CN110444766B - Ternary positive pole piece and method for improving high-temperature cycle performance of positive pole piece - Google Patents
Ternary positive pole piece and method for improving high-temperature cycle performance of positive pole piece Download PDFInfo
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/028—Positive electrodes
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- 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 ternary positive pole piece and a method for improving the high-temperature cycle performance of the positive pole piece. The method for improving the high-temperature cycle performance of the positive pole piece is to spray a mixed liquid crystal of hexabenzocoronene disc-shaped liquid crystal and triphenylene disc-shaped liquid crystal on the surface of the ternary positive pole piece to form a liquid crystal film coated on the surface of the positive pole piece. After the surface of the ternary positive pole piece is coated with the liquid crystal film, the high-temperature cycle performance of the pole piece can be effectively improved.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a ternary positive pole piece with excellent high-temperature cycle performance and a method for improving the high-temperature cycle performance of the positive pole piece.
Background
Ternary composite positive electrode material (LiNi)xMnyCo1-x-yO2) In the alloy, nickel, cobalt and manganese belong to adjacent elements in the same period, and LiCoO2And LiNiO2All have alpha-NaFeO2Layered structures, which can be mixed in any ratio to form a solid solution and remain unchanged. Ni and Co participate in electrochemical action in the charging and discharging process, and Mn is Mn4+The catalyst does not participate in electrochemical reaction, and only plays a role in stabilizing a crystal structure as a material framework. With the change of the composition ratio of Ni, Co and Mn, the writing performance of the material such as capacity, safety and the like can be controlled to a certain extent, and the industry is used to naming according to the ratio of the material, such as 111, 442 and 532 (representing three types of Ni, Co and Mn)Element ratio), and the like, and is influenced by the mutual occupation of nickel and lithium, and the structural stability of the material is better when the ratio of Ni, Mn and Co is 1:1:1 and 4:4: 2. However, in order to obtain more reversible capacity, the development direction of ternary materials tends to increase the content of ternary materials, such as 532, 622, 721, 811, etc.
In order to improve the cycle performance of the ternary cathode material, a surface modification method is mostly adopted at present, namely, a stable thin film substance is coated on the surface of the cathode material, and a modification layer with proper thickness and uniformity can improve the electronic conductivity, reduce the corrosion of electrolyte to cathode active substances, protect the material structure, and inhibit the boundary of the electrolyte under high voltage, thereby improving the cycle stability and the rate performance of the cathode material. After coating modification, the charge and discharge capacity of the battery is improved to different degrees, the cycle performance is greatly improved, and especially under high temperature and high rate, the battery capacity attenuation is obviously reduced after multiple cycles. At present, most of researches for improving the high-temperature cycle performance of the ternary composite material positive pole piece mainly focus on modifying the surface of the positive pole material, such as those described in chinese patent publications with publication numbers CN108682822A, CN108682822A, CN108807950A and CN 108987681A.
The ternary cathode material NCM811 has excellent comprehensive properties such as high energy density, good cycle performance, moderate price and the like, and is the most promising cathode material in the current Lithium Ion Batteries (LIBs). However, in the conventional battery system, the ternary cathode material can undergo drastic structural change and interface side reaction at high voltage and high temperature, which brings great challenges to practical application, especially the cycle life and safety of the ternary material. Therefore, it is important to find a method for improving the structural stability, high temperature and high pressure performance of the ternary material.
Disclosure of Invention
The invention aims to provide a ternary positive pole piece with better high-temperature cycling stability and excellent electrochemical performance.
The invention also aims to provide a method for improving the high-temperature cycle performance of the positive pole piece.
The surface of the ternary positive pole piece provided by the invention is coated with a liquid crystal film, and the liquid crystal film is made of a material formed by mixing Hexacyanoferrate (HBC) disc-shaped liquid crystal and triphenylene disc-shaped liquid crystal to form a binary CPI (complementary polytopic interaction).
Discotic liquid crystals are liquid crystal phases that are represented by discotic molecules. Discotic liquid crystal molecules are generally composed of a rigid central core portion having a large benzene ring planar structure or a nearly planar structure and a plurality of flexible side chains attached to the periphery. The rigid core is mainly anthraquinone, phthalocyanine, ethynylbenzene, benzophenanthrene, porphyrin, hexabenzocoronene and the like.
Hexabenzocoronene (HBC) has a large pi-conjugated structure, consists of 13 inlaid benzene rings, and has D6hSymmetry, also known as "super benzene". The binary CPI formed by mixing the hexacyanoferrate discotic liquid crystal and the triphenylene discotic liquid crystal is very superior in the performances of order, carrier mobility and the like, and after the binary CPI is coated on the surface of the positive pole piece, the coating layer on the surface can keep the stability of the positive pole piece structure, effectively improve the interface contact of the positive pole and the electrolyte, improve the ion transmission capability at the interface and prevent Ni from being in contact with the positive pole piece and the electrolyte+And Mn2+And (4) precipitating. The liquid crystal film meets the requirement of flexible processing of the battery pole piece.
