CN102087921B - Self-supporting super capacitor electrode material and preparation method thereof - Google Patents
Self-supporting super capacitor electrode material and preparation method thereof Download PDFInfo
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
Abstract
The invention discloses a self-supporting super capacitor electrode material and a preparation method thereof, belonging to the field of super capacitor electrode materials. The method is characterized by preparing a nano-micro fiber felt from polymer solution through high-voltage electrospinning, carrying out hot pressing and carbonizing to obtain a carbon nano fiber felt, soaking the carbon nano fiber felt in potassium permanganate solution at a certain temperature for a period of time, then washing the sheet with deionized water and ethanol several times to remove impurities, and drying at 60-110 DEG C for 8-24 hours, thus obtaining the manganese dioxide and carbon nano fiber composite electrode material. The manganese dioxide and carbon nano fiber composite electrode material prepared by the method dispenses with extra current collectors, conductive additives and binders, can be directly used, and has the characteristics of high electrode mechanical stability, self current collection, high active substance loading, excellent electrochemical performance and the like.
Description
Technical field
The invention belongs to the electrode material for super capacitor field, be specifically related to a kind of self-supporting super capacitor electrode material and preparation method thereof.
Background technology
Ultracapacitor is a kind of novel energy-storing device between classic flat-plate capacitor and chemical power source, there is high power density, large capacity, fast charging and discharging, overlength cycle life, pollute the advantage such as little, high reliability, its capacitance can reach a farad rank, at aspects such as mobile communication, information technology, electric power system, electric automobile, Aero-Space, all has broad application prospects.According to energy storage mechanism, ultracapacitor can be divided into double electric layer capacitor and fake capacitance device, the former is the electrostatic attraction stored energy of utilizing between electrode surface and electrolyte, this type of electrode material is mainly the carbon-based material with high-specific surface area, comprise active carbon, carbon aerogels, carbon nano-tube, carbon fiber and Graphene etc., but specific capacitance is lower; The latter relies on the redox reaction generation faraday electric charge between electrode material and electrolyte to carry out storing electricity, and the capacitance of generation is 10-100 times of electric double layer capacitance capacity, and such electrode material has metal oxide (as RuO
2, MnO
2, NiO, Co
3o
4deng) and conducting polymer (as polyaniline, polythiophene, polypyrrole etc.), wherein RuO
2the specific capacitance of electrode material is up to 720F/g, and has good conductivity, is a kind of material of excellent combination property, but because its price is high and toxic, thereby restriction RuO
2commercial application.Meanwhile, the poorly conductive of transition group metallic oxide, the cyclical stability of conduction high polymer is poor.Therefore, can prepare a kind of new electrode material for super capacitor with good electric chemical property by overcoming these electrode materials shortcoming separately, be expected to provide a kind of electrode material of high performance-price ratio in industrialization.
In transition group metallic oxide, MnO
2the advantage such as have aboundresources, environmental friendliness, higher than electric capacity, preparation cost is low, calculate its specific capacitance up to 1370F/g according to theory.Yet in actual applications, along with MnO
2the increase of loading, MnO
2specific capacitance only has 1/10th of theoretical value.
Recent study personnel have developed the multiple nanometer MnO for preparing bigger serface
2synthetic method, but its surface activity site still is difficult to take full advantage of; For this reason by MnO
2can solve preferably MnO with electric conducting material (as carbon nano-tube) is compound
2the problem that utilance is low, however the preparation cost of carbon nano-tube is very high and MnO
2loading limited, therefore, find a kind of cheap efficient composite preparation process extremely urgent.
Summary of the invention
The object of the invention is to provide a kind of and has the good electrical chemical property, process transplanting is strong, with low cost and eco-friendly self-supporting super capacitor electrode material, with two-way raising MnO
2ratio electric capacity and loading.
The present invention also aims to provide a kind of preparation method of self-supporting super capacitor electrode material.
