CN111082050A - Lithium ion battery cathode material and preparation method thereof - Google Patents
Lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN111082050A CN111082050A CN201911325775.5A CN201911325775A CN111082050A CN 111082050 A CN111082050 A CN 111082050A CN 201911325775 A CN201911325775 A CN 201911325775A CN 111082050 A CN111082050 A CN 111082050A
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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 cathode material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) pretreating the carbon cloth; (2) with Co (No)3)2·6H20. Urea and NH4Synthesizing Co (CO) by using F as raw material and using hydrothermal method3)0.5(OH)0.11H2O, performing hydrothermal condition of 6-10 h at 100 ℃; (3) 2-methylimidazole is used as a raw material to synthesize the MOF material by a chemical vapor deposition method, and the growth condition is 20-60 min at 100 ℃. The invention has the advantages that: (1) the MOF material is directly synthesized by using a chemical vapor deposition method,the obtained MOF material is not conductive, but has a porous structure, and the porous structure is favorable for electrolyte permeation and lithium ion transmission, so that the active sites of the reaction are increased, and the electrochemical performance of the battery is improved; (2) the obtained MOF material does not need to be annealed and calcined, and the original appearance is kept, so that the adverse effect on the battery is reduced; (3) the carbon cloth is used as a substrate to provide a conductive channel, so that the whole cathode material is ensured to have a conductive function.
Description
Technical Field
The invention relates to a lithium ion battery cathode material and a preparation method thereof, belonging to the technical field of lithium ion batteries.
Background
Lithium Ion Batteries (LIBs) stand out of numerous energy storage devices due to the advantages of high theoretical energy density, low self-discharge, long service life, small memory effect and the like, are increasingly paid attention to and are energy storage devices with great development prospects.
So far, the lithium battery materials widely researched by people comprise three types of graphite, silicon and transition metal oxide, but have defects. For example: theoretical specific capacity of graphite material (372mAh g)-1) Lower and less satisfactory for the development of lithium ion batteries, in contrast to transition metal oxides which can achieve high theoretical specific capacities by conversion reactions (>600mAh·g-1). Research shows that the transition metal oxide has better conductivity and is cheaper, so that the transition metal oxide is more and more concerned, but the transition metal oxide has the problems of volume expansion and the like in the charging and discharging processes, and the application of the transition metal oxide is limited.
The metal organic framework compounds (MOFs) are novel crystal materials, are assembled by the coordination of metal ions and organic ligands, and show good application prospects in the fields of gas storage and separation, proton conduction, catalysis, sensors, energy storage and conversion and the like. The nano porous metal organic framework compound (MOF) has the advantages of adjustable pore diameter, large specific surface area, various framework structures, surface modification and the like, so that the synthesis of the lithium ion battery anode material by taking the MOF as a template is a challenging research direction.
When most of the MOF materials are applied to the lithium ion battery, annealing and calcining are carried out, so that organic ligands of the MOF become porous carbon, and the electrochemical performance of the lithium ion battery is improved. However, annealing and calcining can change the original morphology of the MOF material, so that the MOF material is easy to agglomerate, and further the electrochemical performance of the lithium ion battery can be influenced to a certain extent.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a negative electrode material which can enable an MOF material to have a porous structure without annealing and calcining the MOF material so as to improve the electrochemical performance of a lithium ion battery, and a preparation method of the negative electrode material.
In order to achieve the above object, the present invention adopts the following technical solutions:
the preparation method of the lithium ion battery negative electrode material is characterized by comprising the following steps of:
step 1: pretreating the carbon cloth
Sequentially putting the carbon cloth into acetone, alcohol and deionized water for ultrasonic cleaning and drying;
step 2: synthesis of Co (CO) by hydrothermal method3)0.5(OH)0.11H2O
Mixing Co (No)3)2·6H 20. Urea, NH4F, mixing with deionized water, stirring at room temperature to obtain a hydrothermal solution, transferring the hydrothermal solution into a liner of a hydrothermal kettle, putting the hydrothermal solution into the carbon cloth pretreated in the step 1, wherein the hydrothermal condition is 100 ℃ for 6-10 hours, and growing pink Co (CO) on the carbon cloth after the reaction is finished3)0.5(OH)0.11H2O, drying;
and step 3: synthesis of MOF-coated Co (CO) by chemical vapor deposition3)0.5(OH)0.11H2O material
Co (CO) to be grown on carbon cloth3)0.5(OH)0.11H2Putting O into a glass bottle, spreading an organic ligand 2-methylimidazole at the bottom of the glass bottle, putting the glass bottle into an oven at 100 ℃, growing for 20min to 1h, and growing purple MOF-coated Co (CO) on carbon cloth after the reaction is finished3)0.5(OH)0.11H2O, as Co (CO)3)0.5(OH)0.11H2O@ZIF-67。
The preparation method of the lithium ion battery cathode material is characterized in that in the step 1, the ultrasonic cleaning time is 30min each time.
