CN102093712A - Preparation method of composite super capacitor electrode material - Google Patents
Preparation method of composite super capacitor electrode material Download PDFInfo
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- CN102093712A CN102093712A CN 201010552735 CN201010552735A CN102093712A CN 102093712 A CN102093712 A CN 102093712A CN 201010552735 CN201010552735 CN 201010552735 CN 201010552735 A CN201010552735 A CN 201010552735A CN 102093712 A CN102093712 A CN 102093712A
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Abstract
The invention discloses a preparation method of a composite super capacitor electrode material. The technical scheme comprises the following steps of: (1) preparing spiral carbon nanofiber by a liquid phase flame method; (2) purifying and activating a sample obtained by the step (1); and (3) adding deionized water into the sample obtained in the step (2), ultrasonically dispersing for 1 hour, adjusting pH to be between 1 and 2 with HCl (Hydrogen Chloride), adding an aniline monomer solution, stirring under magnetic force, adding an ammonium persulfate solution for a polymerization reaction, washing with acetone and deionized water respectively after the reaction ends, filtering, and drying to obtain the spiral carbon nanofiber/polyaniline composite material. The super capacitor electrode material prepared by the method has low cost and is easy to operate, and expensive equipment is not needed.
Description
One, technical field:
The present invention relates to a kind of preparation method of hybrid supercapacitor electrode materials, relate to a kind of preparation of spiral carbon nanofiber/polyaniline composite material more specifically, function of dominant material and energy field.
Two, background technology:
Ultracapacitor is a kind of novel energy-storing device that occurs in recent years, and it has the advantage that conventional capacitor power density is big, the rechargeable battery energy density is high concurrently.In addition, ultracapacitor also has advantages such as long cycle life and environmentally safe, thus it can be used for satisfying automobile quicken, start, superpower requirement during climbing, with the protection battery system; Also can be used in the other system, as the startup power of the battery that acts as a fuel, do the electric power support of mobile communication and computer etc., is most promising green energy resource in this century.
Electrode materials as ultracapacitor comprises unitary electrode material and combination electrode materials such as carbon-based material, metal oxide and conductive polymers, and wherein the research of carbon-based electrode material mainly concentrates on gac, charcoal-aero gel, carbon fiber and carbon nanotube etc.Gac is to study the earliest and maximum electrode for super capacitor materials, because micro content is higher thereby the specific surface area utilization ratio is lower in its pore size distribution.Characteristics such as carbon nanotube is concentrated because of its good conductivity, mesopore aperture and specific surface area is big are used having potential aspect the electric chemical super capacitor electrode materials.Employing KOH such as Deng Meigen are that promoting agent carries out activation treatment to carbon nanotube, have increased the specific surface area of carbon nanotube, make it bring up to 73F/g than electric capacity by the preceding 43F/g of activation.Wu Fayu etc. are reference with straight charcoal fiber, comparative study hydrocarbon oxidation catalyst decompose the microtexture and the energy storage characteristic of the micron spiral type charcoal fiber of preparation, the electrochemical capacitor of finding micron coiled carbon fiber dimension is 3-4 a times of the straight charcoal fiber of similar sizes.
People such as E.Frackowiak utilize various conductive polymers and the compound preparation electrical double layer capacitor electrodes of multi-walled carbon nano-tubes, experimental result shows that suitable CNTs content can effectively improve the electric capacity of electrode, do capacitor cathode with CNTs/PPy, CNTs/PANI does capacitor anode, and can obtain condenser capactiance is 320F/g.Employing sol-gel methods such as Wang Xiaofeng have prepared ultra-fine ruthenium oxide super capacitor material.Electro-chemical test proof ruthenium oxide/carbon nano-tube combination electrode has the above electrochemistry capacitance of 860F/g and has good high power discharge characteristic.But RuO
2XH
2The amount of O accounts for more than 70% of gross weight, does not fundamentally reduce cost and its application is restricted.
