CN108010726A - A kind of ultracapacitor nucleocapsid porous electrode material and preparation method thereof - Google Patents
A kind of ultracapacitor nucleocapsid porous electrode material and preparation method thereof Download PDFInfo
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- CN108010726A CN108010726A CN201610985810.6A CN201610985810A CN108010726A CN 108010726 A CN108010726 A CN 108010726A CN 201610985810 A CN201610985810 A CN 201610985810A CN 108010726 A CN108010726 A CN 108010726A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 119
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 123
- 238000000034 method Methods 0.000 claims abstract description 49
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 43
- 239000002002 slurry Substances 0.000 claims abstract description 31
- 238000010000 carbonizing Methods 0.000 claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 claims abstract description 25
- 238000004220 aggregation Methods 0.000 claims abstract description 12
- 230000002776 aggregation Effects 0.000 claims abstract description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 21
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
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- 239000002245 particle Substances 0.000 claims description 13
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000005453 pelletization Methods 0.000 claims description 8
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- 238000001035 drying Methods 0.000 claims description 7
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229940070765 laurate Drugs 0.000 claims description 6
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- 239000011148 porous material Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 5
- 229930006000 Sucrose Natural products 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
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- 238000001694 spray drying Methods 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 235000000346 sugar Nutrition 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 2
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- 229910052743 krypton Inorganic materials 0.000 claims description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 238000010008 shearing Methods 0.000 claims description 2
- 229910052724 xenon Inorganic materials 0.000 claims description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000178 monomer Substances 0.000 abstract description 33
- 230000032683 aging Effects 0.000 abstract description 10
- 238000003466 welding Methods 0.000 abstract description 9
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- 238000003483 aging Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 25
- 230000008569 process Effects 0.000 description 22
- 239000002243 precursor Substances 0.000 description 19
- 229910021393 carbon nanotube Inorganic materials 0.000 description 18
- 239000002041 carbon nanotube Substances 0.000 description 18
- 239000003610 charcoal Substances 0.000 description 18
- 239000011246 composite particle Substances 0.000 description 15
- 229910021389 graphene Inorganic materials 0.000 description 14
- 238000005253 cladding Methods 0.000 description 10
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- 239000002253 acid Substances 0.000 description 6
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 239000011149 active material Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 5
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- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
- 239000006258 conductive agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
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- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 238000005470 impregnation Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910021392 nanocarbon Inorganic materials 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 235000013339 cereals Nutrition 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 239000008121 dextrose Substances 0.000 description 1
- 235000013681 dietary sucrose Nutrition 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229940093476 ethylene glycol Drugs 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229960002737 fructose Drugs 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
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- 238000003303 reheating Methods 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a kind of ultracapacitor nucleocapsid porous electrode material and preparation method thereof.The method of the present invention includes following steps：(1) electrode active material and Organic carbon source solution are mixed, obtains the slurry that viscosity is 500cP~2500cP；(2) slurry is granulated and dried, obtain electrode material presoma；(3) electrode material presoma is moved on in rotary furnace, is carbonized under inert gas shielding, obtain electrode material.The electrode material of the present invention is core shell structure, kernel is the aggregation of electrode active material, shell is porous carbonizing production, stable structure is formed between kernel and shell, 115F is not less than using capacity after 22 × 45 welding needle type ultracapacitor monomer agings of Φ that the electrode material is prepared into electrode and is assembled into, internal resistance is less than 12.2m Ω, and capacity attenuation rate is less than 30% after 65 DEG C of load 1500h, and internal resistance increase rate is also below 88.5%.
Description
Technical field
The invention belongs to supercapacitor technologies field, is related to a kind of electrode material and preparation method thereof, more particularly to one
Kind ultracapacitor nucleocapsid porous electrode material and preparation method thereof.
Background technology
Ultracapacitor is a kind of energy storage device between traditional capacitor and battery, according to energy stores mechanism
Ultracapacitor can be divided into electric double layer type ultracapacitor and fake capacitance type ultracapacitor by difference.The super electricity of electric double layer type
Container is to store energy by the double electrical layers formed after polarized electrolytic matter using electrode and electrolyte, due to this energy storage
Simply on two porous electrodes reversible ionic adsorption occurs for process, and therefore, electric double layer type ultracapacitor can be repeatedly
Up to a million times of discharge and recharge.
