CN106683902A - High-specific-capacity cobaltosic oxide nanowire carbon aerogel hybrid supercapacitor anode material and preparation method thereof - Google Patents

High-specific-capacity cobaltosic oxide nanowire carbon aerogel hybrid supercapacitor anode material and preparation method thereof Download PDF

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Publication number
CN106683902A
CN106683902A CN201611244213.4A CN201611244213A CN106683902A CN 106683902 A CN106683902 A CN 106683902A CN 201611244213 A CN201611244213 A CN 201611244213A CN 106683902 A CN106683902 A CN 106683902A
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carbon aerogels
appropriate amount
parts
appropriate
graphene
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夏斌
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Tongling City Shengmeida Electronic Manufacturing Co Ltd
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Tongling City Shengmeida Electronic Manufacturing Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • 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

Abstract

The invention discloses a high-specific-capacity cobaltosic oxide nanowire carbon aerogel hybrid supercapacitor anode material. The anode material is prepared from, by weight, 35-38 parts of resorcinol, 70-76 parts of formaldehyde solution, an appropriate amount of sodium carbonate, an appropriate amount of acetone, an appropriate amount of carbon black, an appropriate amount of sodium carboxymethylcellulose, an appropriate amount of butadiene styrene rubber, an appropriate amount of deionized water, an appropriate amount of 14-15 mol/L KOH concentrated solution, 10-12 parts of hydrated cobalt chloride, 56-60 parts of urea, 0.5-0.8 part of nanometer tungsten trioxide, 1.2-1.5 parts of stannic oxide, 0.6-0.7 part of graphene and 10 parts of ethyl alcohol. By adopting stannic oxide and graphene for performing high-temperature expansion, holes in the graphene contain the stannic oxide, and the problems that due to the fact that the volume of the stannic oxide is expanded, an electrode material is powdered, the lithium ion battery capacity is sharply attenuated are solved; meanwhile, nanometer tungsten trioxide is adsorbed, the electrode photoelectric effect is improved, and the electrode energy storage property is improved.

