CN105932297A - Carbon nanotube conductive coating current collector and preparation technology thereof - Google Patents
Carbon nanotube conductive coating current collector and preparation technology thereof Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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Abstract
The invention discloses a carbon nanotube conductive coating current collector, which comprises a metal current collector and a carbon nanotube conductive coating, wherein the carbon nanotube conductive coating coats the surface of the metal current collector; the thickness of the carbon nanotube conductive coating is 1-50 microns; and the surface of the carbon nanotube conductive coating is provided with a mesh micro crack structure and a coarse porous structure. The invention further provides a preparation technology of the carbon nanotube conductive coating current collector. The carbon nanotube conductive coating disclosed by the invention provides a good conductive network for an electrode, and is especially obvious for an electrode material with relatively poor conductivity; meanwhile, dense micro cracks are formed in the surface after the carbon nanotube conductive coating is dried through preparing conductive paste with different dispersion effects; and an electrode coating can be embedded among the micro cracks, so that the contact area of the electrode coating and the conductive coating is greatly improved; the binding force between the electrode coating and the current collector is improved; the internal resistance of a battery is reduced; the lifetime of the battery is prolonged; and the high-rate capability is improved.
Description
Technical field
The present invention relates to technical field of lithium ion, particularly relate to a kind of carbon nanotube conducting coating collector and preparation technology thereof.
Background technology
Lithium ion battery is constantly subjected to the concern of people as the recyclable regenerative energy of a kind of cleaning, its research and application.Existing electrodes of lithium-ion batteries is made up of collector and the electrode material being coated in collection liquid surface.Present business-like affluxion body in lithium ion batteries mainly uses electrolysis Cu paper tinsel or Al paper tinsel, is divided into the several types such as dual light, two-sided hair, one side hair, double-sided coarsening.For improving the adhesion of electrode material and collector, use the binding agent of higher proportion.Embed in electrode material rapidly along with lithium ion in high magnification charge and discharge cyclic process at battery and deviate from, making the volume of electrode material produce violent expansion and contraction, electrode material is damaged, makes the performance of battery decline rapidly.Meanwhile, the electric conductivity of anode material for lithium-ion batteries is poor, causes the internal resistance of battery to have a strong impact on the performance of battery, and novel negative material such as lithium titanate etc. there is also same problem.Therefore the lithium ion battery produced by existing electrodes of lithium-ion batteries, internal resistance is higher, high-rate discharge ability is poor, cyclic process internal resistance raises comparatively fast, cycle life is the most poor.
In order to solve the problems referred to above, research worker improves the most in the following manner: (1) modified both positive and negative polarity active material；(2) conductive agent is improved；(3) electrolyte and barrier film are improved；(4) cell making process is improved；(5) collector is improved.Wherein the most quick to improve collector, effect is notable simultaneously, is wherein most widely used with conductive coating collector.
But conductive coating collector can not improve the contact area between electrode coating and collector in itself greatly, the most blocked up conductive coating can affect this phenomenon of conductive effect of electrode ensemble, it is suppressed that conductive coating collector improves the ability of the electrode material electrodes conduct performance of electric conductivity difference further.The most farthest improving the contact area between electrode coating and collector, weaken the impact on electrode ensemble conductive effect of the conductive coating thickness, the electric conductivity improving electrode further seems extremely important.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of novel carbon nanotube conducting coating collector, while improving the electric conductivity of electrode, by making conductive coating surface produce micro-cracked structure, the contact area of raising electrode coating and conductive coating, to improve the adhesion of electrode material and metal collector, weakens the blocked up impact on electrode ensemble electric conductivity of conductive coating.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
A kind of carbon nanotube conducting coating collector, including metal collector and carbon nanotube conducting coating, described metal collector material is Copper Foil or aluminium foil；Described carbon nanotube conducting coating is coated in metal collector surface, and its thickness is 1 ~ 50 μm, and surface configuration has netted micro-cracked structure and rough porous structure.
Further, the closeness of described micro-cracked structure is inversely proportional to thickness and the dispersion effect of described carbon nanotube conducting coating, the width of described micro-cracked structure is directly proportional to described carbon nanotube conducting coating layer thickness, and the closeness of described rough porous structure is directly proportional to described dispersion effect.
Further, the width of the micro-cracked structure maximum of described carbon nanotube conducting coating surface is 5 ~ 200 μm.
When binding agent is aqueous binders, metal collector material is for using Copper Foil, and when binding agent is oiliness binding agent, metal collector material is for using aluminium foil.
