CN113421995A - Gel-state electrode and preparation method thereof - Google Patents

Gel-state electrode and preparation method thereof Download PDF

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CN113421995A
CN113421995A CN202110703022.4A CN202110703022A CN113421995A CN 113421995 A CN113421995 A CN 113421995A CN 202110703022 A CN202110703022 A CN 202110703022A CN 113421995 A CN113421995 A CN 113421995A
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electrode
gel
state
active material
polymer
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CN113421995B (en
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吴洁
朱蕾
田文生
赵玉辉
韩松益
国洪遥
吴勇民
汤卫平
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Shanghai Institute of Space Power Sources
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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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0407—Methods of deposition of the material by coating on an electrolyte layer
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • 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
    • H01M4/624—Electric conductive fillers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a gel-state electrode and a preparation method thereof, wherein the electrode comprises: electrode active materials, conductive agents, SN, lithium salts, polymers, and additives; the preparation method comprises dissolving lithium salt and additive in SN at 60-80 deg.C, adding polymer, stirring thoroughly to dissolve to form gel state substance; then, the prepared gel state substance, electrode active material and conductive agent are mixed, and after being uniformly stirred or ground, the gel state substance, the electrode active material and the conductive agent are coated on one side of the solid electrolyte to be used as a gel state electrode of the solid-state battery. Whether or not to perform the crosslinking treatment is determined according to the type of the polymer added. The lithium salt can be completely dissolved in SN to form plastic crystal electrolyte, and the selected polymer can be dissolved with the plastic crystal electrolyte. The gel-state electrode provided by the invention can improve the contact performance between the electrode and the solid electrolyte, improve the ion transmission in the electrode and inhibit the negative effect of the volume change of the electrode active material in the charging and discharging process on the battery performance.

Description

Gel-state electrode and preparation method thereof
Technical Field
The invention relates to the technical field of electrochemistry and new energy materials, in particular to a gel-state electrode and a preparation method thereof.
Background
Currently, among various commercial batteries, a lithium ion battery is the battery having the highest energy density, and is widely used in various electronic devices. The rapid development of electric vehicles and large-scale energy storage systems places higher demands on the energy density and safety of lithium ion batteries. However, the conventional lithium ion battery adopts an organic electrolyte, so that the safety risk of liquid leakage, combustion and even explosion exists, the electrochemical window is narrow, and when lithium metal is adopted as a negative electrode, the problem of lithium dendrite is serious, and the safety and the energy density of the lithium ion battery are limited to be improved.
The solid electrolyte has a wider electrochemical window, is not flammable, has high mechanical strength, and can inhibit the growth of lithium dendrites. Therefore, the development of the all-solid-state battery by adopting the solid electrolyte to replace the organic electrolyte is expected to greatly improve the energy density and the safety. However, due to the solid properties, the solid electrolyte has poor contact with the electrode, and the solid electrolyte cannot penetrate into the electrode as well as the organic electrolyte, which greatly affects the capacity exertion, rate capability and cycle life of the electrode material in the solid-state battery.
In order to improve ion transport inside the electrode, composite electrodes have been developed for use in solid-state batteries. In CN201910808588.6, mubin et al add nanoparticles of solid electrolyte to the positive electrode to prepare a composite positive electrode, and construct a dual ion transport channel, which is beneficial to ion transport during charge and discharge. Zhenhao et al prepared a composite electrode in CN201910074271.4, and added LLZO solid electrolyte, and sintered to form an ion conductive layer at the interface between the positive electrode active material and the LLZO particles, thereby reducing the internal resistance of the composite positive electrode. Although these methods have some effect in promoting ion transport inside the electrode, the ion transport speed inside the electrode is still not ideal due to the solid-solid contact characteristics of the solid electrolyte particles and the active material particles, and the composite electrode prepared is in a solid form, not only does not effectively suppress volume change of the electrode, but also is not favorable for interfacial contact between the electrode and the solid electrolyte. In addition, a large amount of organic solvent is needed in the preparation of the conventional electrode, so that the environment is polluted, the raw material cost is increased, the production time is increased due to the drying of the solvent, and the production efficiency is reduced.