Description

A kind of height ratio capacity cobaltosic oxide nano line carbon aerogels hybrid supercapacitor is just Pole material and preparation method thereof
Technical field
The present invention relates to capacitor anode field of material technology, more particularly to a kind of height ratio capacity cobaltosic oxide nano line Carbon aerogels hybrid supercapacitor positive electrode and preparation method thereof.
Background technology
Ultracapacitor is one of most promising electrical source of power of Developing, with having extended cycle life, power density it is big, Assembling mode is simple, the features such as run safer, it is adaptable to electric automobile and hybrid vehicle power supply, portable instrument equipment with And the back-up source of emergency set etc..But with the continuous development of energy storage technology, ultracapacitor is for high-energy-density, high ratio The performance requirement more and more higher of power.Electrode material is one of critical component of ultracapacitor energy storage, and the carbon of commercialization at present Electrode material is mainly activated carbon, there is low electric conductivity, aperture uncontrollability due to activated carbon, specific surface area utilization rate is low asks Topic, therefore it is increasingly urgent to prepare the nanoporous carbon materials of excellent properties.Carbon aerogels are used as a kind of nanoporous carbon materials, quilt It is considered a kind of excellent electrode material for super capacitor, with specific surface area height, pore-size distribution is controllable, density is adjustable, conduction Property the characteristic such as good, attract widespread attention at aspects such as storing up electricity, hydrogen storages.Carbon aerogels are earliest by the U.S. in 1989 LawrenceLivermore National Laboratories PEKALA mixes resorcinol with formaldehyde, in Na2CO3Under catalyst action, Jing Supercritical drying prepares RF aeroges, and carbon aerogels have been obtained after carbonization.It is dry using cheap normal pressure due to industrialization demand Dry technology prepares carbon aerogels and obtains successfully, it might even be possible to prepares the RF and carbon aerogel films of loose structure, is greatly reduced Preparation cost.In order to improve the chemical property of carbon aerogels ultracapacitor, regulation activating process is taken to improve carbon airsetting The pore-size distribution of glue, the method for specific surface area, can increase the capacitance of carbon silica aerogel electrode material, including soak time With active rate etc..Improve carbon aerogels specific surface area and improving the conventional method of chemical property there are KOH wet chemicals to activate And CO2Physical activation method, it is therefore an objective to which pore-creating is obtaining the carbon aerogels of more high-specific surface area.In order to further improve carbon aerogels Specific surface area and specific capacitance, can also use CO2With the step activation methods of KOH two.Match somebody with somebody with catalyst herein by optimization presoma Carbon aerogels of good performance are prepared than parameter, the carbon aerogels for being obtained are activated using 3 kinds of activating process, studied Impacts of the different activating process to carbon aerogels specific surface area and specific capacitance.
Carbon aerogels have the advantages that many materials are difficult to reach, but due to using binding agent, the stability of electrode is poor, Electrical conductivity is relatively low, and energy density is low, and power density is low, needs to improve, in addition it is also necessary to improve the specific capacity of positive electrode.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of height ratio capacity cobaltosic oxide nano line Carbon aerogels hybrid supercapacitor positive electrode and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of height ratio capacity cobaltosic oxide nano line carbon aerogels hybrid supercapacitor positive electrode, by following weight portion Raw material is made：Resorcinol 35-38, formalin 70-76, appropriate sodium carbonate, acetone in proper, appropriate white carbon black, carboxymethyl cellulose Plain sodium is appropriate, appropriate butadiene-styrene rubber, appropriate deionized water, 14-15mol/LKOH concentrated solutions appropriate, hydrated cobalt chloride 10-12, urine Plain 56-60, nano tungsten trioxide 0.5-0.8, tin ash 1.2-1.5, Graphene 0.6-0.7, ethanol -10.
The preparation method of the height ratio capacity cobaltosic oxide nano line carbon aerogels hybrid supercapacitor positive electrode, Comprise the following steps：
（1）By mol ratio for 1: 2 resorcinol and formaldehyde be dissolved in deionized water, add sodium carbonate liquor, uniform stirring 2- 2.3h, resorcinol is 1500 with the mol ratio of sodium carbonate, and Solute mass fraction is 30-32%, and solution sealing is placed in into baking oven, Process at 30 DEG C 1 day, then process 1 day at 50 DEG C, then process 3 days at 90 DEG C, obtain wet gel, then fully replaced with acetone Wet gel, carries out constant pressure and dry, in N2The lower carbonization of protection, then mix with KOH concentrated solutions, it is vacuum dried, in N2It is warming up under protection 900 DEG C of process 2-3 hours, cooling is washed, is dried, and obtains carbon aerogels；
