CN106206060A - 氢氧化钴@碳纤维纳米复合材料的制备及超级电容器电极材料应用 - Google Patents
氢氧化钴@碳纤维纳米复合材料的制备及超级电容器电极材料应用 Download PDFInfo
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- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 title claims abstract description 42
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 title claims abstract description 41
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 239000007772 electrode material Substances 0.000 title claims abstract description 19
- 239000003990 capacitor Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920000742 Cotton Polymers 0.000 claims abstract description 11
- 239000000835 fiber Substances 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 9
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 6
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 6
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 239000012153 distilled water Substances 0.000 claims abstract description 5
- 239000010453 quartz Substances 0.000 claims abstract description 4
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- 238000005406 washing Methods 0.000 claims description 4
- UMAHOFNLHNWTDQ-UHFFFAOYSA-L [C].[Co](O)O Chemical compound [C].[Co](O)O UMAHOFNLHNWTDQ-UHFFFAOYSA-L 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract 1
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- 238000000034 method Methods 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
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- 239000000047 product Substances 0.000 description 4
- 241000219146 Gossypium Species 0.000 description 3
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- 239000001257 hydrogen Substances 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
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- 238000003860 storage Methods 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
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- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
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- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
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- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
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- 230000007246 mechanism Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
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- 230000027756 respiratory electron transport chain Effects 0.000 description 1
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- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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Abstract
本发明公开了一种氢氧化钴@碳纤维纳米复合材料的制备及超级电容器电极材料应用。(1)将2 g市售医用脱脂棉放在石英舟中并置于管式炉中部,在氮气气氛下500 oC焙烧3小时,升温速率为5 oC/min,然后在氮气气氛下自然冷却至室温,得到碳纤维材料;(2)将0.626 g硝酸钴和0.2 g六次甲基四胺加入到40 mL蒸馏水中搅拌溶解,待完全溶解后,加入碳纤维材料,并置于100 mL水热釜中在100 oC下反应12小时;反应结束后,将其自然冷却至室温,对产物进行过滤、30 oC去离子水洗涤;在鼓风干燥箱中80 oC下干燥12小时。本发明制备方法简单,容易实现,所制得的氢氧化钴@碳纤维纳米复合材料在作为超级电容器电极材料应用时表现出了很好的效果。
Description
技术领域
本发明涉及一种超级电容器电极材料的制备方法,特别是一种氢氧化钴@碳纤维纳米复合材料的制备及超级电容器电极材料应用。
背景技术
伴随着社会经济的快速发展及人口的急剧增长,资源和能源的日渐短缺及生态环境的日益恶化成为当今函待解决的问题。为了解决这些问题,发展环保的具有高效利用率和低污染的可持续能源刻不容缓。现在已开发或正在研究开发的新能源包括风能、海洋能、太阳能、氢能、核能等。为了能充分利用这些新能源,需要有与之配套的储能装置。近年来,超级电容器作为一种高性能、无污染的储能器件受到了广泛的关注。目前,超级电容器已经用于电子产品、交通运输、电力、通讯和国防安全等领域,如电动螺丝刀、风能和太阳能发电储能设备。
根据能量的储存与转化机理,超级电容器可以分为双电层电容器和法拉第电容器两类。其中,双电层电容器是在电极表面静电吸附离子而形成双电层进行能量储存;而法拉第电容器是在电极上快速地发生可逆的氧化还原反应而进行能量储存,其储存电荷的过程不仅包括双电层上的存储,同时还包括电解液中的离子在电极活性物质中发生氧化还原反应而将电荷储存于电极中。所以,法拉第电容值要明显大于双电层电容值。
目前,以法拉第电容方式存储能量的电极材料主要包括过渡金属氧化物、氢氧化物及其导电聚合物,如氧化镍、氧化铜、氧化钌、四氧化三铁、氢氧化镍、氢氧化钴等。由于氢氧化钴具有独特的纳米片状结构和良好的电化学性能,同时资源相对丰富、价格低廉、环境友好、导电性比其他氢氧化物好等优点,本发明选取氢氧化钴作为超级电容器电极材料。但是,氢氧化钴在制备过程中容易发生聚集,使其在循环充放电过程中电容性能下降。因此,为解决这一难题,本发明拟将氢氧化钴负载于高比表面积的碳材料上,这样有利于提高活性组分的分散,降低充放电过程的电子转移阻力,从而提高材料的电容性能和循环稳定性能。
以来源广泛的生物质棉花为前驱体通过热处理制备得到的碳纤维是一类质量轻、高导电性、高比表面积的结构材料。利用它作为生长功能纳米材料的基底,一方面可以改善氢氧化钴的导电性,另一方面可以减弱原位生长时活性物质的团聚现象。
发明内容
本发明的目的是以脱脂棉作为基础材料,将脱脂棉在氮气气氛下进行高温热处理得到碳纤维材料;以碳纤维为基底,以硝酸钴为原料,以六次甲基四胺为沉淀剂,采用水热原位合成技术得到氢氧化钴@碳纤维纳米复合材料及作为超级电容器电极材料应用。
具体步骤为:
(1)将2 g市售医用脱脂棉放在石英舟中并置于管式炉中部,在氮气气氛下500 oC焙烧3小时,升温速率为5 oC/min,然后在氮气气氛下自然冷却至室温,得到碳纤维材料。
(2)将0.626 g硝酸钴和0.2 g六次甲基四胺加入到40 mL蒸馏水中搅拌溶解,待完全溶解后,加入步骤(1)所得的碳纤维材料,并置于100 mL水热釜中在100 oC下反应12小时;反应结束后,将其自然冷却至室温,对产物进行过滤、30 oC去离子水洗涤;将洗涤后的样品在鼓风干燥箱中80 oC下干燥12小时,即得到氢氧化钴@碳纤维纳米复合材料。
