CN109734084A - A kind of foam stone ink sheet and preparation method thereof for cathode of lithium battery - Google Patents
A kind of foam stone ink sheet and preparation method thereof for cathode of lithium battery Download PDFInfo
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- CN109734084A CN109734084A CN201811642119.3A CN201811642119A CN109734084A CN 109734084 A CN109734084 A CN 109734084A CN 201811642119 A CN201811642119 A CN 201811642119A CN 109734084 A CN109734084 A CN 109734084A
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- ink sheet
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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 discloses a kind of preparation method of foam stone ink sheet for cathode of lithium battery, include the following steps: graphite composite powder, lithium carbonate particle and Kynoar (0.1~0.5) in mass ratio 1): (0.1~0.8): (0.02~0.1) disperses in a solvent, to obtain graphite slurry;2) graphite slurry is coated on substrate, is dried at 1300~1500 DEG C, after lithium carbonate gasification, form foamy graphite carbon-coating on substrate;3) substrate for being coated with foamy graphite carbon-coating impregnates in the solution, after substrate dissolution, is post-processed to obtain foam stone ink sheet to foamy graphite carbon-coating.The intensity and toughness of foam stone ink sheet can be enhanced by the way that lithium carbonate particle and Kynoar are added in graphite composite powder in the present invention;And it then can be improved the porosity of graphite flake layer by using the mode of lithium carbonate gasification occupy-place, and then promote cathode to the absorbability of electrolyte and the energy density of lithium ion battery.
Description
Technical field
The present invention relates to graphite flake technical field more particularly to a kind of foam stone ink sheets and its system for cathode of lithium battery
Preparation Method.
Background technique
With the development of science and technology mobile device using more and more extensive.It is right due to the rapid growth of mobile device
High energy density cells form wilderness demand.
Negative electrode material is the key components of lithium ion battery, it directly affects the energy density of battery, circulation longevity
Key indexes, following lithium ion battery negative material such as life and security performance must develop to high capacity direction, just can solve
The low problem of existing battery energy density.
For current commercialized negative electrode active material based on graphite, the method for improving its energy density is mainly improved graphite
Change degree come increase lithium ion insertion position and improve cathode pole piece compacted density.The increase of degree of graphitization can reduce graphite
Interlamellar spacing, the polarization for causing lithium ion to be embedded in and deviate from cathode pole piece increase problem.The compacted density of cathode pole piece is excessively high
It can make the reduction of cathode pole piece hole, reduce cathode pole piece significantly to the absorbability of electrolyte, increase lithium ion battery and exist
Polarization during low temperature and high rate charge-discharge.
The technique of high compacted density is improved in the industry, such as Chinese patent application publication number
CN102195029A discloses a kind of lithium ion battery and its cathode pole piece, uses composite graphite layer process, but this technique
It is also reduction of the energy density of lithium ion battery to a certain extent.
In view of this, it is necessory to provide a kind of technical solution to solve the above problems.
Summary of the invention
It is an object of the invention to: in view of the deficiencies of the prior art, and provide that a kind of porosity is high, intensity is high, good toughness
The foam stone ink sheet for cathode of lithium battery preparation method.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of the foam stone ink sheet for cathode of lithium battery, includes the following steps:
1) by graphite composite powder, lithium carbonate particle and Kynoar (0.1~0.5) in mass ratio: (0.1~0.8):
(0.02~0.1) dispersion in a solvent, obtains graphite slurry;
2) graphite slurry is coated on substrate, is dried under the conditions of 1300~1500 DEG C of temperature,
After lithium carbonate gasification, foamy graphite carbon-coating is formed on substrate;
3) substrate for being coated with foamy graphite carbon-coating impregnates in the solution, after substrate dissolution, to foamy graphite
Carbon-coating is post-processed to obtain foam stone ink sheet.
Preferably, in step 1), the partial size of the lithium carbonate particle is 0.1~10 μm.The grain diameter of lithium carbonate will be straight
The size for determining graphite flake layer hole is connect, therefore its partial size needs to control in suitable range.If its partial size is too small, it will shadow
Ring the formation of hole;If its partial size is excessive, it will influence the structural stability of graphite flake layer.
Preferably, in step 1), the partial size of the graphite composite powder is 0.2~5 μm.
Preferably, in step 1), the solvent is N-Methyl pyrrolidone, at least one in n,N-Dimethylformamide
Kind.
Preferably, in step 2), the temperature of the drying process is 1350~1450 DEG C.Wherein, the temperature of drying process
It is most important, if temperature is too low, it is unable to reach the decomposition temperature of lithium carbonate or lithium carbonate is caused to decompose not exclusively, will affect foam
The porosity of graphite flake;If temperature is excessively high, the rock-steady structure of graphitic carbon layer may be will affect, therefore, it is necessary to temperature control exists
In suitable range.
