CN107180667A - A kind of electrocondution slurry and preparation method thereof, application - Google Patents
A kind of electrocondution slurry and preparation method thereof, application Download PDFInfo
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- CN107180667A CN107180667A CN201710291746.6A CN201710291746A CN107180667A CN 107180667 A CN107180667 A CN 107180667A CN 201710291746 A CN201710291746 A CN 201710291746A CN 107180667 A CN107180667 A CN 107180667A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention provides a kind of electrocondution slurry, mainly it is made by following raw material:In parts by weight, 0.1 10 parts of graphene/carbon nanotube hybrid thing, 0.1 10 parts of dispersant, 80 99 parts of solvent.Preparation method includes:After graphene/carbon nanotube hybrid thing and solvent grinding are stirred, addition dispersant grinding more than 5s is produced.The present invention electrocondution slurry can be widely applied to lithium battery positive and negative pole material conductive agent, electrode material for super capacitor, carbon paper in terms of application.
Description
Technical field
The present invention relates to electrocondution slurry preparing technical field, in particular to a kind of electrocondution slurry and preparation method thereof,
Using.
Background technology
CNT can be regarded as the one-dimensional tubular nanometer carbon material crimped by graphene sheet layer.Preferable carbon is received
Carbon atom is sp2 hydridization bonding patterns in nanotube structures, with huge draw ratio.Characteristic on carbon nano tube structure is determined
It has the excellent properties in terms of excellent electromagnetism, mechanics, calorifics.But in actual application, CNT by
In its each other stronger Van der Waals force and easily assemble, so as to be difficult to disperse, seriously hinder filling for its excellent properties
Distribution is waved.
Graphene is as a kind of two-dimentional nano-carbon material, and bonding pattern is similar with CNT between its carbon atom.Stone
Black alkene has the advantages that good toughness, electron mobility height, thermal conductivity are high as " king of new material ", in solar cell, sensing
Device, nanoelectronics, composite, field emmision material and energy storage field are with a wide range of applications.Can be in conductive network
In play wire effect, its huge specific surface area also have electric double layer effect, may be used as the electrode material of ultracapacitor.
But it is easy to assemble as CNT, so as to have influence on the performance of actual use.
Such as, a kind of carbon nanotube conducting slurry, also patent have been recorded in patent CN103886932A
Also a kind of carbon nano tube paste is described in CN103400991B, is typically all to use single CNT material in the prior art
Material or single grapheme material prepare electrocondution slurry, and the defect easily reunited in itself based on CNT, graphene, gesture
Must be to actual electric conductivity and other application performance impact than larger, therefore how to develop a kind of the new of superior performance
Type electrocondution slurry is technical problem urgently to be resolved hurrily in the prior art.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of electrocondution slurry, miscellaneous with graphene-carbon nano tube in the electrocondution slurry
Compound be raw material be prepared from, abandoned it is conventional using single carbon nano-tube material or single grapheme material come
The technology of electrocondution slurry is prepared, electrocondution slurry is prepared by using the compound material progress of this graphene-carbon nano tube, is made
Standby obtained electrocondution slurry dispersive property is stable, the combinations of two kinds of materials has been mutually promoted dispersiveness, it is to avoid agglomeration traits
Occur, improve its electric conductivity, develop a kind of graphene-carbon nano tube hybrid slurry of excellent performance so that the slurry
Material is more beneficial for commercial applications, has filled up correlation technique blank.
The second object of the present invention is the preparation method for providing above-mentioned electrocondution slurry, and the preparation method is simple, operation side
Just, operating condition is gentleer, and front and rear step linking is close, it is easy to operate.
The third object of the present invention is the application for providing above-mentioned electrocondution slurry, using widely, can extensive use
In terms of lithium battery positive and negative pole material conductive agent, electrode material for super capacitor, carbon paper.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme:
The embodiments of the invention provide a kind of electrocondution slurry, mainly it is made by following raw material:In parts by weight, graphene-
0.1-10 parts of carbon nano-tube hybridization thing, 0.1-10 parts of dispersant, 80-99 parts of solvent.
