CN102157271A - Super capacitor - Google Patents

Super capacitor Download PDF

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Publication number
CN102157271A
CN102157271A CN201110003537XA CN201110003537A CN102157271A CN 102157271 A CN102157271 A CN 102157271A CN 201110003537X A CN201110003537X A CN 201110003537XA CN 201110003537 A CN201110003537 A CN 201110003537A CN 102157271 A CN102157271 A CN 102157271A
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oxide
ultracapacitor
metallic element
super capacitor
compound
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唐伟
田舒
李琳琳
刘丽丽
施轶
朱凯
吴宇平
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Fudan University
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Fudan University
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    • 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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  • Electric Double-Layer Capacitors Or The Like (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention belongs to the technical field of chemical power sources, in particular to a super conductor. Negative electrode active substances of the super capacitor are oxide which has metal elements with two oxidation states except vanadium, and modified compounds of the oxide. The electrolyte of the super capacitor is aqueous solution containing alkaline metal ion. The negative active substance is the known active material. Compared with the conventional aqueous solution system super capacitor, the super capacitor has higher energy density and better safety performance. In addition, the capacitor also has excellent rate performance and better cycle performance. The super conductor has strong operability and good repeatability; and products produced by the super capacitor have stable product quality and good performance.

Description

A kind of ultracapacitor
Technical field
The invention belongs to technical field of chemical power, be specifically related to a kind of ultracapacitor.
Background technology
Along with the continuous expansion of information-intensive society and the appearance of environment and energy crisis, store energy and transformation efficiency problem become more and more important.As everyone knows, ultracapacitor have characteristics such as power density is big, good cycle, memory-less effect (referring to Wu Yuping, etc., " green power supply material ". Beijing: Chemical Industry Press, 2008).But along with the development of technology, the energy density that presses for ultracapacitor can improve constantly, and will have excellent cycle performance and high security performance simultaneously.
Ultracapacitor at present commonly used has two kinds of water solution system and organic solution systems.But they adopt the raw material of wood-charcoal material as negative material basically, and actual energy density is low, generally are no more than 20 Wh/kg, mainly contain active carbon // active carbon, active carbon // metal oxide, active carbon //Ni (OH) 2Wherein metal oxide is as positive electrode, mainly comprises RuO 2, PbO 2, MoO 3And MnO 2Deng.
In order to improve the energy density of ultracapacitor, 2005 patent of invention (CN200510025269.6) a kind of ultracapacitor of water solution system, the embedding compound such as the LiMn that just very contain lithium in this ultracapacitor are disclosed 2O 4Canadian Patent (CA 2413453) discloses the Nb that a kind of employing contains vanadium 2O 5Positive active material as ultracapacitor.But disclosing of non-carbon cathode material arranged seldom.2006 the 16th volumes of publication Adv. Mater. disclose the negative material of the compound of VN as ultracapacitor for the 1178th page-1182 pages, but the non-constant of cycle performance; A kind of oxide that adopts vanadium or their modified compound are disclosed in applicant's in 2010 the patent of invention (CN201010162397.6) as negative electrode active material.Based on above series of studies, the inventor is through for many years effort, find except that vanadium, to have the oxide of metallic element of two kinds of oxidation state and the active material that modified compound can be used as super capacitor anode thereof, and have energy density height, advantage that power density is high.
Summary of the invention
In order to overcome the at present existing low density problem of capacity of super capacitor, the invention provides the ultracapacitor that a kind of security performance is good, capacity is high, cycle performance is good.
Ultracapacitor provided by the present invention, its negative active core-shell material is the oxide of metallic element that has two kinds of oxidation state except that vanadium or their modified compound.Described metallic element oxide comprises Fe 3O 4, Fe 2O 3, Mn 2O 3, Co 3O 4, MoO 3, MoO 2, WO 3Or WO 2Can be a kind of metallic element oxide, also can be the oxide of two or more metallic element, or the mixture of the modified compound of described oxide, or the hopcalite of they and vanadium.
The modified compound of described metallic element oxide is their coating compound, doped compound or hydrate.
Described coating compound is material with carbon element, polymeric material or other oxide.Wherein polymeric material is a kind of or wherein several mixture in polyaniline, polypyrrole, the polythiophene, and other oxide is ruthenium-oxide, manganese oxide, tungsten oxide or titanium oxide or their mixture.