Three, summary of the invention:
Purpose of the present invention is exactly the above-mentioned defective that exists at prior art, and a kind of preparation method of the hybrid supercapacitor electrode materials that reduces cost is provided.
A kind of preparation method of hybrid supercapacitor electrode materials, its technical scheme is: be composited by spiral carbon nanofiber and polyaniline, comprise following making step:
(1) preparation of spiral carbon nanofiber: adopting the liquid phase flame method to prepare the spiral carbon nanofiber, is carbon source with the organic solvent, SnCl
45H
2O is the catalyzer precursor, and temperature of reaction is 580～640 ℃, and the reaction times is 5～15min, and prepared spiral carbon nanofiber screw diameter is about 100nm, and Fibre diameter is about 50nm;
(2) purifying of spiral carbon nanofiber: will mix with acidic solution by the spiral carbon nanofiber that step (1) makes, supersound process 60min, thin up, post precipitation with deionized water wash repeatedly, filter, drying;
(3) activation of spiral carbon nanofiber: spiral carbon nanofiber and KOH powder thorough mixing in agate mortar that will make by step (2) by the certain mass ratio, place ceramic boat then, be placed on and carry out activation treatment in the silica tube in the horizontal pipe furnace, the active spiral carbon nanofiber of gained washes repeatedly with deionized water and is diluted to PH ≈ 8, filtration, drying;
(4) spiral carbon nanofiber and polyaniline are compound: add deionized water in step (3) gained spiral carbon nanofiber sample, ultrasonic dispersing 1h, regulate PH to 1-2 with HCl, add aniline monomer solution, under the magnetic agitation, add initiator and carry out polyreaction, after reaction finishes, use acetone, deionized water wash respectively, filter, obtain spiral carbon nanofiber/polyaniline composite material after the drying.
Above-mentioned organic solvent is selected from C
2～C
3Monohydroxy-alcohol or C
5～C
6Alkane.
Above-mentioned organic solvent preferred alcohol.
Above-mentioned acidic solution is the hydrochloric acid of mass concentration 38%.
In the above-mentioned step (3) during the activation of spiral carbon nanofiber: the spiral carbon nanofiber is 1: 4～1: 1 with KOH powder quality ratio.
When carrying out activation treatment in the above-mentioned silica tube of spiral carbon nanofiber in horizontal pipe furnace, be earlier the logical nitrogen 10～20min of flow velocity of 30～40mL/min at normal temperatures with flow, heat-up rate with 10 ℃/min is warmed up to 750 ℃～850 ℃ again, under this temperature, be incubated 1h, naturally cool to room temperature then, whole process, nitrogen are passed through silica tube with the flow velocity of 30～40mL/min all the time.
Above-mentioned spiral carbon nanofiber is by the method and the aniline polymerization of in-situ polymerization, and used initiator is an ammonium persulphate, and ammonium persulphate and aniline add-on mol ratio are 1: 1～1: 2.
The invention has the beneficial effects as follows: the spiral carbon nanofiber has open three-dimensional net structure, interlacing mesh is suitable for the turnover of electrolyte ion between fiber and the fiber, its specific surface area and pore volume further increase after the purified and activation treatment, even aperture distribution and concentrate on the mesopore scope is fit to form double electric layer electrochemical capacitors.Spiral carbon nanofiber and polyaniline are compound both can to obtain high energy density, can obtain high specific power again, the spiral carbon nanofiber/polyaniline material that adopts method preparation of the present invention is than electric capacity (360F/g～403F/g) be higher than the carbon nano-tube/poly aniline material of bibliographical information than electric capacity (320F/g).Present method is with low cost, simple to operate, need not expensive device.
Four, description of drawings:
Accompanying drawing 1 is the microscopic appearance figure of the coiled carbon fibers that makes of flame combustion process;
Accompanying drawing 2 is microscopic appearance figure of the spiral carbon nanofiber behind the purifying;
Accompanying drawing 3 is TEM photos of the spiral carbon nanofiber after the activation;
Accompanying drawing 4 is TEM photos of spiral carbon nanofiber/polyaniline.