Disclosure of Invention
The object of the present invention is to prepare a gel-state electrode having good ion transport properties without using an organic solvent, to improve the internal ion transport of the electrode in a solid-state battery and the contact between a solid electrolyte and the electrode, thereby promoting the exertion of the capacity of the electrode material in the solid-state battery, the rate capability and the improvement of the cycle life. The room temperature ionic conductivity of the nitrile-based plastic crystal electrolyte is extremely high and can reach 10-3Of the order of S/cm, and has good thermal stability and non-flammability. The deformable nitrile plastic crystal electrolyte is added into the electrode material to prepare the gel-state electrode, so that the interface contact between the solid electrolyte and the electrode can be improved, the volume change of an electrode active material in the charge-discharge process can be relieved, and the ion transmission in the electrode can be promoted.
In order to achieve the above object, the present invention provides a gel state electrode comprising: electrode active materials, conductive agents, plastic crystal molecules, Succinonitrile (SN), lithium salts, polymers and additives; the lithium salt can be completely dissolved in the butanedinitrile to form a plastic crystal electrolyte; the polymer is dissolved with the plastic crystal electrolyte; wherein the mass fraction of the electrode active material in the gel electrode is 10-90%; the mass fraction of the conductive agent in the gel-state electrode is 5-20%; the total mass of the polymer, the butadiene-dinitrile plastic-crystal electrolyte and the additive accounts for 5-85% of the mass of the composite electrode; the lithium salt accounts for 0-30% of the mol fraction of the succinonitrile; the mass ratio of the polymer to the butadiene-dinitrile plastic crystal electrolyte is 1: 50-2: 1; the mass fraction of the additive in the butadiene-acrylonitrile plastic crystal electrolyte is 0-15%.
Optionally, the electrode active material comprises: a positive electrode material active material and/or a negative electrode material active material, wherein the positive electrode material active material is selected from LiCoO2、LiNi0.8Co0.1Mn0.1O2(NCM811)、LiFePO4Any one or a combination of any two or more of them, and the negative electrode material active material is Li4Ti5O12(ii) a The mass fraction of the electrode active material in the gel electrode is 20-80%.
Optionally, the conductive agent includes one or more of conductive carbon black SP, graphite, ketjen black, and Carbon Nanotubes (CNTs), and the mass fraction of the conductive agent in the gel electrode is 5-15%.
Optionally, the lithium salt comprises LiClO4、LiTFSI、LiBOB、LiPF6And LiFSI.
Optionally, the lithium salt comprises 1-20% of succinonitrile by mole.
Optionally, the polymer comprises one or more of polyvinyl alcohol (PVA), polyethylene oxide (PEO), cyanoethylated polyvinyl alcohol (PVA-CN), ethoxylated trimethylolpropane triacrylate (ETPTA), and the like.
Optionally, the mass ratio of the polymer to the butadiene-acrylonitrile plastic crystal electrolyte is 1: 50-1: 2.
Optionally, the additive comprises fluoroethylene carbonate (FEC) which accounts for 1-10% of the mass fraction of the butadiene-based plastocytic electrolyte and mainly acts to improve the electrochemical oxidation resistance of components other than the electrode active material.
Optionally, the total mass of the polymer, the butadiene-nitrile plastic crystal electrolyte and the additive accounts for 15-80% of the mass of the composite electrode.
The invention also provides a method for preparing the gel-state electrode, which comprises the following steps:
step 1, dissolving lithium salt and an additive in succinonitrile at 60-80 ℃ (heating is to melt the succinonitrile and promote the uniform mixing of the components, but the temperature is too high, the additive can be evaporated), adding a polymer, and fully stirring and mixing to obtain a gel-state substance;
step 2, adding the gel-state substance obtained in the step 1 into an electrode active material and a conductive agent, and uniformly stirring or grinding;
and 3, coating the mixture obtained by uniformly stirring in the step 2 on one side of the solid electrolyte, and optionally performing polymer crosslinking treatment to obtain the gel-state electrode.
