CN114975994A - Low-temperature quick-charging lithium ion battery cathode material and preparation method and application thereof - Google Patents

Low-temperature quick-charging lithium ion battery cathode material and preparation method and application thereof Download PDF

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CN114975994A
CN114975994A CN202210691457.6A CN202210691457A CN114975994A CN 114975994 A CN114975994 A CN 114975994A CN 202210691457 A CN202210691457 A CN 202210691457A CN 114975994 A CN114975994 A CN 114975994A
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lithium ion
ion battery
low
negative electrode
electrode material
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CN114975994B (en
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王�华
程李巍
郭林
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Beihang University
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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • 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
    • H01M4/625—Carbon or graphite
    • 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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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a lithium ion battery cathode material capable of being rapidly charged and discharged at a low temperature, a preparation method and application thereof, and belongs to the technical field of electrochemical energy storage materials. The invention uses sulfur group elements including sulfur, selenium, tellurium and SxSe y 、S x Te y 、Se x Te y The chalcogenide material is used as a raw material, and the chalcogenide material is amorphized by a metal doping method, so that a novel amorphous sulfur-based lithium ion battery cathode material capable of being rapidly charged and discharged in a low-temperature environment is developed. The amorphous chalcogenide negative electrode material of the lithium ion battery can be rapidly charged and discharged within the temperature range of-60 ℃ to 60 ℃, and simultaneously shows higher specific charge-discharge capacity and cycling stability. The novel cathode can be matched with a cathode material and is applied to a low-temperature lithium ion battery full cell. The sulfur family material is rich in reserves, green and environment-friendly; the preparation process of the cathode material is simple, and the cost is lowLow cost and is suitable for large-scale production.

Description

Low-temperature quick-charging lithium ion battery cathode material and preparation method and application thereof
Technical Field
The invention relates to the technical field of energy storage materials, in particular to a low-temperature quick-charging lithium ion battery cathode material and a preparation method and application thereof.
Background
In recent years, electrochemical energy storage technology is widely applied along with the development of electric automobiles, power energy storage and portable electronic products. Among them, the lithium ion battery with high energy density, high power density and high cycle stability is the most mature energy storage mode at present, and is widely used in various industries.
However, a decrease in ambient temperature typically results in a decay of ion transport kinetics in the cell, with problems including a dramatic decrease in energy density, power density, and cycle life. The negative electrode material of the lithium ion battery has a vital influence on the performance of the battery at low temperature, the resistance of the traditional graphite negative electrode SEI film is increased under the low-temperature environment, the electrochemical polarization is obviously intensified, and Li + The diffusion rate in graphite is reduced, and metallic lithium is easily precipitated on the surface of the negative electrode, so that the traditional graphite negative electrode is not an ideal negative electrode material of a low-temperature lithium ion battery.
Compared with the traditional graphite cathode, the chalcogenide material has higher theoretical capacity, for example, the theoretical capacity of elemental sulfur is up to 1675mAh g -1 Meanwhile, the amorphous disordered structure is beneficial to promoting the transmission of ions, and the amorphous chalcogenide material is expected to be a potential low-temperature lithium ion negative electrode material capable of being rapidly charged and discharged.
Therefore, how to provide a lithium ion battery negative electrode material which can be rapidly charged and discharged in a low-temperature environment and has excellent energy density, excellent power density and excellent cycle stability, and a preparation method and application thereof are technical problems to be solved by those skilled in the art.
Disclosure of Invention
In view of this, the invention provides a lithium ion negative electrode material capable of being rapidly charged and discharged at a low temperature and a preparation method thereof. The negative electrode material can be reversibly charged and discharged in a temperature environment of-60 ℃ to 60 ℃, and has excellent rate performance and cycle stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
the lithium ion battery cathode material capable of being rapidly charged and discharged at low temperature comprises an active substance, wherein the active substance is obtained by doping 0.1-50% of metal in percentage by weight in a chalcogenide material.