（2）Hydrated cobalt chloride, carbamide are added in deionized water, is stirred to dissolving and is obtained solution, cobalt chloride concentration is 0.04mol/L, urea concentration are 0.2mol/L, by volume carbon aerogels：Solution=1:2-2.5 adds carbon aerogels, is put into dry In dry case, 8-9 hours are reacted at 94-97 DEG C, take out carbon aerogels, be dried at 45-48 DEG C, then be placed in muffle furnace 2-2.5 hours are processed at 250-260 DEG C, natural cooling obtains modified carbon aerogels；
（3）Tin ash, Graphene mixed grinding is uniform, to heat 15-20 minutes at 850-880 DEG C, cooling adds ethanol In, nano tungsten trioxide is added while stirring, 3-4 hours are stirred, obtain mixed material；
（4）By carbon aerogels: white carbon black: sodium carboxymethyl cellulose: butadiene-styrene rubber=84: 10: 1: 5 weighings, send into ball mill ball milling 0.5-0.7h, adds water and butadiene-styrene rubber, mixed material, and again ball milling 2-2.3h obtains slurry, and slurry is uniform with coating machine To be coated on thickness be on 20-22 μm of aluminium foil, in 85-90 DEG C of drying, to obtain positive electrode.
Negative material proportioning is MCMB: white carbon black: sodium carboxymethyl cellulose: butadiene-styrene rubber=90: 6: 2: 2, prepare Technique is identical with positive plate, after obtaining uniform sizing material, is uniformly coated on the Copper Foil that thickness is 12-13 μm, 85-90 DEG C of baking It is dry.The positive/negative plate for obtaining is washed into respectively the disk of a diameter of 13mm and the rectangle of 35mm × 40mm, powder at lug is scraped off, Pole piece is compacted with tablet machine；Electrolyte is the LiPF6 of 1mol/L.
It is an advantage of the invention that：The present invention generates four oxidations three using hydrated cobalt chloride, carbamide in carbon aerogels hole Cobalt nanowire so that the specific capacitance of capacitor is raised, carbon aerogels are difficult to subside, and increase discharge and recharge number of times, keep good storage Electrical property；By using tin ash and Graphene high-temperature expansion, the hole of Graphene accommodates tin ash, solves titanium dioxide Stannum volumetric expansion, causes electrode material efflorescence, makes the problem of capacity of lithium ion battery sharp-decay, while having adsorbed the oxygen of nanometer three Change tungsten, improve the photoelectric effect of electrode, improve the energy-storage property of electrode.
Specific embodiment
A kind of height ratio capacity cobaltosic oxide nano line carbon aerogels hybrid supercapacitor positive electrode, by following weight Part（Kilogram）Raw material make：Resorcinol 35, formalin 70, appropriate sodium carbonate, acetone in proper, appropriate white carbon black, carboxymethyl Appropriate sodium cellulosate, appropriate butadiene-styrene rubber, appropriate deionized water, 14mol/LKOH concentrated solutions are appropriate, hydrated cobalt chloride 10, carbamide 56th, nano tungsten trioxide 0.5, tin ash 1.2, Graphene 0.6, ethanol.
The preparation method of the height ratio capacity cobaltosic oxide nano line carbon aerogels hybrid supercapacitor positive electrode, Comprise the following steps：
（1）By mol ratio for 1: 2 resorcinol and formaldehyde be dissolved in deionized water, add sodium carbonate liquor, uniform stirring 2h, Resorcinol is 1500 with the mol ratio of sodium carbonate, and Solute mass fraction is 30%, solution sealing is placed in into baking oven, at 30 DEG C Reason 1 day, is then processed 1 day at 50 DEG C, is then processed 3 days at 90 DEG C, obtains wet gel, then fully replaces wet gel with acetone, Constant pressure and dry is carried out, in N2The lower carbonization of protection, then mix with KOH concentrated solutions, it is vacuum dried, in N2It is warming up under protection at 900 DEG C Reason 2 hours, cooling is washed, is dried, and obtains carbon aerogels；
（2）Hydrated cobalt chloride, carbamide are added in deionized water, is stirred to dissolving and is obtained solution, cobalt chloride concentration is 0.04mol/L, urea concentration are 0.2mol/L, by volume carbon aerogels：Solution=1:2 add carbon aerogels, are put into drying baker In, react 8 hours at 94 DEG C, carbon aerogels are taken out, it is dried at 45 DEG C, then be placed in muffle furnace and process 2 little at 250 DEG C When, natural cooling obtains modified carbon aerogels；
（3）Tin ash, Graphene mixed grinding is uniform, heat 15 minutes at 850 DEG C, cooling, in adding ethanol, while stirring Mix side and add nano tungsten trioxide, stir 3 hours, obtain mixed material；
（4）By carbon aerogels: white carbon black: sodium carboxymethyl cellulose: butadiene-styrene rubber=84: 10: 1: 5 weighings, send into ball mill ball milling 0.5h, adds water and butadiene-styrene rubber, mixed material, and again ball milling 2h obtains slurry, and slurry is uniformly coated to coating machine Thickness is on 20 μm of aluminium foil, in 85 DEG C of drying, to obtain positive electrode.
Negative material proportioning is MCMB: white carbon black: sodium carboxymethyl cellulose: butadiene-styrene rubber=90: 6: 2: 2, prepare Technique is identical with positive plate, after obtaining uniform sizing material, is uniformly coated on the Copper Foil that thickness is 12 μm, 85 DEG C of drying.Will To positive/negative plate be washed into the disk of a diameter of 13mm and the rectangle of 35mm × 40mm respectively, scrape off powder at lug, use tabletting Machine is compacted pole piece；Electrolyte is the LiPF6 of 1mol/L.
The specific capacitance of capacitor made by the electrode material of the embodiment is 359F/g, when electric current density is 20A/g, is followed Ring 1000 times, specific capacitance maintains the 85.4% of initial specific capacitance, good cycling stability.