Five, embodiment:
Further specify the present invention with embodiment below, but protection scope of the present invention is not limited in embodiment.The variation and the modification of other that those skilled in the art is made in the case of without departing from the spirit and scope of protection of the present invention still are included within the protection domain of the present invention.
Embodiment 1: adopt the carbon source of ethanol as combustion medium and spiral carbon nanofiber.Baseplate material is the pure nickel sheet, at first with SnCl
45H
2O is dissolved in and forms saturated solution in the dehydrated alcohol, is coated in substrate surface then.After the liquid drying to be applied, the coating of substrates reaction surface is inserted downwards in the flame, keep taking out after 10 minutes, the substrate surface atrament is coiled carbon fibers (CNCs-1), with reference to accompanying drawing 1, wherein, (a) is electron scanning micrograph; (b) be the transmission electron microscope photo.With mass concentration be that 38% concentrated hydrochloric acid soaks, ultrasonic 1h to be to remove the catalyst particle among the CNCs-1, again with deionized water wash repeatedly, filter, drying, obtain the sample CNCs-2 behind the purifying, with reference to accompanying drawing 2, (a) be electron scanning micrograph; (b) be the transmission electron microscope photo.
Press mass ratio 1: 2 with CNCs-2 and KOH powder thorough mixing in agate mortar, place ceramic boat then, be placed on and carry out activation treatment in the silica tube in the horizontal pipe furnace.Earlier be the logical nitrogen 15min of flow velocity of 40mL/min at normal temperatures with the flow, the heat-up rate with 10 ℃/min is warmed up to 850 ℃ again, is incubated 1h under this temperature, cools to room temperature then naturally, whole process, and nitrogen passes through silica tube with the flow velocity of 40mL/min all the time.The active spiral carbon nanofiber of gained again with deionized water wash repeatedly, filter, drying, obtain CNCs-3, with reference to accompanying drawing 3.
In CNCs-3, add deionized water, ultra-sonic dispersion 1h.Regulate PH to 1 with HCl.Add aniline monomer solution, under the magnetic agitation, add initiator ammonium persulfate and carry out polyreaction.Reaction is used acetone, deionized water wash respectively after finishing, and filters, and obtains spiral carbon nanofiber/polyaniline composite material after the drying, with reference to accompanying drawing 4.
Resulting CNCs-1 and spiral carbon nanofiber/polyaniline composite material are applied to electric chemical super capacitor as electrode materials respectively, the electrochemistry capacitance of finding matrix material after tested improves greatly, brings up to 360.2F/g than electric capacity by the 40F/g of CNCs-1.
Embodiment 2: adopt the carbon source of ethanol as combustion medium and spiral carbon nanofiber.Baseplate material is the pure nickel sheet, at first with SnCl
45H
2O is dissolved in and forms saturated solution in the dehydrated alcohol, is coated in substrate surface then.After the liquid drying to be applied, the coating of substrates reaction surface is inserted downwards in the flame, keep taking out after 10 minutes, the substrate surface atrament is coiled carbon fibers (CNCs-1).With mass concentration be that 38% concentrated hydrochloric acid soaks, ultrasonic 1h to be to remove the catalyst particle among the CNCs-1, again with deionized water wash repeatedly, filter, drying, obtain the sample CNCs-2 behind the purifying.Press mass ratio 1: 4 with CNCs-2 and KOH powder thorough mixing in agate mortar, place ceramic boat then, be placed on and carry out activation treatment in the silica tube in the horizontal pipe furnace.Earlier be the logical nitrogen 15min of flow velocity of 40mL/min at normal temperatures with the flow, the heat-up rate with 10 ℃/min is warmed up to 850 ℃ again, is incubated 1h under this temperature, cools to room temperature then naturally, whole process, and nitrogen passes through silica tube with the flow velocity of 40mL/min all the time.The active spiral carbon nanofiber of gained again with deionized water wash repeatedly, filter, drying, obtain CNCs-3.In CNCs-3, add deionized water, ultra-sonic dispersion 1h.Regulate PH to 1-2 with HCl.Add aniline monomer solution, under the magnetic agitation, add initiator ammonium persulfate and carry out polyreaction.Reaction is used acetone, deionized water wash respectively after finishing, and filters, and obtains spiral carbon nanofiber/polyaniline composite material after the drying.Resulting spiral carbon nanofiber/polyaniline composite material is applied to electric chemical super capacitor as electrode materials, and what find matrix material after tested is than electric capacity 403.7F/g.
