CN106986324A - It is a kind of for hollow porous carbon ball electrode material of ultracapacitor and preparation method thereof - Google Patents
It is a kind of for hollow porous carbon ball electrode material of ultracapacitor and preparation method thereof Download PDFInfo
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- CN106986324A CN106986324A CN201710144357.0A CN201710144357A CN106986324A CN 106986324 A CN106986324 A CN 106986324A CN 201710144357 A CN201710144357 A CN 201710144357A CN 106986324 A CN106986324 A CN 106986324A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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 kind of for hollow porous carbon ball electrode material of ultracapacitor and preparation method thereof, belong to field of new energy technologies.The electrode material uses the method for layer assembly to prepare hollow (Fe) nano materials of MIL 100 for presoma, and hollow porous carbon ball is obtained after thermally treated in an inert atmosphere and hydrofluoric acid treatment.When preparing electrode of super capacitor, by above-mentioned electrode material and acetylene black, Kynoar mixing is applied on stainless steel collector as working electrode.The electrode material for super capacitor of the present invention, with the higher specific capacitance of relative one-component and broader test potential window and high electrochemical stability, service life cycle is long, environment-friendly;Working electrode is prepared simply, and chemical property is good, has broad application prospects.
Description
Technical field
The present invention relates to a kind of for hollow porous carbon ball electrode material of ultracapacitor and preparation method thereof, specifically relate to
And a kind of hollow MIL-100 (Fe) nanosphere is the side that presoma prepares hollow porous Nano carbon balls electrode material for super capacitor
Method.
Background technology
With continuing to develop for economic society, the energy is constantly consumed, and is caused lack of energy and is brought substantial amounts of ring therewith
Border problem, in order to solve these problems, new clean energy resource turns into the emphasis of scientific research.Ultracapacitor is used as accumulator
Part, because with high power density, the charging interval is short, the advantages of having extended cycle life, by extensive concern.According to its energy stores machine
The difference of reason, ultracapacitor can be divided into:Double electric layers supercapacitor and faraday's ultracapacitor (super electricity of fake capacitance
Hold).Carbon material is as the most frequently used electrode material of double electric layers supercapacitor by extensive concern.
The porosity features of carbon material cause it to have faster reacting dynamics characteristic, and higher specific surface area is smaller
Pore-size distribution, higher pore volume and preferable electric conductivity etc. are widely used such as adsorbent, catalysis at many aspects
Carrier and ultracapacitor etc..Preparing the method for porous carbon materials has a lot, such as laser ablation method, arc light method, chemical gaseous phase
Sedimentation and template and the method activated by physical chemistry.In the above-mentioned methods, template is most effective side
Method.Template can be divided into two classes according to the difference of template:Soft template method and hard template method.The wherein preparation process of hard template method
Including:The preparation and carbonization of template, and whether Additional carbon sources are introduced according to carbonisation, it is divided into two classes:(1) the direct carbon of predecessor
Change, this method does not need Additional carbon sources, the porous carbon of acquisition generally has higher specific surface area and pore volume, but its yield
It is relatively low.(2) Additional carbon sources such as glucose, melamine etc. are introduced, such a method is high relative to the first yield, Er Qieke
To be contained by selection, heteroatomic carbon source is such as nitrogenous, and the carbon source of sulfur-bearing prepares the porous carbon materials of Heteroatom doping.
Research report, hollow ball-shape structure are because can be effectively big with relatively low density and low body surface area ratio
Width improves the electro-chemical properties of energy storage device.The inner chamber of hollow ball-shape structure can store electrolyte and substantially reduce electrolyte
Ion transmission path.So that the cyclical stability of its device, specific capacitance and multiplying power property are all greatly improved.Synthesis is hollow
The spherical structural carbon material of nanometer has had template, hydro-thermal method, catalysis method etc..
The report that hollow porous chondritic is prepared using metal organic framework compound as presoma is still less, prepares
The carbon ball of porous hollow structure, plays more preferable chemical property, will be an of great value research topic.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of hollow porous Nano carbon balls for ultracapacitor and surpassed
Level capacitor electrode material and preparation method thereof, the electrode material for super capacitor that the present invention is prepared has high specific capacitance
With good electrochemical stability;Preparation manipulation is simple, and hollow ball wall thickness can control, it is not necessary to complex device, it is easy to industrialize
Production.
