CN108134093A - A kind of carbon nanotube paper-metal or alloy composite current collector and preparation method thereof - Google Patents
A kind of carbon nanotube paper-metal or alloy composite current collector and preparation method thereof Download PDFInfo
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- CN108134093A CN108134093A CN201711464943.XA CN201711464943A CN108134093A CN 108134093 A CN108134093 A CN 108134093A CN 201711464943 A CN201711464943 A CN 201711464943A CN 108134093 A CN108134093 A CN 108134093A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/665—Composites
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of carbon nanotube paper metal or alloy composite current collectors and preparation method thereof.The present invention first by carbon nanotube powder stirring or ultrasound by way of uniformly disperse in a solvent, by the Van der Waals force between Thermodynamics treatmont destroying carbon nanometer tube, then be filtered by vacuum, vacuum drying obtains carbon nanotube paper；Then by chemical plating method carbon nanotube paper one layer of metal of surface uniform fold, finally by electro-deposition mode in its required metal or alloy of surface homoepitaxial, so as to obtain carbon nanotube paper metal or alloy composite current collector.By collector good conductivity made from this method, and it is compound after afflux bulk conductivity vary with temperature fluctuation very little, be suitable as the collector of large current density.Its carrier as lithium battery lithium anode makes lithium battery have good cycle performance and high security performance, also has higher energy density.
Description
Technical field
The invention belongs to battery afflux liquid technical fields, specifically, it is multiple to be related to a kind of carbon nanotube paper-metal or alloy
Intersection fluid and preparation method thereof.
Background technology
The P of carbon atom electronically forms large-scale delocalized pi-bond in carbon nanotube, since conjugation is notable, carbon nanotube
With some special electrical properties.Carbon nanotube has good electric conductivity, due to the structure and graphite of carbon nanotube
Lamellar structure is identical, so with good electric property.Carbon nanotube has good heat transfer property, and CNT has very big
Draw ratio, thus its heat exchange performance alongst is very high, and the heat exchange performance of its opposite vertical direction is relatively low,
By being suitably orientated, carbon nanotube can synthesize the heat conducting material of high anisotropy.In addition, carbon nanotube have it is higher
Thermal conductivity, as long as adulterating micro carbon nanotube in the composite, the thermal conductivity of the composite material will be likely to be obtained very greatly
Improvement.
In recent years, lithium battery is quickly grown, and country dominates the development of new energy industry, traditional lithium battery collector energetically
Requirement of the energy density to its performance at this stage can not have been met, the development of high specific energy collector has become main trend,
And conventional graphite also can not meet the energy density required by present battery as cathode, and lithium metal is as cathode application
In battery be trend of the times.
Simple CNT paper can improve the capacity and energy density of battery, but have the shortcomings that notable, head as collector
Secondary capacitance loss is very big, so must be with the Material cladding of good conductivity.The advantage of lithium anode, it is close with high capacity
(3860mAh/g) and minimum potential (- 3.040vs standard hydrogen electrodes) are spent, but when lithium metal is as battery cathode, in charge and discharge
In the process since current density and lithium ion such as are unevenly distributed at the factors, lithium ion forms dendrite in negative terminal surface nonuniform deposition,
Dendritic growth can not only pierce through diaphragm and cause short circuit, but also battery can consume electrolyte repeatedly in cyclic process, reduce cathode
Utilization rate, so as to cause, cycle performance of lithium ion battery is poor, security performance is low.
Invention content
For overcome the deficiencies in the prior art, the technical problem to be solved in the present invention is to provide a kind of carbon nanotube paper-gold
Category or alloy composite current collector and preparation method thereof.Pass through the not only eager to do well in everything degree of flexibility of carbon nanotube paper made from the method for the present invention
Height, and electric conductivity is high.By composite current collector made from this method, not only increase the electric conductivity of CNT paper, and it is compound after
Afflux bulk conductivity vary with temperature fluctuation very little, be suitable as the collector of large current density.
The present invention uniformly disperses in a solvent by way of by carbon nanotube powder stirring or ultrasound first, passes through heating power
Learn processing destroying carbon nanometer tube between Van der Waals force, then be filtered by vacuum, vacuum drying obtains carbon nanotube paper；Then passing through
The one layer of metal of surface uniform fold of electroplating method in carbon nanotube paper is learned, finally by electro-deposition mode in its surface homoepitaxial
Required metal or alloy, so as to obtain carbon nanotube paper-metal or alloy composite current collector.
Technical scheme of the present invention is specifically described as follows.
