CN110534748A - A kind of preparation method of flexible lithium ion battery negative battery collector - Google Patents
A kind of preparation method of flexible lithium ion battery negative battery collector Download PDFInfo
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- CN110534748A CN110534748A CN201910820656.0A CN201910820656A CN110534748A CN 110534748 A CN110534748 A CN 110534748A CN 201910820656 A CN201910820656 A CN 201910820656A CN 110534748 A CN110534748 A CN 110534748A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/666—Composites in the form of mixed materials
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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
- H01M4/70—Carriers or collectors characterised by shape or form
- H01M4/72—Grids
- H01M4/74—Meshes or woven material; Expanded metal
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
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Abstract
The present invention relates to a kind of preparation methods of flexible lithium ion battery negative current collector comprising has following steps: S1, pre-processing cloth as base material, is ultrasonically treated, is sensitized, is activated later；S2, one layer of nano nickle granules layer is grown on step S1 treated cloth using chemically coated nickel method, prepare nickel plating cloth as flexible current-collecting body；S3, growth in situ Ni (OH) is carried out to nickel plating cloth2Nano-chip arrays；S4, pass through heat treatment method Ni (OH)2Nano-chip arrays are changed into nanoscale nickel array, while flexible cloth substrate being changed into the flexible carbon substrate of nitrogen, phosphor codoping.Flexible lithium ion battery negative electrode active material NiO prepared by the present invention and conductive substrates binding force be strong, nickel carbon support collector has good electric conductivity, stability and flexibility, and preparation method is easy.
Description
Technical field
The present invention relates to a kind of preparation methods of flexible lithium ion battery negative battery collector, belong to electrochmical power source technology
Field.
Background technique
In the energy storage devices such as battery and supercapacitor, the function of collector is the electricity for generating cell active materials
Stream collects and is transmitted.Existing commercialization negative current collector is copper foil, because will cause irreversible shape in metal copper foil deformation process
Become, therefore metal copper foil is not suitable as flexible current-collecting body；Copper foil surface is smooth, and poor adhesion easily causes in deformation process
Active material falls off；Density is larger to be not suitable for light-weighted flexible battery.Traditional preparation method has coating, coating rolling, water
Thermal method growth in situ, absorption etc., but cause since active material is easy to fall off, conductivity is low, is not suitable for the disadvantages of large area preparation
The collector prepared is difficult to meet the requirements.
Summary of the invention
(1) technical problems to be solved
In order to solve the problems such as at high cost, flexible poor, conductivity is low in the prior art, the present invention provide a kind of flexible lithium from
The preparation method of sub- battery cathode collector, the collector of this method preparation not only have flexible, high conductivity, but also preparation side
Method is easy, can also be achieved waste utilization, saves preparation cost.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include:
A kind of preparation method of flexible lithium ion battery negative current collector comprising following steps:
S1, it is pre-processed cloth as base material, is ultrasonically treated, is sensitized, is activated later；
S2, one layer of nano nickel nano-particle layer, preparation are grown on step S1 treated cloth using chemically coated nickel method
Nickel plating cloth is as flexible current-collecting body out；
S3, the nickel plating cloth growth in situ Ni (OH) that step S2 is obtained2Nano-chip arrays；
S4, pass through heating means for Ni (OH)2Nano-chip arrays are changed into nickel oxide nano chip arrays active material, simultaneously
Flexible cloth substrate is changed into the flexible carbon substrate of nitrogen, phosphor codoping.
In a preferred embodiment, in step sl, the cloth is cotton, can also be waste and old cotton, described
Pretreatment refers to using cleaning, then uses dipping by lye, then rinse after being impregnated with deionized water.
In a preferred embodiment, the lye is the NaOH solution of 1~2mol/L, after impregnating 5~20min,
To increase the asperity of cellulose fibre, increase the contact area of the coat of metal and fiber to enhance coating and substrate
Then binding force is impregnated and is cleaned with deionized water.
In a preferred embodiment, in step sl, the ultrasonic treatment is molten using the mixing of ethyl alcohol and acetone
Liquid, the ethyl alcohol are that 1:1 is mixed with acetone by volume；It is rinsed twice after 20~60min of ultrasound with clear water, is dried later
It is dry.