In the prior art, CNT can be regarded as the one-dimensional tubular nanometer carbon materials crimped by graphene sheet layer
Material.Carbon atom is sp2 hydridization bonding patterns in preferable carbon nano tube structure, with huge draw ratio.Carbon nano tube structure
On characteristic determine that it has the excellent properties in terms of excellent electromagnetism, mechanics, calorifics.But in actual application
In, CNT due to its each other stronger Van der Waals force and easily assemble, so as to be difficult to disperse, seriously hinder it
Excellent properties give full play to.
Graphene is as a kind of two-dimentional nano-carbon material, and bonding pattern is similar with CNT between its carbon atom.Stone
Black alkene has the advantages that good toughness, electron mobility height, thermal conductivity are high as " king of new material ", in solar cell, sensing
Device, nanoelectronics, composite, field emmision material and energy storage field are with a wide range of applications.Can be in conductive network
In play wire effect, its huge specific surface area also have electric double layer effect, may be used as the electrode material of ultracapacitor.
But it is easy to assemble as CNT, so as to have influence on the performance of actual use.
General is all to be led using single carbon nano-tube material or single grapheme material to prepare in the prior art
Plasma-based material, and the defect easily reunited in itself based on CNT, graphene, will certainly to actual electric conductivity and other should
With performance impact than larger, therefore it is urgently to be resolved hurrily in the prior art for how developing a kind of Novel conductive paste of superior performance
Technical problem.
In order to solve the technical problem appeared above, the invention provides a kind of Novel conductive paste of excellent performance, its
Using graphene-carbon nano tube hybrid as major ingredient, as a result of composite as raw material, the electrocondution slurry prepared
Dispersive property is excellent, the problem of be not in reunion, and other corresponding performances also increase, and do not use also in the prior art
The compound material of graphene-carbon nano tube prepares the relevant report of electrocondution slurry, and the present invention still belongs to pioneering, filled up correlation technique
Blank.
And the graphene-carbon nano tube hybrid of the present invention is to utilize special catalyst by chemical vapour deposition technique
Graphene and carbon nano tube compound material that grain is grown, such CNT is the surface for being grown directly upon graphene, and
It is not simple mixing, dual structure and property with graphene and CNT, using such graphene-carbon nano tube
The electrocondution slurry electric conductivity that hybrid is prepared is more excellent, has unusual excellent in mechanics, electricity, calorifics and magnetics
Performance.
Specifically, the preparation method of graphene-carbon nano tube hybrid comprises the following steps:
1) sheet layer material of catalyst activity component will be loaded with as catalyst, the active component of the catalyst is
Fe, Co, Ni, Cu, Mo or W, its content account for the 0.1%~50% of catalyst quality;
2) catalyst is placed in reactor, by chemical vapor deposition processes, carbon is deposited on the surface of the catalyst
The product of gained, is then placed in product purification device and is purified, obtain CNT and graphite by nanotube and graphene
CNT is grown directly upon on the surface of graphene in alkene compound, CNT and graphene complex.
Preferably, in chemical vapor deposition processes, temperature control at 500-1200 DEG C, it is more excellent control 800-1000 DEG C it
Between.
In addition, the stability of graphene-carbon nano tube hybrid itself can be strengthened by introducing hetero-atoms, then graphite
Preferably include the hetero atom of doping in alkene-carbon nano-tube hybridization thing, the hetero atom is preferably included in boron, nitrogen phosphate and sulfur atom
One or more of combinations.
It should be noted that the present invention program protection focus on using graphene-carbon nano tube hybrid with it is scattered
Agent, solvent carry out rational 5 with the electrocondution slurry for preparing excellent properties, except being by inventor using the species of raw material
Strictly select, the proportion relation between three kinds of raw materials is also inventor by largely groping to obtain, it is necessary to be strict controlled in this
In the range of invention.