Described ultracapacitor adopts the aqueous solution, organic solution or ionic liquid as electrolyte, and positive active material is existing ultracapacitor known material commonly used.Wherein electrolyte contains alkali metal ion, a kind of or wherein several as in lithium ion, sodium ion, potassium ion, the rubidium ion; The concentration of alkali metal ion is 0.001 mol/l-15 mol/l; Positive active material is a kind of or wherein several mixture in active carbon, ruthenium-oxide, manganese oxide, tungsten oxide, niobium oxide, polyaniline, polypyrrole, the polythiophene or their doped compound.
Have specific energy height, high rate during charging-discharging is good, cycle performance is good characteristics by ultracapacitor provided by the invention, have good security performance.And strong operability of the present invention, favorable reproducibility, steady quality.
Description of drawings
The molybdenum trioxide scanning of materials Electronic Speculum figure of the different nanostructures of preparation among Fig. 1: the embodiment 1,2,3.
The cyclic voltammetry curve of molybdenum trioxide material under 1 mV/s sweep speed of the different nanostructures of preparation among Fig. 2: the embodiment 1,2,3.
The specific capacity of molybdenum trioxide material under different scanning speed of the different nanostructures of preparation among Fig. 3: the embodiment 1,2,3.
Ultracapacitor is at 400 W/kg charging and discharging curves among Fig. 4: the embodiment 1.
Cycle performance when ultracapacitor discharges and recharges under 2200 W/kg for a long time among Fig. 5: the embodiment 1.
The power density of ultracapacitor among Fig. 6: the embodiment 1,3.
Embodiment
Further describe the present invention below by specific embodiment.
Comparative Examples 1
Active carbon with aperture 2 nanometers is a negative electrode active material, mixes with the conductive black (conductive agent) of 15wt.% (is benchmark with the negative electrode active material) and the polytetrafluoroethylene (adhesive) of 5wt.%, is compressed on the nickel screen, as the negative pole of ultracapacitor; Active carbon with aperture 2 nanometers is a positive active material, mixes with the conductive black (conductive agent) of 15wt.% (is benchmark with the positive active material) and the polytetrafluoroethylene (adhesive) of 5wt.%, is compressed on the nickel screen, as the positive pole of ultracapacitor; Electrolyte is that to contain 0.5 mol/l lithium ion, pH be that 8 sulfate liquor is as electrolyte; Barrier film is a nonwoven fabrics; Form ultracapacitor.
Electrochemical property test: above-mentioned capacitor is discharged and recharged between 0V-1.2V (because liberation of hydrogen can't reach 1.8V), current density is that (weight is benchmark with total component of above-mentioned capacitor for 10 W/kg, 1000 W/kg and 2000 W/kg, do not contain the ultracapacitor shell, down together), the energy density of gained is respectively 3.8 Wh/kg, 2.1 Wh/kg and 1.6 Wh/kg.
Embodiment 1:
Take by weighing a certain amount of simple substance molybdenum and put into round-bottomed flask, add a certain amount of 30% hydrogen peroxide in flask under the ice-water bath condition, stirring reaction obtains yellow transparent peroxide molybdic acid colloidal sol.Adding crystal grain is the polystyrene moulding of 200nm-250nm, adsorbs 1 hour, and ageing is spent the night, and puts into crucible, in Muffle furnace, with 1 oC/min speed is warming up to 450 oC keeps half an hour, is cooled to room temperature, obtains the MoO of nano-sheet 3(the ESEM collection of illustrative plates is shown in accompanying drawing 1a), nanometer sheet size are 1 mm ', 1 mm ', 100 nm.
Adopting the molybdenum trioxide nano sheet is the active material of negative pole, mixes with the acetylene black (conductive agent) of 10 wt.% (is benchmark with the negative electrode active material) and the polytetrafluoroethylene (adhesive) of 10 wt.%, is compressed on the nickel screen, as the negative pole of ultracapacitor; Use the nickel screen conduct to electrode, saturated calomel electrode as reference electrode and to contain 0.5 mol/l lithium ion, pH be 8 sulfate liquor as electrolyte form three-electrode system-0.1 ~-carry out cyclic voltammetry scan between 0.85V, be shown in accompanying drawing 2 and Fig. 3 at cyclic voltammetry curve under 1 mV/s and the specific capacity under the different scanning speed; Active carbon with aperture 2 nanometers is the active material of positive pole, mixes with the acetylene black (conductive agent) of 10wt.% (is benchmark with the positive active material) and the polytetrafluoroethylene (adhesive) of 10wt.%, is compressed on the nickel screen, as the positive pole of ultracapacitor; Electrolyte be contain 0.5 mol/l lithium ion, pH be 8 sulfate liquor as electrolyte, barrier film is identical with Comparative Examples 1, forms ultracapacitor.
