CN108172412A - 聚吡咯/氢氧化镍超级电容器复合电极材料的制备方法 - Google Patents
聚吡咯/氢氧化镍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 20
- 239000003990 capacitor Substances 0.000 title claims abstract description 19
- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 19
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 title claims abstract description 17
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000178 monomer Substances 0.000 claims abstract description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 19
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 19
- 239000003792 electrolyte Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 150000002500 ions Chemical class 0.000 claims abstract description 5
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims 1
- 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
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 17
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 16
- 229940078494 nickel acetate Drugs 0.000 description 16
- 238000000151 deposition Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000004070 electrodeposition Methods 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
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-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
- 230000008021 deposition Effects 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
- 150000002815 nickel Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
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- 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
- H01G11/46—Metal oxides
-
- 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
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- 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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- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
本发明公开了一种聚吡咯/氢氧化镍超级电容器复合电极材料的制备方法。将吡咯单体加入到镍离子浓度为0.1~2M的水溶液中,室温搅拌2h直至吡咯单体完全溶解,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,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,即制得聚吡咯/氢氧化镍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吡咯/氢氧化镍超级电容器复合电极材料的办法,具体的来说,涉及一种聚吡咯/氢氧化镍超级电容器复合电极材料的制备方法。
背景技术
聚吡咯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吡咯,由于其粒径极小、比表面积大、极快的电子转移速率等性质,赋予了纳米导电聚吡咯材料具有传统块体所不具备的许多独特性能。
氢氧化镍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).)
虽然氢氧化镍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。聚吡咯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。本发明以吡咯单体和镍盐水溶液为电解液,通过循环伏安的办法在同一电极上同时进行阳极沉积聚吡咯和阴极沉积氢氧化镍,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
本发明的目的在于提供一种聚吡咯/氢氧化镍超级电容器复合电极材料的制备方法。
具体步骤为:
(1)将吡咯单体加入到镍离子浓度为0.1~2M的水溶液中,室温搅拌2h直至吡咯单体完全溶解,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,取下步骤(2)的工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚吡咯/氢氧化镍超级电容器复合电极材料。
所述吡咯单体和镍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,所制得的聚吡咯/氢氧化镍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中制得的聚吡咯/氢氧化镍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中制得的聚吡咯/氢氧化镍超级电容器复合电极材料在氢氧化钾溶液中的交流阻抗图。
具体实施方式
实施例1:
(1)配置硝酸镍和吡咯的水溶液,镍离子浓度为0.2M,吡咯单体浓度为0.02M。室温搅拌2h直至吡咯单体完全溶解,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,取下步骤(2)的工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚吡咯/氢氧化镍超级电容器复合电极材料。
实施例2:
重复实施例1的步骤,镍离子浓度为0.2M,将吡咯单体浓度配置为0.04M。(吡咯单体的和镍离子的物质的量之比为0.2)
实施例3:
重复实施例1的步骤,镍离子浓度为0.2M,将吡咯单体浓度配置为0.05M。(吡咯单体的和镍离子的物质的量之比为0.25)
实施例4:
重复实施例1的步骤,镍离子浓度为0.2M,将吡咯单体浓度配置为0.1M。(吡咯单体的和镍离子的物质的量之比为0.5)
实施例5:
重复实施例1的步骤,镍离子浓度为0.2M,将吡咯单体浓度配置为0.2M。(吡咯单体的和镍离子的物质的量之比为1)
实施例6:
重复实施例1的步骤,镍离子浓度为0.2M,将吡咯单体浓度配置为0.4M。(吡咯单体的和镍离子的物质的量之比为2)
实施例7:
重复实施例1的步骤,镍离子浓度为0.2M,将吡咯单体浓度配置为0.8M。(吡咯单体的和镍离子的物质的量之比为4)
实施例8:
重复实施例1的步骤,镍离子浓度为0.2M,将吡咯单体浓度配置为1M。(吡咯单体的和镍离子的物质的量之比为5)
实施例9:
重复实施例1的步骤,将硝酸镍换成乙酸镍。
实施例10:
重复实施例2的步骤,将硝酸镍换成乙酸镍。
实施例11:
重复实施例3的步骤,将硝酸镍换成乙酸镍。
实施例12:
重复实施例4的步骤,将硝酸镍换成乙酸镍。
实施例13:
重复实施例5的步骤,将硝酸镍换成乙酸镍。
实施例14:
重复实施例6的步骤,将硝酸镍换成乙酸镍。
实施例15:
重复实施例7的步骤,将硝酸镍换成乙酸镍。
实施例16:
重复实施例8的步骤,将硝酸镍换成乙酸镍。
实施例17:
重复实施例1的步骤,将压实碳纸换成石墨烯纸。
实施例18:
重复实施例2的步骤,将压实碳纸换成石墨烯纸。
实施例19:
重复实施例3的步骤,将压实碳纸换成石墨烯纸。
实施例20:
重复实施例4的步骤,将压实碳纸换成石墨烯纸。
实施例21:
重复实施例5的步骤,将压实碳纸换成石墨烯纸。
实施例22:
重复实施例6的步骤,将压实碳纸换成石墨烯纸。
实施例23:
重复实施例7的步骤,将压实碳纸换成石墨烯纸。
实施例24:
重复实施例8的步骤,将压实碳纸换成石墨烯纸。
实施例25:
重复实施例1的步骤,将硝酸镍换成乙酸镍,将压实碳纸换成石墨烯纸。
实施例26:
重复实施例2的步骤,将硝酸镍换成乙酸镍,将压实碳纸换成石墨烯纸。
实施例27:
重复实施例3的步骤,将硝酸镍换成乙酸镍,将压实碳纸换成石墨烯纸。
实施例28:
重复实施例4的步骤,将硝酸镍换成乙酸镍,将压实碳纸换成石墨烯纸。
实施例29:
重复实施例5的步骤,将硝酸镍换成乙酸镍,将压实碳纸换成石墨烯纸。
实施例30:
重复实施例6的步骤,将硝酸镍换成乙酸镍,将压实碳纸换成石墨烯纸。
实施例31:
重复实施例7的步骤,将硝酸镍换成乙酸镍,将压实碳纸换成石墨烯纸。
实施例32:
重复实施例8的步骤,将硝酸镍换成乙酸镍,将压实碳纸换成石墨烯纸。
Claims (1)
1.一种聚吡咯/氢氧化镍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)将吡咯单体加入到镍离子浓度为0.1~2M的水溶液中,室温搅拌2h直至吡咯单体完全溶解,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,取下步骤(2)的工作电极和对电极,用去离子水浸泡过夜以去除杂质离子,在60℃下烘干24h,即制得聚吡咯/氢氧化镍超级电容器复合电极材料;
所述吡咯单体和镍离子的物质的量之比为0.1~5:1。
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CN115394564A (zh) * | 2022-08-23 | 2022-11-25 | 江苏科技大学 | 一种三氮唑铜/聚吡咯复合电极材料的制备方法及其应用 |
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