CN111969185B - Coated TiO2Graphite double-ion battery composite positive electrode material and preparation method thereof - Google Patents

Coated TiO2Graphite double-ion battery composite positive electrode material and preparation method thereof Download PDF

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CN111969185B
CN111969185B CN202010645237.0A CN202010645237A CN111969185B CN 111969185 B CN111969185 B CN 111969185B CN 202010645237 A CN202010645237 A CN 202010645237A CN 111969185 B CN111969185 B CN 111969185B
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陈玉喜
韩方超
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Hunan 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
    • H01M4/362—Composites
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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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/583—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
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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    • H01M4/625—Carbon or graphite
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention provides a coated TiO2The preparation method of the graphite double-ion battery composite positive electrode material comprises the following steps: s1: tetrabutyl titanate as TiO2Uniformly mixing the tetrabutyl titanate and graphite powder, and putting the mixture into absolute ethyl alcohol to obtain a solid-liquid mixture; s2: continuously stirring the solid-liquid mixture in a water bath magnetic stirrer until absolute ethyl alcohol is completely evaporated to obtain a sample; s3: heating and preserving the temperature of the sample under inert protective atmosphere to obtain the coated TiO2The graphite double-ion battery composite positive electrode material. The coated TiO provided by the invention2The graphite double-ion battery composite anode material has good cycle performance.