Electrode active material is one of critical material for determining ultracapacitor electrical property, and electric double layer type ultracapacitor is normal
Electrode active material mainly active charcoal, activated carbon fibre, graphene and carbon nanotube etc..Wherein, activated carbon and activity
Not graphited amorphous carbonaceous component is included in the microstructure of Carbon fibe, graphene and carbon nanotube are easy to be produced from reunion now
As so that the electrical conductivity of these electrode active materials is relatively low.
Therefore, when electrode active material is prepared into electrode, it usually needs addition metal dust, conductive black, furnace black,
The conductive agents such as acetylene black, Ketjen black or electrically conductive graphite improve the electric conductivity of electrode.For example, it is CN102569719 in publication No.
In the Chinese patent of A, activated carbon, conductive charcoal and binding agent are added the V- mixers equipped with high intensity stirring rod by inventor at the same time
Middle ground and mixed is simultaneously further prepared into electrode.But according to this side by activated carbon, conductive charcoal and binding agent ground and mixed
The electrode that formula is prepared has following problem：It is physically held together between activated carbon and conductive charcoal by binding agent, this knot
Credit union makes to produce larger contact resistance between activated carbon and conductive charcoal, therefore the additive amount of conductive charcoal is generally more, more to lead
The addition of electric charcoal significantly reduces the content of electrode active material, so that the capacity of ultracapacitor is substantially relatively low.
In electrode active material surface cladding Organic carbon source, carbonizing production is the effective ways for improving electrode material electrical conductivity.
Chinese patent CN105000544 A disclose a kind of preparation method of ultracapacitor high conductivity porous carbon material, first will
Water-soluble charcoal source obtains the synthetic product of charcoal precursor coated graphite alkene with graphene oxide solution reaction, then this synthesis is produced
Thing is transferred to tube furnace high temperature and sinters to obtain high conductivity porous carbon material.High conductivity porous carbon is prepared with this technique
The experimentation of material has following problem：After charcoal source is reacted with graphene oxide solution, the granularity of gained synthetic product is difficult to control
System, when this synthetic product is transferred to tube furnace high temperature sintering, since charcoal precursor relies on model moral to the cladding of graphene
Wals force combine, charcoal precursor before charing can from graphene surface occur fusing come off so that sintering obtain it is highly conductive
Porous carbon material is uneven in the cladding of graphene surface in property porous carbon material.
Chinese patent CN105261487 A disclose a kind of nucleocapsid porous nano Carbon Materials for electrode of super capacitor
Preparation method.Charcoal source solution and the stirring reaction of carbon nanotube dispersion liquid first obtains to the carbon nanotube of charcoal source cladding, then by charcoal
The charing of oxidized property acid, alkali activation, acid neutralize, obtain that nucleocapsid is porous to be received after vacuum freeze drying the carbon nanotube of source cladding successively
Rice Carbon Materials.The experimentation for preparing nucleocapsid porous nano Carbon Materials with this technique has following problem：The charcoal of charcoal source cladding
After the oxidized property acid charing of nanotube, since bond strength is low between amorphous carbon shell and carbon nanotube, so that being activated with alkali
Amorphous carbon shell is easy to layering occurs from carbon nanotube to come off during the carbon nanotube of unformed charcoal shell cladding.
The content of the invention
Electricity low for the electrical conductivity of electrode for super capacitor active material of the prior art, being combined by binding agent
Contact resistance is big between pole active material and conductive agent, bond strength between electrode active material and Organic carbon source carbonizing production
Low, Organic carbon source carbonizing production is uneven in electrode active material surface cladding, and using existing as caused by the above problem
A series of problems, such as internal resistance of ultracapacitor monomer made of the electrode active material of technology is high, capacity is low and self discharge is big.
It is an object of the invention to provide a kind of ultracapacitor of excellent performance nucleocapsid porous electrode material and preparation method thereof, adopt
With in the electrode material that is prepared of method of the present invention, the porous carbonizing production that Organic carbon source is transformed equably coats
Nucleocapsid mechanism is formed on the surface of electrode active material, bond strength is high between carbonizing production and electrode active material, and electrode
The electrical conductivity of material is high, particle diameter distribution is uniform, the Φ 22 × 45 that electrode material using the present invention is prepared into electrode and is assembled into
Capacity is not less than 115F after welding needle type ultracapacitor monomer aging, and internal resistance is less than 12.2m Ω, and passes through 65 DEG C of load 1500h
Capacity attenuation rate is less than 30% afterwards, and internal resistance increase rate is also below 88.5%.