For proportion optimizing, preferably according to following consumption proportion:In terms of mass fraction, graphene-carbon nano tube hybrid
2-8 parts, 0.2-8 parts of dispersant, 85-95 parts of solvent, more excellent for 5 parts of graphene-carbon nano tube hybrid, 1 part of dispersant is molten
90 parts of agent, it can in addition contain for, 0.3 part of graphene-carbon nano tube hybrid, 0.4 part, 0.5 part, 0.6 part, 0.7 part etc., disperse
0.15 part of agent, 0.16 part, 0.17 part, 0.18 part etc., 81 parts, 82 parts, 83 parts etc. of solvent.
In the present invention, dispersant includes polyvinylpyrrolidone, polyethylene glycol, sodium cellulose glycolate, dodecyl
One or more in benzene sulfonic acid sodium salt, dodecyl sodium sulfate, cellulose derivative, fatty acid polyethylene glycol ester.
Solvent includes one or both of organic solvent, inorganic solvent, organic solvent include methanol, ethanol, isopropanol,
Ether, expoxy propane, styrene, perchloroethylene, trichloro ethylene, ethylene glycol ether, triethanolamine, glycol dimethyl ether, benzene,
Toluene, dimethylbenzene, chlorobenzene, dichloro-benzenes, dichloromethane, methyl acetate, ethyl acetate, propyl acetate, acetone, espeleton, first
One or several kinds in base isobutyl ketone, pyrimidine, phenol, 1-METHYLPYRROLIDONE, DMA, inorganic solvent can
Think water.By from specific dispersant, solvent be combined collocation can so that prepare electrocondution slurry stability, lead
It is more excellent in terms of electrically.
The embodiment of the present invention is except there is provided a kind of formula of electrocondution slurry, additionally providing the preparation side of the electrocondution slurry
Method, specifically includes following steps:After graphene-carbon nano tube hybrid and solvent grinding are stirred, addition dispersant is ground
More than 5s is ground, is produced.
The preparation method of the electrocondution slurry of the present invention is simple to operate, and operating condition is gentleer, by using the present invention's
The electrocondution slurry dispersive property that preparation method is prepared is good, and internal resistance is small and does not have the generation of the phenomenon of sedimentation, and phase is subsequently made
Product such as lithium battery is closed, the use scope of lithium battery can be significantly extended, extends the service life of lithium battery.
Preferably, the time control ground after addition dispersant is more excellent for 20-40s, also one between 10s-24h
As add after solvent the time control ground in 5min or so.
Preferably, the Task-size Controlling ground after addition dispersant is between 0.01-10 μm;More excellent control 2-8 μm it
Between, it can cause be sufficiently mixed uniformly between each raw material by the convenient grinding condition of control ratio, obtain excellent performance
Electrocondution slurry.
Preferably, the abrasive media is included in bead, zirconium silicate pearl, zirconia beads, titanium dioxide aluminium pill, steel ball
One or several kinds of combinations, can carry out unrestricted choice according to actual conditions.
Performance is more excellent in all fields for the electrocondution slurry prepared using the embodiment of the present invention, and application
Than wide, it is widely used in lithium battery positive and negative pole material conductive agent, electrode material for super capacitor, carbon paper aspect.
Being for explanation is needed, the material that may be added in the electrocondution slurry of the present invention has:Conductive black, many wall carbon
Nanotube, graphite, graphene, graphite nano plate, Argent grain, copper particle, as long as but including primary raw material graphite of the invention
The electrocondution slurry of alkene hybrid is within the scope of the present invention.