Another aspect of the present invention provides the preparation technology of a kind of coating collector of carbon nanotube conducting as mentioned, comprises the following steps:
(1) weighing CNT or CNT and one or more conductive agents as raw material, and carry out raw material respectively drying pretreatment, drying time is 3h, and it is 200 DEG C ~ 300 DEG C that the temperature of drying controls；
(2) metal collector selected being carried out surface cleaning pretreatment, the greasy dirt etc. removing surface affects the material that slurry is combined with metal collector；
(3) being mixed according to certain ratio with binding agent, dispersant and solvent by raw material after pretreatment in step (1), stir 5 ~ 20h, the conductive coating slurry preparing dispersion effect different is standby；
(4) the conductive coating slurry prepared in step (3) being carried out vacuum degassing bubble process, the bubble removing time is 5 ~ 10min；
(5) the conductive coating slurry after being processed by step (4) bubble removing uses coating machine to arrange the different coating thickness of 1 ~ 100 μm and coats collection liquid surface, dries 6 ~ 12h, and it is 60 DEG C ~ 120 DEG C that the temperature of drying controls；
(6) make, after drying, the collector that conductive coating thickness is different, standby as affluxion body in lithium ion batteries.
Further, the solvent described in step (3) be NMP, deionized water or volume fraction be the ethanol solution of 20 ~ 40%, the solid content of described conductive coating slurry is 2 ~ 20%.
Further, the dispersion effect of conductive coating slurry described in step (3) is directly proportional to the consumption of dispersant and mixing time.
Further, the carbon nanotube conducting coating collector after step (5) described drying and processing does not carry out compaction treatment, retains conductive coating rough surface loose structure.
Further, the component of described carbon nanotube conducting coating includes by weight percentage: CNT 50% ~ 99%, binding agent 1% ~ 10%, conductive agent 0% ~ 40%, dispersant 0% ~ 10%.
Further, described CNT includes one or more of SWCN, multi-walled carbon nano-tubes and modified carbon nano-tube；Described binding agent is one or more of aqueous binders or oiliness binding agent；Described conductive agent is one or more in conductive black, superconduction white carbon black, conductive carbon fibre, electrically conductive graphite；Described dispersant is the one in TNWDIS, TNADIS, TNDDIS, TNEDIS.
Described carbon nanotube conducting coating collector is used for lithium ion cell positive or negative pole.Described lithium ion cell positive function of tonic chord material includes one or more of the positive electrodes such as cobalt acid lithium, LiFePO4, LiMn2O4；Described lithium ion battery negative function of tonic chord material includes one or more of the negative material such as carbonaceous mesophase spherules, Delanium.
The preparation technology of the carbon nanotube conducting coating collector of the present invention, it thes improvement is that described collector is by using less dispersive agent ratio (0% ~ 10%) and binding agent ratio (1 ~ 10%), dispersant dosage is strictly less than making the fully decentralized optimum amount of CNT, prepare the electrocondution slurry that dispersion effect is different, the solid content of conductive coating slurry is between 2 ~ 20% simultaneously, make conductive coating form intensive micro-cracked structure after the drying, provide the micro-crack improving adhesion for the main slurry of electrode.The one side thickness of conductive coating is 1 ~ 50 μm, and along with the reduction of coating layer thickness, the micro-crack that coating surface is formed is the most intensive.The width of the micro-crack maximum on surface is between 5 ~ 200 μm.Carbon nanotube conducting coating collector after drying and processing does not carry out compaction treatment, retains the shaggy loose structure of conductive coating, improves electrode coating and the contact area of conductive coating to greatest extent.
Compared with prior art, the invention has the beneficial effects as follows:
1. using CNT as the major function material of conductive coating, electric conductivity is better than existing major part lithium ion battery conductive agent, and the tubular structure of its uniqueness is that electrode provides good conductive network, improves electrode performance under high magnification charge and discharge.
2. use the binding agent of small percentage, given full play to the electric conductivity of conductive agent, farthest reduce the internal resistance of battery, improve battery cycle life and high rate performance.
3. coating surface forms intensive micro-cracked structure, add the contact area of electrode function of tonic chord material and conductive coating, improve the adhesion of electrode function of tonic chord material and collector, provide the contact point of electrode function of tonic chord material and metal collector simultaneously, avoid monolithic conductive that is blocked up due to conductive coating and that cause not sufficiently effective, add conductive coating regulation thickness, significantly improve the electric conductivity of the electrode of the electrode function of tonic chord material using electric conductivity difference.