A kind of hollow porous Nano carbon balls electrode material for super capacitor for ultracapacitor, with MIL-100 (Fe)
Hollow ball is presoma, is made after being heat-treated under inert atmosphere after hydrofluoric acid treatment.The diameter of nanosphere is about 300nm,
Nanosphere ball wall is made up of high-graphitized porous carbon, forms loose structure.The porous hollow Nano carbon balls wall thickness can be by preceding
Body regulation is driven, controlled range is 10-50nm.
A kind of hollow porous Nano carbon balls electrode material for super capacitor for ultracapacitor produced by the present invention,
In three-electrode system test, specific capacitance value can reach 271~310F/g, with very excellent specific capacitance.
Present invention also offers the preparation method for preparing the above-mentioned hollow porous Nano carbon balls for ultracapacitor, bag
Include:Methods described is used as presoma using hollow MIL-100 (Fe) nanosphere, it is characterised in that the described method comprises the following steps:
(1) it is carbonized:Under nitrogen protection, by hollow MIL-100 (Fe) the nanosphere presomas through two benches carbonization at
Reason, obtains carbonized product;Described two benches carbonization treatment is:First stage in 200-400 DEG C be incubated 1-5h, second stage in
800-1000 DEG C of insulation 3-7h;
(2) acid treatment:The product that step (1) is obtained uniformly is mixed with hydrofluoric acid aqueous solution, and gained mixture is put
Bubble is no longer produced in being heated to mixture on 80-120 DEG C of warm table;
(3) by gained activation after acid treatment, material is neutralized, deionized water is washed to neutrality, then is placed in 80-100 DEG C of vacuum
12-24h is dried in drying box, hollow porous carbon ball is made;
Wherein, in above-mentioned steps (1), described two benches carbonization treatment is carried out in temperature programmed control tube furnace.
In above-mentioned steps (1), described two benches carbonization treatment is carried out in temperature programmed control tube furnace, and heating rate is 5
~20 DEG C/min conditions.
Described inert atmosphere be nitrogen, argon gas, carbon dioxide in one or more, wherein mixed gas stream
Measure as 3-300mL/min.
In above-mentioned steps (2), the hydrofluoric acid aqueous solution that described hydrofluoric acid aqueous solution is 10wt%.
Ultrasonic power used is 40-60KHz in above-mentioned steps (2)
Centrifuge speed used is 8000-10000r/min in aforesaid operations
Absolute ethyl alcohol washing times are 1~3 time in above-mentioned steps (3)
Hollow porous Nano carbon balls electrode material for super capacitor prepared by the present invention, is made with metal organic framework compound
The report for preparing hollow porous chondritic for presoma is still less, prepares the carbon ball of porous hollow structure.In the middle of hollow ball
Cavity effectively combined with the loose structure of carbon wall, give full play to the synergy of the two.Found by electrochemical property test,
The material can preferably improve the specific capacitance of ultracapacitor and forthright again.And can be adjusted by changing presoma self assembly number of times
The wall thickness of the whole hollow porous Nano carbon balls of end-product, the chemical property so as to adjusting the material.In addition, carbon prepared by the present invention
The carbon material (such as graphene) that based super capacitor electrode material is outstanding compared to some performances but price is sufficiently expensive, has
Relatively good cost advantage.
Brief description of the drawings
The transmission electron microscope picture of the hollow porous carbon balls of Fig. 1:(a) 15, (b) 30,60 layers of (c) 45 and (d)
The X-ray powder diffraction style of the hollow porous carbon balls of Fig. 2
(a) cyclic voltammetry curve of the hollow porous carbon balls of Fig. 3;(b) charging and discharging curve;(c) curve of double curvature;(d) 2000 connect
The change curve of continuous circulation specific capacitance recoverable amount.
Specific embodiment
In order to be better understood from the present invention, the present invention is further detailed below by specific embodiment, but
Protection scope of the present invention is not limited to that.
1st, the preparation of hollow porous Nano carbon balls
(1) preparation of the polystyrene nanospheres of sulfonation
2g diameters about 200nm polystyrene nanospheres are taken to be added in the 50mL concentrated sulfuric acids, under the conditions of 40 DEG C, stirring reaction
After 2h, washed after centrifugation, that is, obtain the polystyrene nanospheres that surface carries sulfonic acid group, products therefrom is needed in ethanol
Save backup.
