CN114464776A - Preparation method of ultra-high power ultra-thin negative plate capable of being produced in batch - Google Patents

Preparation method of ultra-high power ultra-thin negative plate capable of being produced in batch Download PDF

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Publication number
CN114464776A
CN114464776A CN202210056346.8A CN202210056346A CN114464776A CN 114464776 A CN114464776 A CN 114464776A CN 202210056346 A CN202210056346 A CN 202210056346A CN 114464776 A CN114464776 A CN 114464776A
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ultra
negative electrode
high power
slurry
negative plate
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Chinese (zh)
Inventor
唐月娇
班宵汉
刘富亮
刘江涛
陈晓涛
袁再芳
胡锦飞
刁思强
苏纪宏
周雄
陈安国
向斌
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Chongqing University
Guizhou Meiling Power Supply Co Ltd
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Chongqing University
Guizhou Meiling Power Supply Co Ltd
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy

Abstract

The application discloses a preparation method of an ultra-high power ultra-thin negative plate capable of being produced in batch in the technical field of chemical energy storage batteriesOne or more of carbon microspheres, lithium titanate, silicon carbon and silicon monoxide, a negative electrode active substance D90 is not more than 5 mu m, and the specific surface area is not less than 5m2(ii) in terms of/g. Mixing the raw materials of the negative plate together, kneading by adopting a kneading process to form slurry, finishing kneading when the fineness of the slurry is less than or equal to that of a negative active material D90, adding a binder and water into the kneaded slurry for dilution regulation, sieving and loading into a coating machine, performing double-sided coating on a current collector, wherein the total thickness of the double-sided coating is less than or equal to 60 mu m, and performing high-temperature drying after coating to obtain the high-power ultrathin negative plate. The negative plate realizes 1500C limit discharge, and provides a new solution for mass production of ultrahigh power supplies.