The gel-state substance prepared from the polymer has better viscosity, not only can be used as a binder of an electrode, but also can enhance the contact between the electrode and a solid electrolyte. The in-situ crosslinking treatment is carried out on the electrode on the solid electrolyte, so that the interface contact between the electrode and the solid electrolyte can be further improved, the interface impedance is reduced, and the mechanical strength of the electrode can also be improved.
The invention has the following technical effects:
(1) compared with the traditional method for preparing the electrode, the preparation of the gel-state electrode provided by the invention does not need to use an organic solvent, thereby avoiding the environmental pollution and the increase of the raw material cost.
(2) In the preparation method, the gel-state substance prepared in the step 1 can form an ion conductor with high ionic conductivity due to the existence of plastic crystal succinonitrile (a butadiene-dinitrile plastic crystal electrolyte), so that the ion transmission in the gel-state electrode can be promoted, and the rate capability of the solid-state battery can be improved.
(3) Compared with the traditional solid electrode, the gel-state electrode can improve the interface contact between the electrode and the solid electrolyte, and because the gel-state substance has elastic deformation capacity, the gel-state electrode has large contact area with the electrode material, thereby being beneficial to the formation of a continuous ion channel network in the electrode and relieving the problem caused by the volume change of the electrode active material in the charging and discharging process.
Drawings
Fig. 1 is a room temperature ac impedance spectrum of a gel state material consisting of LiTFSI, succinonitrile, FEC and PEO prepared in example 1.
FIG. 2 is a linear sweep voltammogram of the gel state material prepared in example 1, with a sweep rate of 0.1 mV/s.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a gel state electrode comprising: the electrode comprises an electrode active material, a conductive agent, plastic crystal molecules, namely Succinonitrile (SN), lithium salt, a polymer and an additive.
The lithium salt can be completely dissolved in the butanedinitrile to form a plastic crystal electrolyte; the polymer is dissolved with the plastic crystal electrolyte.
The mass fraction of the electrode active material in the gel electrode is 10-90%, preferably 20-80%. The electrode active material includes: a positive electrode material active material and/or a negative electrode material active material, wherein the positive electrode material active material is selected from LiCoO2、LiNi0.8Co0.1Mn0.1O2(NCM811)、LiFePO4Any one or a combination of any two or more of them, and the negative electrode material active material is Li4Ti5O12。
The conductive agent comprises one or more of SP, graphite, Ketjen black and CNT, and accounts for 5-20% by mass of the gel-state electrode, preferably 5-15% by mass of the gel-state electrode.
The total mass of the polymer, the butadiene-dinitrile plastic-crystal electrolyte and the additive accounts for 5-85 percent of the mass of the gel-state electrode, and the mass percent is preferably 15-80 percent.
The lithium salt comprises LiClO4、LiTFSI、LiBOB、LiPF6And LiFSI, the lithium salt accounts for 0-30% of the molar fraction of the succinonitrile, and preferably 1-20%.
The polymer comprises one or more of polyvinyl alcohol (PVA), polyethylene oxide (PEO), cyanoethylated polyvinyl alcohol (PVA-CN), ethoxylated trimethylolpropane triacrylate (ETPTA) and the like. The mass ratio of the polymer to the butadiene-dinitrile plastic crystal electrolyte is 1: 50-2: 1, preferably 1: 50-1: 2; the additive can be fluoroethylene carbonate (FEC), and the mass fraction of the fluoroethylene carbonate (FEC) in the butadiene-acrylonitrile plastic crystal electrolyte is 0-15%, preferably 1-10%.