Description

Coated TiO2Graphite double-ion battery composite positive electrode material and preparation method thereof
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of energy storage and conversion materials, in particular to a coated TiO2The graphite double-ion battery composite anode material and the preparation method thereof.
[ background of the invention ]
The theoretical specific capacity of the embedded anions of the graphite material adopted by the positive electrode of the double-ion battery is 120mAhg-1But the intercalation of the anion will result in a volume expansion of about 130%. Meanwhile, since the decomposition of the electrolyte is inevitably caused by the operating voltage of about 5V, the actual specific cycle capacity of the graphite positive electrode is smaller than the theoretical cycle capacity, and the cycle performance is poor, which is difficult to be put into practical use.
In the related art, in order to solve the above problems, at present, a high-voltage resistant additive is generally added into an electrolyte, or other types of negative electrode materials are adopted to replace a graphite negative electrode to improve the cycle stability of the bi-ion battery. However, the above method cannot effectively improve the problem of poor battery cycle stability caused by volume expansion of the graphite positive electrode; in addition, the addition of the additive in the electrolyte inevitably leads to the increase of the viscosity of the electrolyte, and influences the rapid charge and discharge performance of the dual-ion battery.
Therefore, there is a need to provide a coated TiO2The graphite double-ion battery composite positive electrode material and the preparation method thereof solve the problems.
[ summary of the invention ]
The present invention has been made to overcome the above problems and an object of the present invention is to provide a coated TiO having excellent cycle characteristics2The graphite double-ion battery composite anode material and the preparation method thereof.
In order to achieve the above object, the present invention provides a coated TiO2The preparation method of the graphite double-ion battery composite positive electrode material comprises the following steps:
s1: tetrabutyl titanate as TiO2Uniformly mixing the tetrabutyl titanate and graphite powder, and putting the mixture into absolute ethyl alcohol to obtain a solid-liquid mixture;
s2: continuously stirring the solid-liquid mixture in a water bath magnetic stirrer until absolute ethyl alcohol is completely evaporated to obtain a sample;
s3: heating and preserving the temperature of the sample under inert protective atmosphere to obtain the coated TiO2The graphite double-ion battery composite positive electrode material.
Preferably, the mass ratio of the tetrabutyl titanate to the graphite powder is (0.05-0.15): 1.
preferably, the temperature of the water bath in the step S2 is 40-70 ℃.
Preferably, in the step S4, the heating temperature is 400-600 ℃, and the heat preservation time is 3-6 hours.
The invention also provides a coated TiO2The graphite double-ion battery composite positive electrode material is prepared by the preparation method.
Compared with the related technology, the technical scheme provided by the invention utilizes a liquid phase method to mix the nano TiO2The particles are coated on the surface of the graphite particles, so that the interface structure of graphite/electrolyte is optimized and improved, and the following beneficial effects are achieved:
(1)TiO2the oxide is chemically stable and high-voltage-resistant, and the coating on the surface of graphite can effectively inhibit mechanical stress caused by the insertion of anions into the graphite, so that the cycling stability of the battery is improved;
(2)TiO2is a wide bandgap semiconductor with very low electron conductivity (10)-12Scm-1) The coating on the surface of the graphite particles can isolate the electrolyte from the graphite particles to a certain extent, and prevent the conduction of electrons between the graphite particles and the carbonate electrolyte, so that the oxidative decomposition of the electrolyte under high potential is effectively slowed down, and the cycle stability of the bi-ion battery is further improved;
(3) TiO on the surface of graphite particles2Can inhibit the co-intercalation phenomenon of the solvent caused by the intercalation of anions in the graphite in the charging process and effectively reduce the surface breakage of graphite particles. Therefore, the surface of the graphite powder is coated with TiO2The composite anode material has the advantages of long cycle life up to ten thousand times, high cycle capacity and excellent high-current charge and discharge performance which are far higher than that of the anode material without TiO2Electrochemical performance of the coated graphite positive electrode.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 shows a coated TiO provided by the present invention2The flow chart of the steps of the preparation method of the graphite double-ion battery composite anode material;
FIG. 2(a) shows a TiO coating layer in the first embodiment2Graphite double-ion battery composite positive electrode material and uncoated TiO2The positive electrode material of the graphite bi-ion battery has an X-ray diffraction spectrum (XRD) contrast diagram;
FIG. 2(b) is an enlarged view of a diffraction peak at a diffraction angle 2 θ of 20 ° to 40 ° in FIG. 2 (a);
FIG. 2(c) and FIG. 2(d) show the TiO coating in the first embodiment2The low-power and high-power Scanning Electron Microscope (SEM) morphology graphs of the graphite double-ion battery composite positive electrode material;
FIG. 2(e) is a diagram showing the coating of TiO in the first embodiment2The morphology of the graphite double-ion battery composite anode material is shown in a Transmission Electron Microscope (TEM);
FIG. 2(f) shows the current density of 0.5Ag in the first embodiment-1(5C) Under the condition, coating TiO2Graphite double-ion battery composite positive electrode material and uncoated TiO2The cycle performance diagram of the graphite double-ion battery anode material is shown;
FIG. 2(g) shows the uncoated TiO of the first example2The positive electrode material of the graphite double-ion battery and the coated TiO2The cycle performance diagram of the graphite double-ion battery composite positive electrode material under different multiplying power conditions is shown;
FIG. 3(a) shows the TiO coating in the second embodiment2The SEM topography of the graphite double-ion battery composite anode material;
FIG. 3(b) is a diagram showing the coating of TiO in example two2The cycle performance diagram of the graphite double-ion battery composite positive electrode material under the current density of 2C;
FIG. 4(a) shows the TiO coating in example III2The SEM topography of the graphite double-ion battery composite anode material;
FIG. 4(b) is the TiO coating in example III2The graphite double-ion battery composite positive electrode material has a cycle performance diagram under the current density of 5C.
[ detailed description ] embodiments
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.
Referring to FIG. 1, the present invention provides a coated TiO2The preparation method of the graphite double-ion battery composite positive electrode material comprises the following steps:
s1: tetrabutyl titanate as TiO2Uniformly mixing the tetrabutyl titanate and graphite powder, and putting the mixture into absolute ethyl alcohol to obtain a solid-liquid mixture;
s2: continuously stirring the solid-liquid mixture in a water bath magnetic stirrer until absolute ethyl alcohol is completely evaporated to obtain a sample;
s3: heating and preserving the temperature of the sample under inert protective atmosphere to obtain the coated TiO2The graphite double-ion battery composite positive electrode material.
Preferably, the mass ratio of the tetrabutyl titanate to the graphite powder is (0.05-0.15): 1.
preferably, the temperature of the water bath in the step S2 is 40-70 ℃.
Preferably, in the step S4, the heating temperature is 400-600 ℃, and the heat preservation time is 3-6 hours.
The invention also provides a coated TiO2The graphite double-ion battery composite positive electrode material is prepared by the preparation method.
Example one
Mixing tetrabutyl titanate and graphite powder according to the mass ratio of 0.15:1, adding the mixture into absolute ethyl alcohol with a proper volume, and placing the mixture into a water bath kettle at the temperature of 60 ℃ to continuously magnetically stir until the absolute ethyl alcohol is completely evaporated; carbonizing the collected sample at 600 ℃ for 3 hours in argon atmosphere to obtain the coated TiO2The graphite double-ion battery composite positive electrode material.
