CN102683037A - Manganese dioxide asymmetric super capacitor and manufacturing method thereof - Google Patents
Manganese dioxide asymmetric super capacitor and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to a manganese dioxide asymmetric super capacitor and a manufacturing method of the super capacitor; the manganese dioxide asymmetric super capacitor is characterized in that a positive pole of the super capacitor is made of flower-like manganese dioxide or nano manganese dioxide/ active carbon composite material with higher pseudocapacitance, and a negative pole of the super capacitor is made of porous carbon with large specific surface area; a water solution system containing univalent or divalent cation is adopted as electrolyte of the super capacitor; and the asymmetric super capacitor formed by encapsulation has the characteristics of being higher in energy density, low in cost, safe and free from pollution.
Description
Technical field
The present invention relates to asymmetric ultracapacitor of a kind of manganese dioxide and preparation method thereof, belong to battery and ultracapacitor technical field.
Background technology
Ultracapacitor be a kind ofly have the specific power density height, have extended cycle life, the novel energy-storing device of characteristics such as charge-discharge magnification height, have a wide range of applications in fields such as electric automobile, aviation national defence, telecommunications.Ultracapacitor mainly contains positive pole, barrier film, negative pole, electrolyte and encapsulating housing to be formed, and wherein electrode active material directly influences the ultracapacitor performance.
According to ultracapacitor energy storage mechanism; Can material be divided into two types: the one, utilize electric double layer mechanism to come the electric double layer material of storage power; Like active carbon, NACF, CNT, charcoal gel etc., this type material is to rely on the Electrostatic Absorption electrolyte ion to form the purpose that electric double layer reaches energy storage; The 2nd, utilize itself and electrolyte ion generation redox reaction to come the fake capacitance material of energy storage; Like ruthenium-oxide, vanadium oxide, nickel oxide and manganese dioxide etc.; Because this type material relates to absorption/desorption or oxidation/reduction reaction; Therefore having higher ratio electric capacity, is an important directions that improves the research of ultracapacitor energy density.Ruthenium-oxide is wherein most typical representative, and up to 720F/g, still because the price of ruthenium is more expensive, the fake capacitance that the amorphous aquation ruthenium of report produces in the document does not suit large-scale production than electric capacity.
Manganese dioxide since its wide material sources, cheap, chemical property good, eco-friendly characteristics receive the researcher concern (like CN1438181; CN1715460; CN1792820; CN1758468; CN1758468; CN101372363; CN101417820; CN101700912A; CN101597086; CN101531402; CN101607740), the reaction mechanism of manganese dioxide in ultracapacitor is to rely on fast transition between manganese dioxide and the water manganese stone to store and discharge electric charge, because this process is reversible highly fast; Therefore it can realize high current charge-discharge; Have high energy density and power density, therefore, manganese dioxide is expected to as electrode material for super capacitor; Realization reduces cost, and improves the purpose of specific energy.Must adopt the strong acid and strong base electrolyte with respect to other metal oxides or carbon back ultracapacitor, the manganese dioxide based super capacitor can adopt neutral electrolyte solution, and this makes the assembling of manganese dioxide based super capacitor and uses safer, more convenient.Therefore, the manganese dioxide based super capacitor is a kind of safety, cost is low, energy density is high, free of contamination novel power supply device, has broad prospects in fields such as new-energy automobiles.
Summary of the invention
The object of the present invention is to provide asymmetric ultracapacitor of a kind of manganese dioxide and preparation method thereof, ultracapacitor that particularly a kind of flower-shaped manganese dioxide or nano-manganese dioxide/absorbent charcoal composite material and active carbon are formed and preparation method thereof, its manganese bioxide material have the flower-like structure of rule; Form asymmetric ultracapacitor with porous carbon material; Can further improve energy density, adopt neutral electrolyte, have bigger electromotive force window; Safety, cost are low, pollution-free; Preparation technology is simple, and cost is lower, is expected to be used for new-energy automobile.