The ternary positive pole piece is prepared from a ternary positive pole material, an adhesive and a conductive agent.
Optionally or preferably, in the ternary positive electrode plate, the thickness of the liquid crystal film is 0.1-50.0 nm.
Optionally or preferably, in the ternary positive electrode plate, the thickness of the liquid crystal film is 1.0-10.0 nm.
Optionally or preferably, in the ternary positive electrode plate, the hexabenzocoronene discotic liquid crystal is a phenyl-coupled hexabenzocoronene (HBC-Ph) discotic liquid crystal, and the triphenylene discotic liquid crystal is a Hexaalkoxytriphenylene (HAT) discotic liquid crystal.
The benzene-coupled hexabenzocoronene discotic liquid crystal and hexaoxyalkyltriphenylene discotic liquid crystal are mixed to form the binary CPI. The liquid crystal film has good toughness and strong ion conduction capability, and the existence of the liquid crystal film can effectively protect the SEI film on the surface of the anode from being damaged in the charging and discharging processes; when the thickness of the liquid crystal film is controlled to be a specific value, the thickness of the whole SEI + liquid crystal film can be minimized, and the cycle performance of the battery cell is not influenced; at the moment, the minimum irreversible capacity consumed in the formation process can be realized, and the purposes of improving the first efficiency, reversible capacity and energy density of the battery cell are finally achieved.
Optionally or preferably, in the ternary positive electrode plate, the molecular structure of the phenyl-coupled hexabenzocoronene-like discotic liquid crystal is HBC-PhCn(n-10-12). The hexaalkoxy benzophenanthrene discotic liquid crystal molecular structure is HAT-Cn(n＝2-7)。
Optionally or preferably, the liquid crystal film of the ternary positive electrode plate is formed by mixing two phenyl-coupled hexabenzocoronene disc-shaped liquid crystals and triphenylene, and the mass ratio of the two liquid crystals is 1:1-1:10, so that a binary CPI is formed.
Optionally or preferably, the ternary positive electrode plate is prepared from a ternary positive electrode material, an adhesive and a conductive agent, and the ternary positive electrode material is a ternary composite material NCM811, NCM523, NCM721, NCM333 or NCM 622. Namely, the mass ratios of Ni, Mn and Co in the ternary composite material are respectively 8:1:1, 5:2:3, 7:2:1, 3:3:3 and 6:2: 2.
Optionally or preferably, in the ternary positive electrode plate, the binder is PVDF (polyvinylidene fluoride), and the conductive agent is acetylene black.
The invention also provides a method for improving the high-temperature cycle performance of the positive pole piece, which is characterized in that hexabenzocoronene disc-shaped liquid crystal and triphenylene disc-shaped liquid crystal are sprayed on the surface of the positive pole piece and mixed to form double-body CPI liquid crystal liquid, and a liquid crystal film coated on the surface of the positive pole piece is formed; the positive pole piece is a ternary positive pole piece.
Optionally or preferably, the method comprises the following specific steps: accurately weighing a mixed material of hexabenzocoronene disc-shaped liquid crystal and triphenylene disc-shaped liquid crystal in a flask according to a certain design proportion, heating to dissolve, cooling to just above a clearing point of the liquid crystal material to obtain liquid crystal liquid, spraying the liquid crystal liquid to the surface of a ternary positive pole piece, and forming a liquid crystal film at room temperature.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the purpose of improving the high-temperature cycle performance can be achieved by directly spraying liquid crystal on the outer surface of the positive pole piece to form a liquid crystal film without coating and modifying the positive pole material, and the product has a simple structure and is easy to manufacture.
The positive pole piece with the surface coated with the liquid crystal film has smaller overall impedance and better high-temperature cycle performance, and the coating layer on the surface can keep the stability of the positive pole piece structure and can not prevent Li+Is being migrated. Not only reduces the oxidation rate of the electrolyte on the surface of the anode, but also improves the electrochemical performance of the ternary material under high voltage.
Drawings
Fig. 1 is a graph of the cycle comparison of the cells of example 2 and comparative example 1 at 55 ℃.
Detailed Description
The technical solutions of the present invention are described in detail below with reference to specific examples, so that those skilled in the art can better understand the present invention and implement the present invention.