将所制得的氢氧化钴@碳纤维复合材料作为超级电容器电极材料的应用。
氢氧化钴@碳纤维复合材料能在6.0 mol/L KOH电解液中室温下使用,适用于超级电容器工作电极电极,其电容性能远远优于采用同种方法制备得到的未添加基底的氢氧化钴材料,是一种有效的超级电容器电极材料。
本发明制备方法简单,容易实现,所制得的氢氧化钴@碳纤维纳米复合材料,以来源广泛的生物质棉花作为基础材料,棉花纤维的交织结构使其高温热处理后还能保持一定的整体结构,利用它作为生长电极材料的基底,一方面可以改善氢氧化钴的导电性,另一方面可以减弱原位生长时活性物质的团聚现象。
附图说明
图1为本发明所制的未添加基底的氢氧化钴材料和氢氧化钴@碳纤维纳米复合材料的扫描电镜图,a:未添加基底的氢氧化钴材料,b:氢氧化钴@碳纤维纳米复合材料。
图2为本发明所制的未添加基底的氢氧化钴材料和氢氧化钴@碳纤维纳米复合材料的比电容随电流密度的变化曲线图。
具体实施方式
实施例:
(1)将2 g市售医用脱脂棉放在石英舟中并置于管式炉中部,在氮气气氛下500 oC焙烧3小时,升温速率为5 oC/min,然后在氮气气氛下自然冷却至室温,得到碳纤维材料。
(2)将0.626 g硝酸钴和0.2 g六次甲基四胺加入到40 mL蒸馏水中搅拌溶解,待完全溶解后,加入步骤(1)所得的碳纤维材料,并置于100 mL水热釜中在100 oC下反应12小时;反应结束后,将其自然冷却至室温,对产物进行过滤、30 oC去离子水洗涤;将洗涤后的样品在鼓风干燥箱中80 oC下干燥12小时,即得到氢氧化钴@碳纤维纳米复合材料,氢氧化钴@碳纤维纳米复合材料的扫描电镜图如图1(b)所示,棉花碳纤维错综复杂地交织成网状结构,提供了很大的空间位置,而氢氧化钴如同花瓣一样,独立均匀地镶嵌在其表面上。这表明本发明制备的氢氧化钴@碳纤维纳米复合材料可以克服传统方法制备过程中氢氧化钴易聚集的问题,从而有利于其作为电极材料时电容性能的提高。
(3)取尺寸为2×3 cm的泡沫镍并将其对折,之后将所制备的氢氧化钴@碳纤维纳米复合材料夹在对折的泡沫镍中间,置于6.0 mol/L KOH电解液中,常温下在CHI660D电化学工作站分别进行循环伏安曲线、恒电流充放电曲线和稳定性的测试。经测试发现,所得氢氧化钴@碳纤维纳米复合材料的电容性能大大增加,在不同电流密度下的比电容值见图2。
对比例:
(1)将0.626 g硝酸钴和0.2 g六次甲基四胺加入到40 mL蒸馏水中搅拌溶解,待完全溶解后,置于100 mL水热釜中在100 oC下反应12小时;反应结束后,将其自然冷却至室温,对产物进行过滤、去离子水洗涤;将洗涤后的样品在鼓风干燥箱中80 oC下干燥12小时,即得到未添加基底的氢氧化钴超级电容器电极材料,未添加基底的氢氧化钴材料的扫描电镜图如图1(a)所示。
(2)按照未添加基底的氢氧化钴材料:聚偏二氟乙烯:炭黑的质量比80:10:10,分别称取未添加基底的氢氧化钴材料、聚偏二氟乙烯和炭黑并置于500 μL N-甲基-2-吡咯烷酮中,搅拌均匀后涂在泡沫镍1 cm2的表面上,然后在100 oC下干燥12小时,在10 MPa下进行压片、称重并置于6.0 mol/L KOH电解液中,常温下在CHI660D电化学工作站分别进行循环伏安曲线、恒电流充放电曲线和稳定性的测试。经测试发现,所得未添加基底的氢氧化钴超电极材料有一定的电容性能,在不同电流密度下的比电容值见图2。
从图2中可以看出,氢氧化钴@碳纤维纳米复合材料具有较大的比电容,而未添加基底的氢氧化钴材料比电容较小。这表明,与传统方法制备的氢氧化钴相比,本发明制备的氢氧化钴@碳纤维纳米复合材料是一种高效的超级电容器电极材料。
与未添加基底的氢氧化钴相比,氢氧化钴@碳纤维纳米复合材料的电化学性能明显增强。因此以脱脂棉为前驱体采用原位生长法制备得到的氢氧化钴@碳纤维纳米复合材料是一种有较大应用前景的高效超级电容器电极材料。
Claims (2)
1.一种氢氧化钴@碳纤维纳米复合材料的制备方法,其特征在于具体步骤为:
(1)将2 g市售医用脱脂棉放在石英舟中并置于管式炉中部,在氮气气氛下500 oC焙烧3小时,升温速率为5 oC/min,然后在氮气气氛下自然冷却至室温,得到碳纤维材料;
(2)将0.626 g硝酸钴和0.2 g六次甲基四胺加入到40 mL蒸馏水中搅拌溶解,待完全溶解后,加入步骤(1)所得的碳纤维材料,并置于100 mL水热釜中在100 oC下反应12小时;反应结束后,将其自然冷却至室温,对产物进行过滤、30 oC去离子水洗涤;将洗涤后的样品在鼓风干燥箱中80 oC下干燥12小时,即得到氢氧化钴@碳纤维纳米复合超级电容器电极材料。
2.根据权利要求1所述的氢氧化钴@碳纤维纳米复合材料的应用,其特征在于氢氧化钴@碳纤维纳米复合材料作为超级电容器电极材料应用。
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