Claims (7)
1. the preparation method of a hybrid supercapacitor electrode materials is characterized in that: be composited by spiral carbon nanofiber and polyaniline, comprise following making step:
(1) preparation of spiral carbon nanofiber: adopting the liquid phase flame method to prepare the spiral carbon nanofiber, is carbon source with the organic solvent, SnCl
45H
2O is the catalyzer precursor, and temperature of reaction is 580～640 ℃, and the reaction times is 5～15min, and prepared spiral carbon nanofiber screw diameter is about 100nm, and Fibre diameter is about 50nm;
(2) purifying of spiral carbon nanofiber: will mix with acidic solution by the spiral carbon nanofiber that step (1) makes, supersound process 60mins, thin up, post precipitation with deionized water wash repeatedly, filter, drying;
(3) activation of spiral carbon nanofiber: spiral carbon nanofiber and KOH powder thorough mixing in agate mortar that will make by step (2) by the certain mass ratio, place ceramic boat then, be placed on and carry out activation treatment in the silica tube in the horizontal pipe furnace, the active spiral carbon nanofiber of gained washes repeatedly with deionized water and is diluted to PH ≈ 8, filtration, drying;
(4) spiral carbon nanofiber and polyaniline are compound: add deionized water in step (3) gained spiral carbon nanofiber sample, ultrasonic dispersing 1h, regulate PH to 1-2 with HCl, add aniline monomer solution, under the magnetic agitation, add initiator and carry out polyreaction, after reaction finishes, use acetone, deionized water wash respectively, filter, obtain spiral carbon nanofiber/polyaniline composite material after the drying.
2. the preparation method of hybrid supercapacitor electrode materials according to claim 1 is characterized in that: described organic solvent is selected from C
2～C
3Monohydroxy-alcohol or C
5～C
6Alkane.
3. the preparation method of hybrid supercapacitor electrode materials according to claim 2 is characterized in that: described organic solvent preferred alcohol.
4. the preparation method of hybrid supercapacitor electrode materials according to claim 1 is characterized in that: described acidic solution is the hydrochloric acid of mass concentration 38%.
5. the preparation method of hybrid supercapacitor electrode materials according to claim 1 is characterized in that: in the described step (3) during the activation of spiral carbon nanofiber: the spiral carbon nanofiber is 1: 4～1: 1 with KOH powder quality ratio.
6. the preparation method of hybrid supercapacitor electrode materials according to claim 1, it is characterized in that: when carrying out activation treatment in the silica tube of described spiral carbon nanofiber in horizontal pipe furnace, be earlier the logical nitrogen 10～20min of flow velocity of 30～40mL/min at normal temperatures with flow, heat-up rate with 10 ℃/min is warmed up to 750 ℃～850 ℃ again, under this temperature, be incubated 1h, naturally cool to room temperature then, whole process, nitrogen are passed through silica tube with the flow velocity of 30～40mL/min all the time.