Preferably, the chalcogenide material is selected from sulfur and seleniumTellurium, S x Se y 、S x Te y 、Se x Te y One of (1); the metal is any one of Cr, Mn, Fe, Co, Ni, Cu, Zn, Mo, Ru, Rh, Pd, Ag, Pt and Au, wherein the range of x is more than 0 and less than 1; the y range is 0 < y < 1.
More preferably, the metal-doped amorphous chalcogenide material is Fe-doped elemental sulfur.
Preferably, the negative electrode material further comprises a conductive agent and a binder, wherein the mass ratio of the active material to the conductive agent to the binder is (6-9.6): (0.2-2): (0.2-2).
More preferably, the mass ratio of the active material to the conductive agent to the binder is 7: 2: 1.
preferably, the conductive agent is one or more of SuperP, acetylene black, Ketjen black, conductive graphite, carbon nanotubes, graphene and carbon fibers.
More preferably, the conductive agent is SuperP.
Preferably, the binder is selected from one or more of polyvinylidene fluoride (PVDF), Polytetrafluoroethylene (PTFE), polyacrylic acid (PAA), carboxymethylcellulose/sodium carboxymethylcellulose (CMC), styrene butadiene rubber (GR-S), Sodium Alginate (SA), LA132 or gelatin.
More preferably, the binder is LA 132.
Another object of the present invention is to provide a method for preparing the above lithium ion battery negative electrode material capable of being rapidly charged and discharged at a low temperature, comprising the following steps:
s1, weighing each raw material in the anode material for later use;
s2, mixing the chalcogenide material with metal, adding water, and fully grinding to obtain an active substance;
s3, adding a conductive agent into the active substance, and continuously and fully grinding to uniformly mix the active substance and the conductive agent to obtain a first solid mixture;
s4, adding a binder into the solid mixture I, and continuously and fully grinding to uniformly mix the solid mixture I and the binder to obtain a solid mixture II;
s5, adding a solvent into the solid mixture II, continuously and fully grinding and uniformly mixing to obtain composite slurry;
and S6, coating the composite slurry on a copper current collector, and drying in vacuum to obtain the negative electrode material.
Preferably, the grinding time in steps S2-S5 is 30-60min, and the solvent in step S5 is deionized water.
More preferably, the grinding time in steps S2-S5 is 60 min.
The invention also aims to provide application of the low-temperature quick-charging lithium ion battery negative electrode material in a lithium ion battery.
Preferably, the lithium ion battery negative electrode material capable of being rapidly charged at low temperature can also be used for sodium ion batteries and potassium ion batteries.
Preferably, the lithium ion battery further comprises an electrolyte and a positive electrode material, wherein the electrolyte comprises a lithium salt, an organic solvent and an additive.
Preferably, the lithium salt is selected from the group consisting of LiTFSI, LiFSI, LiCF 3 SO 3 、LiPF 6 、LiClO 4 、LiNO 3 、LiBF 4 At least one of LiDFOB and LiBOB;
the organic solvent is at least one selected from dimethyl ether, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, polyethylene glycol dimethyl ether, ethylene glycol diethyl ether, diethylene glycol diethyl ether, 1,3 dioxolane, dioxane, tetrahydrofuran, 2-methyltetrahydrofuran, fluoroethylene carbonate, propylene carbonate, ethyl methyl carbonate, dimethyl carbonate, diethyl carbonate, ethylene carbonate and vinylene carbonate;
the additive is at least one of 1-10% by volume of 2,2, 2-trifluoroethyl-1, 1,2, 2-tetrafluoroethyl ether, 1,1,1,3,3, 3-hexafluoroisopropyl methyl ether, 1,1,2, 2-tetrafluoroethyl-2, 2,3, 3-tetrafluoropropyl ether and 1H,1H, 5H-octafluoropentyl-1, 1,2, 2-tetrafluoroethyl ether.