A kind of self-supporting super capacitor electrode material, is characterized in that, the compound that described electrode material is manganese dioxide and carbon nano-fiber.
A kind of preparation method of self-supporting super capacitor electrode material, is characterized in that, comprises the steps:
(1) prepare the high polymeric solution of the dispersed 0.1-2% of having carbon nano-tube or Graphene;
(2) by regulation voltage, receiving range, solution flow rate, ambient humidity, ambient temperature, become nanometer to arrive the micron order fibrofelt high polymeric solution electrospinning;
(3) fibrofelt is carried out to hot pressing, hot pressing temperature is 60～200 ℃, and the time is 20～300s, and pressure is 0.25～10MPa;
(4) the fibrofelt carbonization after hot pressing is obtained to carbon nanofiber felt, carburizing atmosphere is nitrogen or argon gas, and temperature is 800～1500 ℃, and the time is 60～240min;
(5) preparation liquor potassic permanganate, its concentration is 0.005～2mol/L, by adding the concentrated sulfuric acid or red fuming nitric acid (RFNA) or concentrated hydrochloric acid regulator solution pH, is 0～7, utilizes heating water bath that solution temperature is adjusted to 0～90 ℃;
(6) carbon nanofiber felt be impregnated in the liquor potassic permanganate that step (5) prepares, after magnetic agitation reaction certain hour, carbon nanofiber felt is taken out, use deionized water and absolute ethanol washing for several times, until pH equals 7;
(7) carbon nanofiber felt after washing is put into to dry 8-24h under baking oven 60-110 ℃, obtain the combination electrode material of manganese dioxide and carbon nano-fiber.
High polymer in described high polymeric solution is polyacrylonitrile, polyimides, polyvinyl alcohol, Kynoar or pitch.
Beneficial effect of the present invention: 1, preparation technology is simple, and the operating condition gentleness is portable strong.2, the Electrospun productive rate is high, and the reagent of employing is common agents, with low cost.3, electrode material of the present invention, without extra collector, conductive additive and binding agent, has saved complicated electrode production process.4, MnO
2with the compound of carbon nano-fiber as electrode of super capacitor have mechanical stability high, from afflux, the characteristics such as the active material loading is high and chemical property is good.
The accompanying drawing explanation
Accompanying drawing 1 is preparation technology's of the present invention schematic diagram;
MnO prepared for the present invention by accompanying drawing 2
2combination electrode material XRD diffraction pattern with carbon nano-fiber;
MnO prepared for the present invention by accompanying drawing 3
2scanning electron microscope (SEM) photograph with the combination electrode material of carbon nano-fiber;
MnO prepared for the present invention by accompanying drawing 4
2transmission electron microscope picture with the combination electrode material of carbon nano-fiber;
MnO prepared for the present invention by accompanying drawing 5
2the cyclic voltammetry curve of combination electrode material under different scanning rates with carbon nano-fiber;
MnO prepared for the present invention by accompanying drawing 6
2combination electrode material constant current charge-discharge curve with carbon nano-fiber;
MnO prepared for the present invention by accompanying drawing 7
2the specific capacity of combination electrode material under the 50mV/s sweep speed and the graph of a relation of cycle-index with carbon nano-fiber.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described:
