CN110683576A - Lithium ion battery - Google Patents
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- CN110683576A CN110683576A CN201910962377.8A CN201910962377A CN110683576A CN 110683576 A CN110683576 A CN 110683576A CN 201910962377 A CN201910962377 A CN 201910962377A CN 110683576 A CN110683576 A CN 110683576A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M2004/027—Negative electrodes
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- 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 lithium ion battery, the cathode of which is TiO2Self-supporting films of TiO2The nano wires composed of nano sheets form the self-supporting film, TiO2The preparation of the self-supporting film adopts titanium dioxide powder as a titanium source, sodium hydroxide solution as a solvent and a reaction regulator, and a hydrothermal method is used to successfully obtain TiO2The nano-sheet self-supporting thin film material. The raw materials required for preparation are rich, and the cost is low. The preparation process is simple and has good repeatability. The TiO being2The nanosheet self-supporting film is used as a negative electrode material for a lithium ion battery, and shows good rate capability and cycling stability.
Description
Technical Field
The invention belongs to the field of preparation and application of nano materials, and particularly relates to a negative electrode material of a lithium ion battery.
Background
With the rapid development of economy, the increasingly severe energy crisis and environmental deterioration have become the biggest problems facing all mankind. Lithium ion batteries are increasingly used as energy storage devices because of their advantages of portability, high capacity, long life, and the like. In recent years, due to the increasing demand for power performance of electronic products and electric vehicles, performance such as power density of lithium ion batteries has been improvedHigher demands, and electrode materials are the determining factor for the performance improvement of lithium ion batteries. In the aspect of negative electrode materials, the rate capability of the current commercialized negative electrode material graphite of the lithium ion battery cannot meet the requirements of people on the battery performance. And TiO 22The material has the advantages of environmental friendliness, higher reversible electrochemical capacity, stable cycle efficiency and coulombic efficiency, very small volume effect (only 4 percent) and the like; in particular TiO2The nano material has high lithium ion transmission efficiency, so the nano material has excellent rate performance, namely large-current charge and discharge capacity, and is a lithium ion battery cathode material with important application prospect. However, conventional TiO2The nanometer negative electrode material needs to prepare an electrode by means of a binder and a conductive agent, and the use of the binder reduces the effective contact area of the nanometer material and an electrolyte, so that the lithium ion intercalation/deintercalation efficiency is reduced. Thus, how to realize TiO2The ordered assembly of nanomaterials so as to avoid the use of binders is a problem which is urgently needed to be solved at present.
Disclosure of Invention
In order to solve the above problems, the present invention provides a lithium ion battery.
The technical scheme of the invention is as follows: a lithium ion battery comprises a positive electrode, a negative electrode, electrolyte and a diaphragm; the negative electrode is TiO2A self-supporting film; the titanium oxide is made of TiO2The self-supporting film is made of TiO2The nano sheets are mutually cross-linked and wound to form a one-dimensional nanowire penetrating and penetrating two-dimensional self-supporting structure.
Further, the TiO2The preparation method of the self-supporting film comprises the following steps: and (3) putting 0.05g of titanium dioxide powder, 60ml of water and 15g of sodium hydroxide into a 100ml reaction kettle, uniformly dispersing, and then reacting for 3d under the hydrothermal condition of 220 ℃ to obtain the self-supporting film self-assembled by the sodium titanate nanosheets. Repeatedly washing the self-supporting film to be neutral by using deionized water, drying, putting the self-supporting film into a tubular furnace, calcining for 2 hours at 400 ℃ in air atmosphere to obtain TiO2A nanosheet self-supporting film.
Further, the electrolyte adopts 1mol/L LiPF6A solution, wherein the solvent is a mixed solution of Ethylene Carbonate (EC) and diethyl carbonate (DEC) in a volume ratio of 1: 1;
the invention has the beneficial effects that: the method of the invention can simply and stably obtain TiO2And the nano-sheet cathode is a self-supporting film and is further assembled into the lithium ion battery. The titanium oxide powder is made of TiO2The two-dimensional self-supporting film formed by interpenetration of the one-dimensional nanowires formed by mutually crosslinking and winding the nanosheets not only has the advantages of three-dimensional interpenetrating structure, high porosity, large specific surface area, good solution permeability and the like, but also has the advantages that the nanowires are formed by crosslinking and winding the nanosheets, so that the nanowires have a hollow structure, the specific surface area of the nanowires is further increased, and the prepared lithium ion battery has higher capacity, circulation stability and excellent rate capability, so that the lithium ion battery has wide application prospect in the field of lithium ion batteries.