7. the preparation method of hybrid supercapacitor electrode materials according to claim 1, it is characterized in that: described spiral carbon nanofiber is by the method and the aniline polymerization of in-situ polymerization, used initiator is an ammonium persulphate, and ammonium persulphate and aniline add-on mol ratio are 1: 1～1: 2.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105118686A (en) * | 2015-08-27 | 2015-12-02 | 桂林理工大学 | Graphite alkene /polyaniline/manganese dioxide ternary composite electrode material preparation method |
| CN105254876A (en) * | 2015-11-25 | 2016-01-20 | 黑龙江省科学院大庆分院 | Preparation method of polyaniline-coated carbon fiber hybrid gas-sensitive material with cross-linked structure |
| CN105679554A (en) * | 2016-01-05 | 2016-06-15 | 新疆大学 | Preparation method for needle-shaped polyaniline/coal-based carbon nanofiber flexible supercapacitor |
| CN105869901A (en) * | 2016-03-30 | 2016-08-17 | 北京化工大学 | Carbon nanofiber composite material with controllable structure and preparation method and application therefor |
| CN108505144A (en) * | 2018-05-10 | 2018-09-07 | 芜湖市创源新材料有限公司 | A kind of preparation method of composite regenerated cellulose fibre |
| CN108622991A (en) * | 2017-03-17 | 2018-10-09 | 南开大学 | A kind of method of novel nitrating charcoal-aero gel catalysis persulfate degradation of organic waste water |
| CN109103029A (en) * | 2018-08-27 | 2018-12-28 | 四川理工学院 | A kind of spiral nanometer carbon fiber/TiO2Composite material and its application |
| CN117638063A (en) * | 2023-11-29 | 2024-03-01 | 西安理工大学 | Preparation method of heteroatom doped hard carbon negative electrode material for sodium ion battery |
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| CN100999315A (en) * | 2006-12-26 | 2007-07-18 | 华东理工大学 | Method of preparing spiral nanometer carbon fiber |
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Cited By (11)
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|---|---|---|---|---|
| CN105118686A (en) * | 2015-08-27 | 2015-12-02 | 桂林理工大学 | Graphite alkene /polyaniline/manganese dioxide ternary composite electrode material preparation method |
| CN105118686B (en) * | 2015-08-27 | 2017-12-12 | 桂林理工大学 | The preparation method of graphene/polyaniline/manganese dioxide ternary composite electrode material |
| CN105254876A (en) * | 2015-11-25 | 2016-01-20 | 黑龙江省科学院大庆分院 | Preparation method of polyaniline-coated carbon fiber hybrid gas-sensitive material with cross-linked structure |
| CN105679554A (en) * | 2016-01-05 | 2016-06-15 | 新疆大学 | Preparation method for needle-shaped polyaniline/coal-based carbon nanofiber flexible supercapacitor |
| CN105869901A (en) * | 2016-03-30 | 2016-08-17 | 北京化工大学 | Carbon nanofiber composite material with controllable structure and preparation method and application therefor |
| CN105869901B (en) * | 2016-03-30 | 2018-07-06 | 北京化工大学 | A kind of carbon nano-fiber composite material of structure-controllable and its preparation method and application |
| CN108622991A (en) * | 2017-03-17 | 2018-10-09 | 南开大学 | A kind of method of novel nitrating charcoal-aero gel catalysis persulfate degradation of organic waste water |
| CN108505144A (en) * | 2018-05-10 | 2018-09-07 | 芜湖市创源新材料有限公司 | A kind of preparation method of composite regenerated cellulose fibre |
| CN109103029A (en) * | 2018-08-27 | 2018-12-28 | 四川理工学院 | A kind of spiral nanometer carbon fiber/TiO2Composite material and its application |
| CN109103029B (en) * | 2018-08-27 | 2020-12-11 | 四川理工学院 | Spiral nano carbon fiber/TiO2Composite material and use thereof |
| CN117638063A (en) * | 2023-11-29 | 2024-03-01 | 西安理工大学 | Preparation method of heteroatom doped hard carbon negative electrode material for sodium ion battery |
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Application publication date: 20110615 |