The invention also provides a method for preparing the gel-state electrode, which comprises the following steps:
step 1, dissolving lithium salt and an additive in succinonitrile at 60 ℃, adding a polymer, and fully stirring and mixing to obtain a gel-state substance;
step 2, adding the gel-state substance obtained in the step 1 into an electrode active material and a conductive agent, and uniformly stirring or grinding;
and 3, coating the mixture obtained by uniformly stirring in the step 2 on one side of the solid electrolyte, and optionally performing polymer crosslinking treatment to obtain the gel-state electrode. When the crosslinking treatment is needed, the selected crosslinking mode is photo-crosslinking or thermal crosslinking.
The following examples are given for illustrative purposes.
Example 1
At 60 ℃, 5 mol% of LiTFSI is dissolved in succinonitrile to prepare the nitrile-based plastic crystal electrolyte, then 7 wt% of FEC is added, PEO (polyethylene oxide) is added after full and uniform stirring. The mass ratio of the PEO to the butadiene-nitrile plastic crystal electrolyte is 1: 20.After sufficiently stirring and dissolving, a transparent gel-state ion-conductive substance was obtained. In LiCoO2Adding 35 wt% of gel state substance into 10 wt% of SP, grinding uniformly, and coating the composite anode slurry on Li uniformly6.4La3Zr1.4Ta0.6O12And sticking an aluminum foil as a current collector on one side of the ceramic wafer, and standing in an oven at 60 ℃ for a period of time. The mass of the composite positive electrode can be obtained by weighing the mass of the ceramic sheet before and after coating.
According to FIG. 1 and the formula σ ═ L/(R · S), where L, R and S are the thickness (0.6mm), impedance and cross-sectional area (0.50 cm) of the gel state substance prepared in example 1, respectively2) The room-temperature ionic conductivity of the gel-state material prepared in example 1 was 2.18X 10-3S/cm, and the high ionic conductivity of the solid-state battery is favorable for promoting the ion transmission in the electrode and improving the rate capability of the solid-state battery.
Fig. 2 shows that the electrochemical stability window of the gel-state material prepared in example 1 is as high as-4.6V, and the gel-state material can be used with a high-voltage cathode material.
Example 2
At 60 ℃, 5 mol% of LiTFSI is dissolved in succinonitrile to prepare the nitrile-based plastic crystal electrolyte, then 5 wt% of FEC is added, and PEO is added after full and uniform stirring. The mass ratio of the PEO to the butadiene-nitrile plastic crystal electrolyte is 1: 20. After sufficiently stirring and dissolving, a transparent gel-state ion-conductive substance was obtained. In LiCoO2Adding 45 wt% of gel state substance into 10 wt% of SP, grinding uniformly, and coating the composite anode slurry on Li uniformly6.4La3Zr1.4Ta0.6O12And (3) sticking a stainless steel net on one side of the ceramic plate as a current collector, and standing in a 60 ℃ oven for a period of time.
Example 3
At 60 ℃, 5mol percent of LiTFSI and 1mol percent of LiPF are added6Dissolving in succinonitrile to prepare the nitrile-based plastic crystal electrolyte, and then adding 5 wt% of FEC. After stirring well, cyanoethylated polyvinyl alcohol (PVA-CN) was added at 50 ℃. The PVA-CN accounts for 5 percent of the mass fraction of the butyronitrile-based plastic crystal electrolyteAfter sufficiently stirring and dissolving, 50 wt% LiCoO was added2Uniformly grinding the powder and 10 wt% of SP, and uniformly coating the composite anode slurry on Li6.4La3Zr1.4Ta0.6O12And an aluminum foil is pasted on one side of the ceramic plate to be used as a current collector. Then, the PVA-CN was crosslinked by heat treatment at 70 ℃ for 6 hours in an oven.
Due to the similarity of the structure, PVA-CN is easily dissolved in the molten nitrile plastic crystal electrolyte. During the heat treatment, LiPF6PF produced by decomposition5Crosslinking of the PVA-CN can be initiated.