In a preferred embodiment, the drying uses low temperature drying (50 DEG C) or natural drying.
In a preferred embodiment, in step sl, the sensitization uses the 10mmol/L SnCl of stanniferous grain2
After being mixed in the HCI solution of liquor capacity content 0.6%, 10min is stirred, cleans 2 after impregnating 10min with deionized water
Time, water is drained after being rinsed with water later.
Tin is for preventing SnCl2Oxidation, so being added with tin grain.
In a preferred embodiment, in step sl, the cloth being activated will to drain is in activating solution
Middle immersion, is impregnated in deionized water later, is pulled out and is drained, drying.
In a preferred embodiment, the activating solution is the PbCl of 2mmol/L2Solution impregnates 10min, finally uses
Deionized water is impregnated, soaking time 10min.
In a preferred embodiment, in step s 2, the chemically coated nickel method refers to the cloth after sensitization, activation
Material is put into plating solution, and plating solution is 30mmol nickel sulfate, 0.1mol hypophosphorous acid Asia hydrogen sodium, 70mmol ammonium chloride, 15mmol citric acid
The aqueous solution of trisodium adjusts pH to 4~5 with ammonium hydroxide.
In a preferred embodiment, in step s3, the growth in situ Ni (OH)2Nano-chip arrays use water
Thermal method, method are the H for using reaction solution to be 6:1 for volume ratio2O and H2O2Solution, be added step S2 obtain nickel plating cloth
It is placed in polytetrafluoroethylliner liner together, then is put into baking oven after being sealed with rustless steel container, keeps the temperature 14 hours at 140 DEG C, then
Natural cooling, the process can make to show nano nickel particles layer portions turn Ni (OH)2Nano-chip arrays.
In a preferred embodiment, in step s 4, the heating means are to obtain step S3 in Muffle furnace
The Ni (OH) obtained2Nano-chip arrays are heated to 250 DEG C, keep the temperature 3 hours.Nickel hydroxide dehydration is set to be changed into porous nickel oxide in this way
Nano-chip arrays, while the carbonization of cotton substrate being made to be porous structure flexibility carbon substrate, due to containing ammonia and phosphate in the solution,
Two kinds of compositions are attracted to cloth substrate, after heat treatment ammonia and phosphate decomposition, and nitrogen and phosphorus are mixed in substrate, realize nitrogen,
The flexible carbon substrate of phosphor codoping.
(3) beneficial effect
The beneficial effects of the present invention are:
It selects the nickel oxide with high theoretical capacity as research object in the present invention, is substrate using cotton flexible,
The deposition for being carried out metallic nickel in cotton surface using chemical plating method is etched in situ by hydro-thermal method, is obtained in layer on surface of metal
Persursor material makes flexible cotton templating through Overheating Treatment, and persursor material is changed into the nickel oxide of high theoretical capacity
Nano-chip arrays structure-activity substance, while realizing the nitrogen of carbon substrate, phosphorus doping, preparation method is easy, strong operability.Simultaneously
Waste and old cotton can also be used as flexible substrates in the present invention, facilitates energy-saving and emission-reduction, realizes the low of waste utilization and flexible electrode
Cost preparation.
Detailed description of the invention
Fig. 1 is that the flexible electrode of preparation tests the binding force of active material NiO and conductive substrates under the sticking of adhesive tape
Figure；
Fig. 2 is the conductivity of the four electrode method measuring resistance of chemical nickel plating cotton；
Fig. 3 is photo of the flexible electrode of preparation under the conditions of bending；
Fig. 4 is the scanning electron microscope diagram of the nickel oxide nano chip arrays of growth in situ；
Fig. 5 is the spectrogram that x-ray photoelectron spectroscopy tests nitrogen；
Fig. 6 is the spectrogram that x-ray photoelectron spectroscopy tests P elements；
Fig. 7 is capacity and voltage curve of the flexible electrode as button cell cathode.