Technical scheme of the present invention is achieved in that the asymmetric ultracapacitor of manganese dioxide; Be superimposed as power brick successively by positive pole, barrier film and negative pole and put into encapsulating housing; Electrolyte pours into encapsulating housing inside; It is characterized in that its preparation method is following: positive active material, conductive agent, binding agent evenly apply on the nickel foam according to after quality ratio of components 70 ~ 90:5 ~ 20:1 ~ 10 adding absolute ethyl alcohols are dispersant, and positive pole is processed in 80 ℃ of oven dry, roll-in, sections; Negative electrode active material, conductive agent, binding agent evenly apply on the nickel foam according to after quality ratio of components 65 ~ 95:5 ~ 20:1 ~ 10 adding absolute ethyl alcohols are dispersant, and negative pole is processed in 80 ℃ of oven dry, roll-in, sections; Wherein positive active material is for to process through the flower-shaped manganese dioxide or the nano-manganese dioxide/absorbent charcoal composite material of Hydrothermal Preparation: (1) flower-shaped manganese dioxide: take by weighing potassium permanganate 1.0g and hydrated manganese sulfate 0.5g, be dissolved in respectively then and obtain solution 15ml and 5ml in the deionized water; Under the condition of strong mixing, manganese sulfate solution is dropped in the liquor potassic permanganate, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, obtained brownish black to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate and precipitate; Dry 24h under deionized water wash, the 80 ℃ of conditions makes flower-shaped manganese dioxide; (2) nano-manganese dioxide and absorbent charcoal composite material: take by weighing the 0.5g active carbon at 15ml deionized water for ultrasonic 1h, add potassium permanganate 1.0g, ultrasonic 2h; The 0.5g hydrated manganese sulfate is dissolved in the 5ml deionized water ultrasonic 2h; Under the condition of strong mixing, manganese sulfate solution is dropped in potassium permanganate/Actidose, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate, deionized water wash, dry 24h under 80 ℃ of conditions makes nano-manganese dioxide/absorbent charcoal composite material;
Negative electrode active material is a kind of in rice hull carbon, apricot shell charcoal, coconut husk charcoal, bamboo matter charcoal, asphalt based active carbon, coal mass active carbon, activated carbon fiber, CNT, the Graphene.
Described conductive agent is a kind of in conductive black, electrically conductive graphite, gas-phase growth of carbon fibre (VGCF), CNT or the acetylene black.
Described binding agent is polytetrafluoroethylene, gather a kind of in inclined to one side tetrafluoroethene or the sodium carboxymethylcellulose.
Described barrier film is a kind of in the composite membrane, polyethene microporous membrane, polypropylene non-woven fabric of PP and PE.
Described electrolyte is the aqueous solution that contains monovalence or bivalent cation, and electrolyte is potassium sulfate, sodium sulphate, potassium chloride, sodium chloride, lithium sulfate, calcium nitrate, potassium hydroxide, and its concentration of electrolyte is 0.1 ~ 6mol/L.
Described encapsulating housing is metal shell or non-metal shell.
Good effect of the present invention is that its manganese bioxide material has the flower-like structure and the porous carbon material of rule and forms asymmetric ultracapacitor, can further improve energy density; Adopt neutral electrolyte; Have bigger electromotive force window, safety, cost are low, pollution-free, and preparation technology is simple; Cost is lower, is expected to be used for new-energy automobile.
Description of drawings
Fig. 1 is the flower-shaped manganese bioxide material SEM of a positive active material of the present invention picture.
Fig. 2 is the present invention's cyclic voltammogram in the 0.5mol/L metabisulfite solution when sweep speed is 10mV/s.
Fig. 3 is the present invention's cyclic voltammogram in the 0.5mol/L metabisulfite solution when sweep speed is 10mV/s.