Embodiment 1: take a certain amount of polyacrylonitrile (PAN), add in dimethyl formamide (DMF) solvent of the dispersed 0.1-2% of having carbon nano-tube or Graphene, the PAN-DMF solution that to be mixed with mass fraction be 10wt.%, regulation voltage is 16kV, receiving range is 18cm, the solution feed rate is 0.6ml/h, and the solution electrospinning is become to fibrofelt.Hot press is heated to 100 ℃, puts into after fibrofelt is forced into 5MPa and be incubated 5min, obtain the fibrofelt thin slice of combining closely.Then the fibrofelt thin slice is put into to box atmosphere furnace, under the protection of nitrogen, with the heating rate of 5 ℃/min, be heated to 250 ℃ and 1000 ℃, be incubated respectively 2h and carry out pre-oxidation and carbonization, obtain the carbon nano-fiber thin slice.Preparation 0.1mol/L liquor potassic permanganate, add the concentrated sulfuric acid that solution is adjusted to pH=2, then the carbon nano-fiber thin slice of above-mentioned preparation be impregnated in solution after 15min, take out and use deionized water and absolute ethyl alcohol repeatedly to wash to pH=7, then put into the dry 12h of vacuum drying oven of 90 ℃, obtain MnO
2with the combination electrode material of carbon nano-fiber, calculate MnO by weighing
2loading be 1.03mg/cm
2.XRD diffraction picture, scanning and the transmission electron microscope picture of gained composite material are shown in respectively accompanying drawing 2,3 and 4.Prepared electrode material is carried out under different scanning rates to cyclic voltammetry and constant current charge-discharge test, its specific capacity is 400-500F/g, and the test result curve is as shown in accompanying drawing 5,6.Prepared electrode material is carried out under the sweep speed of 50mV/s to the cyclical stability test, as shown in Figure 7, after 1000 circulations, its specific capacity still keeps 95% to test result.
Embodiment 2: take a certain amount of polyvinyl alcohol (PVA), add in the deionized water of the dispersed 0.1-2% of having carbon nano-tube or Graphene, the PVA aqueous solution that to be mixed with mass fraction be 15wt.%, regulation voltage is 18kV, receiving range is 18cm, the solution feed rate is 0.8ml/h, and the solution electrospinning is become to fibrofelt.Then the fibrofelt thin slice is put into to box atmosphere furnace, under the protection of nitrogen, with the heating rate of 5 ℃/min, be heated to 1200 ℃, insulation 1.5h carries out carbonization, obtains the carbon nano-fiber thin slice.Preparation 0.25mol/L liquor potassic permanganate, add red fuming nitric acid (RFNA) that solution is adjusted to pH=1, then the carbon nano-fiber thin slice of above-mentioned preparation be impregnated in solution after 20min, take out and use deionized water and absolute ethyl alcohol repeatedly to wash to pH=7, then put into the dry 8h of vacuum drying oven of 100 ℃, obtain MnO
2combination electrode material with carbon nano-fiber.Calculate MnO by weighing
2loading be 1.56mg/cm
2.The specific capacity of prepared electrode material under the sweep speed of 5mV/s is 428F/g, and after 1000 circulations, its specific capacity still remains on more than 94%.
Embodiment 3: take a certain amount of Kynoar (PVDF) powder, add in dimethyl formamide (DMF) solvent of the dispersed 0.1-2% of having carbon nano-tube or Graphene, the PVDF-DMF solution that to be mixed with mass fraction be 10wt.%, regulation voltage is 20kV, receiving range is 15cm, the solution feed rate is 0.5ml/h, and the solution electrospinning is become to fibrofelt.Then the fibrofelt thin slice is put into to box atmosphere furnace, under the protection of nitrogen, with the heating rate of 5 ℃/min, be heated to 1100 ℃, insulation 2.5h carries out carbonization, obtains the carbon nano-fiber thin slice.Preparation 0.05mol/L liquor potassic permanganate, add the concentrated sulfuric acid that solution is adjusted to pH=1, then the carbon nano-fiber thin slice of above-mentioned preparation be impregnated in solution after 10min, take out and use deionized water and absolute ethyl alcohol repeatedly to wash to pH=7, then put into the dry 8h of vacuum drying oven of 100 ℃, obtain MnO
2combination electrode material with carbon nano-fiber.Calculate MnO by weighing
2loading be 0.77mg/cm
2.The specific capacity of prepared electrode material under the sweep speed of 5mV/s is 459F/g, and after 1000 circulations, its specific capacity still remains on more than 90%.