Specific embodiment
Discovery first cleans cotton before chemical nickel plating in research in the present invention, activates.Using palladium chloride solution conduct
Activator, palladium metal ion are restored as the divalent tin ion that oxidant is adsorbed by fabric surface, restore the precious metals pd of generation,
It is attached to fabric surface in colloidal particle, there can be stronger catalytic activity, in subsequent chemical plating, these particles will be at
For catalytic center, enable the spontaneous progress of chemical plating.
Chemical nickel-plating plating solution is mainly by nickel sulfate, reducing agent sodium hypophosphite, ammonium hydroxide as pH buffer and complexing agent.
The reaction mechanism is as follows for it.In acidic environment:
Ni2++H2PO2+H2O—Ni+H2PO3-+2H+
The evolution reaction of phosphorus is as follows:
H2PO2-+2H+—P+2H2O
2H2PO2-—P+HPO3 2-+H++H2O
H2PO2-+4H+H+—PH3+2H2O
The deposition velocity of chemical nickel plating is influenced maximum by pH value, to reaction speed, the utilization rate of reducing agent, the property of coating
All have a great impact.The nickel of every reduction lmol, need to consume the hypophosphites of 3mol.Meanwhile a part of hypophosphite is in nickel
Surface catalyzed decomposition.The usage factor of hypophosphite is related with the property of solution composition such as buffer and ligand and concentration.
When other conditions are identical, in the high solution of nickel reduction rate, usage factor is also high.Usage factor adds with loading density
It improves greatly.
In acidic environment, the solution chemistry nickel plating containing only nickel ion and hypophosphite can be used, but in order to make work
Skill is stablized, it is necessary to buffer and complexing agent be added.The buffer that the present invention selects is ammonium hydroxide, and complexing agent is trisodium citrate.Cause
Hydrogen ion to generate in nickel process makes reaction speed decline or even stop.Complex compound can be when bath pH value increases
Also its reducing power is kept, if the stability of plating solution can sharply decline without enough complexing agents.
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
Embodiment 1
A kind of preparation method of flexible battery collector, has specifically included following steps:
(1) cotton directly bought on the market is cut into 5cm × 5cm size, is impregnated with the NaOH solution of 1.25mol/L
After 5min, spends and rinsed well after being impregnated from water；
(2) cotton is put into the solution of ethyl alcohol, acetone volume ratio 1:1 one by one, is sealed with preservative film, ultrasonic cleaning is put into
It is cleaned 30 minutes in instrument；It is rinsed twice with clear water, 50 DEG C of low temperature drying；
(3) cotton sensitized treatment: is put into the 10mmol/L SnCl containing 3 tin grains2With liquor capacity content 0.6%
HCI solution in stir 10 minutes, with deionized water impregnate after ten minutes, cleaning after be rinsed with water 2 times, pick up and water dripped
It is dry；
(4) it is activated: the cotton drained is put into the PbCl of 2mmol/L2It is impregnated in 10min in hydrochloric acid solution, hydrochloric acid
Content is the 1% of overall solution volume, picks up to be put into deionized water after sufficiently impregnating and impregnates 10min, pulls out and drain, low temperature drying
Or natural drying.
After sensitization, activation, cotton surface color is ecru at this time.Flavescence is a large amount of due to having in sensitization activation process
Palladium ion is attached to cotton surface.Softening is to remove the glue dust spot of design on fabric surface in the process of cleaning, oil removing degreasing,
So that cloth surface is become hydrophily, while keeping design on fabric surface coarse.
(5) 30mmol nickel sulfate, 0.1mol hypophosphorous acid Asia hydrogen sodium, 70mmol ammonium chloride, 15mmol trisodium citrate are prepared
Aqueous solution, with ammonium hydroxide adjust pH to 4~5, be put into draught cupboard and start chemical nickel plating, nickel plating 5 was as a child pulled out afterwards, spend from
After sub- water impregnates 10min, then water rinses repeatedly to remove the remaining plating solution on surface, and nickel plating cotton fabric i.e. nickel plating cloth is obtained after drying
Material is used as flexible current-collecting body；Wherein, there are two effects for nickel coating: first is that as conductive layer, second is that the nickel as active material NiO
Source.