Fig. 4 is the charging and discharging curve of the present invention under constant current 10mA.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further: the asymmetric ultracapacitor of manganese dioxide; Be superimposed as power brick successively by positive pole, barrier film and negative pole and put into encapsulating housing; Electrolyte pours into encapsulating housing inside; It is characterized in that its preparation method is following: positive active material, conductive agent, binding agent evenly apply on the nickel foam according to after quality ratio of components 70 ~ 90:5 ~ 20:1 ~ 10 adding absolute ethyl alcohols are dispersant, and positive pole is processed in 80 ℃ of oven dry, roll-in, sections; Negative electrode active material, conductive agent, binding agent evenly apply on the nickel foam according to after quality ratio of components 65 ~ 95:5 ~ 20:1 ~ 10 adding absolute ethyl alcohols are dispersant, and negative pole is processed in 80 ℃ of oven dry, roll-in, sections; Positive active material is for to process through the flower-shaped manganese dioxide or the nano-manganese dioxide/absorbent charcoal composite material of Hydrothermal Preparation: (1) flower-shaped manganese dioxide: take by weighing potassium permanganate 1.0g and hydrated manganese sulfate 0.5g, be dissolved in respectively then and obtain solution 15ml and 5ml in the deionized water; Under the condition of strong mixing, manganese sulfate solution is dropped in the liquor potassic permanganate, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, obtained brownish black to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate and precipitate; Dry 24h under deionized water wash, the 80 ℃ of conditions makes flower-shaped manganese dioxide; (2) nano-manganese dioxide and absorbent charcoal composite material: take by weighing the 0.5g active carbon at 15ml deionized water for ultrasonic 1h, add potassium permanganate 1.0g, ultrasonic 2h; The 0.5g hydrated manganese sulfate is dissolved in the 5ml deionized water ultrasonic 2h; Under the condition of strong mixing, manganese sulfate solution is dropped in potassium permanganate/Actidose, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate, deionized water wash, dry 24h under 80 ℃ of conditions makes nano-manganese dioxide and absorbent charcoal composite material; Negative electrode active material is a kind of in rice hull carbon, apricot shell charcoal, coconut husk charcoal, bamboo matter charcoal, asphalt based active carbon, coal mass active carbon, activated carbon fiber, CNT, the Graphene.
Described conductive agent is a kind of in conductive black, electrically conductive graphite, gas-phase growth of carbon fibre (VGCF), CNT or the acetylene black.
Described binding agent is polytetrafluoroethylene, gather a kind of in inclined to one side tetrafluoroethene or the sodium carboxymethylcellulose.
Described barrier film is a kind of in the composite membrane, polyethene microporous membrane, polypropylene non-woven fabric of PP and PE.
Described electrolyte is the aqueous solution that contains monovalence or bivalent cation, and electrolyte is potassium sulfate, sodium sulphate, potassium chloride, sodium chloride, lithium sulfate, calcium nitrate, potassium hydroxide, and its concentration of electrolyte is 0.1 ~ 6mol/L.
Described encapsulating housing is metal shell or non-metal shell.
Embodiment 1
Take by weighing potassium permanganate 1.0g and hydrated manganese sulfate 0.5g, be dissolved in respectively then and obtain solution 15ml and 5ml in the deionized water; Under the condition of strong mixing, manganese sulfate solution is dropped in the liquor potassic permanganate, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, obtained brownish black to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate and precipitate; Dry 24h under deionized water wash, the 80 ℃ of conditions makes flower-shaped manganese dioxide.
With the absolute ethyl alcohol is dispersant, and flower-shaped manganese dioxide and conductive agent VGCF with preparation after polyfluortetraethylene of binding element is the mixed of 80:15:5 by mass ratio, evenly apply on the nickel foam, and 80 ℃ of oven dry make positive pole.
With the absolute ethyl alcohol is dispersant, with active carbon and conductive agent VGCF, after polyfluortetraethylene of binding element is the mixed of 80:15:5 by mass ratio, evenly applies on the nickel foam, and negative pole is processed in 80 ℃ of oven dry.