4., in lithium ion battery, can relatively reduce in electrode coating in the case of conductive agent content, the effective rising suppressing the internal resistance of cell, the surface density of the electrode function of tonic chord material of increase, improves the capacity of electrode unit area.
Accompanying drawing explanation
Fig. 1 is the lithium ion cell electrode profile using carbon nanotube conducting coating collector of embodiment.
Fig. 2 is 30 μ m-thick coating surface microstructures of embodiment two；
Fig. 3 is 25 μ m-thick coating surface microstructures of embodiment two；
Fig. 4 is 20 μ m-thick coating surface microstructures of embodiment two；
Fig. 5 is the multi-walled carbon nano-tubes conductive coating collection liquid surface rough porous structure SEM figure of embodiment two；
Fig. 6 is embodiment two and comparative example one and comparative example two AC impedance comparison diagram；
Fig. 7 is embodiment two and cycle charge-discharge specific capacity comparison diagram under comparative example one and comparative example two different multiplying.
Shown in figure it is: 1-metal collector；2-carbon nanotube conducting coating；3-electrode coating；4-micro-crack.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further described, but the present invention is not limited in following example.Described method is conventional method without special instruction.
Embodiment one
A kind of carbon nanotube conducting coating collector, including metal collector 1 and carbon nanotube conducting coating 2, described carbon nanotube conducting coating 2 is coated in metal collector 1 surface.The thickness of described carbon nanotube conducting coating is 1 ~ 50 μm.The surface configuration of described carbon nanotube conducting coating has netted micro-cracked structure 4 and rough porous structure.
The closeness of described micro-cracked structure 4 is inversely proportional to thickness and the dispersion effect of described carbon nanotube conducting coating 2, the width of described micro-cracked structure 4 is directly proportional to described carbon nanotube conducting coating 2 thickness, and the closeness of described rough porous structure is directly proportional to described dispersion effect.
The width of micro-cracked structure 4 maximum on described carbon nanotube conducting coating 2 surface is 5 ~ 200 μm.
Described carbon nanotube conducting coating 2 surface-coated electrode coating 3, for lithium ion cell positive or negative pole, described lithium ion cell positive function of tonic chord material includes one or more of the positive electrodes such as cobalt acid lithium, LiFePO4, LiMn2O4；Described lithium ion battery negative function of tonic chord material includes one or more of the negative material such as carbonaceous mesophase spherules, Delanium.Electrode coating 3 can be embedded between micro-cracked structure 4, greatly increase the contact area between electrode coating 3 and carbon nanotube conducting coating 2, improve the adhesion between collector, greatly reduce the internal resistance of battery, improve life-span and the high rate capability of battery.
Described metal collector 1 according to use binding agent kind select, when binding agent is aqueous binders use Copper Foil, when binding agent be oiliness binding agent be use aluminium foil.
Embodiment two
A kind of preparation technology of carbon nanotube conducting coating collector, select butadiene-styrene rubber (SBR) and sodium carboxymethyl cellulose (CMC) as the binding agent of conductive coating, only use multi-walled carbon nano-tubes as conductive agent, without other conductive agents, and use the part by weight modulation electrocondution slurry of 3:3:94, the ethanol solution of use 20% is as solvent simultaneously, and final conductive coating slurry solid content is about 6%, and concrete preparation process is as follows:
(1) multi-walled carbon nano-tubes is dried in advance process, 120 DEG C of dry 12h；Metal collector is carried out surface cleaning pretreatment；
(2) use magnetic stirring apparatus to dissolve CMC at 80 DEG C, after CMC is completely dissolved, add SBR emulsion, continue stirring 0.5h, make binder solution；
(3) multi-walled carbon nano-tubes is added in the binder solution that step (2) is made in four times, be continuing with magnetic stirrer, every minor tick 1h, and observe the viscosity of slurry, after feeding for the last time, high-speed stirred 6h；
(4) slurry prepared in step (3) being carried out vacuum degassing bubble process, the bubble removing time is 10min；
(5) infrared drying vacuum flow-casting coating machine is used to carry out conductive coating coating, coating thickness is 150 μm, 125 μm, 100 μm, dry 12h for 80 DEG C, carbon nanotube conducting coating collector after drying and processing does not carry out compaction treatment, retains the shaggy loose structure of conductive coating (see Fig. 5)；
(6) standby as collector after drying.