Description

Preparation method of ultra-high power ultra-thin negative plate capable of being produced in batch
Technical Field
The invention relates to the technical field of chemical energy storage batteries, in particular to a preparation method of ultra-high power ultra-thin negative plates capable of being produced in batch.
Background
With the development of science and technology, the military and civil energy storage markets have higher and higher requirements on power, and in the preparation direction of pole pieces, the following approaches are mainly used for improving the rate performance of a battery at present: namely, the preparation of the high-performance super-thick pole piece is carried out by taking the super capacitor as a direction, and the load of active substances is improved so as to improve the specific power and specific energy of the super capacitor. Based on the above, the discharge of the current high-specific energy lithium ion battery, such as high-power lithium ion batteries for model airplanes and unmanned aerial vehicles, is 30 ℃, but the thickness of the negative electrode plate is about 100 μm, and the specific power of the battery is 3-5 Kw/kg. But the multiplying power performance of the weapon can not meet the use requirements of the weapon requiring ultrahigh power, such as an electronic gun, a laser weapon, a microwave weapon and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention designs the high-power ultrathin negative plate.
One of the purposes of the invention is to provide a preparation method of an ultra-high power ultra-thin negative electrode sheet capable of being produced in batch, the raw materials comprise a negative electrode active substance, the negative electrode active substance is one or more of hard carbon, soft carbon, graphite, mesocarbon microbeads, lithium titanate, silicon carbon and silicon oxide, the negative electrode active substance D90 is less than or equal to 5 microns, and the specific surface area is greater than or equal to 5m2/g。
Further, the raw materials also comprise a conductive agent, a thickening agent and a binder, the negative active material, the conductive agent and the thickening agent are mixed together, a kneading process is adopted to knead the mixture to form slurry, when the fineness of the slurry is smaller than or equal to that of the negative active material D90, the kneading is finished, the binder is added to be uniformly mixed, deionized water is added to dilute and regulate, the slurry is sieved, the slurry is placed into a coating machine, two surfaces of a current collector are coated respectively, the total thickness of the two-surface coating is smaller than or equal to 60 mu m, and high-temperature drying is carried out after the coating, so that the high-power ultrathin negative plate is obtained.
Further, the μ/σ of the slurry is <1 s/m. Where μ is the slurry viscosity and σ is the surface tension of the slurry fluid.
Further, the coating machine is a transfer type coating machine or a squeeze type coating machine.
Further, high-temperature drying is carried out in a vacuum drying oven, the drying temperature is 100-200 ℃, the drying time is 2-100 hours, and the vacuum degree is more than or equal to 85 Mpa.
Further, the conductive agent is superconducting carbon black SP, the thickening agent is CMC, and the binder is SBR.
Further, the current collector is a copper foil.
The invention also aims to provide a high-power ultrathin negative plate prepared by the method.
The invention also aims to provide the application of the high-power ultrathin negative plate in an ultrahigh-power supply.
The working principle of the invention is as follows: the raw materials of the invention are selected from materials with small particle size, the transmission path of ions and electrons in the materials is greatly shortened, meanwhile, the lithium ion battery anode material is prepared by a high-hole ultrathin pole piece, the transmission channel of lithium ions in the pole piece is widened, the transmission distance of the lithium ions in the pole piece is shortened, the transmission distance of the electrons in the pole piece is also shortened, the particle-particle interaction is realized by combining the kneading principle and mechanical stirring, the problem that the anode material with high specific surface area and small particle size is easy to agglomerate in the pulping process is solved, then, the slurry is regulated and controlled to prepare the anode slurry for ultrathin coating of a transfer type coating machine or an extrusion type coating machine, the ultrahigh-power anode sheet with thickness deviation lower than 1 mu m and no obvious coating defect is prepared, the 1500C limit discharge of the anode sheet is realized, and a new solution way is provided for mass production of ultrahigh-power supplies.
Drawings
FIG. 1 is a diagram showing the fineness of the slurry successfully kneaded in example 1 of the present invention;
FIG. 2 is a test chart of the thickness of both sides of the high-power ultrathin pole piece (thickness of the current collector) in the embodiment 1 of the invention;
FIG. 3 is a 1500C second charging and discharging curve chart of the pole piece prepared by the embodiment 1-2 and the comparative example 3-5 of the invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments thereof, but the present invention is not limited to these embodiments, and any modifications or substitutions within the basic spirit of the present invention are intended to be included within the scope of the present invention as defined by the appended claims.
The high-power ultrathin pole pieces of the embodiment cases 1-2 and the negative pole pieces 1-3 of the comparison case were prepared as follows:
example 1
D90 was weighed to be 5 μm and the specific surface area to be 6m2The graphite material per gram, together with the conductive agent SP, is added to the CMC water solution (mass ratio of CMC to water is1:40), wherein the raw materials of the negative electrode sheet comprise a graphite material, a conductive agent SP, a binder SBR and a thickening agent CMC in a mass ratio of 95:1:2: 2. And (3) sampling every 1 hour of stirring, performing fineness test, as shown in figure 1, until the fineness of the slurry is 5 micrometers, ensuring that the slurry is free of agglomeration, adding a certain amount of SBR (styrene butadiene rubber) to continue stirring after kneading is finished, adding water to dilute until the mu/sigma is 0.3s/m, sieving, respectively coating the two sides of the current collector by using a transfer coater, wherein the total thickness of the two-side coating is 30 micrometers, as shown in figure 2, finally, the thickness of the two sides of the high-power ultrathin pole piece (the thickness of the current collector is removed) is 30 micrometers, and drying the coated pole piece for 12 hours in an environment with the vacuum degree of 85MPa and the temperature of 150 ℃ to obtain the ultrathin high-power negative pole piece.