Above-mentioned ultracapacitor is discharged and recharged between 0V-1.8V, and current density range is 400-2200 W/kg (weight is benchmark with total component of above-mentioned capacitor, does not contain the ultracapacitor shell).The ultracapacitor that is assembled into is shown in Fig. 4 at 400 W/kg charging and discharging curves, and the cycle performance when discharging and recharging for a long time under 2200 W/kg is illustrated in Fig. 5.Test its energy density under different current densities, and calculate its power density, the results are shown in Fig. 6.Under the current density of 428 W/kg, energy density is 45 Wh/kg; Under the current density of 1928 W/kg, energy density is 29.5 Wh/kg.
Embodiment 2:
Polystyrene moulding is carried out preliminary treatment, processing method is specifically: get the PDDA(poly(diallyldimethyl-ammonium chloride that a certain amount of polystyrene powder is scattered in) in (molecular weight is 100000, concentration be 2.0 wt.%) solution, soaked 30 minutes, centrifugal back is standby.
Prepare molybdenum trioxide according to method identical among the embodiment 1, resulting molybdenum trioxide is nano bar-shape structure (the ESEM collection of illustrative plates is shown in accompanying drawing 1b), and this nano structured unit size is 200 nm ', 200 nm ', 2 mm.
Carry out electrochemical property test according to method identical among the embodiment 1, be shown in accompanying drawing 2 and Fig. 3 at cyclic voltammetry curve that obtains under the sweep speed of 1mV/s and the specific capacity under the different scanning speed.
Embodiment 3:
Take by weighing a certain amount of simple substance molybdenum and put into round-bottomed flask, add a certain amount of 30% hydrogen peroxide in flask under the ice-water bath condition, stirring reaction obtains yellow transparent peroxide molybdic acid colloidal sol.Ageing is spent the night, and puts into crucible, in Muffle furnace, with 1 oC/min speed is warming up to 450 oC keeps half an hour, is cooled to room temperature, and obtaining is the MoO of the big thin, soft plain-weave silk fabric taper of 1 mm 3(the ESEM collection of illustrative plates is shown in accompanying drawing 1c).Carry out electrochemical property test according to method identical among the embodiment 1, specific capacity under resulting cyclic voltammetry curve and the different scanning speed is shown in accompanying drawing 2 and Fig. 3 equally, test its energy density under different current densities, and calculate its power density, the results are shown in Fig. 6.Energy density is 31 Wh/kg under the power density of 421 W/kg.
Embodiment 4:
With a certain amount of phosphomolybdic acid (H 3PMo 12O 40.6H 2O) be dissolved in the 5ml absolute ethyl alcohol, obtain bright yellow solution, add 3.0g phenolic resins then, ultrasonic dispersion, magnetic agitation is volatilized fully until ethanol.The gained material is calcining at a certain temperature under inert gas shielding, takes out behind the natural cooling, obtains the molybdenum trioxide spheroidal particle that the raw material of wood-charcoal material package is covered, and average grain diameter is 3 mm.
Carry out electrochemical property test according to method identical among the embodiment 1, the result shows that its energy density under the power density of 436 W/kg is 46 Wh/kg.
Embodiment 5:
The molybdenum trioxide nano sheet of getting preparation among the embodiment 1 carries out polypyrrole and coats, and polypyrrole coats thickness 20 nm, and concrete encapsulation steps is as follows:
Material is immersed in the certain density neopelex solution, stirs a period of time, drip ferric chloride solution (FeCl 3) and pyrrole monomer ,-30 oC stirred 1 hour down, and suction filtration, washing, alcohol are washed, drying, can obtain the molybdenum trioxide nano sheet that polypyrrole coats.
Change the Li that uses lithium doping into except positive electrode xMnO 2(x=0.5), other with embodiment 1 in identical method carry out electrochemical property test, the result shows that its energy density under the power density of 450 W/kg is 75 Wh/kg.
Embodiment 6:
With 1 mol/l ferric chloride aqueous solutions, add the biphosphate sodium water solution of equal-volume 0.2 mol/l then, after stirring, change closed reactor over to, the sealing back is 200 oConstant temperature was handled 24 hours under the C, took out reactor then, and natural cooling in air is separated red precipitate in the still, washed 3 times, in the air 80 oThe C oven dry promptly gets a-di-iron trioxide nano wire.