Preferably, in step 2), the graphite slurry is coated on the substrate by the way of layered coatings, if coating
Counting is N, and N >=2, and wherein the partial size of the lithium carbonate particle in n-th layer is greater than the partial size of the lithium carbonate particle in N-1 layers.It is logical
The lithium carbonate grain diameter crossed by the way of multi-layer coated and the lithium carbonate grain diameter of rear coating layer is made to be greater than preceding coating layer,
In this way after the gasification of lithium carbonate particle, divide the pore size of graphite carbon-coating from the gradient formed from small to large far from orientation substrate
Cloth structure.The quick deintercalation for not only improving lithium ion in this way, improves the high rate performance of battery, while can prevent to a certain extent again
The only dilatancy of negative electrode tab.
Preferably, in step 2), the substrate is copper foil or aluminium foil.
Preferably, in step 3), the solution is any in liquor ferri trichloridi, silver nitrate solution and sulfuric acid mercury solution
Kind;Wherein, the concentration of liquor ferri trichloridi is 1~3mol/L;The concentration of silver nitrate solution is 2~5mol/L;Sulfuric acid mercury solution
Concentration be 2~5mol/L.
Preferably, in step 3), described the step of post-processing to foamy graphite carbon-coating includes: using deionized water pair
After the foamy graphite carbon-coating cleaning, drying and processing is carried out.
In addition, the foam stone ink sheet is by above-mentioned the present invention also provides a kind of foam stone ink sheet for cathode of lithium battery
The preparation method of foam stone ink sheet described in either segment for cathode of lithium battery is prepared.
Compared with the prior art, the present invention at least has the advantages that the system of foam stone ink sheet provided by the invention
The strong of foam stone ink sheet can be enhanced by the way that lithium carbonate particle and Kynoar (PVDF) are added in graphite composite powder in Preparation Method
Degree and toughness;And made of coating is dissolved in solvent graphite composite powder, lithium carbonate particle and PVDF on substrate
Graphite slurry makes graphite slurry be coated on progress heated drying processing on substrate, lithium carbonate is made to gasify to form foamy graphite carbon-coating, then
The method that substrate removes is prepared into foamy graphite lamella, this preparation method can overcome the frangible spy of foam stone ink sheet well
Point substantially increases the intensity and toughness of foam stone ink sheet, also provides possibility to prepare lithium ion battery flexible;And pass through
The porosity of graphite flake layer can be then greatly improved in such a way that lithium carbonate gasifies occupy-place, and then effectively promotes negative electrode tab to electricity
The absorbability of liquid and the energy density of lithium ion battery, and preparation method simple process of the invention are solved, operation is easy, cost
It is low, it is suitable for enterprise scale and produces.
Specific embodiment
To keep technical solution of the present invention and advantage clearer, below in conjunction with specific embodiment, to skill of the invention
Art scheme is clearly and completely described, it is clear that and described embodiments are some of the embodiments of the present invention, rather than all
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art institute without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of foam stone ink sheet for cathode of lithium battery, preparation method include the following steps:
1) by partial size be 0.2 μm graphite composite powder, the lithium carbonate particle that partial size is 0.1 μm and Kynoar in mass ratio
0.1:0.1:0.02 is dispersed in N-Methyl pyrrolidone solvent, obtains graphite slurry;
2) graphite slurry is coated on copper clad laminate, is dried under the conditions of 1300 DEG C of temperature, to
After the lithium carbonate gasification, foamy graphite carbon-coating is formed on copper clad laminate;
3) copper clad laminate for being coated with foamy graphite carbon-coating is immersed in the liquor ferri trichloridi that concentration is 2mol/L, to
After the copper clad laminate dissolution, after being cleaned using deionized water to the foamy graphite carbon-coating, drying and processing is carried out, foam is obtained
Graphite flake.
Embodiment 2
A kind of foam stone ink sheet for cathode of lithium battery, preparation method include the following steps:
1) by partial size be 5 μm graphite composite powder, the lithium carbonate particle that partial size is 10 μm and Kynoar in mass ratio
0.5:0.8:0.1 is dispersed in n,N-Dimethylformamide solvent, obtains graphite slurry;
2) graphite slurry is coated on copper clad laminate, is dried under the conditions of 1500 DEG C of temperature, to
After the lithium carbonate gasification, foamy graphite carbon-coating is formed on copper clad laminate;
3) copper clad laminate for being coated with foamy graphite carbon-coating is immersed in the silver nitrate solution that concentration is 3.5mol/L, to
After the copper clad laminate dissolution, after being cleaned using deionized water to the foamy graphite carbon-coating, drying and processing is carried out, foam is obtained
Graphite flake.
