CN102087921A - 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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- 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
- Y02E60/10—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 electrode material for super capacitor and preparation method thereof.
Background technology
Ultracapacitor is a kind of novel energy-storing device between classic flat-plate capacitor and chemical power source, have high power density, big capacity, fast charging and discharging, overlength cycle life, pollute advantage such as little, high reliability, its capacitance can reach a farad rank, all has broad application prospects at aspects such as mobile communication, information technology, electric power system, electric automobile, Aero-Space.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 the electrolyte, this type of electrode material mainly is 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 the electrolyte to come storing electricity, and the capacitance of generation is 10-100 a 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 electrical 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, be expected in industrialization, provide a kind of electrode material of high performance-price ratio by overcoming these electrode materials shortcoming separately with good electric chemical property.
In transition group metallic oxide, MnO
2Have aboundresources, environmental friendliness, than advantage such as electric capacity height, preparation cost be low, according to its specific capacitance of Theoretical Calculation up to 1370F/g.Yet in actual applications, along with MnO
2The increase of loading, MnO
2Specific capacitance has only 1/10th of theoretical value.
Recent study personnel have developed the nanometer MnO of multiple preparation bigger serface
2Synthetic method, but its surface activity site still is difficult to make full use of; For this reason with MnO
2Can solve MnO preferably 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, it is extremely urgent to seek a kind of cheap composite preparation process efficiently.
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 electrode material for super capacitor, 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 electrode material for super capacitor.
A kind of self-supporting electrode material for super capacitor is characterized in that, described electrode material is the compound of manganese dioxide and carbon nano-fiber.
A kind of preparation method of self-supporting electrode material for super capacitor is characterized in that, comprises the steps:
(1) preparation evenly is dispersed with the high polymeric solution of 0.1-2% 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 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 the hot pressing is obtained 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, is 0～7 by adding the concentrated sulfuric acid or red fuming nitric acid (RFNA) or concentrated hydrochloric acid regulator solution pH, utilizes the water-bath heating that solution temperature is adjusted to 0～90 ℃;
(6) carbon nanofiber felt be impregnated in the liquor potassic permanganate that step (5) prepares, behind the magnetic agitation reaction certain hour, carbon nanofiber felt is taken out, use deionized water and absolute ethanol washing for several times, equal 7 until pH;
(7) carbon nanofiber felt after will washing is put into baking oven 60-110 ℃ of dry 8-24h down, promptly obtains the combination electrode material of manganese dioxide and carbon nano-fiber.
High polymer in the 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, electrospinning silk productive rate height, the reagent of employing is common agents, and is with low cost.3, electrode material of the present invention need not 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 the mechanical stability height, from characteristics such as afflux, active material loading height and chemical property be good.
Description of drawings
Accompanying drawing 1 is preparation technology's of the present invention schematic diagram;
Accompanying drawing 2 is the MnO of the present invention's preparation
2Combination electrode material XRD diffraction pattern with carbon nano-fiber;
Accompanying drawing 3 is the MnO of the present invention's preparation
2Sem photograph with the combination electrode material of carbon nano-fiber;
Accompanying drawing 4 is the MnO of the present invention's preparation
2Transmission electron microscope picture with the combination electrode material of carbon nano-fiber;
Accompanying drawing 5 is the MnO of the present invention's preparation
2The cyclic voltammetry curve of combination electrode material under different scanning rates with carbon nano-fiber;
Accompanying drawing 6 is the MnO of the present invention's preparation
2Combination electrode material constant current charge-discharge curve with carbon nano-fiber;
Accompanying drawing 7 is the MnO of the present invention's preparation
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
The present invention will be further described below in conjunction with the drawings and specific embodiments:
Embodiment 1: take by weighing a certain amount of polyacrylonitrile (PAN), add in dimethyl formamide (DMF) solvent, being mixed with mass fraction is the PAN-DMF solution of 10wt.%, regulation voltage is 16kV, receiving range is 18cm, and the solution feed rate is 0.6ml/h, and the solution electrospinning is become fibrofelt.Hot press is heated to 100 ℃, puts into and be incubated 5min after fibrofelt is forced into 5MPa, obtain the fibrofelt thin slice of combining closely.Then the fibrofelt thin slice is put into box atmosphere furnace, under protection of nitrogen gas, be heated to 250 ℃ and 1000 ℃, be incubated 2h respectively and carry out pre-oxidation and carbonization, obtain the carbon nano-fiber thin slice with the heating rate of 5 ℃/min.Preparation 0.1mol/L liquor potassic permanganate, add the concentrated sulfuric acid solution is adjusted to pH=2, then the carbon nano-fiber thin slice of above-mentioned preparation be impregnated in the solution behind the 15min, take out and repeatedly wash to pH=7 with deionized water and absolute ethyl alcohol, put into 90 ℃ the dry 12h of vacuum drying oven then, obtain MnO
2With the combination electrode material of carbon nano-fiber, calculate MnO by weighing
2Loading be 1.03mg/cm
2XRD diffraction picture, scanning and the transmission electron microscope picture of gained composite material are seen accompanying drawing 2,3 and 4 respectively.Prepared electrode material is carried out cyclic voltammetric test and constant current charge-discharge test under different scanning rates, its specific capacity is 400-500F/g, and the test result curve is shown in accompanying drawing 5,6.Prepared electrode material is carried out the stable circulation property testing under the sweep speed of 50mV/s, test result as shown in Figure 7, through 1000 times the circulation after its specific capacity still keep 95%.