FIG. 2(a) shows a TiO coating2Graphite double-ion battery composite positive electrode material and uncoated TiO2The positive electrode material of the graphite bi-ion battery has an X-ray diffraction spectrum (XRD) contrast diagram, wherein a curve chart I is a coated TiO2The graphite double-ion battery composite anode material has an X-ray diffraction spectrum (XRD) pattern; graph II shows uncoated TiO2The positive electrode material of the graphite bi-ion battery has an X-ray diffraction spectrum (XRD) pattern. Uncoated TiO2The positive electrode material of the graphite double-ion battery only has graphite diffraction peaks (PDF #41-1487) and is coated with TiO2Anatase type TiO appears in the graphite double-ion battery composite anode material sample2The diffraction peak (PDF #21-1272) and that of graphite, and in addition, there is no diffraction peak of other phases, indicating that TiO is produced by the production method provided by the present invention2Successfully coated on the surface of the graphite.
FIG. 2(b) is an enlarged view of a diffraction peak between 20 DEG and 40 DEG at a diffraction angle 2 theta in FIG. 2(a), in which the curve isLine drawing I is coating TiO2The enlarged view of the diffraction peak of the graphite double-ion battery composite positive electrode material; graph II shows uncoated TiO2The enlarged view of the diffraction peak of the graphite bi-ion battery positive electrode material. Anatase type TiO can be clearly seen from the figure2The (101) crystal plane diffraction peak of (a).
FIG. 2(c) and FIG. 2(d) are each a TiO-coated film2The low-power and high-power Scanning Electron Microscope (SEM) morphology images of the graphite double-ion battery composite anode material clearly show that the surface of graphite is uniformly coated with nano TiO2Particles having a particle size of about 10 nm.
FIG. 2(e) shows the coating of TiO2The Transmission Electron Microscope (TEM) morphology of the graphite double-ion battery composite anode material further proves that the TiO is2And (3) uniformly coating the nano particles on the surface of the graphite.
FIG. 2(f) shows the current density at 0.5Ag-1(5C) Under the condition, coating TiO2Graphite double-ion battery composite positive electrode material and uncoated TiO2The cycle performance diagram of the graphite double-ion battery anode material. Wherein the graph I shows that the TiO is not coated2The coulomb efficiency curve diagram of the graphite bi-ion battery anode material; graph II for coating TiO2The coulomb efficiency curve diagram of the graphite double-ion battery composite anode material; graph III for uncoated TiO2The cycle capacity curve diagram of the graphite double-ion battery anode material; graph IV shows the coating of TiO2The cycle capacity curve diagram of the graphite double-ion battery composite anode material. Uncoated TiO2The graphite bi-ion battery anode material has poor cycle stability, and the charge-discharge cycle capacity is attenuated to zero less than one thousand times. In contrast, coated TiO2The graphite double-ion battery composite positive electrode material has the cycle capacity of 75 percent of the first cycle capacity even after ten thousand charge-discharge cycles, shows extremely stable cycle performance, and is more stable than that of the graphite double-ion battery composite positive electrode material without TiO coating2The cycling stability of the graphite double-ion battery anode material is greatly improved. FIG. 2(g) shows uncoated TiO2The positive electrode material of the graphite double-ion battery and the coated TiO2The graphite double-ion battery composite anode materialThe cycle performance under different multiplying power conditions is shown in the graph I, and the graph I is a coating TiO2The cycle capacity curve diagram of the graphite double-ion battery composite anode material under different multiplying power conditions; graph II shows uncoated TiO2The cycle capacity curve chart of the graphite double-ion battery anode material under different multiplying power conditions shows that the graphite double-ion battery anode material is coated with TiO under the conditions of large-current charge and discharge2The cycle capacity of the graphite double-ion battery composite anode material is obviously higher than that of the uncoated TiO2The positive electrode material of the graphite bi-ion battery.
Example two
Mixing tetrabutyl titanate and graphite powder according to the mass ratio of 0.05:1, adding the mixture into absolute ethyl alcohol with a proper volume, and placing the mixture into a water bath kettle at 40 ℃ for continuous magnetic stirring until the absolute ethyl alcohol is completely evaporated; carbonizing the collected sample at 400 ℃ for 6 hours in argon atmosphere to obtain the coated TiO2The graphite double-ion battery composite positive electrode material.
FIG. 3(a) shows a TiO coating2The SEM topography of the graphite double-ion battery composite anode material, TiO2The nano particles are uniformly coated on the surface of the graphite. FIG. 3(b) shows the coating of TiO2The graphite double-ion battery composite positive electrode material has a cycle performance diagram under 2C current density, wherein a curve chart I is a TiO coating layer2The coulomb efficiency curve diagram of the graphite double-ion battery composite anode material; graph II for coating TiO2The charging capacity curve diagram of the graphite double-ion battery composite anode material; graph III for coating TiO2The discharge capacity curve chart of the graphite double-ion battery composite anode material. The cycle capacity retention rate after 500 charge-discharge cycles was as high as 95%, showing extremely excellent cycle stability.
EXAMPLE III
Mixing tetrabutyl titanate and graphite powder according to the mass ratio of 0.1:1, adding the mixture into absolute ethyl alcohol with a proper volume, and placing the mixture into a water bath kettle at 50 ℃ for continuous magnetic stirring until the ethyl alcohol is completely evaporated; carbonizing the collected sample at 500 ℃ for 5 hours in argon atmosphere to obtain the coated TiO2The graphite double-ion battery composite positive electrode material.
FIG. 4(a) shows a TiO coating2The SEM topography of the graphite double-ion battery composite anode material, TiO2The nano particles are uniformly coated on the surface of the graphite. FIG. 4(b) shows a TiO coating2The graphite double-ion battery composite positive electrode material has a cycle performance diagram under the current density of 5C, wherein a curve chart I is a coated TiO2The coulomb efficiency curve diagram of the graphite double-ion battery composite anode material; graph II for coating TiO2The charging capacity curve diagram of the graphite double-ion battery composite anode material; graph III for coating TiO2The discharge capacity curve chart of the graphite double-ion battery composite anode material. After 1000 times of charge-discharge cycles, the discharge cycle capacity was maintained at 80mAhg-1And the cycle stability is excellent.
Compared with the related technology, the technical scheme provided by the invention utilizes a liquid phase method to mix the nano TiO2The particles are coated on the surface of the graphite particles, so that the interface structure of graphite/electrolyte is optimized and improved, and the following beneficial effects are achieved:
(1)TiO2the oxide is chemically stable and high-voltage-resistant, and the coating on the surface of graphite can effectively inhibit mechanical stress caused by the insertion of anions into the graphite, so that the cycling stability of the battery is improved;
(2)TiO2is a wide bandgap semiconductor with very low electron conductivity (10)-12Scm-1) The coating on the surface of the graphite particles can isolate the electrolyte from the graphite particles to a certain extent, and prevent the conduction of electrons between the graphite particles and the carbonate electrolyte, so that the oxidative decomposition of the electrolyte under high potential is effectively slowed down, and the cycle stability of the bi-ion battery is further improved;
(3) TiO on the surface of graphite particles2Can inhibit the co-intercalation phenomenon of the solvent caused by the intercalation of anions in the graphite in the charging process and effectively reduce the surface breakage of graphite particles. Therefore, the surface of the graphite powder is coated with TiO2The composite anode material has the advantages of long cycle life up to ten thousand times, high cycle capacity and excellent high-current charge and discharge performance which are far higher than that of the anode material without TiO2Electrochemical performance of coated graphite positive electrode。
While the foregoing is directed to embodiments of the present invention, it will be understood by those skilled in the art that various changes may be made without departing from the spirit and scope of the invention.