Embodiment 3
A kind of foam stone ink sheet for cathode of lithium battery, preparation method include the following steps:
1) by partial size be 2 μm graphite composite powder, the lithium carbonate particle and Kynoar in mass ratio 0.3 that partial size is 5 μm:
0.5:0.06 is dispersed in n,N-Dimethylformamide solvent, obtains graphite slurry;
2) graphite slurry is coated on copper clad laminate, is dried under the conditions of 1350 DEG C of temperature, to
After the lithium carbonate gasification, foamy graphite carbon-coating is formed on copper clad laminate;
3) copper clad laminate for being coated with foamy graphite carbon-coating is immersed in the sulfuric acid mercury solution that concentration is 3.5mol/L, to
After the copper clad laminate dissolution, after being cleaned using deionized water to the foamy graphite carbon-coating, drying and processing is carried out, foam is obtained
Graphite flake.
Embodiment 4
A kind of foam stone ink sheet for cathode of lithium battery, preparation method include the following steps:
1) by partial size be 1 μm graphite composite powder, the lithium carbonate particle that partial size is 2.5~5 μm and Kynoar by quality
It is dispersed in n,N-Dimethylformamide solvent than 0.2:0.3:0.04, obtains graphite slurry;
2) graphite slurry is coated on the copper clad laminate by the way of layered coatings, floating coat number is 2
Layer, the partial size of the lithium carbonate particle in the 2nd layer is greater than the partial size of the lithium carbonate particle in the 1st layer, in 1450 DEG C of temperature condition
Under be dried, after the lithium carbonate gasification after, on copper clad laminate formed foamy graphite carbon-coating;
3) copper clad laminate for being coated with foamy graphite carbon-coating is immersed in the sulfuric acid mercury solution that concentration is 3.5mol/L, to
After the copper clad laminate dissolution, after being cleaned using deionized water to the foamy graphite carbon-coating, drying and processing is carried out, foam is obtained
Graphite flake.
Embodiment 5
A kind of foam stone ink sheet for cathode of lithium battery, preparation method include the following steps:
1) by partial size be 0.8 μm graphite composite powder, the lithium carbonate particle that partial size is 0.5~1.5 μm and Kynoar by
Mass ratio 0.5:0.2:0.08 is dispersed in N-Methyl pyrrolidone solvent, obtains graphite slurry;
2) graphite slurry is coated on the copper clad laminate by the way of layered coatings, apply the number of plies is 3 layers altogether,
Wherein the partial size of the lithium carbonate particle in the 2nd layer is greater than the partial size of the lithium carbonate particle in the 1st layer, the lithium carbonate in the 3rd layer
The partial size of grain is greater than the partial size of the lithium carbonate particle in the 2nd layer, is dried under the conditions of 1450 DEG C of temperature, to described
After lithium carbonate gasification, foamy graphite carbon-coating is formed on copper clad laminate;
3) copper clad laminate for being coated with foamy graphite carbon-coating is immersed in the silver nitrate solution that concentration is 5mol/L, to institute
After stating copper clad laminate dissolution, after being cleaned using deionized water to the foamy graphite carbon-coating, drying and processing is carried out, foam stone is obtained
Ink sheet.
Embodiment 6
A kind of foam stone ink sheet for cathode of lithium battery, preparation method include the following steps:
1) by partial size be 5 μm graphite composite powder, the lithium carbonate particle that partial size is 5~10 μm and Kynoar in mass ratio
0.4:0.3:0.05 is dispersed in N-Methyl pyrrolidone solvent, obtains graphite slurry;
2) graphite slurry is coated on the aluminum foil substrate by the way of layered coatings, apply the number of plies is 4 layers altogether,
Wherein the partial size of the lithium carbonate particle in the 2nd layer is greater than the partial size of the lithium carbonate particle in the 1st layer, the lithium carbonate in the 3rd layer
The partial size of grain is greater than the partial size of the lithium carbonate particle in the 2nd layer, and the partial size of the lithium carbonate particle in the 4th layer is greater than in the 3rd layer
The partial size of lithium carbonate particle is dried under the conditions of 1450 DEG C of temperature, after lithium carbonate gasification, in copper foil base
Foamy graphite carbon-coating is formed on plate;
3) aluminum foil substrate for being coated with foamy graphite carbon-coating is immersed in the sulfuric acid mercury solution that concentration is 5mol/L, to institute
After stating aluminum foil substrate dissolution, after being cleaned using deionized water to the foamy graphite carbon-coating, drying and processing is carried out, foam stone is obtained
Ink sheet.
