CN107731567A - 柔性碳布负载空心球状1T‑MoS2超级电容器电极材料的制备方法 - Google Patents
柔性碳布负载空心球状1T‑MoS2超级电容器电极材料的制备方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 49
- 239000004744 fabric Substances 0.000 title claims abstract description 49
- 239000007772 electrode material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000003990 capacitor Substances 0.000 title abstract description 10
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 13
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 229920000742 Cotton Polymers 0.000 claims abstract description 7
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 4
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 4
- 235000018417 cysteine Nutrition 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 4
- 239000005864 Sulphur Substances 0.000 abstract description 4
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 4
- 239000011733 molybdenum Substances 0.000 abstract description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 230000014759 maintenance of location Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 229910052976 metal sulfide Inorganic materials 0.000 description 3
- 230000001052 transient effect Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000007825 activation reagent Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005406 washing Methods 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
- H01G11/84—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
-
- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
-
- 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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- 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
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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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- Microelectronics & Electronic Packaging (AREA)
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- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
本发明涉及一种柔性碳布负载空心球状1T‑MoS2超级电容器电极材料的制备方法,具体涉及一种将棉布碳化制备为碳布并活化,利用球形模板,碳布,钼源,硫源,进行水热反应并去除模板以制备超级电容器用柔性碳布负载空心球状1T‑MoS2超级电容器电极材料的新方法。本发明包括具体步骤如下:首先将棉布碳化制备为碳布并活化,再将球形模板嵌入碳布中,所得碳布放入钼源,硫源混合液进行水热反应并去除球形模板以制备超级电容器用柔性碳布负载空心球状1T‑MoS2超级电容器电极材料。
Description
技术领域
本发明涉及一种柔性碳布负载空心球状1T-MoS2超级电容器电极材料的制备方法,具体涉及一种首先将棉布碳化制备为碳布并活化,再将球形模板嵌入碳布中,所得碳布放入钼源,硫源混合液,水热反应后去除模板以制备超级电容器用柔性碳布负载空心球状1T-MoS2超级电容器电极材料的新方法。
背景技术
可再生能源技术在解决能源危机和全球环境变化方面具有重要意义。在各种电化学能量储存和转换系统中,超级电容器近年来得到了广泛的研究,因为其具有高功率,充放电速率快,循环稳定性好等多种优势。近年来,可穿戴电子设备迅猛发展,常规形式的超级电容器已不能完全满足实际的需求,储能装置的要求扩大。各种柔性智能可穿戴电子设备朝着小巧轻便、可穿戴折叠、具有柔性的方向发展,这就要求电子设备的储能装置必须兼具柔性可弯曲、可拉伸、轻质舒适、安全稳定等特点。
碳布是双电层电容材料,它是集导电性,柔性,高稳定性,高使用寿命于一体的理想集流体和电极材料,而超级电容器中的电极是构建高效器件的关键部件,但以纯碳布作为电极的超级电容器比电容偏低,所以通过在碳布上负载其他金属,引入赝电容是来提高碳布电极比电容的有效途径。过渡金属硫化物与其相应的金属氧化物相比,电容量更高,氧化还原电位高,电导率提高,因此过渡金属硫化物受到了极大关注,在过渡金属硫化物中,二硫化钼作为热门的二维材料,具有类石墨烯的片层结构,受到了极大的关注。相对于自然界常见的半导体相的2H-MoS2,金属相的1T-MoS2具有更高的导电性,亲水性和比电容,是更为理想的超级电容器电极材料,同时,空心球的特征形状能使二硫化钼获得更大的比表面积,提高活性材料与电解液的接触面积,以提高超级电容器性能。
本专利是以棉布为碳布的原料,将其碳化为碳布,再通过氢氧化钾使碳布活化,使碳布获得更大比表面积并引入-OH基团以提升后续水热反应时的1T-MoS2负载量。本路线原料来源广泛、合成方法简便,通过调节活化试剂的量来调整碳布的导电性,比表面积和孔隙率并引入表面基团,以钼酸钠为钼源,半胱氨酸为硫源,硅球为球形模板,在200℃下水热反应合成球状1T-MoS2并负载于活化碳布上,最后去除模板获得负载于碳布上的空心球状1T-MoS2电极材料。
发明内容
本发明目的是提供一种制备柔性碳布负载空心球状1T-MoS2超级电容器电极材料的新方法。
本发明首先将棉布700~900℃碳化为碳布,将碳布与活化试剂按质量比1∶1~1∶4混合,于120℃下保温2小时活化,再将二氧化硅嵌入活化碳布,之后将所得碳布放入钼酸钠,半胱氨酸,二甲基甲酰胺和去离子水的混合液中并放置于聚四氟乙烯内衬的水热反应釜中,180~220℃下反应12~24小时,之后将产物取出,去除模板后洗涤、干燥。
本发明的特征在于:碳布同时作为集流体和电极材料,硅球作为球形模板,最终复合材料中的空心球状MoS2为金属相的1T-MoS2。
具体实施方式
实施例1:首先将棉布在管式炉中800℃,氮气保护下碳化2h,将得到的碳布与活化试剂(碳布与KOH的质量比为1∶3)混合,向其中加入适量蒸馏水混合均匀,将混合物充分浸渍后在120℃烘箱中烘干12小时,之后将产物在800℃氮气保护下的管式炉中高温活化1.5h,所得固体洗涤、干燥,得到的活化碳布进行电化学性能测试,以氢氧化钾为电解液,测得面积比容量为273F/g,循环5000次容量保持率97%。
实施例2:将已嵌入球形模板碳布,钼酸钠,半胱氨酸,二甲基甲酰胺混合液放入水热反应釜,200℃反应6小时,得到生长于碳布和球形模板上的花状微球1T-MoS2,比电容为439F/g,循环5000次容量保持率95%。
实施例3:改变水热反应时间为12小时,将已嵌入球形模板碳布,钼酸钠,半胱氨酸,二甲基甲酰胺混合液放入水热反应釜,200℃下,得到生长于碳布和球形模板上,数量减少但形状增大的纳米花状微球1T-MoS2,比电容为516F/g,循环5000次容量保持率95%。
实施例4:改变水热反应时间为24小时,将已嵌入球形模板碳布,钼酸钠,半胱氨酸,二甲基甲酰胺混合液放入水热反应釜,200℃下,得到垂直排列于实心硅球和碳布上的1T-MoS2,比电容为576F/g,循环5000次容量保持率95%。
实施例5:将实施例4所得产物去除模板后,所得的柔性碳布负载空心球状1T-MoS2电极材料测得比电容602F/g,循环5000次容量保持率91%。
Claims (2)
1.一种柔性碳布负载空心球状1T-MoS2的制备方法,其具体步骤如下:首先将棉布700~900℃碳化为碳布,将碳布与活化试剂按质量比1∶1~1∶4(g/g)混合后在110℃~130℃下活化,再将球形模板嵌入碳布,将所得碳布放入钼酸钠,半胱氨酸,二甲基甲酰胺,去离子水混合液中,180~220℃下进行水热反应12~24h,将产物取出并清洗,干燥。
2.一种如权利要求1所述的柔性碳布负载空心球状1T-MoS2的制备方法,其特征在于:碳布同时作为集流体和电极材料,硅球作为球形模板,最终复合材料中的空心球状MoS2为金属相的1T-MoS2。
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CN116072879B (zh) * | 2023-04-07 | 2023-07-07 | 河南工学院 | 一种锂离子电池电极材料及其制备方法 |
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