A kind of preparation method of carbon nanotube paper-metal or alloy composite current collector, includes the following steps：
1) CNT suspension is prepared；
2) CNT suspension is put into autoclave and handled；
3) treated CNT suspension is filtered by vacuum, then vacuum drying obtains CNT paper；
4) CNT paper is put into and preliminary CNT- metal collectors is obtained in electroless metal plating solution；
5) it is cathode, using metal or metal alloy as anode using the preliminary CNT- metal collectors obtained in step 4),
Using metal plating liquid or alloy as electroplate liquid, carbon nanotube paper-metal or alloy composite current collector is obtained by plating.
In the present invention, in step 1), the mass fraction of CNT suspension is 0.001%-0.1%.
In the present invention, in step 1), the solvent used in CNT suspension is polar aprotic solvent.
In the present invention, in step 2), treatment temperature is 50-250 DEG C, processing time 0.5-10h.
In the present invention, in step 4), chemical plating can be in CNT paper surface uniform deposition one layer of silver, copper, nickel, gold so that
CNT paper electric conductivity increases substantially, and prepares for follow-up plating, otherwise follow-up plating step makes since current density is unevenly distributed
CNT paper surface deposition it is uneven, alloy can be ormolu, copper-tin alloy, corronil etc..
In the present invention, in step 4), electroless metal plating solution is nickel chemical plating solution or copper chemical plating solution.
In the present invention, in step 5), the metal thickness of galvanization coating is 0.5-2 μm.
In the present invention, in step 5), common metal or alloy electroplating formula, selects according to actual needs on the market.Root
Suitable current density is selected, for example the current density of Technology Bright Acidic copper electrolyte is 1-5A/ according to actually used plating solution formula
cm2, plate the time and converted and obtained according to required thickness of coating.
A kind of carbon nanotube paper being prepared the present invention also provides above-mentioned preparation method-metal or alloy composite current collecting
Body.
Compared to the prior art, the beneficial effects of the present invention are：
Carbon nanotube paper-metal or alloy composite current collector of the present invention is three-dimensional structure, is used as lithium battery lithium metal
The carrier of cathode, lithium metal preferentially fill up the gap of collector, avoid the life of lithium metal plane along carbon cannon born frame deposition growing
Long point effect so as to inhibit the growth of Li dendrite, reduces the reversible capacity loss of lithium battery, has lithium battery good
Good cycle performance and high security performance also have higher energy density；More than, carbon nanotube paper-metal of the invention
Or alloy composite current collector can not only meet requirement of the large current charge to collector performance, or lithium metal provides limit
Position effect, will not form Li dendrite in high current charge-discharge, not only battery safety be made to be greatly enhanced, also make battery
Energy density greatly promotes.In addition afflux bulk conductivity varies with temperature fluctuation very little, is suitable as the afflux of large current density
Body.
Description of the drawings
The SEM figures of CNT paper prepared by Fig. 1 embodiments 1.
The XRD diagram of CNT paper prepared by Fig. 2 embodiments 1.
The AFM figures of CNT-Cu prepared by Fig. 3 embodiments 1.
Fig. 4 is the obtained composite current collectors of embodiment 1-3 and independent CNT and blank copper foil current collector cycle performance
Figure.
Specific embodiment
The present invention is expanded on further, but be not intended to limit the present invention below by specific embodiment and with reference to attached drawing.
Embodiment 1
1) the CNT alcohol suspensions that mass fraction is 0.05% are prepared；
2) it takes in the above-mentioned suspension of 90mL and 100mL autoclaves；
3) reaction kettle is put into 200 DEG C of insulating boxs and handles 5h；
4) the above-mentioned treatment fluids of 30mL is taken to be filtered by vacuum with the PTFE filter membranes of a diameter of 5cm；
5) PTFE filter membranes obtained above and the CNT being attached to above are put into togerther in 60 DEG C of vacuum drying ovens and handled
6h obtains the CNT paper with certain flexibility and mechanical strength；
6) obtained CNT paper is placed in prepared chemical copper plating solution, is placed at room temperature for 5min, obtained at this time preliminary
CNT-Cu collectors；
7) using above-mentioned preliminary CNT-Cu collectors as cathode, metallic copper anode, using acid bright copper plating liquid as plating solution, electricity
Current density is 3A/cm2, galvanization coating thickness is 2 μm, so as to obtain CNT-Cu collectors.