(2) the polystyrene nanospheres 2g for the process sulfonation for stating preparation is taken to be put into 50mL centrifuge tubes, it is equal through ultrasonic disperse
It is even, obtain sulfonated polystyrene nanosphere dispersion liquid.
(3) FeCl that molar concentration is 2mM is respectively configured3·6H2O and trimesic acid (H3BTC ethanol solution).Will
(2) sulfonated polystyrene nanosphere dispersion liquid adds 16mL FeCl in3·6H2After O ethanol solution is fully dispersed, 70 DEG C of standings
15min is reacted, absolute ethyl alcohol washed once after centrifugation, then add the ethanol solution of 16mL trimesic acids, 70 DEG C quiet
Reaction 30min is put, absolute ethyl alcohol washed once after same centrifugation, circulate aforesaid operations, prepare 30 layers of PS@MIL-100
(Fe) nucleocapsid structure material.
(4) after PS@MIL-100 (Fe) the nucleocapsid structures material of above-mentioned preparation is centrifuged, N, N- dimethyl are added
Formamide, dissolving removes polystyrene moulding, obtains hollow MIL-100 (Fe) hollow ball.
2nd, the preparation of hollow porous carbon ball nano-electrode material
(5) 2g predecessors MIL-100 (Fe) hollow ball is taken to insert in clean quartz boat, under nitrogen protection, hollow MIL-
100 (Fe) nanometer ball warp two benches carbonization treatments, obtain carbonized product;Described two benches carbonization treatment is:First stage in
300 DEG C of insulation 1-5h, second stage is incubated 5h in 900 DEG C;
(6) acid activation is handled:The product that step (5) is obtained uniformly is mixed with hydrofluoric acid, water, and gained mixture is put
Bubble is no longer produced in being heated to mixture on 90 DEG C of warm tables.
(7) after acid activation processing gained activation material is neutralized, deionized water is washed to neutrality, then be placed in 80 DEG C of vacuum and do
12h is dried in dry case, hollow porous Nano carbon balls are made.
Ultrasonic power used is 60KHz in above-mentioned steps (2)
Centrifuge speed used is 8000r/min in aforesaid operations
Heating rate is 5-10 DEG C/min in above-mentioned steps (5).
3rd, the electrochemical property test of 20 layers of hollow porous Nano carbon balls of self assembly.
The hollow porous carbon ball nano material that synthesis is obtained, Kynoar (PVDF), acetylene black is according to mass ratio:
80:15:5 ratio mixing.Detailed process is first by hollow porous carbon ball nano material and the acetylene black mixing of certain mass
And ground 20 minutes in mortar, quantitative poly- segregation PVF is added afterwards, plus a small amount of 1-METHYLPYRROLIDONE continues to grind 10
Minute, the mixture obtained after being fully ground is redispersed in NMP, to be applied in foamed nickel current collector.Afterwards, electrode exists
Stay overnight to remove NMP in vacuum drying oven at a temperature of 120 DEG C.Generally, total load amount of the electrode material in foamed nickel current collector
About 2mg.Cyclic voltammetry, constant current charge-discharge is with electrochemical impedance spectroscopy (EIS) in Shanghai Chen Hua (CHI660D) electrochemical operation
Obtained in standing.In test, using three-electrode system, to load the foamed nickel current collector of hollow porous carbon ball nano material as work
Electrode, platinum guaze is that, to electrode, Hg/HgO is reference electrode, and electrolyte is 6M KOH.
Understood according to calculating, be 1A g in current density-1When, the specific capacitance of hollow porous carbon ball material can reach
306.2F g-1Even if current density increases to 10A g-1When, specific capacitance remains to reach 271.6F g-1, multiplying power reaches 88.7%.
Data above illustrates that hollow porous Nano carbon balls prepared by the inventive method have excellent electrochemical capacitance performance, is potential super
Level capacitor electrode material candidate.