Carry out electrochemical property test according to method identical among the embodiment 1, the result shows that its energy density under the power density of 2 kW/kg is 32 Wh/kg.
Embodiment 7:
The a-di-iron trioxide nano wire that embodiment 6 obtains is put into a high temperature process furnances, feed reducing gases, be warming up to 600 oC, heat treatment is 5 hours under this temperature, naturally cools to room temperature, promptly gets the ferriferrous oxide nano line.
Carry out electrochemical property test according to method identical among the embodiment 1, the result shows that its energy density under the power density of 2 kW/kg is 29 Wh/kg, shows good high-power performance.
Embodiment 8:
With 2 mol/l ferric chloride aqueous solutionses, add the ammonia spirit of equal-volume 6 mol/l then, after stirring, then 80 oConstant temperature was handled 2 hours under the C, obtained red precipitate, with deionized water wash 3 times, in air 100 oThe C drying promptly obtains spherical a-di-iron trioxide particle, and average grain diameter is 3 mm.
Carry out electrochemical property test according to method identical among the embodiment 1, the result shows that its energy density under the power density of 2 kW/kg is 18 Wh/kg, shows good high-power performance.
Comparative Examples 2
Except electrolyte is 1 mol/l LiPF 6Vinyl carbonate/Methylethyl carbonate solution (volume ratio 1:1), barrier film be outside the porous polypropylene, other conditions are identical with Comparative Examples 1 with material, form ultracapacitor in the glove box of anhydrous and oxygen-free.
Electrochemical property test: above-mentioned capacitor is discharged and recharged between 0V-3 V, current density is that (weight is benchmark with total component of above-mentioned capacitor for 10 W/kg, 1000 W/kg and 2000 W/kg, do not contain the ultracapacitor shell, down together), the energy density of gained is respectively 3.1 Wh/kg, 1.4 Wh/kg and 1.2 Wh/kg.
Embodiment 9
Except electrolyte is 1 mol/l LiPF 6Vinyl carbonate/Methylethyl carbonate solution (volume ratio 1:1), barrier film be outside the porous polypropylene, other conditions are identical with embodiment 2 with material, form ultracapacitor in the glove box of anhydrous and oxygen-free.
Carry out electrochemical property test according to method identical in the Comparative Examples 2, the result shows it under the power density of 302 W/kg, and energy density is 25.8 Wh/kg, is higher than the energy density in the Comparative Examples 2.
By the contrast of the foregoing description and Comparative Examples, as can be seen: embodiments of the invention have good electrochemical, the energy density height, and under high-power, also have high energy density.

Claims (8)

1. a ultracapacitor is characterized in that negative electrode active material is the oxide that has the metallic element of two kinds of oxidation state except that vanadium, or the modified compound of metallic element oxide.
2. ultracapacitor according to claim 1, the metallic element oxide that wherein has two kinds of oxidation state except that vanadium is Fe 3O 4, Fe 2O 3, Mn 2O 3, Co 3O 4, MoO 3, MoO 2, WO 3Or WO 2
3. ultracapacitor according to claim 1 and 2 is characterized in that negative electrode active material is the oxide of two or more described metallic element, or the mixture of its modified compound, or the hopcalite of described metallic element oxide and vanadium.
4. ultracapacitor according to claim 1 is characterized in that coating compound, doped compound or the hydrate of the modified compound of metallic element oxide for them.
5. ultracapacitor according to claim 4 is characterized in that described coating compound is material with carbon element, polymeric material or other oxide; Wherein, described polymeric material is a kind of or wherein several mixture in polyaniline, polypyrrole, the polythiophene; Described other oxide is ruthenium-oxide, manganese oxide, tungsten oxide or titanium oxide, or their mixture.
6. ultracapacitor according to claim 1 is characterized in that adopting the aqueous solution, organic solution or ionic liquid as electrolyte.
7. ultracapacitor according to claim 6 is characterized in that described electrolyte contains a kind of or wherein several in following alkali metal ion lithium ion, sodium ion, potassium ion, the rubidium ion; The concentration of alkali metal ion is 0.001 mol/l-15 mol/l.
8. according to any one described ultracapacitor among the claim 1-7, it is characterized in that described positive active material is a kind of or wherein several mixture in active carbon, ruthenium-oxide, manganese oxide, tungsten oxide, niobium oxide, polyaniline, polypyrrole, the polythiophene, or their doped compound.