Compared with prior art, beneficial effects of the present invention are:
1) it is prepared from the electrocondution slurry of the embodiment of the present invention using graphene-carbon nano tube hybrid as raw material,
The conventional technology that electrocondution slurry is prepared using single carbon nano-tube material or single grapheme material has been abandoned, has been passed through
Electrocondution slurry is prepared using the compound material progress of this graphene-carbon nano tube, the electrocondution slurry dispersiveness prepared
Can be stable;
2) present invention develops the graphene-carbon nano tube hybrid slurry of excellent performance a kind of, passes through two kinds of materials
With reference to dispersiveness of having mutually promoted, it is to avoid the generation of agglomeration traits, its electric conductivity is improved so that the slurry is more beneficial for
Commercial applications, have filled up correlation technique blank;
3) preparation method of electrocondution slurry provided in an embodiment of the present invention, preparation method is simple, easy to operate, operating condition
Compare gentle, front and rear step linking is close, it is easy to operate.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described.
Fig. 1 is that 1-3,6,7 and comparative example 1-3 of the embodiment of the present invention compound the button ultracapacitor ratio prepared with activated carbon
The graph of relation of capacity and discharge current density.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, be
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
0.1g graphene-carbon nano tubes hybrid, 80g ethanol are added in sand mill, sanding media is 0.6mm zirconiums
5min is sanded in pearl, low speed, then adds 0.1g polyvinylpyrrolidones, is sanded at a high speed after 5s, sand milling and obtains particle diameter less than 10 μm
Graphene hybrid electrocondution slurry, the electrocondution slurry be used for prepare lithium battery positive and negative pole material conductive agent, super capacitor electrode
Pole material and carbon paper.
Wherein, the preparation method of graphene-carbon nano tube hybrid includes:
1) sheet layer material of catalyst activity component will be loaded with as catalyst, the active component of the catalyst is
Fe, its content accounts for the 0.1% of catalyst quality;
2) catalyst is placed in reactor, by chemical vapor deposition processes, carbon is deposited on the surface of the catalyst
The product of gained, is then placed in product purification device and is purified, produced by nanotube and graphene.
Embodiment 2
10g graphene-carbon nano tubes hybrid, 99g methanol and ethanol are added in sand mill, sanding media is
5min is sanded in 0.6mm zirconia beads, low speed, then adds 10g sodium cellulose glycolates, is obtained after 10s, sand milling is sanded at a high speed
The graphene hybrid electrocondution slurry of 8 μm of particle diameter, the electrocondution slurry is used to prepare lithium battery positive and negative pole material conductive agent, super electricity
Container electrode material and carbon paper.
Wherein, the preparation method of graphene-carbon nano tube hybrid includes:
1) sheet layer material of catalyst activity component will be loaded with as catalyst, the active component of the catalyst is
Mo, its content accounts for the 20% of catalyst quality;
2) catalyst is placed in reactor, by chemical vapor deposition processes, be catalyzed under the conditions of 500-1200 DEG C
The product of gained, is then placed in product purification device and is purified, i.e., by deposition of carbon nanotubes and graphene on the surface of agent
.
Embodiment 3
2g graphene-carbon nano tubes hybrid, 95g methanol and ethanol are added in sand mill, sanding media is
5min is sanded in 0.6mm zirconia beads, low speed, then adds 0.2g sodium cellulose glycolates, is sanded at a high speed after 24h, sand milling and obtains
To 0.01 μm of graphene hybrid electrocondution slurry of particle diameter, the electrocondution slurry be used to preparing lithium battery positive and negative pole material conductive agent,
Electrode material for super capacitor and carbon paper.
Wherein, the preparation method of graphene-carbon nano tube hybrid includes:
1) sheet layer material of catalyst activity component will be loaded with as catalyst, the active component of the catalyst is
Ni, its content accounts for the 20% of catalyst quality;
2) catalyst is placed in reactor, by chemical vapor deposition processes, be catalyzed under the conditions of 800-1000 DEG C
The product of gained, is then placed in product purification device and is purified, i.e., by deposition of carbon nanotubes and graphene on the surface of agent
.