Example 1
The ternary positive electrode material is prepared by mixing PVDF (polyvinylidene fluoride) and acetylene black in a certain ratio, taking NMP (N-methyl pyrrolidone) as a solvent of the PVDF, and performing the working procedures of coating, drying, tabletting and the like.
Preparing a liquid crystal mixed solution: weighing HBC-C according to the mass ratio of 1:1010And HAT-C2The mixture was placed in a flask and mixed on a magnetic stirrer with a heating temperature control device. The mixed liquid crystal is heated to be completely dissolved, and after stirring, the temperature is reduced to be just above the clearing point. And continuously stirring at constant temperature to obtain the mixed liquid crystal.
And uniformly spraying liquid crystal liquid on the surface of the positive pole piece, and forming a liquid crystal state film by the mixed liquid at room temperature. The thickness of the liquid crystal film was 1 nm. And then winding or laminating the prepared positive pole piece, the prepared negative pole piece and the prepared isolating film to obtain the bare cell. And (4) loading the naked electric core into a steel shell.
And adding the electrolyte into the steel shell to soak the bare cell, and assembling the battery. The cells were tested at 55 ℃ and the cycling program was 1C charged to 4.3V and 1C discharged to 2.5V.
Example 2
The positive electrode sheet was prepared as in example 1.
Preparing a liquid crystal mixed solution: weighing HBC-PhC according to the mass ratio of 1:114And HAT-C7The mixture was placed in a flask and mixed on a magnetic stirrer with a heating temperature control device. The mixed liquid crystal is heated to be completely dissolved, and after stirring, the temperature is reduced to be just above the clearing point. And continuously stirring at constant temperature to obtain the mixed liquid crystal.
And uniformly spraying liquid crystal liquid on the surface of the positive pole piece, and forming a liquid crystal state film by the mixed liquid at room temperature. The thickness of the liquid crystal film was 10 nm. And then winding or laminating the prepared positive pole piece, the prepared negative pole piece and the prepared isolating film to obtain the bare cell. And (4) loading the naked electric core into a steel shell.
And adding the electrolyte into the steel shell to soak the bare cell, and assembling the battery. The cells were tested at 55 ℃ and the cycling program was 1C charged to 4.3V and 1C discharged to 2.5V.
Example 3
The positive electrode sheet was prepared as in example 1.
Preparing a liquid crystal mixed solution: weighing HBC-C according to the mass ratio of 1:112And HAT-C6The mixture was placed in a flask and mixed on a magnetic stirrer with a heating temperature control device. The mixed liquid crystal is heated to be completely dissolved, and after stirring, the temperature is reduced to be just above the clearing point. And continuously stirring at constant temperature to obtain the mixed liquid crystal.
And uniformly spraying liquid crystal liquid on the surface of the positive pole piece, and forming a liquid crystal state film by the mixed liquid at room temperature. The thickness of the liquid crystal film was 0.1 nm. And then winding or laminating the prepared positive pole piece, the prepared negative pole piece and the prepared isolating film to obtain the bare cell. And (4) loading the naked electric core into a steel shell.
And adding the electrolyte into the steel shell to soak the bare cell, and assembling the battery. The cells were tested at 55 ℃ and the cycling program was 1C charged to 4.3V and 1C discharged to 2.5V.
Example 4
The positive electrode sheet was prepared as in example 1.
Preparing a liquid crystal mixed solution: weighing HBC-C according to the mass ratio of 1:510And HAT-C3The mixture was placed in a flask and mixed on a magnetic stirrer with a heating temperature control device. The mixed liquid crystal is heated to be completely dissolved, and after stirring, the temperature is reduced to be just above the clearing point. And continuously stirring at constant temperature to obtain the mixed liquid crystal.
And uniformly spraying liquid crystal liquid on the surface of the positive pole piece, and forming a liquid crystal state film by the mixed liquid at room temperature. The thickness of the liquid crystal film was 50 nm. And then winding or laminating the prepared positive pole piece, the prepared negative pole piece and the prepared isolating film to obtain the bare cell. And (4) loading the naked electric core into a steel shell.
And adding the electrolyte into the steel shell to soak the bare cell, and assembling the battery. The cells were tested at 55 ℃ and the cycling program was 1C charged to 4.3V and 1C discharged to 2.5V.
Example 5
The positive electrode sheet was prepared as in example 1.
Preparing a liquid crystal mixed solution: weighing HBC-C according to the mass ratio of 1:514And HAT-C6The mixture was placed in a flask and mixed on a magnetic stirrer with a heating temperature control device. The mixed liquid crystal is heated to be completely dissolved, and after stirring, the temperature is reduced to be just above the clearing point. And continuously stirring at constant temperature to obtain the mixed liquid crystal.