Example 2
D90 was weighed to be 4 μm and the specific surface area was 8m2The hard carbon material per gram and the conductive agent SP are added into a CMC aqueous solution (the mass ratio of the CMC to the water is 1:40) to be kneaded, wherein the hard carbon material, the conductive agent SP, the binder SBR and the thickening agent CMC in the raw materials of the negative plate are 95:1:2:2 in the mass ratio. Sampling every 1h of stirring, performing fineness test until the fineness of the slurry is 4 mu m, ensuring that the slurry is free of agglomeration, adding a certain amount of SBR (styrene butadiene rubber) to continue stirring after kneading is finished, adding water to dilute until the mu/sigma is 0.3s/m, sieving, respectively coating the two sides of a current collector by adopting a transfer coater, wherein the total thickness of the two-side coating is 30 mu m, and drying the coated pole piece for 12h in an environment with the vacuum degree of 85Mpa and the temperature of 150 ℃ to obtain the high-power ultrathin negative pole piece.
Comparative example 1
D90 was weighed to 21 μm and the specific surface area was 1m2The graphite material per gram and the conductive agent SP are added into a CMC aqueous solution (the mass ratio of the CMC to the water is 1:40) to be kneaded, and the graphite material, the conductive agent SP, the binder SBR and the thickening agent CMC in the raw materials of the negative plate are 95:1:2:2 according to the mass ratio. Sampling every 1h of stirring, performing fineness test until the fineness of the slurry is less than 21 mu m, adding a certain amount of SBR, stirring, adding water to dilute mu/sigma to be 0.3s/m, sieving, coating the current collector by adopting a transfer coater, and drying the coated pole piece for 12h in an environment with the vacuum degree of 85Mpa and the temperature of 150 ℃ to obtain the negative pole piece.
Comparative example 2
D90 was weighed to be 5 μm and the specific surface area to be 6m2The graphite material per gram and the conductive agent SP are added into a CMC aqueous solution (the mass ratio of the CMC to the water is 1:40), and the graphite material, the conductive agent SP, the binder SBR and the thickening agent CMC in the raw materials of the negative plate are 95:1:2:2 according to the mass ratio. Stirring and mixing, wherein the fineness of the slurry is 18 mu m, adding a certain amount of SBR, stirring, adding water to dilute until the mu/sigma is 0.3s/m, sieving, coating the current collector by adopting a transfer coater, and drying the coated pole piece for 12 hours in an environment with the vacuum degree of 85Mpa and the temperature of 150 ℃ to obtain the cathode piece.
Comparative example 3
D90 was weighed to 10 μm and the specific surface area was 1m2The graphite material per gram and the conductive agent SP are added into a CMC aqueous solution (the mass ratio of the CMC to the water is 1:40) to be kneaded, and the graphite material, the conductive agent SP, the binder SBR and the thickening agent CMC in the raw materials of the negative plate are 95:1:2:2 according to the mass ratio. Sampling every 1h of stirring, performing fineness test until the fineness of the slurry is less than 10 mu m, adding a certain amount of SBR, stirring, adding water to dilute until the mu/sigma is 0.3s/m, sieving, coating the two sides of the current collector by adopting a transfer coater, wherein the total thickness of the coated two sides is 30 mu m, and drying the coated pole piece for 12h in an environment with the vacuum degree of 85Mpa and the temperature of 150 ℃ to obtain the cathode piece.
Comparative example 4
Weighing the following options of D90 being 5 μm and specific surface area being 6m2Adding the graphite material and SP into CMC aqueous solution (the mass ratio of CMC to water is 1:40) to be kneaded, wherein the mass ratio of the material layer of the negative plate, the conductive agent SP, the binder SBR and the thickening agent CMC is 95:1:2: 2. Sampling every 1h of stirring, performing fineness test until the fineness of slurry is 5 mu m, adding a certain amount of SBR, stirring, adding water to dilute to 0.3s/m, sieving, respectively coating the two sides of a current collector by adopting a transfer coater, wherein the total thickness of the coated two sides is 30 mu m, and drying the coated pole piece for 12h in an environment with the vacuum degree of 85Mpa and the temperature of 85 ℃ to obtain the cathode piece.
Comparative example 5
Weighing the following options of D90 being 5 μm and specific surface area being 6m2Adding the graphite material per gram and SP into CMC water solution (the mass ratio of CMC to water is 1:40) for kneadingAnd the mass ratio of the material layer of the negative electrode sheet, the conductive agent SP, the binder SBR and the thickening agent CMC is 95:1:2: 2. Sampling every 1h of stirring, performing fineness test until the fineness of the slurry is 5 mu m, adding a certain amount of SBR, stirring, adding water to dilute to 0.3s/m, coating by using a transfer coater, wherein the total thickness of the two surfaces of the coated slurry is 80 mu m, drying at 120 ℃ for 12h, and the vacuum degree is 85 Mpa.
In examples 1 to 2 and comparative examples 1 to 5, copper foil of 9 μm was selected as the current collector, and current collectors of other thicknesses or materials are also suitable.
Table 1 relevant parameters of the negative electrode sheets provided in examples 1 to 2 and comparative examples 1 to 5.
Figure BDA0003476649960000041
As can be seen from Table 1, in example 1 and comparative examples 1 and 2, it can be seen that the material particles are too large, or the slurry is agglomerated, so that the fineness of the slurry is too large, and uniform ultrathin pole piece preparation cannot be carried out.
Application example
The lithium ion capacitors of the embodiment examples 1-2 and the comparative examples 3-4 were prepared as follows, and negative electrode sheets were coated on both sides, and the laminated cells of about 1Ah were assembled according to the company production process.
As can be seen from FIG. 3, 1500C discharge can be performed in the embodiments 1-2, which shows that the weight of the active material has little influence on pulse charge and discharge, the comparative example 3 can not perform 1500C discharge, which shows that the particle size and specific surface area of the material are limiting factors of the limit discharge, and the comparative example 4 can perform 1500C second charge and discharge, but has large voltage drop, which shows that the drying temperature has influence on the limit discharge of the pole piece, high temperature pore-forming can be realized at high temperature, and widening of Li is increased+The comparison case 5 in the transmission channel can not be charged and discharged for 1500C seconds, which shows that the thickness of the pole piece is a limiting factor of the very high-rate discharge.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.