To use following technical scheme up to the purpose, the present invention：
In the present invention, it is core shell structure that " nucleocapsid ", which refers to the electrode material,；The shell that " porous " refers to the electrode material is to carry
The structure of large number of orifices, porosity is 25%~70%, such as 25%, 30%, 35%, 38%, 40%, 44%, 48%, 52%,
56%th, 60%, 65%, 68% or 70% etc..
In a first aspect, the present invention provides a kind of electrode material, the electrode material includes kernel and shell, and the kernel is
The aggregation of electrode active material, the shell for Organic carbon source through obtained from charing carry pore structure carbonizing production, should
Bond strength between carbonizing production and the aggregation of electrode active material is high.
Preferably, the electrode material is positive electrode or negative material.
The electrode material stable structure of the present invention, is core shell structure, and kernel is the aggregation of electrode active material, and shell is
Loose structure, and bond strength is high between kernel and shell, the electrical conductivity height of the electrode material, particle diameter distribution are uniform, this knot
The electrode material that structure is unique, stablizes is prepared particularly suitable for preparing high performance ultracapacitor using the electrode material
Capacity is not less than 115F after into electrode and 22 × 45 welding needle type ultracapacitor monomer agings of Φ that are assembled into, and internal resistance is less than
12.2m Ω, and capacity attenuation rate is less than 30% after 65 DEG C of load 1500h, internal resistance increase rate is also below 88.5%.
Second aspect, the present invention provide the preparation method of electrode material as described in relation to the first aspect, the described method includes with
Lower step：
(1) electrode active material and Organic carbon source solution are mixed, obtains slurry, wherein, the viscosity of the slurry is
500cP~2500cP；
(2) slurry obtained to step (1) is granulated and dries, and obtains electrode material presoma；
(3) step (2) obtained electrode material presoma is moved on in rotary furnace, charcoal is carried out under inert gas shielding
Change, obtain electrode material.
The viscosity of step (1) the of the present invention slurry is 500cP~2500cP, for example, 500cP, 600cP, 750cP,
850cP、900cP、1000cP、1100cP、1300cP、1500cP、1600cP、1700cP、1750cP、1850cP、2000cP、
2100cP, 2200cP, 2350cP or 2500cP etc., are preferably 650cP~2400cP, in this preferred scope 650cP~2400cP
It is interior, it is easy to accomplish the granulation process of step (1) described slurry, and the associativity for being granulated obtained electrode material presoma is good.
The present invention obtains the slurry of appropriate viscosity, is made by the way that Organic carbon source solution is mixed with electrode active material
Grain, forms the composite particles of even particle size distribution, and in composite particles, the electrode active material being made of electrode active material
Aggregation be uniformly coated with Organic carbon source.
The electrode material that the method for the present invention is prepared includes kernel and shell, and the kernel is by electrode active material structure
Into electrode active material aggregation, the shell for Organic carbon source by charing obtained from pore structure charing produce
Thing, the bond strength between the aggregation and shell carbonizing production of the kernel electrode active material are high.
Preferably, the Organic carbon source in step (1) the Organic carbon source solution is selected from glucose sugar, sucrose, fructose, lemon
Any a kind or at least two kinds of of combination in acid, laurate, ethylene glycol, polyvinyl alcohol, phenolic resin or polyacrylonitrile, typical case but
Nonrestrictive example has：Glucose, sucrose, polyethylene glycol, polyacrylonitrile, the mixture of dextrose and saccharose, glucose and
The mixture of fructose, the mixture of citric acid, laurate and polyacrylonitrile, glucose sugar, sucrose, fructose, citric acid, laurate,
Mixture of polyethylene glycol and phenolic resin etc..
Preferably, it is sub- to be selected from water, ethanol, ether, acetone or dimethyl for the solvent in step (1) the Organic carbon source solution
Any a kind or at least two kinds of of combination in sulfone, typical but non-limiting example have：Water, ethanol, ethanol and dimethyl sulfoxide (DMSO)
Mixture, the mixture of acetone and dimethyl sulfoxide (DMSO), ethanol, ether, the mixture etc. of acetone and dimethyl sulfoxide (DMSO), but not
It is limited to above-mentioned solvent, other solvents that can dissolve Organic carbon source can also be used for the present invention.
Preferably, the mass ratio of the Organic carbon source in step (1) the Organic carbon source solution and solvent is (1~3):(240
, such as 1~400):240、2:250、3:250、1:280、2:280、3:280、1:300、2:300、3:300、1:320、2:320、
3:320、1:350、2:350、3:350、1:370、2:370、3:370、1:400、2:400 or 3:400 etc..