Drawings
FIG. 1 shows TiO prepared in example 12A nitrogen adsorption and desorption curve graph of the nanosheet self-supporting film;
FIG. 2 is a high rate cycle test plot for the lithium ion battery prepared in example 1;
FIG. 3 shows TiO prepared in example 22A nitrogen adsorption and desorption curve graph of the nanosheet self-supporting film;
FIG. 4 is a graph showing the rate capability test of the lithium ion battery prepared in example 2;
FIG. 5 shows TiO of the present invention2SEM pictures of the nanoplate self-supporting film;
FIG. 6 shows TiO of the present invention2TEM picture of the nanosheet self-supporting thin film;
FIG. 7 shows TiO of the present invention2AFM pictures of the nanosheet self-supporting thin film;
FIG. 8 shows TiO of the present invention2Macroscopic pictures of the nanosheet self-supporting film;
FIG. 9 shows TiO prepared in example 32A nitrogen adsorption and desorption curve graph of the nanosheet self-supporting film;
fig. 10 is a rate capability test chart of the lithium ion battery prepared in example 3.
Detailed Description
The invention will be further elucidated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention will occur to those skilled in the art after reading the present disclosure, and such equivalents will fall within the scope of the appended claims.
Examples 1 and 2 used a sheet of lithium metal as the counter electrode to TiO2The lithium storage performance of the nano-sheet self-supporting film as a half electrode is tested, which shows that TiO2The two-dimensional self-supporting structure formed by interpenetration of the one-dimensional nanowires formed by cross-linking and winding the nanosheets has excellent lithium storage performance.
Example 1
TiO 22The preparation method of the nano-sheet self-supporting film comprises the following steps: placing 0.01g of titanium dioxide powder, 40mL of water and 5g of sodium hydroxide in a 100mL hydrothermal reaction kettle, carrying out ultrasonic treatment for 10min at room temperature, and reacting in an oven at 180 ℃ for 1d to obtain the film self-assembled by the sodium titanate nanosheets. Repeatedly washing the self-supporting film to be neutral by using deionized water, drying, putting the film into a tubular furnace, and calcining for 1h at 300 ℃ in air atmosphere to obtain TiO2(B) A nanosheet film.
Characterized by being TiO2(B) The nano sheets are bent, cross-linked and interpenetrated into nano wires, a three-dimensional interpenetrating network structure is formed, a self-supporting film is formed after the whole network reaches a certain thickness, and the specific surface area of the film is as high as 36.4 m2g-1As shown in fig. 1. The self-supporting film is used as a working electrode, a metal lithium sheet is used as a counter electrode, and 1mol/L LiPF is adopted as an electrolyte6The solvent of the solution is a mixed solution of Ethylene Carbonate (EC) and diethyl carbonate (DEC) in a volume ratio of 1:1, and the diaphragm is assembled by adopting a Celgard2400 diaphragm to obtain the lithium ion battery. It was tested for cell performance at 6.7A g-1After circulating for 1000 times under the current density of (1), the current density of the copper-based alloy still can keep 150.5 mAh g-1As shown in fig. 2.
Example 2
TiO 22The preparation method of the nano-sheet self-supporting film comprises the following steps: placing 0.2g of titanium dioxide powder, 80mL of water and 32g of sodium hydroxide in a 100mL hydrothermal reaction kettle, performing ultrasonic treatment at room temperature for 60min, and reacting in an oven at 250 ℃ for 6d to obtain the self-supporting film self-assembled by the sodium titanate nanosheets. Repeatedly washing the self-supporting film to be neutral by using deionized water, drying, putting the film into a tubular furnace, calcining for 3 hours at 500 ℃ in air atmosphere to obtain TiO2(B) A nanosheet self-supporting film.
Characterized by being TiO2(B) The nano sheets are bent, cross-linked and interpenetrated into nano wires, a three-dimensional interpenetrating network structure is formed, a self-supporting film is formed after the whole network reaches a certain thickness, and the specific surface area of the film is as high as 83.8m2g-1As shown in fig. 3. The self-supporting film is used as a working electrode, a metal lithium sheet is used as a counter electrode, and 1mol/L LiPF is adopted as an electrolyte6The solvent of the solution is a mixed solution of Ethylene Carbonate (EC) and diethyl carbonate (DEC) in a volume ratio of 1:1, and the diaphragm is assembled by adopting a Celgard2400 diaphragm to obtain the lithium ion battery. The performance of the battery is tested and is 0.1A g-1Has a capacity of 323.2 mAh g at current density-1As shown in fig. 4; when the current density is increased to 6.7A g-1When the water is used, the capacity of the water still reaches up to 180.5 mAh g-1Showing good rate performance.
Example 3 TiO was further treated using commercial lithium cobaltate as the positive electrode2Assembling the nano-sheet self-supporting film to obtain the lithium ion battery, and directly proving that TiO is adopted2TiO of two-dimensional self-supporting structure formed by interpenetration of one-dimensional nanowires formed by cross-linking and winding nanosheets2The nano-sheet self-supporting film can assemble a lithium ion battery with excellent performance.