Embodiment 4: take a certain amount of pyromellitic acid anhydride and 4-4 diaminodiphenyl ether, add in dimethyl formamide (DMF) solvent of the dispersed 0.1-2% of having carbon nano-tube or Graphene, be mixed with the polyamic acid solution that mass fraction is 20wt.%, regulation voltage is 35kV, receiving range is 18cm, the solution feed rate is 2ml/h, and the solution electrospinning is become to fibrofelt.Again fibrofelt is put into to 350 ℃ of imidizations of baking oven and obtained the polyimide fiber felt after 0.5 hour.Then the fibrofelt thin slice is put into to box atmosphere furnace, under the protection of nitrogen, with the heating rate of 5 ℃/min, be heated to 1000 ℃, insulation 3h carries out carbonization, obtains the carbon nano-fiber thin slice.Preparation 0.15mol/L liquor potassic permanganate, add the concentrated sulfuric acid that solution is adjusted to pH=0, then the carbon nano-fiber thin slice of above-mentioned preparation be impregnated in solution after 30min, take out and use deionized water and absolute ethyl alcohol repeatedly to wash to pH=7, then put into the dry 8h of vacuum drying oven of 100 ℃, obtain MnO
2combination electrode material with carbon nano-fiber.Calculate MnO by weighing
2loading be 1.58mg/cm
2.Prepared electrode material specific capacity after 500 circulations under the sweep speed of 10mV/s is 317F/g, and the specific capacity conservation rate is 96%.
MnO prepared by above embodiment
2with the combination electrode material of carbon nano-fiber, MnO
2can evenly wrap in the carbon nano-fiber surface, thereby MnO
2loading is high and can be fully utilized, and the continuous carbon fiber of long-range can play good electric action simultaneously; In addition, carbon fiber has higher intensity, except as MnO
2support substrate, can also directly be used as stable electrode.Adopt three electrode test MnO
2chemical property with the combination electrode material of carbon nano-fiber, reference electrode is saturated calomel electrode, to electrode, it is platinum filament, the metabisulfite solution that electrolyte is 0.1mol/L, result shows that this novel self-supporting electrode material has the capacitance of 200-600F/g and good cyclical stability, and after 1000 circulations, capacitance can remain on more than 90%.
Claims (1)
1. the preparation method of a self-supporting super capacitor electrode material, is characterized in that, comprises the steps:
(1) prepare the high polymeric solution of the dispersed 0.1-2% of having carbon nano-tube or Graphene; High polymer in described high polymeric solution is polyacrylonitrile, polyimides, polyvinyl alcohol, Kynoar or pitch;
(2) by regulation voltage, receiving range, solution flow rate, ambient humidity, ambient temperature, become nanometer to arrive the micron order fibrofelt high polymeric solution electrospinning;
(3) fibrofelt is carried out to hot pressing, hot pressing temperature is 60～200 ℃, and the time is 20～300s, and pressure is 0.25～10MPa;
(4) the fibrofelt carbonization after hot pressing is obtained to carbon nanofiber felt, carburizing atmosphere is nitrogen or argon gas, and temperature is 800～1500 ℃, and the time is 60～240min;
(5) preparation liquor potassic permanganate, its concentration is 0.005～2mol/L, by adding the concentrated sulfuric acid or red fuming nitric acid (RFNA) or concentrated hydrochloric acid regulator solution pH, is 0～7, utilizes heating water bath that solution temperature is adjusted to 0～90 ℃;
(6) carbon nanofiber felt be impregnated in the liquor potassic permanganate that step (5) prepares, after magnetic agitation reaction certain hour, carbon nanofiber felt is taken out, use deionized water and absolute ethanol washing for several times, until pH equals 7;
(7) carbon nanofiber felt after washing is put into to dry 8-24h under baking oven 60-110 ℃, obtain the combination electrode material of manganese dioxide and carbon nano-fiber.
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