Positive pole, barrier film, the negative pole encapsulating housing of packing into that superposes successively is that electrolyte pours into encapsulating housing and processes capacitor with the 0.5mol/L metabisulfite solution.
Take by weighing the 0.5g active carbon at 15ml deionized water for ultrasonic 1h, add potassium permanganate 1.0g, ultrasonic 2h; The 0.5g hydrated manganese sulfate is dissolved in the 5ml deionized water ultrasonic 2h; Under the condition of strong mixing, manganese sulfate solution is dropped in potassium permanganate/Actidose, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate, deionized water wash, dry 24h under 80 ℃ of conditions makes nano-manganese dioxide/absorbent charcoal composite material.
With the absolute ethyl alcohol is dispersant; With nano-manganese dioxide and the flower-shaped manganese dioxide of absorbent charcoal composite material and the conductive agent VGCF of preparation, polyfluortetraethylene of binding element evenly applies on the nickel foam after being the mixed of 85:10:5 by mass ratio; 80 ℃ of oven dry make positive pole.
With the absolute ethyl alcohol is dispersant, with active carbon and conductive agent VGCF, after polyfluortetraethylene of binding element is the mixed of 85:10:5 by mass ratio, evenly applies on the nickel foam, and negative pole is processed in 80 ℃ of oven dry.
Positive pole, barrier film, the negative pole encapsulating housing of packing into that superposes successively is that electrolyte pours into encapsulating housing and processes capacitor with the 2mol/L metabisulfite solution.
Embodiment 3
Take by weighing potassium permanganate 1.0g and hydrated manganese sulfate 0.5g, be dissolved in respectively then and obtain solution 15ml and 5ml in the deionized water; Under the condition of strong mixing, manganese sulfate solution is dropped in the liquor potassic permanganate, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, obtained brownish black to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate and precipitate; Dry 24h under deionized water wash, the 80 ℃ of conditions makes flower-shaped manganese dioxide.
With the absolute ethyl alcohol is dispersant, and flower-shaped manganese dioxide and conductive agent VGCF with preparation after polyfluortetraethylene of binding element is the mixed of 90:5:5 by mass ratio, evenly apply on the nickel foam, and 80 ℃ of oven dry make positive pole.
With the absolute ethyl alcohol is dispersant, with active carbon and conductive agent VGCF, after polyfluortetraethylene of binding element is the mixed of 90:5:5 by mass ratio, evenly applies on the nickel foam, and negative pole is processed in 80 ℃ of oven dry.
Positive pole, barrier film, negative pole are superposeed successively, and soldering polar ear soaks 24h at the 1mol/L metabisulfite solution, takes out, and wipes the unnecessary electrolyte in surface away, installs to then in the encapsulating housing of plastic housing to encapsulate, and processes ultracapacitor.