Preferably, step (1) electrode active material and the mass ratio in the Organic carbon source in the solution of the Organic carbon source
For (95~110):(1~3), such as 95:1、95:2、95:3、98:1、98:2、98:3、100:1、100:1.5、100:2、100:
2.2、100:2.5、100:3、105:1、105:2、105:3、110:1、110:2 or 110:3 etc..
Preferably, the equipment that step (1) mixing uses is selected from vacuum dispersion machine, planetary mixer, high shear dispersion
Any a kind or at least two kinds of of group in mulser, agitating ball mill, sand mill, ultrasonic dispersing machine, sand mixer or refiner
Close.
Preferably, the temperature of step (2) described granulation be 100 DEG C~250 DEG C, be, for example, 100 DEG C, 105 DEG C, 110 DEG C,
115 DEG C, 120 DEG C, 130 DEG C, 135 DEG C, 145 DEG C, 150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C, 190 DEG C, 200 DEG C, 220 DEG C or 250
DEG C etc., it is preferably 100 DEG C~200 DEG C.
Preferably, step (2) method used that is granulated is selected from spray drying granulation method, extruding pelletization method, fluid bed
Any a kind in comminution granulation or melt pelletization method.
Preferably, the temperature of step (2) described drying is 200 DEG C.
Preferably, the particle diameter of step (2) the electrode material presoma is at 5 μm~50 μm, for example, 5 μm, 8 μm, 10 μm, 15
μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 43 μm, 46 μm, 48 μm or 50 μm etc..
Preferably, step (3) described inert gas in nitrogen, helium, neon, argon gas, Krypton or xenon any 1
Kind or at least two kinds of combinations.
Preferably, the temperature of step (3) described charing is at 400 DEG C~800 DEG C, be, for example, 400 DEG C, 410 DEG C, 430 DEG C,
450℃、475℃、500℃、525℃、550℃、580℃、600℃、620℃、640℃、680℃、710℃、750℃、775℃
Or 800 DEG C etc..
Preferably, the time of step (3) described charing is in 2h~8h, for example, 2h, 2.5h, 3h, 3.3h, 3.6h, 4h,
4.2h, 4.5h, 5h, 5.5h, 6h, 6.4h, 6.8h, 7.2h, 7.6h or 8h etc..
The present invention method in, the carbonization process of step (3) carries out in rotary furnace, select rotary furnace the reason for be：Bag
The Organic carbon source for overlaying on the aggregate surface of electrode active material is melted in carbonization process, selects rotary furnace can be to avoid
The Organic carbon source of fusing settles, and realizes the carbonizing production in Organic carbon source to the uniform of the aggregate surface of electrode active material
Cladding.
Under the conditions of the carbonization temperature and carbonization time of the present invention, the Organic carbon source can occur charing and produce gas, make
Obtained organic carbonizing production is presented loose structure, the shell of the carbonizing production of the loose structure as final electrode material.
The third aspect, the present invention provide a kind of electrode, and the preparing raw material of the electrode includes the electricity described in first aspect
Pole material.The electrode can be used for the negative or positive electrode of ultracapacitor.
The preparation of electrode of the present invention is referred to the preparation method of electrode for super capacitor in the prior art, preferably
Preparation method it is as follows：
By the nucleocapsid porous electrode material of the present invention with polyacrylonitrile according to nucleocapsid porous electrode material：Polyacrylonitrile=
90:10 proportioning is mixed and made into the electrode for super capacitor (cathode and anode) that thickness is 200 μm, and cathode is cut into width
35mm, length 570mm；Anode is cut into wide 35mm, length 525mm；It is stand-by.
Fourth aspect, the present invention provide a kind of ultracapacitor, and the ultracapacitor includes the electricity described in second aspect
Pole material.
The preparation of ultracapacitor of the present invention is referred to the preparation method of ultracapacitor in the prior art, preferably
Preparation method it is as follows：
The special TF4035 types membrane of ultracapacitor produced using Japanese NKK companies and one roll set of positive and negative anodes cut
It is coiled into battery core.Battery core is placed in solution of the 1M tetraethyl ammonium tetrafluoro boric acids in acetonitrile vacuum impregnation to saturation imbibition state,
The battery core impregnated is loaded in shell, sealing, obtains Φ 22*45 welding needle type ultracapacitor monomers.