Toughness, the intensity of the foam stone ink sheet of Examples 1 to 6 preparation are tested respectively, it is specific as follows: by embodiment
1~6 foam stone ink sheet (2cm*2cm) sample prepared is dipped into respectively in 50ml ethanol solution, ultrasonic disperse
30min, supersonic frequency 40Hz observe the integrality of ultrasound front and back pole piece, and whether there are cracks etc..
It is observed that the foam stone ink sheet sample of Examples 1 to 6 preparation has almost no change after ultrasound, shape has been kept
It is whole, occur without crackle, this illustrates the foam stone ink sheet integrality with higher and intensity of this method preparation.
The cathode of lithium ion battery is made in the foam stone ink sheet that Examples 1 to 6 is respectively adopted, and then uses common process system
At lithium ion battery, the chemical property of lithium ion battery is tested.Test result is shown in Table 1.
By the test result of table 1 it is found that the present invention not only increases battery energy density, the forthright again of battery is also improved
Energy and service life cycle.This is because the special composed structure and table of foam stone ink sheet made from preparation method of the present invention
Porosity is seen, is that the performance of high energy lithium ion cell plays, has built good battery core microstructure.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and is modified.Therefore, the invention is not limited to above-mentioned specific embodiment, all those skilled in the art exist
Made any conspicuous improvement, replacement or modification all belong to the scope of protection of the present invention on the basis of the present invention.This
Outside, although using some specific terms in this specification, these terms are merely for convenience of description, not to the present invention
Constitute any restrictions.
Claims (10)
1. a kind of preparation method of the foam stone ink sheet for cathode of lithium battery, which comprises the steps of:
1) by graphite composite powder, lithium carbonate particle and Kynoar (0.1~0.5) in mass ratio: (0.1~0.8): (0.02~
0.1) dispersion in a solvent, obtains graphite slurry;
2) graphite slurry is coated on substrate, is dried under the conditions of 1300~1500 DEG C of temperature, to institute
After stating lithium carbonate gasification, foamy graphite carbon-coating is formed on substrate;
3) substrate for being coated with foamy graphite carbon-coating impregnates in the solution, after substrate dissolution, to foamy graphite carbon-coating
It is post-processed to obtain foam stone ink sheet.
2. the preparation method of the foam stone ink sheet according to claim 1 for cathode of lithium battery, it is characterised in that: step
1) in, the partial size of the lithium carbonate particle is 0.1~10 μm.
3. the preparation method of the foam stone ink sheet according to claim 1 for cathode of lithium battery, it is characterised in that: step
1) in, the partial size of the graphite composite powder is 0.2~5 μm.
4. the preparation method of the foam stone ink sheet according to claim 1 for cathode of lithium battery, it is characterised in that: step
1) in, the solvent is at least one of N-Methyl pyrrolidone, n,N-Dimethylformamide.
5. the preparation method of the foam stone ink sheet according to claim 1 for cathode of lithium battery, it is characterised in that: step
2) in, the temperature of the drying process is 1350~1450 DEG C.
6. the preparation method of the foam stone ink sheet according to claim 1 for cathode of lithium battery, it is characterised in that: step
2) in, the graphite slurry is coated on the substrate by the way of layered coatings, if the painting number of plies is N, and N >=2, wherein the
The partial size of lithium carbonate particle in N layers is greater than the partial size of the lithium carbonate particle in N-1 layers.
7. the preparation method of the foam stone ink sheet according to claim 1 for cathode of lithium battery, it is characterised in that: step
2) in, the substrate is copper foil or aluminium foil.
8. the preparation method of the foam stone ink sheet according to claim 1 for cathode of lithium battery, it is characterised in that: step
3) in, the solution is any one of liquor ferri trichloridi, silver nitrate solution and sulfuric acid mercury solution;Wherein, ferric trichloride is molten
The concentration of liquid is 1~3mol/L;The concentration of silver nitrate solution is 2~5mol/L;The concentration of sulfuric acid mercury solution is 2~5mol/L.
9. the preparation method of the foam stone ink sheet according to claim 1 for cathode of lithium battery, it is characterised in that: step
3) in, described the step of post-processing to foamy graphite carbon-coating includes: clear to the foamy graphite carbon-coating using deionized water
After washing, drying and processing is carried out.
10. a kind of foam stone ink sheet for cathode of lithium battery, it is characterised in that: the foam stone ink sheet is by claim 1~9
The preparation method of described in any item foam stone ink sheets for cathode of lithium battery is prepared.
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