Example 3
TiO 22The preparation method of the nano-sheet self-supporting film comprises the following steps: placing 0.05g of titanium dioxide powder, 60mL of water and 15g of sodium hydroxide in a 100mL hydrothermal reaction kettle, carrying out ultrasonic treatment for 30min at room temperature, and reacting in an oven at 220 ℃ for 3d to obtain the film self-assembled by the sodium titanate nanosheets. Then deionized water is used for mixingRepeatedly washing the self-supporting film to be neutral, drying, putting the film into a tubular furnace, calcining for 2h at 400 ℃ in air atmosphere to obtain TiO2(B) A nanosheet film.
The self-supporting film is used as a negative electrode, commercial lithium cobaltate is used as a positive electrode, and 1mol/L LiPF is used as an electrolyte6The solvent of the solution is a mixed solution of Ethylene Carbonate (EC) and diethyl carbonate (DEC) in a volume ratio of 1:1, and the diaphragm is assembled by adopting a Celgard2400 diaphragm to obtain the lithium ion battery.
FIG. 5 is an SEM picture of a self-supporting film, from which it can be seen that TiO was prepared2The structure is a rough one-dimensional nanometer multilevel structure, the size is uniform, and the appearance is regular.
FIG. 6 is a TEM image of a free-standing film from which it can be seen that TiO is produced2The nano sheets are intertwined with each other to form a one-dimensional nano multilevel structure, and the one-dimensional nano multilevel structure is further woven into the self-supporting film in fig. 5.
FIG. 7 is an AFM picture of nanoplates comprising a free-standing film from which the TiO produced can be seen2The thickness of the nano-sheet is only about 5 nm.
FIG. 8 is a macroscopic picture of a self-supporting film, from which it can be seen that TiO is produced2The nano sheets are self-assembled into a film structure with an ultra-large area.
FIG. 9 shows TiO prepared in example 32(B) The nitrogen absorption and desorption curve chart of the nano-sheet self-supporting film shows that the specific surface area of the nano-sheet self-supporting film is up to 117.0 m through measurement and calculation2g-1。
FIG. 10 is a graph formed by TiO2The rate capability test chart of the lithium ion battery assembled by the nanosheet self-supporting film shows that the prepared lithium ion battery has higher rate capability which is 0.3A g-1Has a capacity of 246.8 mAh g-1When the current density was increased to 3.4A g-1When the water is used, the capacity of the water still reaches 136.3 mAh g-1。
Claims (5)
1. A lithium ion battery comprises an anode, a cathode and electrolyteAnd a diaphragm; characterized in that the negative electrode is TiO2A self-supporting film; the TiO is2The self-supporting film is made of TiO2The nano sheets are mutually cross-linked and wound to form a one-dimensional nanowire penetrating and penetrating two-dimensional self-supporting structure.
2. The lithium ion battery of claim 1, wherein the TiO is selected from the group consisting of2The preparation method of the self-supporting film comprises the following steps: placing titanium dioxide powder, water and sodium hydroxide in a reaction kettle, wherein the mass ratio of the titanium dioxide powder to the water to the sodium hydroxide is as follows: 0.01-0.2:40-80: 5-32; after being dispersed uniformly, the mixture reacts for 1 to 6 days under the hydrothermal condition of 180 ℃ and 250 ℃ to obtain the self-supporting film self-assembled by the sodium titanate nano-sheets; then repeatedly washing the self-supporting film to be neutral by deionized water, drying, then putting the self-supporting film into a tubular furnace, calcining for 1-3h at the temperature of 500 ℃ in the air atmosphere to obtain TiO2A nanosheet self-supporting film.
3. The lithium ion battery of claim 2, wherein the mass ratio of titanium dioxide powder, water and sodium hydroxide is: 0.05:60:15, the hydrothermal reaction temperature is 220 ℃, and the reaction time is 3 d.
4. The lithium ion battery of claim 2, wherein the tube furnace calcination temperature is 400 ℃ and the calcination time is 2 h.
5. The lithium ion battery of claim 1, wherein the electrolyte is 1mol/L LiPF6The solvent of the solution is a mixed solution of Ethylene Carbonate (EC) and diethyl carbonate (DEC) in a volume ratio of 1: 1.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113511638A (en) * | 2021-06-30 | 2021-10-19 | 南京邮电大学 | Preparation method of TiN-S composite anode material by plasma chemical vapor codeposition |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113511638A (en) * | 2021-06-30 | 2021-10-19 | 南京邮电大学 | Preparation method of TiN-S composite anode material by plasma chemical vapor codeposition |
CN113511638B (en) * | 2021-06-30 | 2022-12-06 | 南京邮电大学 | Preparation method of TiN-S composite anode material by plasma chemical vapor codeposition |
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