Compared with the prior art, the present invention has the advantages that：
(1) slurry of appropriate viscosity is made by using Organic carbon source solution and electrode active material by the present invention, to slurry
It is granulated, the surface that Organic carbon source is uniformly coated on the aggregation of electrode active material is obtained composite particles, and it is compound
The particle diameter distribution of particle is uniform, further obtains the electrode material presoma of even particle size distribution, is then being closed using rotary furnace
Charing process is carried out under the conditions of suitable temperature and time, the carbonizing production that Organic carbon source changes into loose structure is coated on electrode
The surface of the aggregation of active material, forms the electrode material of core shell structure, and the bond strength between kernel and shell is high.
(2) electrode material of the invention is core shell structure, and kernel is the electrode active material formed by electrode active material
Aggregation, shell is the carbonizing production in the Organic carbon source of loose structure, and bond strength is high between kernel and shell.The present invention
Electrode material electrical conductivity is high, particle diameter distribution is uniform, the Φ 22 that electrode is prepared into using the electrode material and is assembled into ×
Capacity is not less than 115F after 45 welding needle type ultracapacitor monomer agings, and internal resistance is less than 12.2m Ω, and passes through 65 DEG C of loads
Capacity attenuation rate is less than 30% after 1500h, and internal resistance increase rate is also below 88.5%.
(3) technical solution using the present invention, can effectively solve the electrical conductivity of electrode for super capacitor active material
Contact resistance is big between low, the electrode active material and conductive agent that are combined by binding agent, Organic carbon source carbonizing production is in electrode
Surface of active material cladding is uneven, Organic carbon source carbonizing production is easy to ask from what the generation layering of electrode active material surface came off
Topic.
Embodiment
Technical scheme is further illustrated below by embodiment.
Embodiment 1
The preparation of electrode material：
1) take 1g glucose to be scattered in 300g water and form glucose solution, 100g activated carbons are added into glucose solution
In, it is uniformly mixed with vacuum dispersion machine, obtains the slurry that viscosity is 1650cP；
2) by slurry spray drying granulation at 160 DEG C obtained by step 1), composite particles is obtained, are done with 200 DEG C of temperature
Dry composite particles, obtain the activated carbon of coated with uniform glucose as electrode material precursor；
3) step 2) the electrode obtained material precursor is transferred in rotary furnace, under nitrogen protection with 600 DEG C of pyrocarbons
Change 3h, it is more to obtain the nucleocapsid being made of the glucose carbonizing production of activated carbon and the loose structure for being evenly coated at activated carbon surface
Pore electrod material.
The preparation of electrode：
The nucleocapsid porous electrode material that the present embodiment is obtained is with polyacrylonitrile by nucleocapsid porous active Carbon Materials：Polypropylene
Nitrile=90:10 proportioning mixing, be prepared into thickness be 200 μm electrode for super capacitor (not only as cathode and as bear
Pole).Cathode is cut into wide 35mm, length 570mm；Anode is cut into wide 35mm, length 525mm is stand-by.
The assembling of ultracapacitor monomer：
The special TF4035 types membrane of ultracapacitor produced using Japanese NKK companies and one roll set of positive and negative anodes cut
It is coiled into battery core.Battery core is placed in solution of the 1M tetraethyl ammonium tetrafluoro boric acids in acetonitrile vacuum impregnation to saturation imbibition state,
The battery core impregnated is loaded in shell, sealing, obtains Φ 22*45 welding needle type ultracapacitor monomers.
The test of ultracapacitor monomer：
By ultracapacitor monomer with 2.7V aging 10h, the appearance of the ultracapacitor monomer after test aging at 65 DEG C
Amount and internal resistance.To assess the electrical properties in high temperatures of ultracapacitor monomer, ultracapacitor monomer is continued at 65 DEG C with 2.7V
Load 1500h, the capacity of ultracapacitor monomer and internal resistance after testing load, the capacity of ultracapacitor monomer after calculated load
Attenuation rate and internal resistance increase rate.Ultracapacitor monomer is discharged to below 0.1V after being completed.The test result such as institute of table 1
Show.