Using super depth of field equipment to observe conductive coating collection liquid surface prepared by above-described embodiment, as shown in Fig. 2 ~ 4, due to the evaporation of solvent, slurry volume is shunk, and it is 30 μm, 25 μm, the coating structure of 20 μm that three kinds of different coating thickness form average thickness.It can be seen that coating defines intensive micro-cracked structure, comparison diagram 2, Fig. 3 and Fig. 4 are it is found that along with the width of coating layer thickness reduction micro-crack reduces the most therewith, micro-crack is the most intensive simultaneously.Through measuring the coating micro-crack maximum width of 30 μ m-thick between 20 ~ 80 μm, the coating of 25 μm and 20 μ m-thick is respectively between 10 ~ 40 μm and 10 ~ 30 μm simultaneously, embeds the space providing abundance for the negative or positive electrode material below micron order.
The present embodiment uses MCMB (carbonaceous mesophase spherules graphite) prepare lithium ion battery negative as function of tonic chord material, and with metal lithium sheet for button half-cell being prepared by electrode.Selecting aqueous binders SBR and CMC as binding agent, Super-P conductive black, as conductive agent, uses 2:2:3:93(SBR:CMC:Super-P:MCMB) ratio prepare cathode size, concrete preparation scheme is as follows:
(1) MCMB and Super-P is dried pretreatment, 120 DEG C of dry 12h；
(2) use magnetic stirring apparatus to dissolve CMC at 80 DEG C, after CMC is completely dissolved, add SBR emulsion, continue stirring 0.5h, make binder solution；
(3) Super-P is added in the binder solution that step (2) is made, use ball mill dispersed with stirring 1h；
(4) MCMB is added in four times, every minor tick 1h, and observe the viscosity of slurry, add appropriate deionized water, after feeding for the last time, continue stirring 6h；
(5) slurry prepared in step (3) being carried out vacuum degassing bubble process, the bubble removing time is 10min；
(6) cathode size using infrared drying vacuum flow-casting coating machine that step (4) is made is applied on the above-mentioned multi-walled carbon nano-tubes conductive layer collector prepared, and coating film thickness is 100 μm, 80 DEG C of dry 12h；
(7) dried electrode in step (5) being carried out 25Mpa compaction treatment, the dwell time is 5min；
(8) electrode after compaction treatment in step (6) is made the entelechy sheet of 16mm, then proceed to 60 DEG C of dry 12h.
Using the anode plate for lithium ionic cell of above-mentioned preparation, install button half-cell in the glove box under argon shield, battery case model is 2032；A series of performance test such as cycle charge-discharge, AC impedance is carried out after battery standing 12h.
Comparative example one
The preparation technology of a kind of carbon nanotube conducting coating collector, this comparative example is not use above-mentioned new current collector with the difference of embodiment two.Selecting aqueous binders SBR and CMC as binding agent, multi-walled carbon nano-tubes, as conductive agent, uses 2:2:3:93(SBR:CMC: multi-walled carbon nano-tubes: MCMB) ratio prepare cathode size, concrete preparation scheme is as follows:
(1) MCMB and multi-walled carbon nano-tubes are dried pretreatment, 120 DEG C of dry 12h, metal collector 1 is carried out surface cleaning pretreatment simultaneously；
(2) use magnetic stirring apparatus to dissolve CMC at 80 DEG C, after CMC is completely dissolved, add SBR emulsion, continue stirring 0.5h, make binder solution；
(3) multi-walled carbon nano-tubes is added in the binder solution that step (2) is made, use ball mill dispersed with stirring 1h；
(4) MCMB is added in four times, every minor tick 1h, and observe the viscosity of slurry, add appropriate deionized water, after feeding for the last time, continue stirring 6h；
(5) slurry prepared in step (3) being carried out vacuum degassing bubble process, the bubble removing time is 10min；
(6) cathode size using infrared drying vacuum flow-casting coating machine that step (4) is made is applied on the above-mentioned multi-walled carbon nano-tubes conductive layer collector prepared, and coating film thickness is 100 μm, 80 DEG C of dry 12h；
(7) dried electrode in step (5) being carried out 25Mpa compaction treatment, the dwell time is 5min；
(8) electrode after compaction treatment in step (6) is made the entelechy sheet of 16mm, then proceed to 60 DEG C of dry 12h.
Using the anode plate for lithium ionic cell of above-mentioned preparation, install button half-cell in the glove box under argon shield, battery case model is 2032；A series of performance test such as cycle charge-discharge, AC impedance is carried out after battery standing 12h.
Comparative example two
The preparation technology of a kind of carbon nanotube conducting coating collector, this comparative example is not use above-mentioned new current collector with the difference of embodiment two.Selecting aqueous binders SBR and CMC as binding agent, Super-P conductive black, as conductive agent, uses 2:2:3:93(SBR:CMC:Super-P:MCMB) ratio prepare cathode size, its specific solution is identical with comparative example one.