More preferably, the electrolyte comprises a solution of a LITFSI salt and DME, and the additive is 1 volume percent of 2,2, 2-trifluoroethyl-1, 1,2, 2-tetrafluoroethyl ether.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the chalcogenide material provided by the invention is rich in reserve, green and environment-friendly, and is a promising active material of a lithium ion battery.
2. The amorphous chalcogenide material doped with metal has an amorphous disordered structure which is beneficial to promoting the transmission of lithium ions, so that the amorphous chalcogenide material is a potential low-temperature lithium ion negative electrode material capable of being rapidly charged and discharged.
3. The metal-doped amorphous chalcogenide negative electrode material can be reversibly and rapidly charged and discharged within the temperature range of-60 ℃ to 60 ℃, and the charge and discharge multiplying power can reach 5 ℃ under the environment of-40 ℃.
4. The metal-doped amorphous chalcogenide negative electrode material has excellent energy density, excellent power density and excellent cycling stability at the low temperature of-40 ℃.
5. The preparation method provided by the invention is simple to operate, low in production cost, mature in technology, easy to industrialize and capable of being put into production without large amount of capital and technical investment. The preparation method of the amorphous chalcogenide-based anode material has a huge application prospect in the large-scale production process of the battery anode material.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a graph of the capacity of the negative electrode material of the present invention at different current densities at room temperature;
FIG. 2 is a charge-discharge curve of the negative electrode material of the present invention under room temperature conditions at different current densities;
FIG. 3 is a charge-discharge curve of the negative electrode material of the present invention at a low temperature of-40 ℃ and different current densities;
FIG. 4 is a cycle performance diagram of the negative electrode material of the present invention at-40 ℃ and 0.2 ℃.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
A lithium ion negative electrode material capable of being rapidly charged and discharged at low temperature comprises the following steps:
a. 99mg of elemental sulfur and 1mg of iron powder are added into a small amount of water and fully ground for 60min, and then the mixture is dried in a vacuum drying oven at 60 ℃ for 6h in vacuum, so that solid 1 is obtained.
b. 70mg of solid 1 were taken, 20mg of superP were added and milled for 60min, followed by 10mg of PAA and milling continued for 60 min.
c. And c, adding a small amount of deionized water as a solvent into the solid obtained in the step b, and fully stirring for 60min to obtain uniform cathode slurry.
d. And (c) uniformly coating the slurry obtained in the step (c) on a Cu current collector by using a scraper, and then putting the Cu current collector into a vacuum drying oven at 60 ℃ for drying for 12h to obtain the negative electrode 1.
Example 2
A lithium ion negative electrode material capable of being rapidly charged and discharged at low temperature comprises the following steps:
a. 95mg of selenium simple substance and 5mg of zinc powder are added into a small amount of water to be fully ground for 60min, and then the mixture is dried in a vacuum drying oven at 60 ℃ for 6h in vacuum, so that solid 2 is obtained.
b. 70mg of solid 1 are taken, 20mg of conductive graphite are added and ground for 60min, then 10mg of PTFE are added and grinding is continued for 60 min.
c. And c, adding a small amount of deionized water serving as a solvent into the solid obtained in the step b, and fully stirring for 60min or uniformly stirring the slurry.
d. And (c) uniformly coating the slurry obtained in the step (c) on a Cu current collector by using a scraper, and then putting the Cu current collector into a vacuum drying oven at 60 ℃ for drying for 12h to obtain the negative electrode 2.
Example 3
A lithium ion negative electrode material capable of being rapidly charged and discharged at low temperature comprises the following steps:
a. 99mg of elemental sulfur and 1mg of nickel powder are added into a small amount of water to be fully ground for 60min, and then the mixture is dried in a vacuum drying oven at the temperature of 60 ℃ for 6h in vacuum, so that solid 1 is obtained.
b. 80mg of the solid 1 is taken, 10mg of the carbon nano tubes are added and ground for 60min, and then 10mg of CMC is added and the grinding is continued for 60 min.
c. And c, adding a small amount of deionized water serving as a solvent into the solid obtained in the step b, and fully stirring for 60min or uniformly stirring the slurry.
d. And (c) uniformly coating the slurry obtained in the step (c) on a Cu current collector by using a scraper, and then putting the Cu current collector into a vacuum drying oven at 60 ℃ for drying for 12h to obtain a negative electrode 3.