Claims (7)
1. a kind of hollow porous Nano carbon balls electrode material for ultracapacitor, it is characterised in that:The hollow porous carbon
The a diameter of 300nm of nanosphere, ball wall by the trimesic acid in presoma hollow MIL-100 (Fe) nanosphere by being carbonized what is formed
Height graphite alkylene carbon is constituted, and with loose structure, wall thickness range is 10-50nm.
2. a kind of hollow porous Nano carbon balls electrode material for ultracapacitor according to claim 1, its feature
It is:The specific capacitance value of the material reaches 271~310F/g.
3. a kind of method of the hollow porous Nano carbon balls electrode material prepared described in claim 1-2, methods described is with hollow
MIL-100 (Fe) nanosphere is used as presoma, it is characterised in that the described method comprises the following steps:
(1) it is carbonized:Under nitrogen protection, hollow MIL-100 (Fe) the nanosphere presomas are obtained through two benches carbonization treatment
To carbonized product;Described two benches carbonization treatment is:First stage is incubated 1-5h in 200-400 DEG C, and second stage is in 800-
1000 DEG C of insulation 3-7h;
(2) acid activation is handled:The product that step (1) is obtained uniformly is mixed with hydrofluoric acid aqueous solution, and gained mixture is put
Bubble is no longer produced in being heated to mixture on 80-120 DEG C of warm table;
(3) activation material obtained by after acid activation is handled is neutralized, deionized water is washed to neutrality, then is placed in 80-100 DEG C of vacuum
12-24h is dried in drying box, hollow porous carbon ball is made.
4. method according to claim 3, it is characterised in that in step (1), described two benches carbonization treatment is in program
Carried out in temperature control tube furnace.
5. method according to claim 3, it is characterised in that in step (1), described two benches carbonization treatment is in program
Carried out in temperature control tube furnace, heating rate is 5~20 DEG C/min conditions.
6. method according to claim 3, it is characterised in that described inert atmosphere is nitrogen, argon gas, carbon dioxide gas
The flow of one or more in body, wherein mixed gas is 3-300mL/min.
7. method according to claim 3, it is characterised in that in step (2), described hydrofluoric acid aqueous solution is 5-
15wt% hydrofluoric acid aqueous solution.
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CN109607510A (en) * | 2019-01-15 | 2019-04-12 | 广西大学 | ZIF base nitrogen-doped porous carbon material and preparation method thereof |
CN109659158A (en) * | 2018-12-07 | 2019-04-19 | 武汉工程大学 | A kind of nitrogen-doped carbon nanometer pipe/cobaltosic oxide composite aerogel and its preparation method and application |
CN110165210A (en) * | 2019-05-14 | 2019-08-23 | 中国民航大学 | A kind of preparation method of the fluorocarbons positive electrode with height ratio capacity |
CN110436441A (en) * | 2019-08-12 | 2019-11-12 | 青岛大学 | A kind of meso-porous hollow carbon sphere and its preparation and the application in electromagnetic absorption |
CN112017868A (en) * | 2020-08-28 | 2020-12-01 | 陕西科技大学 | Mesoporous hollow carbon micron cage material and preparation method and application thereof |
CN112591734A (en) * | 2020-12-29 | 2021-04-02 | 陕西科技大学 | Nano carbon spheres based on in-situ growth of nano lignin and preparation method thereof |
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CN109659158A (en) * | 2018-12-07 | 2019-04-19 | 武汉工程大学 | A kind of nitrogen-doped carbon nanometer pipe/cobaltosic oxide composite aerogel and its preparation method and application |
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CN110165210A (en) * | 2019-05-14 | 2019-08-23 | 中国民航大学 | A kind of preparation method of the fluorocarbons positive electrode with height ratio capacity |
CN110165210B (en) * | 2019-05-14 | 2021-12-24 | 中国民航大学 | Preparation method of carbon fluoride anode material with high specific capacity |
CN110436441A (en) * | 2019-08-12 | 2019-11-12 | 青岛大学 | A kind of meso-porous hollow carbon sphere and its preparation and the application in electromagnetic absorption |
CN112017868A (en) * | 2020-08-28 | 2020-12-01 | 陕西科技大学 | Mesoporous hollow carbon micron cage material and preparation method and application thereof |
CN112591734A (en) * | 2020-12-29 | 2021-04-02 | 陕西科技大学 | Nano carbon spheres based on in-situ growth of nano lignin and preparation method thereof |
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