Embodiment two contrasts as shown in Figure 6 with the AC impedance of comparative example one and comparative example two, can be seen that, the impedance of comparative example one (curve is the longest) and comparative example two (curve vice-minister) is the highest, contrast with both, embodiment two (curve is the shortest) is much smaller, and the internal resistance of battery is greatly reduced.
Charging and discharging capacity change under different multiplying contrasts as shown in Figure 7 embodiment two with comparative example one and comparative example two, can be seen that, the embodiment two specific capacity under each multiplying power all reaches the maximum of three, along with the advantage of the increase embodiment of multiplying power is more significantly, it is 2 ~ 3 times of comparative example specific capacity under 0.5C high magnification.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted by the embodiments; the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify; all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (9)
1. a carbon nanotube conducting coating collector, it is characterised in that: include that metal collector and carbon nanotube conducting coating, described metal collector material are Copper Foil or aluminium foil；Described carbon nanotube conducting coating is coated in metal collector surface, and its thickness is 1 ~ 50 μm, and surface configuration has netted micro-cracked structure and rough porous structure.
Carbon nanotube conducting coating collector the most according to claim 1, it is characterized in that: the closeness of described micro-cracked structure is inversely proportional to thickness and the dispersion effect of described carbon nanotube conducting coating, the width of described micro-cracked structure is directly proportional to described carbon nanotube conducting coating layer thickness, and the closeness of described rough porous structure is directly proportional to described dispersion effect.
Carbon nanotube conducting coating collector the most according to claim 1, it is characterised in that: the width of the micro-cracked structure maximum of described carbon nanotube conducting coating surface is 5 ~ 200 μm.
4. the preparation technology of a carbon nanotube conducting coating collector as claimed any one in claims 1 to 3, it is characterised in that comprise the following steps:
(1) weighing CNT or CNT and one or more conductive agents as raw material, and carry out raw material respectively drying pretreatment, drying time is 3h, and it is 200 DEG C ~ 300 DEG C that the temperature of drying controls；
(2) metal collector selected being carried out surface cleaning pretreatment, the greasy dirt etc. removing surface affects the material that slurry is combined with metal collector；
(3) being mixed according to certain ratio with binding agent, dispersant and solvent by raw material after pretreatment in step (1), stir 5 ~ 20h, the conductive coating slurry preparing dispersion effect different is standby；
(4) the conductive coating slurry prepared in step (3) being carried out vacuum degassing bubble process, the bubble removing time is 5 ~ 10min；
(5) the conductive coating slurry after being processed by step (4) bubble removing uses coating machine to arrange the different coating thickness of 1 ~ 100 μm and coats collection liquid surface, dries 6 ~ 12h, and it is 60 DEG C ~ 120 DEG C that the temperature of drying controls；
(6) make, after drying, the collector that conductive coating thickness is different, standby as affluxion body in lithium ion batteries.
The preparation technology of carbon nanotube conducting coating collector the most according to claim 4, it is characterized in that: the solvent described in step (3) be NMP, deionized water or volume fraction be the ethanol solution of 20 ~ 40%, the solid content of described conductive coating slurry is 2 ~ 20%.
The preparation technology of carbon nanotube conducting coating collector the most according to claim 4, it is characterised in that: the dispersion effect of conductive coating slurry described in step (3) is directly proportional to the consumption of dispersant and mixing time.
The preparation technology of carbon nanotube conducting coating collector the most according to claim 4, it is characterised in that: the carbon nanotube conducting coating collector after step (5) described drying and processing does not carry out compaction treatment, retains conductive coating rough surface loose structure.
The preparation technology of carbon nanotube conducting coating collector the most according to claim 4, it is characterised in that: the component of described carbon nanotube conducting coating includes by weight percentage: CNT 50% ~ 99%, binding agent 1% ~ 10%, conductive agent 0% ~ 40%, dispersant 0% ~ 10%.
The preparation technology of carbon nanotube conducting coating collector the most according to claim 4, it is characterised in that: described CNT includes one or more of SWCN, multi-walled carbon nano-tubes and modified carbon nano-tube；Described binding agent is one or more of aqueous binders or oiliness binding agent；Described conductive agent is one or more in conductive black, superconduction white carbon black, conductive carbon fibre, electrically conductive graphite；Described dispersant is the one in TNWDIS, TNADIS, TNDDIS, TNEDIS.
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