Example 4
Carrying out room temperature electrochemical performance test on the cathode material
The negative electrode 1 and a lithium sheet are added with a diaphragm and electrolyte to be assembled into a half cell, wherein the diaphragm adopts a Celgard2325 diaphragm of a lithium ion cell; the electrolyte is prepared by dissolving 1M LiTFSI and 1% of 2,2, 2-trifluoroethyl-1, 1,2, 2-tetrafluoroethyl ether in DME.
The battery is subjected to a rate performance test at room temperature of 25 ℃, and the current density is 0.2C, 1C, 2C, 5C, 10C and 15C respectively, wherein 1C is 1675 mA/g. The capacity graph (figure 1) of the negative electrode material under the condition of room temperature under different current densities and the charge-discharge curve graph (figure 2) of the negative electrode material under the condition of room temperature under different current densities are obtained. As can be seen from the figure, the negative electrode material has the capacity of about 800mAh/g at 0.2C, the specific discharge capacity of about 400mAh/g at 15C, and the rapid charge and discharge performance is excellent.
Example 5
Carrying out temperature-changing electrochemical performance test on the cathode material
The negative electrode 1 and a lithium sheet are added with a diaphragm and electrolyte to be assembled into a half cell, wherein the diaphragm adopts a Celgard2325 diaphragm of a lithium ion cell; the electrolyte is prepared by dissolving 1M LiTFSI and 3 % volume content 2,2, 2-trifluoroethyl-1, 1,2, 2-tetrafluoroethyl ether in DME.
The battery was tested for rate capability at-40 ℃ with current densities of 0.1C, 1C, and 5C, respectively, to obtain the charge and discharge curves of the negative electrode material shown in fig. 3 at-40 ℃ under different current densities. As can be seen from the figure, when the current density is 5C, the negative electrode material can be reversibly charged and discharged under the low-temperature environment of-40 ℃, and the discharge specific capacity is as high as about 350mAh/g, which indicates that the negative electrode material is a lithium ion negative electrode material which can be rapidly charged and discharged at low temperature.
Example 6
The cycle performance of the negative electrode material is tested in a low-temperature environment of-40 DEG C
The negative electrode 1 and a lithium sheet are added with a diaphragm and electrolyte to be assembled into a half cell, wherein the diaphragm adopts a Celgard2325 diaphragm of a lithium ion cell; the electrolyte is prepared by dissolving 1M LiTFSI and 3 % volume content 2,2, 2-trifluoroethyl-1, 1,2, 2-tetrafluoroethyl ether in DME.
The battery is subjected to a cycle performance test at a current density of 0.2C in a low-temperature environment of-40 ℃. And obtaining a cycle performance diagram of the negative electrode material at the low temperature of-40 ℃ and 0.2C (figure 4). It can be seen from the figure that when the current density is 0.2C, the capacity of the negative electrode material is not obviously attenuated after 50 cycles of charge and discharge under the low temperature condition of-40 ℃, which indicates that the negative electrode material has excellent cycle stability in a low temperature environment.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. The low-temperature fast-chargeable lithium ion battery cathode material is characterized by comprising an active substance, wherein the active substance is obtained by doping 0.1-50% of metal in percentage by weight in a chalcogenide material.
2. The negative electrode material of low-temperature fast-chargeable lithium ion battery as claimed in claim 1, wherein the chalcogenide material is selected from sulfur, selenium, tellurium, and S x Se y 、S x Te y 、Se x Te y One of (1); the metal is one or more of Cr, Mn, Fe, Co, Ni, Cu, Zn, Mo, Ru, Rh, Pd, Ag, Pt and Au, wherein x is more than 0 and less than 1; the y range is 0 < y < 1.