Embodiment 4
8g graphene-carbon nano tubes hybrid, 85g triethanolamine are added in sand mill, sanding media is 0.6mm
5min is sanded in titanium dioxide aluminium pill, low speed, then adds 8g sodium cellulose glycolates and neopelex, is sanded at a high speed
The graphene hybrid electrocondution slurry of 2 μm of particle diameter is obtained after 10h, sand milling, the electrocondution slurry is used to prepare lithium battery both positive and negative polarity material
Expect conductive agent, electrode material for super capacitor and carbon paper.
Wherein, the preparation method of graphene-carbon nano tube hybrid includes:
1) sheet layer material of catalyst activity component will be loaded with as catalyst, the active component of the catalyst is
Co, its content accounts for the 50% of catalyst quality;
2) catalyst is placed in reactor, by chemical vapor deposition processes, be catalyzed under the conditions of 800-1000 DEG C
The product of gained, is then placed in product purification device and is purified, i.e., by deposition of carbon nanotubes and graphene on the surface of agent
.
Embodiment 5
5g graphene-carbon nano tubes hybrid, 90g water are added in sand mill, sanding media is 0.6mm titanium dioxides
5min is sanded in aluminium pill, low speed, then adds 8g sodium cellulose glycolates and neopelex, 15h is sanded at a high speed, be sanded
The graphene hybrid electrocondution slurry of 0.01-1 μm of particle diameter is obtained afterwards, and the electrocondution slurry is led for preparing lithium battery positive and negative pole material
Electric agent, electrode material for super capacitor and carbon paper.
The specific preparation method of graphene-carbon nano tube hybrid is consistent with embodiment 4.
Embodiment 6
1g graphene-carbon nano tubes hybrid, 85g ethanol are added in sand mill, sanding media is 0.6mm dioxies
Change aluminium pill, 5min is sanded in low speed, then add 8g sodium cellulose glycolates and neopelex, 15h, sand are sanded at a high speed
The graphene hybrid electrocondution slurry of 0.01-1 μm of particle diameter is obtained after mill, the electrocondution slurry is used to prepare lithium battery positive and negative pole material
Conductive agent, electrode material for super capacitor and carbon paper.
The specific preparation method of graphene-carbon nano tube hybrid is consistent with embodiment 4.
Embodiment 7
4g graphene-carbon nano tubes hybrid, 396g water are added in sand mill, sanding media is 0.6mm glass
5min is sanded in pearl, low speed, then adds 1g polyvinylpyrrolidones, and the graphite that 10 μm of particle diameter is obtained after 2h, sand milling is sanded at a high speed
Alkene hybrid electrocondution slurry, the electrocondution slurry is used to prepare lithium battery positive and negative pole material conductive agent, electrode material for super capacitor
And carbon paper.
The specific preparation method of graphene-carbon nano tube hybrid is consistent with embodiment 4.
Comparative example 1
The carbon nanotube conducting slurry that embodiment 1 in CN103886932A patents is prepared.
Comparative example 2
The carbon nanotube conducting slurry that embodiment 1 in CN103400991B patents is prepared.
Comparative example 3
Conventional conductive agent conductive black SP is used as conductive agent.
Experimental example 1
By 1-3 of the embodiment of the present invention, 6,7, and the electrocondution slurry prepared of comparative example 1,2 and activated carbon and conductive black,
CMC, SBR are compounded by same ratio, make button cell test data.Simultaneously with conventional conductive agent conductive black SP compounds pair
Than test data being made into figure, concrete outcome is referring to accompanying drawing 1.From accompanying drawing 1 it can be seen that embodiment 1-3,6,7 graphene is miscellaneous
The capacitor that compound is compounded with activated carbon, with the increase of discharge current, special capacity fade trend slows down, the high rate performance of electric discharge
Better than the carbon pipe slurry built reactive charcoal and the high rate performance of the conductive black of comparative example 3 of comparative example 1,2.It is miscellaneous that this is attributed to graphene
The characteristic of the good electric conductivity of compound and large specific surface area, is more suitable for the electrode material or conductive agent of ultracapacitor.