Claims (2)

1. a kind of height ratio capacity cobaltosic oxide nano line carbon aerogels hybrid supercapacitor positive electrode, it is characterised in that： It is prepared by the raw materials in：Resorcinol 35-38, formalin 70-76, appropriate sodium carbonate, acetone in proper, white carbon black are fitted Amount, appropriate sodium carboxymethyl cellulose, appropriate butadiene-styrene rubber, appropriate deionized water, 14-15mol/LKOH concentrated solutions are appropriate, hydration Cobaltous chloride 10-12, carbamide 56-60, nano tungsten trioxide 0.5-0.8, tin ash 1.2-1.5, Graphene 0.6-0.7, ethanol- 10。
2. height ratio capacity cobaltosic oxide nano line carbon aerogels hybrid supercapacitor positive electrode according to claim 1 Preparation method, it is characterised in that comprise the following steps：
（1）By mol ratio for 1: 2 resorcinol and formaldehyde be dissolved in deionized water, add sodium carbonate liquor, uniform stirring 2- 2.3h, resorcinol is 1500 with the mol ratio of sodium carbonate, and Solute mass fraction is 30-32%, and solution sealing is placed in into baking oven, Process at 30 DEG C 1 day, then process 1 day at 50 DEG C, then process 3 days at 90 DEG C, obtain wet gel, then fully replaced with acetone Wet gel, carries out constant pressure and dry, in N2The lower carbonization of protection, then mix with KOH concentrated solutions, it is vacuum dried, in N2It is warming up under protection 900 DEG C of process 2-3 hours, cooling is washed, is dried, and obtains carbon aerogels；
（2）Hydrated cobalt chloride, carbamide are added in deionized water, is stirred to dissolving and is obtained solution, cobalt chloride concentration is 0.04mol/L, urea concentration are 0.2mol/L, by volume carbon aerogels：Solution=1:2-2.5 adds carbon aerogels, is put into dry In dry case, 8-9 hours are reacted at 94-97 DEG C, take out carbon aerogels, be dried at 45-48 DEG C, then be placed in muffle furnace 2-2.5 hours are processed at 250-260 DEG C, natural cooling obtains modified carbon aerogels；
（3）Tin ash, Graphene mixed grinding is uniform, to heat 15-20 minutes at 850-880 DEG C, cooling adds ethanol In, nano tungsten trioxide is added while stirring, 3-4 hours are stirred, obtain mixed material；
（4）By carbon aerogels: white carbon black: sodium carboxymethyl cellulose: butadiene-styrene rubber=84: 10: 1: 5 weighings, send into ball mill ball milling 0.5-0.7h, adds water and butadiene-styrene rubber, mixed material, and again ball milling 2-2.3h obtains slurry, and slurry is uniform with coating machine To be coated on thickness be on 20-22 μm of aluminium foil, in 85-90 DEG C of drying, to obtain positive electrode.
CN201611244213.4A 2016-12-29 2016-12-29 High-specific-capacity cobaltosic oxide nanowire carbon aerogel hybrid supercapacitor anode material and preparation method thereof Pending CN106683902A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1567493A (en) * 2003-07-03 2005-01-19 中国科学院电工研究所 A composite carbon-based electrode material for super capacitor and method for making same
CN101468795A (en) * 2007-12-25 2009-07-01 成都思摩纳米技术有限公司 Preparation of high specific surface carbon aerogel
CN103413695A (en) * 2013-07-19 2013-11-27 北京航空航天大学 Macroscopic-quantity preparation method for macroscopic three-dimensional graphene/tin oxide composite material
CN103449424A (en) * 2012-08-28 2013-12-18 武汉大学 Low temperature preparation method of graphene and graphene-based composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1567493A (en) * 2003-07-03 2005-01-19 中国科学院电工研究所 A composite carbon-based electrode material for super capacitor and method for making same
CN101468795A (en) * 2007-12-25 2009-07-01 成都思摩纳米技术有限公司 Preparation of high specific surface carbon aerogel
CN103449424A (en) * 2012-08-28 2013-12-18 武汉大学 Low temperature preparation method of graphene and graphene-based composite material
CN103413695A (en) * 2013-07-19 2013-11-27 北京航空航天大学 Macroscopic-quantity preparation method for macroscopic three-dimensional graphene/tin oxide composite material

Non-Patent Citations (2)

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Title
FANG ZHANG等: ""Facile growth of mesoporous Co3O4 nanowire arrays on Ni foam for high performance electrochemical capacitors"", 《JOURNAL OF POWER SOURCES》 *
GUANGLIN SUN等: ""Incorporation of homogeneous Co3O4 into a nitrogen-doped carbon aerogel via a facile in situ synthesis method： implications for high performance asymmetric supercapacitors"", 《JOURNAL OF MATERIALS CHEMISTRY A》 *

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