3. The negative electrode material of the low-temperature fast-chargeable lithium ion battery as claimed in claim 2, further comprising a conductive agent and a binder, wherein the mass ratio of the active material to the conductive agent to the binder is (6-9.6): (0.2-2): (0.2-2).
4. The low-temperature fast-chargeable lithium ion battery cathode material as claimed in claim 3, wherein the conductive agent is one or more of SuperP, acetylene black, Ketjen black, conductive graphite, carbon nanotubes, graphene and carbon fibers.
5. The negative electrode material of the low-temperature fast-chargeable lithium ion battery as claimed in claim 3, wherein the binder is selected from one or more of polyvinylidene fluoride, polytetrafluoroethylene, polyacrylic acid, carboxymethyl cellulose/sodium carboxymethyl cellulose, styrene butadiene rubber, sodium alginate, LA132 or gelatin.
6. The preparation method of the negative electrode material of the low-temperature quick-charging lithium ion battery as claimed in any one of claims 3 to 5, characterized by comprising the following steps:
s1, weighing each raw material of claim 3 for later use;
s2, mixing the chalcogenide material with metal, adding water, and fully grinding to obtain an active substance;
s3, adding a conductive agent into the active substance, and continuously and fully grinding to uniformly mix the active substance and the conductive agent to obtain a first solid mixture;
s4, adding a binder into the solid mixture I, and continuously and fully grinding to uniformly mix the solid mixture I and the binder to obtain a solid mixture II;
s5, adding a solvent into the solid mixture II, continuously and fully grinding and uniformly mixing to obtain composite slurry;
and S6, coating the composite slurry on a copper current collector, and drying in vacuum to obtain the negative electrode material.
7. The method for preparing a low-temperature fast-chargeable lithium ion battery cathode material according to claim 6, wherein the grinding time in steps S2-S5 is 30-60min, and the solvent in step S5 is one of N-methylpyrrolidone and deionized water.
8. The use of the negative electrode material of a low-temperature fast-chargeable lithium ion battery as claimed in any one of claims 3 to 5 in a lithium ion battery.
9. The application of the negative electrode material of the low-temperature fast-charging lithium ion battery in the lithium ion battery as claimed in claim 8, wherein the lithium ion battery further comprises a positive electrode material and an electrolyte, and the electrolyte comprises a lithium salt, an organic solvent and an additive.
10. The use of the negative electrode material for a low-temperature fast-rechargeable lithium ion battery as claimed in claim 9, wherein the lithium salt is selected from the group consisting of LiTFSI, LiFSI, LiCF 3 SO 3 、LiPF 6 、LiClO 4 、LiNO 3 、LiBF 4 At least one of LiDFOB and LiBOB;
the organic solvent is at least one selected from ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, polyethylene glycol dimethyl ether, ethylene glycol diethyl ether, diethylene glycol diethyl ether, 1,3 dioxolane, dioxane, tetrahydrofuran, 2-methyltetrahydrofuran, fluoroethylene carbonate, propylene carbonate, ethyl methyl carbonate, dimethyl carbonate, diethyl carbonate, ethylene carbonate and vinylene carbonate;
the additive is one or more of 1,1,2, 2-tetrafluoroethyl-2, 2,3, 3-tetrafluoropropyl ether, 2,2, 2-trifluoroethyl-1, 1,2, 2-tetrafluoroethyl ether, 1,1,1,3, 3-hexafluoroisopropyl methyl ether and 1H,1H, 5H-octafluoropentyl-1, 1,2, 2-tetrafluoroethyl ether with the volume content of 1-10%.
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CN114400321A (en) * 2022-02-15 2022-04-26 北京航空航天大学 Low-temperature charge-discharge lithium ion battery and negative electrode material thereof

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