In conclusion, the deformable nitrile plastic crystal electrolyte is added into the traditional solid-state electrode, so that the contact effect between the solid electrolyte and the electrode is improved, the volume change of an electrode active material in the charging and discharging process is relieved, the ion transmission in the electrode is promoted, and the capacity exertion, the rate capability and the cycle life of the electrode material in the solid-state battery are improved.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.

Claims (10)

1. A gel state electrode, comprising: the electrode comprises an electrode active material, a conductive agent, plastic crystal molecules, succinonitrile, lithium salt, a polymer and an additive; the lithium salt can be completely dissolved in the succinonitrile to form a succinonitrile-based plastic crystal electrolyte, and the polymer can be dissolved with the plastic crystal electrolyte.
2. A gel state electrode according to claim 1, wherein said electrode active material comprises LiCoO as a positive electrode2、LiNi0.8Co0.1Mn0.1O2(NCM811)、LiFePO4Any one or more of the positive electrode materials; when used as a negative electrode, the electrode active material includes Li4Ti5O12A negative electrode material;
the mass fraction of the electrode active material in the gel electrode is 10 to 90%, preferably 20 to 80%.
3. The gel state electrode of claim 1, wherein said conductive agent comprises one or more of SP, graphite, ketjen black, CNT;
the mass fraction of the conductive agent in the gel-state electrode is 5-20%, preferably 5-15%.
4. A gel state electrode according to claim 1, characterized in that the total mass fraction of the polymer, the nitrile plastic crystal electrolyte and the additives in the composite electrode is 5-85%, preferably 15-80%.
5. The gel electrode of any one of claims 1 to 4, wherein said lithium salt comprises LiClO4、LiTFSI、LiBOB、LiPF6And LiFSI, the lithium salt accounts for 0-30% of the molar fraction of the succinonitrile, and preferably 1-20%.
6. The gel electrode according to any one of claims 1 to 4, wherein the polymer comprises one or more of polyvinyl alcohol, polyethylene oxide, cyanoethylated polyvinyl alcohol, and ethoxylated trimethylolpropane triacrylate;
the mass ratio of the polymer to the butadiene-acrylonitrile plastic crystal electrolyte is 1: 50-2: 1, preferably 1: 50-1: 2.
7. A gel state electrode according to any one of claims 1 to 4 wherein the additive comprises fluoroethylene carbonate;
the mass fraction of the additive in the butadiene-acrylonitrile plastic crystal electrolyte is 0-15%, preferably 1-10%.
8. The gel state electrode according to claim 1, which has a deformability similar to that of plasticine, improves interfacial contact performance with a solid electrolyte, and alleviates adverse effects caused by volume change during charge and discharge of an electrode active material.
9. The gel state electrode of claim 1, prepared without the use of N-methyl pyrrolidone organic solvents.
10. A method of preparing a gel state electrode according to any one of claims 1 to 9, comprising the steps of:
step 1, dissolving lithium salt and an additive in succinonitrile at 60-80 ℃, adding a polymer, and fully stirring and mixing to obtain a gel-state substance;
step 2, adding the gel-state substance obtained in the step 1 into an electrode active material and a conductive agent, and uniformly stirring or grinding;
and 3, coating the mixture obtained by uniformly stirring in the step 2 on one side of the solid electrolyte, and optionally performing polymer crosslinking treatment to obtain the gel-state electrode.
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CN115882057A (en) * 2022-09-23 2023-03-31 四川新能源汽车创新中心有限公司 Electrolyte, solid-state battery and preparation method thereof

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CN114759269A (en) * 2022-05-18 2022-07-15 电子科技大学 Integrated all-solid-state battery based on ceramic-based electrolyte sheet and preparation method
CN115882057A (en) * 2022-09-23 2023-03-31 四川新能源汽车创新中心有限公司 Electrolyte, solid-state battery and preparation method thereof
CN115882057B (en) * 2022-09-23 2023-09-08 四川新能源汽车创新中心有限公司 Electrolyte, solid-state battery and preparation method of solid-state battery

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