And uniformly spraying liquid crystal liquid on the surface of the positive pole piece, and forming a liquid crystal state film by the mixed liquid at room temperature. The thickness of the liquid crystal film was 5 nm. And then winding or laminating the prepared positive pole piece, the prepared negative pole piece and the prepared isolating film to obtain the bare cell. And (4) loading the naked electric core into a steel shell.
And adding the electrolyte into the steel shell to soak the bare cell, and assembling the battery. The cells were tested at 55 ℃ and the cycling program was 1C charged to 4.3V and 1C discharged to 2.5V.
Comparative example 1
The positive electrode sheet was prepared as in example 1.
And winding or laminating the prepared anode sheet, the cathode sheet and the isolating film at room temperature to obtain the bare cell. And (4) loading the naked electric core into a steel shell.
And adding the electrolyte into the steel shell to soak the bare cell, and assembling the battery. And adding the electrolyte into the steel shell to soak the bare cell, and assembling the battery. The cells were tested at 55 ℃ and the cycling program was 1C charged to 4.3V and 1C discharged to 2.5V.
The results of the cycling capacity test for each example and comparative example, and the calculated first cell efficiencies are as follows:
please refer to table 1, which shows the first effective value, 80% cycle number of capacity remained and 80% ac impedance value of capacity remained of the battery cell at 55 ℃ for comparison between the examples and the comparative examples. The detection result shows that after the liquid crystal film is sprayed, the coulombic efficiency is improved for the first time, the high-temperature cycle number of 80 percent conservation rate is increased, the impedance is reduced after high-temperature cycle, and the high-temperature cycle performance is obviously improved on the whole. Especially, when the thickness of the liquid crystal film is 5nm, various performances are best.
Please refer to the cycle comparison chart of the cells of example 2 and comparative example 1 at 55 ℃ shown in fig. 1. As can be seen from the figure, the cell coated with the liquid crystal state film has better high temperature cycle stability than comparative example 1.
The results of the test data of each example are shown in table 1 below:
TABLE 1
The inventive concept is explained in detail herein using specific examples, which are given only to aid in understanding the core concepts of the invention. It should be understood that any obvious modifications, equivalents and other improvements made by those skilled in the art without departing from the spirit of the present invention are included in the scope of the present invention.
Claims (7)
1. The ternary positive pole piece is characterized in that the surface of the positive pole piece is coated with a liquid crystal film, and the liquid crystal film is made of a material formed by mixing hexacenzocardamom disc-shaped liquid crystal and triphenylene disc-shaped liquid crystal to form a binary CPI; the hexabenzocoronene-like discotic liquid crystal is phenyl-coupled hexabenzocoronene-like discotic liquid crystal, and the triphenylene discotic liquid crystal is hexaalkoxytriphenylene discotic liquid crystal;
the coating method comprises the following steps:
weighing a mixed liquid crystal material of the hexabenzocoronene discotic liquid crystal and the triphenylene discotic liquid crystal according to a certain proportion, heating and dissolving, then cooling to be just above a clearing point of the liquid crystal material to obtain liquid crystal liquid, spraying the liquid crystal liquid to the surface of the ternary positive pole piece, and forming a liquid crystal film at room temperature.
2. The ternary positive electrode sheet according to claim 1, wherein the thickness of the liquid crystal film is 0.1 to 50.0 nm.
3. The ternary positive electrode sheet according to claim 2, wherein the thickness of the liquid crystal film is 1.0 to 10.0 nm.
4. The ternary positive electrode plate according to claim 1, wherein the mass ratio of the phenyl-coupled hexabenzocoronene-like discotic liquid crystal to the hexaalkoxytriphenylene discotic liquid crystal is 1:1-1: 10.
5. The ternary positive electrode plate according to claim 1, wherein the molecular structure of the phenyl-coupled hexabenzocoronene-like discotic liquid crystal is HBC-PhCnN is 10-12; the molecular structure of the hexa-alkoxy benzophenanthrene discotic liquid crystal is HAT-Cn，n＝2-7。
6. The ternary positive pole piece according to claim 1, wherein the positive pole piece is prepared from a ternary positive pole material, an adhesive and a conductive agent, and the ternary positive pole material is a ternary composite material NCM811, NCM523, NCM721, NCM333 or NCM 622.
7. The ternary positive electrode sheet according to claim 6, wherein the binder is PVDF and the conductive agent is acetylene black.
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| WO2019017846A1 (en) * | 2017-07-20 | 2019-01-24 | Agency For Science, Technology And Research | Hexaazatriphenylene derivative and graphene oxide composites |
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| CN1154102A (en) * | 1994-06-27 | 1997-07-09 | 巴斯福股份公司 | Oligomer liquid crystal triphenylene derivatives and their use as charge carrying substances in electrophoto-graphy |
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