Embodiment 2
The preparation of electrode material：
1) take 1g fructose to be scattered in 320g ethanol and form fructose soln, 100g activated carbon fibre is added into fructose soln
In, it is uniformly mixed with planetary mixer, obtains the slurry that viscosity is 1230cP；
2) by slurry extruding pelletization at 180 DEG C obtained by step 1), composite particles are obtained, it is multiple with 200 DEG C of temperature drying
Particle is closed, obtains the activated carbon fibre of coated with uniform fructose as electrode material precursor；
3) step 2) the electrode obtained material precursor is transferred in rotary furnace, with 550 DEG C of pyrocarbons under helium protection
Change 6h, obtain what is be made of the fructose carbonizing production of activated carbon fibre and the loose structure for being evenly coated at activated carbon fibre surface
Nucleocapsid porous electrode material.
Using the nucleocapsid porous electrode material of the present embodiment prepare the process of electrode, ultracapacitor monomer assembling and
Test process is same as Example 1, and test result is shown in Table 1.
Embodiment 3
The preparation of electrode material：
1) 1g laurate is taken to be scattered in formation bay acid solution in 350g ether, by the dilute addition bay acid solution of 100g graphite
In, it is uniformly mixed with high-shearing dispersion emulsifying machine, obtains the slurry that viscosity is 780cP；
2) slurry obtained by step 1) is granulated in 100 DEG C of fluidized bed at elevated, obtains composite particles, dried with 200 DEG C of temperature
Composite particles, obtain the lauric graphene of coated with uniform as electrode material precursor；
3) step 2) the electrode obtained material precursor is transferred in rotary furnace, with 650 DEG C of pyrocarbons under argon gas protection
Change 4h, it is more to obtain the nucleocapsid being made of the laurate carbonizing production of graphene and the loose structure for being evenly coated at graphene surface
Pore electrod material.
Using the nucleocapsid porous electrode material of the present embodiment prepare the process of electrode, ultracapacitor monomer assembling and
Test process is same as Example 1, and test result is shown in Table 1.
Embodiment 4
The preparation of electrode material：
1) take 1g polyethylene glycol to be scattered in 300g acetone and form polyglycol solution, 100g carbon nanotubes are added into poly- second
In glycol solution, it is uniformly mixed with agitating ball mill, obtains the slurry that viscosity is 1560cP；
2) by slurry melt pelletization at 130 DEG C obtained by step 1), composite particles are obtained, it is multiple with 200 DEG C of temperature drying
Particle is closed, obtains the carbon nanotube of coated with uniform polyethylene glycol as electrode material precursor；
3) step 2) the electrode obtained material precursor is transferred in rotary furnace, under nitrogen protection with 500 DEG C of pyrocarbons
Change 7h, obtain what is be made of the polyethylene glycol carbonizing production of carbon nanotube and the loose structure for being evenly coated at carbon nanotube surface
Nucleocapsid porous electrode material.
Using the nucleocapsid porous electrode material of the present embodiment prepare the process of electrode, ultracapacitor monomer assembling and
Test process is same as Example 1, and test result is shown in Table 1.
Embodiment 5
The preparation of electrode material：
1) take 2g citric acids to be scattered in 270g water and form citric acid solution, 100g activated carbons are added into citric acid solution
In, it is uniformly mixed with sand mill, obtains the slurry that viscosity is 1650cP；
2) by slurry melt pelletization at 200 DEG C obtained by step 1), composite particles are obtained, it is multiple with 200 DEG C of temperature drying
Particle is closed, obtains the activated carbon of coated with uniform citric acid as electrode material precursor；
3) step 2) the electrode obtained material precursor is transferred in rotary furnace, with 400 DEG C of pyrocarbons under helium protection
Change 8h, it is more to obtain the nucleocapsid being made of the citric acid carbonizing production of activated carbon and the loose structure for being evenly coated at activated carbon surface
Pore electrod material.
Using the nucleocapsid porous electrode material of the present embodiment prepare the process of electrode, ultracapacitor monomer assembling and
Test process is same as Example 1, and test result is shown in Table 1.
Embodiment 6
The preparation of electrode material：
1) take 2g polyacrylonitrile to be scattered in 370g dimethyl sulfoxide (DMSO)s and form polyacrylonitrile solution, by 100g activated carbon fibre
Add in polyacrylonitrile solution, be uniformly mixed with ultrasonic dispersing machine, obtain the slurry that viscosity is 660cP；
2) by slurry extruding pelletization at 170 DEG C obtained by step 1), composite particles are obtained, it is multiple with 200 DEG C of temperature drying
Particle is closed, obtains the activated carbon fibre of coated with uniform polyacrylonitrile as electrode material precursor；
3) step 2) the electrode obtained material precursor is transferred in rotary furnace, with 800 DEG C of pyrocarbons under argon gas protection
Change 2h, obtain the polyacrylonitrile by carbonization product structure by activated carbon fibre and the loose structure for being evenly coated at activated carbon fibre surface
Into nucleocapsid porous electrode material.