Embodiment 2: take by weighing a certain amount of polyvinyl alcohol (PVA), add in the deionized water, being mixed with mass fraction is the PVA aqueous solution of 15wt.%, and regulation voltage is 18kV, and receiving range is 18cm, and the solution feed rate is 0.8ml/h, and the solution electrospinning is become fibrofelt.Then the fibrofelt thin slice is put into box atmosphere furnace, under protection of nitrogen gas, be heated to 1200 ℃ with the heating rate of 5 ℃/min, 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) solution is adjusted to pH=1, then the carbon nano-fiber thin slice of above-mentioned preparation be impregnated in the solution behind the 20min, take out and repeatedly wash to pH=7 with deionized water and absolute ethyl alcohol, put into 100 ℃ the dry 8h of vacuum drying oven then, obtain MnO
2Combination electrode material with carbon nano-fiber.Calculate MnO by weighing
2Loading be 1.56mg/cm
2The specific capacity of prepared electrode material under the sweep speed of 5mV/s is 428F/g, still remains on more than 94% through 1000 its specific capacities of circulation back.
Embodiment 3: take by weighing a certain amount of Kynoar (PVDF) powder, add in dimethyl formamide (DMF) solvent, being mixed with mass fraction is the PVDF-DMF solution of 10wt.%, regulation voltage is 20kV, receiving range is 15cm, the solution feed rate is 0.5ml/h, and the solution electrospinning is become fibrofelt.Then the fibrofelt thin slice is put into box atmosphere furnace, under protection of nitrogen gas, be heated to 1100 ℃ with the heating rate of 5 ℃/min, 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 solution is adjusted to pH=1, then the carbon nano-fiber thin slice of above-mentioned preparation be impregnated in the solution behind the 10min, take out and repeatedly wash to pH=7 with deionized water and absolute ethyl alcohol, put into 100 ℃ the dry 8h of vacuum drying oven then, obtain MnO
2Combination electrode material with carbon nano-fiber.Calculate MnO by weighing
2Loading be 0.77mg/cm
2The specific capacity of prepared electrode material under the sweep speed of 5mV/s is 459F/g, still remains on more than 90% through 1000 its specific capacities of circulation back.
Embodiment 4: take by weighing a certain amount of pyromellitic acid anhydride and 4-4 diaminodiphenyl ether, add in dimethyl formamide (DMF) solvent, 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 fibrofelt.Again fibrofelt is put into 350 ℃ of imidizations of baking oven and got the polyimide fiber felt after 0.5 hour.Then the fibrofelt thin slice is put into box atmosphere furnace, under protection of nitrogen gas, be heated to 1000 ℃ with the heating rate of 5 ℃/min, insulation 3h carries out carbonization, obtains the carbon nano-fiber thin slice.Preparation 0.15mol/L liquor potassic permanganate, add the concentrated sulfuric acid solution is adjusted to pH=0, then the carbon nano-fiber thin slice of above-mentioned preparation be impregnated in the solution behind the 30min, take out and repeatedly wash to pH=7 with deionized water and absolute ethyl alcohol, put into 100 ℃ the dry 8h of vacuum drying oven then, obtain MnO
2Combination electrode material with carbon nano-fiber.Calculate MnO by weighing
2Loading be 1.58mg/cm
2Prepared electrode material under the sweep speed of 10mV/s through 500 times the circulation after specific capacity be 317F/g, the specific capacity conservation rate is 96%.
The MnO of above embodiment preparation
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 the favorable conductive effect 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 a saturated calomel electrode, to electrode is platinum filament, electrolyte is the metabisulfite solution of 0.1mol/L, the result shows that this novel self-supporting electrode material has the capacitance of 200-600F/g and good cyclical stability, and 1000 times circulation back capacitance can remain on more than 90%.
Claims (3)
1. a self-supporting electrode material for super capacitor is characterized in that, described electrode material is the compound of manganese dioxide and carbon nano-fiber.
2. the preparation method of a self-supporting electrode material for super capacitor is characterized in that, comprises the steps:
(1) preparation evenly is dispersed with the high polymeric solution of 0.1-2% 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 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 the hot pressing is obtained 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, is 0～7 by adding the concentrated sulfuric acid or red fuming nitric acid (RFNA) or concentrated hydrochloric acid regulator solution pH, utilizes the water-bath heating that solution temperature is adjusted to 0～90 ℃;
(6) carbon nanofiber felt be impregnated in the liquor potassic permanganate that step (5) prepares, behind the magnetic agitation reaction certain hour, carbon nanofiber felt is taken out, use deionized water and absolute ethanol washing for several times, equal 7 until pH;
(7) carbon nanofiber felt after will washing is put into baking oven 60-110 ℃ of dry 8-24h down, promptly obtains the combination electrode material of manganese dioxide and carbon nano-fiber.
3. according to the preparation method of the described a kind of self-supporting electrode material for super capacitor of claim 2, it is characterized in that the high polymer in the described high polymeric solution is polyacrylonitrile, polyimides, polyvinyl alcohol, Kynoar or pitch.
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