CN201110003537XA 2011-01-10 2011-01-10 Super capacitor Pending CN102157271A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103613759A (en) * 2013-12-06 2014-03-05 东华大学 Preparation method of MoO3/polyaniline coaxial nano heterojunction
CN105355460A (en) * 2015-11-27 2016-02-24 中南大学 High-voltage water-based asymmetric super capacitor and preparation method thereof
CN105374577A (en) * 2015-11-23 2016-03-02 太原理工大学 Preparation and application of molybdenum oxide powder electrode material with high specific capacitance characteristics
CN106558423A (en) * 2016-11-21 2017-04-05 华中科技大学 Fe2O3Laminar nano array, the Fe with layer structure2O3/ PPy flexible composites and preparation and application
CN107742588A (en) * 2017-11-09 2018-02-27 安徽大学 A kind of preparation method of high-performance super capacitor electrode
CN108287190A (en) * 2017-01-09 2018-07-17 天津大学 A kind of cubical array electrode and its preparation method and application of polypyrrole cladding cobaltosic oxide nano line
CN108642446A (en) * 2018-06-01 2018-10-12 广东工业大学 A kind of porous C rN coatings and preparation method thereof and a kind of ultracapacitor
CN109243831A (en) * 2017-07-10 2019-01-18 清华大学深圳研究生院 Lithium-ion capacitor and preparation method thereof
CN111883757A (en) * 2020-07-27 2020-11-03 陕西科技大学 Polypyrrole-coated Fe serving as pseudo-capacitor material2O3/Mn2O3Composite material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5426561A (en) * 1992-09-29 1995-06-20 The United States Of America As Represented By The United States National Aeronautics And Space Administration High energy density and high power density ultracapacitors and supercapacitors
CN1420507A (en) * 2002-09-12 2003-05-28 锦州锦容超级电容器有限责任公司 High specific energy super copacitor for vehicle
CN101814379A (en) * 2010-04-28 2010-08-25 复旦大学 Super capacitor
CN101916663A (en) * 2010-08-03 2010-12-15 清华大学 Hybrid micro super capacitor and manufacturing method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5426561A (en) * 1992-09-29 1995-06-20 The United States Of America As Represented By The United States National Aeronautics And Space Administration High energy density and high power density ultracapacitors and supercapacitors
CN1420507A (en) * 2002-09-12 2003-05-28 锦州锦容超级电容器有限责任公司 High specific energy super copacitor for vehicle
CN101814379A (en) * 2010-04-28 2010-08-25 复旦大学 Super capacitor
CN101916663A (en) * 2010-08-03 2010-12-15 清华大学 Hybrid micro super capacitor and manufacturing method thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103613759A (en) * 2013-12-06 2014-03-05 东华大学 Preparation method of MoO3/polyaniline coaxial nano heterojunction
CN103613759B (en) * 2013-12-06 2015-10-28 东华大学 A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction
CN105374577B (en) * 2015-11-23 2018-08-24 太原理工大学 Preparation and application with high specific capacitance characteristic molybdenum oxide powder electrode material
CN105374577A (en) * 2015-11-23 2016-03-02 太原理工大学 Preparation and application of molybdenum oxide powder electrode material with high specific capacitance characteristics
CN105355460B (en) * 2015-11-27 2018-06-01 中南大学 A kind of aqueous Asymmetric Supercapacitor of high voltage and preparation method thereof
CN105355460A (en) * 2015-11-27 2016-02-24 中南大学 High-voltage water-based asymmetric super capacitor and preparation method thereof
CN106558423A (en) * 2016-11-21 2017-04-05 华中科技大学 Fe2O3Laminar nano array, the Fe with layer structure2O3/ PPy flexible composites and preparation and application
CN108287190A (en) * 2017-01-09 2018-07-17 天津大学 A kind of cubical array electrode and its preparation method and application of polypyrrole cladding cobaltosic oxide nano line
CN109243831A (en) * 2017-07-10 2019-01-18 清华大学深圳研究生院 Lithium-ion capacitor and preparation method thereof
CN107742588A (en) * 2017-11-09 2018-02-27 安徽大学 A kind of preparation method of high-performance super capacitor electrode
CN107742588B (en) * 2017-11-09 2019-04-16 安徽大学 A kind of preparation method of high-performance super capacitor electrode
CN108642446A (en) * 2018-06-01 2018-10-12 广东工业大学 A kind of porous C rN coatings and preparation method thereof and a kind of ultracapacitor
CN111883757A (en) * 2020-07-27 2020-11-03 陕西科技大学 Polypyrrole-coated Fe serving as pseudo-capacitor material2O3/Mn2O3Composite material and preparation method thereof

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Application publication date: 20110817