Therefore, it can be seen that the electrocondution slurry electric conductivity that the embodiment of the present invention is prepared is good from accompanying drawing 1, it is super
The high rate performance of capacitor is substantially improved, and is significantly improved in its performance of general electrocondution slurry more of the prior art.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that without departing substantially from the present invention's
Many other changes and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of electrocondution slurry, it is characterised in that be mainly made by following raw material:In parts by weight, graphene-carbon nano tube is miscellaneous
0.1-10 parts of compound, 0.1-10 parts of dispersant, 80-99 parts of solvent.
2. a kind of electrocondution slurry according to claim 1, it is characterised in that 2-8 parts of graphene-carbon nano tube hybrid,
0.2-8 parts of dispersant, 85-95 parts of solvent;
Preferably, 5 parts of graphene-carbon nano tube hybrid, 1 part of dispersant, 90 parts of solvent.
3. a kind of electrocondution slurry according to claim 1 or 2, it is characterised in that the graphene-carbon nano tube hybrid
It is to be combined CNT and graphene by chemical deposition;
Preferably, the preparation method of the graphene-carbon nano tube hybrid includes:
1) sheet layer material of catalyst activity component will be loaded with as catalyst, the active component of the catalyst is Fe, Co,
Ni, Cu, Mo or W, its content account for the 0.1%-50% of catalyst quality;
2) catalyst is placed in reactor, by chemical vapor deposition processes, carbon nanometer is deposited on the surface of the catalyst
The product of gained, is then placed in product purification device and is purified, produced by pipe and graphene;
Preferably, in chemical vapor deposition processes, temperature control is at 500-1200 DEG C, and more excellent control is between 800-1000 DEG C.
4. a kind of electrocondution slurry according to claim 3, it is characterised in that the graphene-carbon nano tube hybrid bag
Hetero atom containing doping, the hetero atom includes the one or more in boron, nitrogen phosphate and sulfur atom.
5. a kind of electrocondution slurry according to claim 3, it is characterised in that the dispersant includes polyvinylpyrrolidine
Ketone, polyethylene glycol, sodium cellulose glycolate, neopelex, dodecyl sodium sulfate, cellulose derivative, fat
One or more in acid polyethylene glycol ester;
The solvent includes one or both of organic solvent, inorganic solvent;
Organic solvent includes methanol, ethanol, isopropanol, ether, expoxy propane, styrene, perchloroethylene, trichloro ethylene, ethene
Glycol ether, triethanolamine, glycol dimethyl ether, benzene,toluene,xylene, chlorobenzene, dichloro-benzenes, dichloromethane, methyl acetate,
Ethyl acetate, propyl acetate, acetone, espeleton, methylisobutylketone, pyrimidine, phenol, 1-METHYLPYRROLIDONE, N, N- diformazans
One or several kinds in yl acetamide;
Inorganic solvent is water.
6. the preparation method of the electrocondution slurry described in claim any one of 1-5, it is characterised in that mainly comprise the following steps:
After graphene-carbon nano tube hybrid and solvent grinding are stirred, addition dispersant grinds more than 5s again, produces.
7. preparation method according to claim 6, it is characterised in that the time control ground after addition dispersant is in 10s-
Between 24h.
8. preparation method according to claim 6, it is characterised in that the Task-size Controlling ground after addition dispersant exists
Between 0.01-10 μm;More excellent control is between 2-8 μm.
9. preparation method according to claim 6, it is characterised in that the abrasive media include bead, zirconium silicate pearl,
One or several kinds of combinations in zirconia beads, titanium dioxide aluminium pill, steel ball.
10. the electrocondution slurry described in claim any one of 1-5 is used as lithium battery positive and negative pole material conductive agent, super capacitor electrode
Application in terms of pole material, carbon paper.
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