Claims (3)

1. Coated TiO2The application of the graphite composite anode material as the anode material of the double-ion battery is characterized in that the graphite composite anode material is coated with TiO2The graphite composite cathode material is prepared by the following steps:
s1: tetrabutyl titanate as TiO2Uniformly mixing the tetrabutyl titanate and graphite powder, and putting the mixture into absolute ethyl alcohol to obtain a solid-liquid mixture;
s2: continuously stirring the solid-liquid mixture in a water bath magnetic stirrer until absolute ethyl alcohol is completely evaporated to obtain a sample;
s3: heating and preserving the temperature of the sample under inert protective atmosphere to obtain the coated TiO2The graphite composite positive electrode material of (1); the mass ratio of the tetrabutyl titanate to the graphite powder is (0.05-0.15): 1.
2. the use according to claim 1, wherein the water bath temperature in step S2 is 40-70 ℃.
3. The use according to claim 1, wherein the heating temperature in step S3 is 400-600 ℃ and the holding time is 3-6 hours.
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CN114188521B (en) * 2021-12-10 2023-10-20 湖南大学 Light coating layer on surface of graphite anode material of double-ion battery and preparation method
WO2023108321A1 (en) * 2021-12-13 2023-06-22 深圳先进技术研究院 Composite modified graphite material, dual-ion battery positive electrode material, dual-ion battery negative electrode material, and dual-ion battery
CN114430029A (en) * 2021-12-13 2022-05-03 深圳先进技术研究院 Composite modified graphite material, positive electrode material of bi-ion battery, negative electrode material of bi-ion battery and bi-ion battery
CN114655951B (en) * 2022-04-17 2022-09-02 晖阳(贵州)新能源材料有限公司 Preparation method of lithium ion battery cathode material

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