Using the nucleocapsid porous electrode material of the present embodiment prepare the process of electrode, ultracapacitor monomer assembling and
Test process is same as Example 1, and test result is shown in Table 1.
Embodiment 7
The preparation of electrode material：
1) take 2g polyvinyl alcohol to be scattered in 280g water and form poly-vinyl alcohol solution, 100g graphenes are added into polyvinyl alcohol
In solution, it is uniformly mixed with sand mixer, obtains the slurry that viscosity is 1940cP；
2) by slurry spray drying granulation at 120 DEG C obtained by step 1), composite particles is obtained, are done with 200 DEG C of temperature
Dry composite particles, obtain the graphene of coated with uniform polyvinyl alcohol as electrode material precursor；
3) step 2) the electrode obtained material precursor is transferred in rotary furnace, under nitrogen protection with 450 DEG C of pyrocarbons
Change 7h, obtain the nucleocapsid being made of the polyvinyl alcohol carbonizing production of graphene and the loose structure for being evenly coated at graphene surface
Porous electrode material.
Using the nucleocapsid porous electrode material of the present embodiment prepare the process of electrode, ultracapacitor monomer assembling and
Test process is same as Example 1, and test result is shown in Table 1.
Embodiment 8
The preparation of electrode material：
1) take 2g phenolic resin dispersions to form phenol resin solution in 260g acetone, 100g carbon nanotubes are added into phenolic aldehyde
In resin solution, it is uniformly mixed with refiner, obtains the slurry that viscosity is 2370cP；
2) slurry obtained by step 1) is granulated in 160 DEG C of fluidized bed at elevated, obtains composite particles, dried with 200 DEG C of temperature
Composite particles, obtain the carbon nanotube of coated with uniform phenolic resin as electrode material precursor；
3) step 2) the electrode obtained material precursor is transferred in rotary furnace, with 700 DEG C of pyrocarbons under argon gas protection
Change 3h, obtain what is be made of the phenolic resin of carbon nanotube and the loose structure for being evenly coated at carbon nanotube surface charing product
Nucleocapsid porous electrode material.
Using the nucleocapsid porous electrode material of the present embodiment prepare the process of electrode, ultracapacitor monomer assembling and
Test process is same as Example 1, and test result is shown in Table 1.
Comparative example 1
Electrode material：
The electrode material of this comparative example is activated carbon.
The preparation of electrode：
Activated carbon, conductive black and polyacrylonitrile are pressed into activated carbon:Conductive black:Polyacrylonitrile=85:5:10 proportioning
It is prepared by mixing into the electrode for super capacitor that thickness is 200 μm.
Ultracapacitor monomer assembles and test process is same as Example 1, and test result is shown in Table 1.
Comparative example 2
Except step 2) is without spray drying granulation the step of, and outside the slurry of convection drying step 1), other preparations
Method and condition are same as Example 1.This comparative example obtained electrode material is the carbon by being coated with polyvinyl alcohol carbonizing production
Nanotube composition, carbonizing production is coated on the surface of single carbon nanotubes, without being coated on carbon nanotube aggregation body surface
Face.
The process of electrode, the assembling of ultracapacitor monomer and test process are prepared using the electrode material of this comparative example
Same as Example 1, test result is shown in Table 1.
Electrical property after electrical property and load 1500h after the aging of 1 Φ 22*45 welding needle type ultracapacitor monomers of table
According to the test result of embodiment 1-8, technical solution using the present invention first pass through granulation reuse rotary furnace into
The electrode assembling that row heat treatment gained nucleocapsid porous electrode material and polyacrylonitrile are mixed with is into the super electricity of Φ 22*45 welding needle types
Container monomer, capacity is not less than 115F after aging, and internal resistance is less than 12.2m Ω, and ultracapacitor monomer is after 65 DEG C of load 1500h
Capacity attenuation rate is less than 30%, and internal resistance increase rate is also below 88.5%.According to the test result of comparative example 1, with activated carbon, conduction
The electrode assembling that carbon black and polyacrylonitrile are mixed with is into Φ 22*45 welding needle type ultracapacitor monomers, and capacity is after aging
111F, internal resistance are 13.6m Ω, and monomer capacity attenuation rate after 65 DEG C of load 1500h is more than 30%, internal resistance increase rate considerably beyond
100%.According to the test result of comparative example 2, with the electrode assembling prepared without being granulated the electrode material of directly heat treatment gained
Into ultracapacitor monomer, electrical property is close with embodiment 1~8 after aging, and still, ultracapacitor monomer is through 65 DEG C of loads
Capacity attenuation rate is still above 30% after 1500h, and internal resistance increase rate is also considerably beyond 100%.Contrast is it is recognised that the present invention adopts
Electrode material of the nucleocapsid porous electrode material than comparative example 1 and comparative example 2 of reheating processing preparation is granulated under suitable parameters with elder generation
The stable structure of material, it is also more preferable for the performance after ultracapacitor monomer.