The SEM figures of CNT paper prepared by Fig. 1 embodiments 1.As seen in Figure 1, CNT is intertwined, and intermediate there are seams
Gap, traditional ultrasound or mechanical agitation are difficult the Van der Waals force destroyed between CNT, so ultrasonic merely without Thermodynamics treatmont
Or mechanical agitation obtain CNT paper be rambling, and mechanical strength is not high, easily tear, the present invention by thermodynamics at
For reason so that CNT dispersions are intertwined after filtering, high mechanical strength has certain flexibility.
The XRD diagram of CNT paper prepared by Fig. 2 embodiments 1.As seen in Figure 2, Thermodynamics treatmont of the invention is not
The structure crystal form and original CNT powder for changing CNT keep the phase isomorphism, maintain the good electrically and thermally performances of CNT.
Fig. 3 is CNT-Cu composite current collectors made from this method, and Cu not only increases the electric conductivity of CNT paper, M-CNT tri-
Carrier of the collector of structure as lithium battery lithium anode is tieed up, lithium metal can be made to be kept away along carbon cannon born frame deposition growing
The point effect of lithium metal planar growth is exempted from, so as to inhibit the growth of Li dendrite, so as to reduce the reversible appearance of lithium battery
Amount loss so as to which lithium battery be made to have good cycle performance and high security performance, also has higher energy density.And
Afflux bulk conductivity after compound varies with temperature fluctuation very little, is suitable as the collector of large current density.
Embodiment 2
1) the CNT alcohol suspensions that mass fraction is 0.05% are prepared；
2) it takes in the above-mentioned suspension of 90mL and 100mL autoclaves；
3) reaction kettle is put into 200 DEG C of insulating boxs and handles 5h；
4) the above-mentioned treatment fluids of 30mL is taken to be filtered by vacuum with the PTFE filter membranes of a diameter of 5cm；
5) PTFE filter membranes obtained above and the CNT being attached to above are put into togerther in 60 DEG C of vacuum drying ovens and handled
6h obtains the CNT paper with certain flexibility and mechanical strength；
6) obtained CNT paper is placed in prepared chemical copper plating solution, is placed at room temperature for 5min, obtained at this time preliminary
CNT-Cu collectors；
7) it is anode using above-mentioned preliminary CNT-Cu collectors as cathode, metallic nickel, using bright nickel plating bath as plating solution, electric current
Density is 1A/cm2, galvanization coating thickness is 2 μm, so as to obtain CNT-Ni collectors.
Embodiment 3
1) the CNT alcohol suspensions that mass fraction is 0.05% are prepared；
2) it takes in the above-mentioned suspension of 90mL and 100mL autoclaves；
3) reaction kettle is put into 200 DEG C of insulating boxs and handles 5h；
4) the above-mentioned treatment fluids of 30mL is taken to be filtered by vacuum with the PTFE filter membranes of a diameter of 5cm；
5) PTFE filter membranes obtained above and the CNT being attached to above are put into togerther in 60 DEG C of vacuum drying ovens and handled
6h obtains the CNT paper with certain flexibility and mechanical strength；
6) obtained CNT paper is placed in prepared chemical nickel-plating solution, is placed at room temperature for 5min, obtained at this time preliminary
CNT-Ni collectors；
7) it is anode using above-mentioned preliminary CNT-Ni collectors as cathode, brass, using Brass Plating Solution as plating solution, current density
For 0.5A/cm2, galvanization coating thickness is 2 μm, so as to obtain CNT-Cu/Zn alloy collectors.
Embodiment 4
1) the CNT alcohol suspensions that mass fraction is 0.05% are prepared；
2) it takes in the above-mentioned suspension of 90mL and 100mL autoclaves；
3) reaction kettle is put into 200 DEG C of insulating boxs and handles 5h；
4) the above-mentioned treatment fluids of 30mL is taken to be filtered by vacuum with the PTFE filter membranes of a diameter of 5cm；
5) PTFE filter membranes obtained above and the CNT being attached to above are put into togerther in 60 DEG C of vacuum drying ovens and handled
6h obtains the CNT paper with certain flexibility and mechanical strength；
6) obtained CNT paper is placed in prepared chemical copper plating solution, is placed at room temperature for 5min, obtained at this time preliminary
CNT-Cu collectors；
7) it is anode using above-mentioned preliminary CNT-Cu collectors as cathode, copper-nickel alloy, using low cyanogen bronze (copper-tin alloy) electroplating plating solution as plating
Liquid, current density 0.5A/cm2, galvanization coating thickness is 2 μm, so as to obtain CNT-Cu/Sn alloy collectors.