(6) show to directly generate Ni (OH) in nickel metal layer by hydro-thermal method oxidizing process (140 DEG C, 14h)2Nanometer sheet battle array
Column.Specific steps are as follows: reaction solution is the H that volume ratio is 6:12O and H2O2Solution, a piece of suitable of step (5) preparation is added
The nickel plating cotton of size is placed in polytetrafluoroethylliner liner together, then is put into baking oven after being sealed with rustless steel container, protects at 140 DEG C
Temperature 14 hours, then natural cooling, that is, obtain Ni (OH)2Nano-chip arrays cloth.To Ni (OH) at a temperature of 250 DEG C2Nanometer sheet
Array cloth carries out heat preservation heat treatment 3 hours, so that surface Ni (OH)2Layer is changed into NiO nano-chip arrays active material, simultaneously
The carbonization of cotton base part is set to become carbon material to enhance electric conductivity and realize flexible carbon support substrate.
(7) by adhesive force of the tape method observational measurement NiO on cotton, to determine that active material nickel oxide and flexibility are led
The binding force of electric substrate.It is pasted onto the surface that growth has NiO with adhesive tape, is rolled using the noon that weight is 2 kilograms above
Pressure for several times, then takes the content that NiO is stained on adhesive tape observation adhesive tape off.Only adhere to a small amount of residue on adhesive tape, has no obvious powder
Residual, it means that the binding force of nickel oxide and substrate is greater than the binding force between nickel oxide and adhesive tape, illustrates in flexible substrates
NiO is preferable with substrate caking power, as a result as shown in Figure 1.Tape method can refer to document Hu L, Pasta M, Mantia F L, et
al.Stretchable,porous,and conductive energy textiles[J].Nano Letters,2010,10
(2): being carried out in 708-714..
(8) using the conductivity of the nickel plating cotton in four probe method measuring process 5.As a result as shown in Fig. 2, can be sent out in figure
The resistivity of existing chemical nickel plating cloth is lower and deviation is lower, and the average resistivity of chemical nickel plating cotton is only 1.08 Ω cm,
As a result illustrate that its is entirely appropriate as flexible conducting substrate.It is also that four probe method, which can be found in document Zheng Li and defend with sodium hypophosphite,
Nylon fabric electroless copper research [D] the Donghua University of former agent, 2010.
Embodiment 2
(1) it is the flexibility of electrode prepared by verifying embodiment 1, it is bent at room temperature, it is anyway curved
Folding, which can return back to original shape, have no falling off for NiO and metallic nickel, as shown in Figure 3.And existing copper foil preparation
Electrode can not carry out repeatedly, wide-angle bending.
(2) using the pattern of NiO obtained by (6) method in scanning electron microscope observation embodiment 1, as shown in figure 4, gained
NiO is nano-chip arrays as a result, being grown directly upon the surface of metal nickel layer.
(3) the contained element of flexible electrode is probed into using x-ray photoelectron spectroscopy, there is a small amount of in electrode kind for discovery
Nitrogen and P elements, as shown in Figure 5,6.After nitrating and phosphorus, nitrogen and phosphorus can partially replace carbon, into carbon lattice structure, can make
Carbon-coating generates a large amount of defect and active site, these defects and active site can capture lithium ion, to improve lithium ion
Embedded quantity, therefore the specific capacity of cathode is improved；Nitrogen and P elements can also change the electronics in carbon-coating around carbon atom
Cloud distribution, so that the carbon-coating of nitrating, phosphorus has superior electric conductivity and more stable electrification compared to the carbon of non-nitrating, phosphorus
Performance is learned, and then improves the high rate performance and cycle performance of cathode.
(4) lithium ion battery is assembled after being sliced flexible electrode.It is the LiPF of 1mol/L with concentration6EC/DEC mixed liquor
For electrolyte, wherein the volume ratio of EC:DEC is that 1:1 is completed in glove box using Celgard2400 polypropylene film as diaphragm
Button cell assembling, this half-cell initial capacity up to 6000 μ Ah/cm2, reversible capacity still up to 3000 μ Ah/cm2, 5
Capacity is still up to 1700 μ Ah/cm after secondary electric discharge2, as shown in fig. 7,1,2,3,5 expression discharge time in Fig. 7.