Claims (7)

1. The preparation method of the ultra-high power ultra-thin negative electrode sheet capable of being produced in batch is characterized in that raw materials comprise a negative electrode active substance, the negative electrode active substance is one or more of hard carbon, soft carbon, graphite, mesocarbon microbeads, lithium titanate, silicon carbon and silicon oxide, the negative electrode active substance D90 is less than or equal to 5 mu m, and the specific surface area is greater than or equal to 5m2/g。
2. The method for preparing ultra-high power ultra-thin negative electrode sheets capable of being mass-produced according to claim 1, wherein the method comprises the following steps: the raw materials also comprise a conductive agent, a thickening agent and a binder, the negative active material, the conductive agent and the thickening agent are mixed together, a kneading process is adopted to knead and form slurry, when the fineness of the slurry is smaller than or equal to that of the negative active material D90, the binder is added and uniformly mixed, deionized water is added to dilute, regulate and control, sieving is carried out, the slurry is put into a coating machine, two surfaces of a current collector are respectively coated, the total thickness of the two coated surfaces is smaller than or equal to 60 mu m, and high-temperature drying is carried out after coating, so that the high-power ultrathin negative plate is obtained.
3. The method for preparing ultra-high power ultra-thin negative electrode sheets capable of batch production according to claim 2, wherein the method comprises the following steps: the μ/σ of the slurry is <1 s/m.
4. The method for preparing ultra-high power ultra-thin negative electrode sheets capable of being produced in batch according to claim 3, wherein the method comprises the following steps: the coating machine is a transfer type coating machine or an extrusion type coating machine.
5. The method for preparing ultra-high power ultra-thin negative electrode sheets capable of being mass-produced according to claim 4, wherein the method comprises the following steps: and (3) carrying out high-temperature drying in a vacuum drying oven, wherein the drying temperature is 100-200 ℃, the drying time is 2-100 h, and the vacuum degree is more than or equal to 85 Mpa.
6. An ultra-high power ultra-thin negative electrode sheet prepared by the method of any one of claims 1 to 5.
7. An application of the ultra-high power ultra-thin negative plate prepared by the method of any one of claims 1 to 5 in an ultra-high power supply.
CN202210056346.8A 2022-01-18 2022-01-18 Preparation method of ultra-high power ultra-thin negative plate capable of being produced in batch Pending CN114464776A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014088084A1 (en) * 2012-12-07 2014-06-12 昭和電工株式会社 Method for producing slurry for negative electrode of lithium-ion secondary cell
US20170084913A1 (en) * 2014-03-25 2017-03-23 Tosoh Corporation Composite active material for lithium ion secondary batteries and method for producing same
CN107834023A (en) * 2017-11-27 2018-03-23 东莞市创明电池技术有限公司 Lithium ion battery cathode slurry and preparation method thereof, negative plate and lithium ion battery
CN111758179A (en) * 2018-04-04 2020-10-09 株式会社东芝 Positive electrode, electrode group, and nonaqueous electrolyte battery
US20200373564A1 (en) * 2018-01-31 2020-11-26 Hitachi Chemical Company, Ltd. Negative electrode active material for lithium ion secondary battery, negative electrode for lithium ion secondary battery, and lithium ion secondary battery

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014088084A1 (en) * 2012-12-07 2014-06-12 昭和電工株式会社 Method for producing slurry for negative electrode of lithium-ion secondary cell
US20170084913A1 (en) * 2014-03-25 2017-03-23 Tosoh Corporation Composite active material for lithium ion secondary batteries and method for producing same
CN107834023A (en) * 2017-11-27 2018-03-23 东莞市创明电池技术有限公司 Lithium ion battery cathode slurry and preparation method thereof, negative plate and lithium ion battery
US20200373564A1 (en) * 2018-01-31 2020-11-26 Hitachi Chemical Company, Ltd. Negative electrode active material for lithium ion secondary battery, negative electrode for lithium ion secondary battery, and lithium ion secondary battery
CN111758179A (en) * 2018-04-04 2020-10-09 株式会社东芝 Positive electrode, electrode group, and nonaqueous electrolyte battery

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