Embodiment 5
1) using embodiment 1 to CNT-Cu as cathode；
2) pole piece size 12mm, electrolyte are molten for the ethylene carbonate and dimethyl carbonate of the lithium hexafluoro phosphate of 1mol/L
Liquid；
3) diaphragm is polypropylene screen (Celgard2400)
4) lithium piece is used as to electrode, assembles 2016 button cells respectively；
5) cyclical stability of cycle half-cell that test is prepared.
6) first in 0.5mA/cm2Current density under deposit 10 hours lithium metals, then in 0.5mA/cm2Electric current it is close
It under degree, first charges to battery 5 hours, then 5 hours constant current charge-discharge tests of discharging.
Fig. 4 is the obtained composite current collectors of embodiment 1-3 and independent CNT and blank copper foil current collector performance comparison,
From data comparison it is found that copper/lithium Symmetrical cells efficiency in cyclic process is substantially unstable, after recycling a period of time, substantially
Efficiency becomes very little, and possible cause is easily to form Li dendrite on smooth copper foil, so as to consume electrolyte, pierces through diaphragm, makes
Into partial short-circuit, CNT or CNT- metal or alloy/lithium Symmetrical cells have preferable cyclical stability, the reason is that three-dimensional structure
Collector specific surface area it is more many than simple untreated copper foil large specific surface area, the current density ratio for causing it practical is not located merely
Reason copper foil is much smaller, and so as to inhibit lithium dendrite growth, and the gap of CNT further limits the life of Li dendrite in CNT paper
It is long, so as to preferable cyclical stability.
It is the specific implementation of the present invention above, description is more specific and detailed, but can not therefore be interpreted as
Limitation to the scope of the claims of the present invention.It should be pointed out that for those of ordinary skill in the art, this hair is not being departed from
Under the premise of bright design, various modifications and improvements can be made, these obvious alternative forms belong to the present invention's
Protection domain.
Claims (7)
1. the preparation method of a kind of carbon nanotube paper-metal or alloy composite current collector, which is characterized in that include the following steps：
1) CNT suspension is prepared；
2) CNT suspension is put into autoclave and handled；
3) treated CNT suspension is filtered by vacuum, then vacuum drying obtains CNT paper；
4) CNT paper is put into and preliminary CNT- metal collectors is obtained in electroless metal plating solution；
5) it is cathode, using metal or metal alloy as anode using the preliminary CNT- metal collectors obtained in step 4), with gold
It is electroplate liquid to belong to plating solution or alloy, and carbon nanotube paper-metal or alloy composite current collector is obtained by plating.
2. preparation method according to claim 1, which is characterized in that in step 1), the mass fraction of CNT suspension is
0.001%-0.1%.
3. preparation method according to claim 1, which is characterized in that in step 1), the solvent used in CNT suspension is pole
Protic solvents.
4. preparation method according to claim 1, which is characterized in that in step 2), treatment temperature is 50-250 DEG C, processing
Time is 0.5-10h.
5. preparation method according to claim 1, which is characterized in that in step 4), electroless metal plating solution is nickel chemistry
One or both of plating liquor or copper chemical plating solution.
6. preparation method according to claim 1, which is characterized in that in step 5), the metal thickness of galvanization coating is
0.5-2μm。
7. a kind of carbon nanotube paper that preparation method according to one of claim 1~6 obtains-metal or alloy Composite Set
Fluid.
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Cited By (6)
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| CN108987796A (en) * | 2018-09-10 | 2018-12-11 | 江西克莱威纳米碳材料有限公司 | A kind of flexible lithium ion battery and preparation method thereof |
| CN110518247A (en) * | 2019-08-19 | 2019-11-29 | 上海交通大学 | Lithium-sulfur cell and preparation method thereof based on carbon photonic crystal metal coating structure |
| CN110777331A (en) * | 2019-11-07 | 2020-02-11 | 苏州第一元素纳米技术有限公司 | Preparation method of metal-coated carbon nano tube |
| CN111430721A (en) * | 2020-02-25 | 2020-07-17 | 蜂巢能源科技有限公司 | Composite electrode and preparation method and application thereof |
| CN115036515A (en) * | 2022-08-12 | 2022-09-09 | 清华大学 | Carbon nano material composite current collector, preparation method thereof, electrode and battery |
| CN117174914A (en) * | 2023-09-20 | 2023-12-05 | 中能鑫储(北京)科技有限公司 | Three-dimensional current collector applied to aluminum ion battery and preparation method thereof |
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