Claims (6)
1. the asymmetric ultracapacitor of manganese dioxide; Be superimposed as power brick successively by positive pole, barrier film and negative pole and put into encapsulating housing; Electrolyte pours into encapsulating housing inside; It is characterized in that its preparation method is following: positive active material, conductive agent, binding agent evenly apply on the nickel foam according to after quality ratio of components 70 ~ 90:5 ~ 20:1 ~ 10 adding absolute ethyl alcohols are dispersant, and positive pole is processed in 80 ℃ of oven dry, roll-in, sections; Negative electrode active material, conductive agent, binding agent evenly apply on the nickel foam according to after quality ratio of components 65 ~ 95:5 ~ 20:1 ~ 10 adding absolute ethyl alcohols are dispersant, and negative pole is processed in 80 ℃ of oven dry, roll-in, sections; Wherein positive active material is for to process through the flower-shaped manganese dioxide or the nano-manganese dioxide/absorbent charcoal composite material of Hydrothermal Preparation: (1) flower-shaped manganese dioxide: take by weighing potassium permanganate 1.0g and hydrated manganese sulfate 0.5g, be dissolved in respectively then and obtain solution 15ml and 5ml in the deionized water; Under the condition of strong mixing, manganese sulfate solution is dropped in the liquor potassic permanganate, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, obtained brownish black to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate and precipitate; Dry 24h under deionized water wash, the 80 ℃ of conditions makes flower-shaped manganese dioxide; (2) nano-manganese dioxide and absorbent charcoal composite material: take by weighing the 0.5g active carbon at 15ml deionized water for ultrasonic 1h, add potassium permanganate 1.0g, ultrasonic 2h; The 0.5g hydrated manganese sulfate is dissolved in the 5ml deionized water ultrasonic 2h; Under the condition of strong mixing, manganese sulfate solution is dropped in potassium permanganate and the Actidose, 10min is added dropwise to complete; Mixed liquor is transferred in the hydrothermal reaction kettle, to 90%, 100 ℃ of following hydro-thermal reaction 3h of filling rate, deionized water wash, dry 24h under 80 ℃ of conditions makes nano-manganese dioxide/absorbent charcoal composite material; Negative electrode active material is a kind of in rice hull carbon, apricot shell charcoal, coconut husk charcoal, bamboo matter charcoal, asphalt based active carbon, coal mass active carbon, activated carbon fiber, CNT, the Graphene.
2. the asymmetric ultracapacitor of manganese dioxide according to claim 1 is characterized in that described conductive agent is a kind of in conductive black, electrically conductive graphite, gas-phase growth of carbon fibre (VGCF), CNT or the acetylene black.
3. the asymmetric ultracapacitor of manganese dioxide according to claim 1 is characterized in that described binding agent is polytetrafluoroethylene, gathers a kind of in inclined to one side tetrafluoroethene or the sodium carboxymethylcellulose.
4. the asymmetric ultracapacitor of manganese dioxide according to claim 1 is characterized in that described barrier film is a kind of in the composite membrane, polyethene microporous membrane, polypropylene non-woven fabric of PP and PE.
5. the asymmetric ultracapacitor of manganese dioxide according to claim 1; It is characterized in that described electrolyte is the aqueous solution that contains monovalence or bivalent cation; Electrolyte is potassium sulfate, sodium sulphate, potassium chloride, sodium chloride, lithium sulfate, calcium nitrate, potassium hydroxide, and its concentration of electrolyte is 0.1 ~ 6mol/L.
6. the asymmetric ultracapacitor of manganese dioxide according to claim 1 is characterized in that described encapsulating housing is metal shell or non-metal shell.
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CN102891280A (en) * | 2012-10-08 | 2013-01-23 | 中国电子科技集团公司第十八研究所 | Preparation method for high-capacity lithium manganese battery positive plate |
CN103121725A (en) * | 2013-03-25 | 2013-05-29 | 华东理工大学 | Preparation method of nanometer manganese sesquioxide with a hollow cone shape |
CN103258656A (en) * | 2013-04-25 | 2013-08-21 | 华中科技大学 | Method for preparing electrodes of super capacitor based on nickel foam and products thereof |
CN103426650A (en) * | 2013-08-22 | 2013-12-04 | 吉林大学 | Asymmetric electrochemical supercapacitor on basis of rice-husk-based activated carbon materials |
CN103545122A (en) * | 2013-10-30 | 2014-01-29 | 中国第一汽车股份有限公司 | Preparation method for manganese dioxide/carbon composite materials used for super capacitor |
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CN105304352A (en) * | 2015-10-12 | 2016-02-03 | 哈尔滨工业大学深圳研究生院 | Method for preparing manganese dioxide/nickel hydroxide composite nano sheet by using nickel foam self-reaction and application of manganese dioxide/nickel hydroxide composite nano sheet to supercapacitor |
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