压实碳纸为工作电极和对电极。饱和甘汞电极为参比电极,配置三电极体系,以100mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描150圈。
(3)反应结束后,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
实施例3:
(1)配置100ml 0.2M的硝酸钴水溶液,加入苯胺单体至苯胺单体浓度为0.05M。室温搅拌2h直至苯胺单体完全溶解,制得电解液。
(2)取50ml步骤(1)制得的电解液置入电解槽,以1×4cm2压实碳纸为工作电极和对电极。饱和甘汞电极为参比电极,配置三电极体系,以100mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描150圈。
(3)反应结束后,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
实施例4:
(1)配置100ml 0.2M的硝酸钴水溶液,加入苯胺单体至苯胺单体浓度为0.1M。室温搅拌2h直至苯胺完全溶解,制得电解液。
(2)取50ml步骤(1)制得的电解液置入电解槽,以1×4cm2压实碳纸为工作电极和对电极。饱和甘汞电极为参比电极,配置三电极体系,以100mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描150圈。
(3)反应结束后,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
实施例5:
(1)配置100ml 0.2M的硝酸钴水溶液,加入苯胺单体至苯胺单体浓度为0.2M。室温搅拌2h直至苯胺完全溶解,制得电解液。
(2)取50ml步骤(1)制得的电解液置入电解槽,以1×4cm2压实碳纸为工作电极和对电极。饱和甘汞电极为参比电极,配置三电极体系,以100mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描150圈。
(3)反应结束后,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
实施例6:
(1)配置100ml 0.2M的硝酸钴水溶液,加入苯胺单体至苯胺单体浓度为0.4M。室温搅拌2h直至苯胺单体完全溶解,制得电解液。
(2)取50ml步骤(1)制得的电解液置入电解槽,以1×4cm2压实碳纸为工作电极和对电极。饱和甘汞电极为参比电极,配置三电极体系,以100mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描150圈。
(3)反应结束后,直接取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
实施例7:
(1)配置100ml 0.2M的乙酸钴水溶液,加入苯胺单体至苯胺单体浓度为0.8M。室温搅拌2h直至苯胺单体完全溶解,制得电解液。
(2)取50ml步骤(1)制得的电解液置入电解槽,以1×4cm2压实碳纸为工作电极和对电极。饱和甘汞电极为参比电极,配置三电极体系,以100mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描150圈。
(3)反应结束后,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
实施例8:
(1)配置100ml 0.2M的乙酸钴水溶液,加入苯胺单体至苯胺单体浓度为1M。室温搅拌2h直至苯胺单体完全溶解,制得电解液。
(2)取50ml步骤(1)制得的电解液置入电解槽,以1×4cm2压实碳纸为工作电极和对电极。饱和甘汞电极为参比电极,配置三电极体系,以100mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描150圈。
(3)反应结束后,直接取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料。
实施例9:
重复实施例1的步骤,仅将硝酸钴换成乙酸钴。
实施例10:
重复实施例2的步骤,仅将硝酸钴换成乙酸钴。
实施例11:
重复实施例3的步骤,仅将硝酸钴换成乙酸钴。
实施例12:
重复实施例4的步骤,仅将硝酸钴换成乙酸钴。
实施例13:
重复实施例5的步骤,仅将硝酸钴换成乙酸钴。
实施例14:
重复实施例6的步骤,仅将硝酸钴换成乙酸钴。
实施例15:
重复实施例7的步骤,仅将硝酸钴换成乙酸钴。
实施例16:
重复实施例8的步骤,仅将硝酸钴换成乙酸钴。
实施例17:
重复实施例1的步骤,仅将压实碳纸换成石墨烯纸。
实施例18:
重复实施例2的步骤,仅将压实碳纸换成石墨烯纸。
实施例19:
重复实施例3的步骤,仅将压实碳纸换成石墨烯纸。
实施例20:
重复实施例4的步骤,仅将压实碳纸换成石墨烯纸。
实施例21:
重复实施例5的步骤,仅将压实碳纸换成石墨烯纸。
实施例22:
重复实施例6的步骤,仅将压实碳纸换成石墨烯纸。
实施例23:
重复实施例7的步骤,仅将压实碳纸换成石墨烯纸。
实施例24:
重复实施例8的步骤,仅将压实碳纸换成石墨烯纸。
实施例25:
重复实施例1的步骤,将硝酸钴换成乙酸钴,将压实碳纸换成石墨烯纸。
实施例26:
重复实施例2的步骤,将硝酸钴换成乙酸钴,将压实碳纸换成石墨烯纸。
实施例27:
重复实施例3的步骤,将硝酸钴换成乙酸钴,将压实碳纸换成石墨烯纸。
实施例28:
重复实施例4的步骤,将硝酸钴换成乙酸钴,将压实碳纸换成石墨烯纸。
实施例29:
重复实施例5的步骤,将硝酸钴换成乙酸钴,将压实碳纸换成石墨烯纸。
实施例30:
重复实施例6的步骤,将硝酸钴换成乙酸钴,将压实碳纸换成石墨烯纸。
实施例31:
重复实施例7的步骤,将硝酸钴换成乙酸钴,将压实碳纸换成石墨烯纸。
实施例32:
重复实施例8的步骤,将硝酸钴换成乙酸钴,将压实碳纸换成石墨烯纸。
Claims (1)
1.一种聚苯胺/氢氧化钴超级电容器复合电极材料的制备方法,其特征在于具体步骤为:
(1)在钴离子的浓度为0.1~2M的水溶液中加入苯胺单体,室温搅拌2h直至苯胺单体完全溶解,制得电解液;
(2)取50mL步骤(1)制得的电解液置入电解槽,以压实碳纸或者石墨烯纸为工作电极和对电极,饱和甘汞电极为参比电极,配置三电极体系,以5~2000mV/s的扫描速率在-1V~1V之间对体系进行循环伏安扫描100~10000圈;
(3)反应结束后,取下工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,最后在60℃下烘干24h,即制得聚苯胺/氢氧化钴超级电容器复合电极材料;
所述苯胺单体与钴离子的物质的量之比为0.1~5:1。
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