The above described is only a preferred embodiment of the present invention, being not the limitation for doing other forms to the present invention, appoint
What those skilled in the art can use the equivalence enforcement that technology contents disclosed above were changed or be modified as equivalent variations
Example.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to the above embodiments
What simple modification, equivalent variations and remodeling, still falls within the protection scope of technical solution of the present invention.
Claims (10)
1. a kind of preparation method of flexible lithium ion battery negative current collector, which is characterized in that it includes the following steps:
S1, it is pre-processed cloth as base material, is ultrasonically treated, is sensitized, is activated later；
S2, one layer of nano nickel nano-particle layer is grown on step S1 treated cloth using chemically coated nickel method, prepare plating
Nickel cloth is as flexible current-collecting body；
S3, the nickel plating cloth growth in situ Ni (OH) that step S2 is obtained2Nano-chip arrays；
S4, pass through heating means for Ni (OH)2Nano-chip arrays are changed into nickel oxide nano chip arrays active material, while will be soft
Property cloth substrate is changed into the flexible carbon substrate of nitrogen, phosphor codoping.
2. preparation method as shown in claim 1, which is characterized in that in step sl, the cloth is cotton, waste and old cotton
Cloth, the pretreatment refers to using cleaning, then uses dipping by lye, then rinse after being impregnated with deionized water.
3. the preparation method as shown in claim 2, which is characterized in that the lye is the NaOH solution of 1~2mol/L, is impregnated
After 5~20min, is impregnated and cleaned with deionized water.
4. preparation method as shown in claim 1, which is characterized in that in step sl, it is described ultrasonic treatment using ethyl alcohol with
The mixed solution of acetone is rinsed twice with clear water after ultrasonic, is dried later.
5. preparation method as shown in claim 1, which is characterized in that in step sl, the sensitization is using stanniferous grain
10mmol/L SnCl2After being mixed with the HCI solution of liquor capacity content 0.6%, 5~20min is impregnated with deionized water,
Water is drained after being rinsed with water later.
6. preparation method as shown in claim 1, which is characterized in that in step sl, the activation processing will drain
Cloth impregnates in activating solution, is impregnated later in deionized water, pulls out and drains, drying.
7. the preparation method as shown in claim 6, which is characterized in that the activating solution is the PbCl of 2mmol/L2Solution impregnates 5
~10min finally impregnates 5~10min with deionized water.
8. preparation method as shown in claim 1, which is characterized in that in step s 2, the chemically coated nickel method refers to will be quick
Change, activation after cloth be put into plating solution, plating solution be 30mmol nickel sulfate, 0.1mol hypophosphorous acid Asia hydrogen sodium, 70mmol ammonium chloride,
The aqueous solution of 15mmol trisodium citrate adjusts pH to 4~5 with ammonium hydroxide.
9. preparation method as shown in claim 1, which is characterized in that in step s3, the growth in situ Ni (OH)2Nanometer
Chip arrays use hydro-thermal method, and method is the H for using reaction solution to be 6:1 for volume ratio2O and H2O2Solution, be added step S2 obtain
The nickel plating cloth obtained is placed in polytetrafluoroethylliner liner together, then is put into baking oven after being sealed with rustless steel container, keeps the temperature at 140 DEG C
14 hours, then natural cooling.
10. preparation method as shown in claim 1, which is characterized in that in step s 4, the heating means are in Muffle furnace
The middle Ni (OH) for obtaining step S32Nano-chip arrays are heated to 250 DEG C, keep the temperature 3 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113517445A (en) * | 2021-05-20 | 2021-10-19 | 上海工程技术大学 | Flexible battery current collector, electrode plate and electrode lug for lithium ion battery |
| CN114388741A (en) * | 2022-02-25 | 2022-04-22 | 电子科技大学 | Sodium titanium phosphate electrode and preparation method thereof |
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