Applicant states that the present invention illustrates the method detailed of the present invention, but not office of the invention by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., all fall within protection scope of the present invention and the open scope.
Claims (10)
1. a kind of electrode material, it is characterised in that the electrode material includes kernel and shell, and the kernel is electrode activity material
The aggregation of material, the shell are Organic carbon source through the carbonizing production with pore structure obtained from charing；
Preferably, the electrode material is positive electrode or negative material.
2. the preparation method of electrode material as claimed in claim 1, it is characterised in that the described method comprises the following steps：
(1) electrode active material and Organic carbon source solution are mixed, obtain slurry, wherein, the viscosity of the slurry for 500cP~
2500cP；
(2) slurry obtained to step (1) is granulated and dries, and obtains electrode material presoma；
(3) step (2) obtained electrode material presoma is moved on in rotary furnace, is carbonized, obtained under inert gas shielding
To electrode material.
3. according to the method described in claim 2, it is characterized in that, Organic carbon source in step (1) the Organic carbon source solution
Appointing in glucose sugar, sucrose, fructose, citric acid, laurate, polyethylene glycol, polyvinyl alcohol, phenolic resin or polyacrylonitrile
The combination of a kind or at least two kinds of of meaning；
Preferably, the solvent in step (1) the Organic carbon source solution is in water, ethanol, ether, acetone or dimethyl sulfoxide (DMSO)
Any a kind or at least two kinds of of combination.
4. according to the method in claim 2 or 3, it is characterised in that the Organic carbon in step (1) the Organic carbon source solution
The mass ratio of source and solvent is (1~3):(240~400)；
Preferably, step (1) electrode active material and the mass ratio in the Organic carbon source in the solution of the Organic carbon source are (95
~110):(1~3).
5. according to claim 2-4 any one of them methods, it is characterised in that the equipment choosing that step (1) mixing uses
From vacuum dispersion machine, planetary mixer, high-shearing dispersion emulsifying machine, agitating ball mill, sand mill, ultrasonic dispersing machine, mulling
Any a kind or at least two kinds of of combination in machine or refiner；
Preferably, the viscosity 650cP~2400cP of step (1) described slurry.
6. according to claim 2-5 any one of them methods, it is characterised in that the temperature of step (2) described granulation is 100 DEG C
~250 DEG C, be preferably 100 DEG C~200 DEG C；
Preferably, step (2) method used that is granulated is selected from spray drying granulation method, extruding pelletization method, fluidized bed prilling
Any a kind in method or melt pelletization method；
Preferably, the temperature of step (2) described drying is 200 DEG C.
7. according to claim 2-6 any one of them methods, it is characterised in that step (2) the electrode material presoma
Particle diameter is at 5 μm~50 μm.
8. according to claim 2-7 any one of them methods, it is characterised in that step (3) described inert gas be selected from nitrogen,
Any a kind or at least two kinds of of combination in helium, neon, argon gas, Krypton or xenon；
Preferably, the temperature of step (3) described charing is at 400 DEG C~800 DEG C；
Preferably, the time of step (3) described charing is in 2h~8h.
9. a kind of electrode, it is characterised in that the preparing raw material of the electrode includes the electrode material described in claim 1；
Preferably, the electrode is the cathode of ultracapacitor or the anode of ultracapacitor.
10. a kind of ultracapacitor, it is characterised in that the ultracapacitor includes the electrode material described in claim 1.
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| CN105244179A (en) * | 2015-11-05 | 2016-01-13 | 宁波南车新能源科技有限公司 | Core-shell porous nanometer carbon material applied to supercapacitor electrode |
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