The preparation method of the lithium ion battery negative electrode material is characterized in that in the step 1 and the step 2, the temperature of an oven is 80 ℃.
The preparation method of the lithium ion battery anode material is characterized in that in the step 2, Co (No)3)2·6H 20. Urea and NH4The molar ratio of F is 2 mmol: 5 mmol: 5 mmol.
The preparation method of the lithium ion battery negative electrode material is characterized in that in the step 2, the stirring time is 20 min.
The lithium ion battery negative electrode material is characterized by being prepared by the preparation method, and the MOF material can have a porous structure without annealing and calcining the MOF material.
The invention has the advantages that:
(1) the MOF material is directly synthesized by using a chemical vapor deposition method, the obtained MOF material is non-conductive, but has a porous structure without annealing and calcining, the porous structure is favorable for permeation of electrolyte and lithium ion transmission, active sites of reaction are increased, electrolyte is stored in the porous structure, so that lithium ions also enter the porous structure, the lithium ions react with cobalt ions coated by the MOF in the porous structure, the effective area of the reaction of the lithium ions and the cobalt ions is increased, and the electrochemical performance of the lithium ion battery is improved;
(2) the obtained MOF material does not need to be annealed and calcined, the original morphology is maintained, the MOF material is not easy to agglomerate, and the adverse effect on the electrochemical performance of the lithium ion battery is reduced;
(3) the cathode material provided by the invention has periodic metal nodes and ligands, so that the transition metal cobalt with a nano structure is uniformly distributed in a porous structure, and further, the transmission of electrons/ions can be promoted, thereby adapting to the change of the volume of the transition metal and keeping the integrity of the porous structure;
(4) the carbon cloth is used as a substrate to provide a conductive channel for transmitting electrons, and the carbon cloth is combined with the non-conductive MOF material to ensure that the whole negative electrode material has a conductive function.
Drawings
FIG. 1 is Co (CO)3)0.5(OH)0.11H2A charge-discharge curve chart of the third circle of O at 0.1C;
FIG. 2 is Co (CO)3)0.5(OH)0.11H2A charge-discharge curve diagram of the third ring of O @ ZIF-67 at 0.1C;
FIG. 3 shows Co (CO) grown at different hydrothermal times3)0.5(OH)0.11H2A graph of rate performance of O;
FIG. 4 shows the Co (CO) at different CVD time3)0.5(OH)0.11H2A multiplying power performance diagram of O @ ZIF-67;
FIG. 5 is Co (CO)3)0.5(OH)0.11H2SEM picture of O;
FIG. 6 is Co (CO)3)0.5(OH)0.11H2SEM picture of O @ ZIF-67;
FIG. 7 is Co (CO)3)0.5(OH)0.11H2TEM image of O @ ZIF-67.
Detailed Description
The invention is described in detail below with reference to the figures and the embodiments.
The lithium ion battery cathode material provided by the invention is prepared by adopting the following method:
step 1: pretreating the carbon cloth
Cutting carbon cloth into circle with radius of 0.8cm, sequentially adding into acetone, alcohol and deionized water, respectively ultrasonic cleaning for 30min, and oven drying at 80 deg.C.
Step 2: synthesis of Co (CO) by hydrothermal method3)0.5(OH)0.11H2O
2mmol of Co (No)3)2·6H 20. 5mmol Urea, 5mmol NH4And F, mixing with 35mL of deionized water, and stirring at room temperature for 20min to obtain a hydrothermal solution. Mixing the aboveTransferring the hydrothermal solution into the inner container of the hydrothermal kettle, putting the pretreated carbon cloth into the hydrothermal kettle, wherein the hydrothermal condition is 6-10 h (6h, 8h and 10h) at 100 ℃, and growing pink Co (CO) on the carbon cloth after the reaction is finished3)0.5(OH)0.11H2And O, putting the mixture into an oven at 80 ℃ for drying.
Co (CO) grown at different hydrothermal times3)0.5(OH)0.11H2The graph of the rate capability of O is shown in fig. 3. As can be seen from FIG. 3, the optimum hydrothermal time was 8 hours.
Co (CO) prepared under the hydrothermal condition of 100 ℃ for 8h3)0.5(OH)0.11H2And (3) performing step 3 on the basis of O.
And step 3: synthesis of MOF (ZIF-67) coated Co (CO) by chemical vapor deposition3)0.5(OH)0.11H2O material
Co (CO) to be grown on carbon cloth3)0.5(OH)0.11H2Putting O into a glass bottle, spreading an organic ligand 2-methylimidazole at the bottom of the glass bottle, putting the glass bottle into an oven at 100 ℃, growing for 20 min-1 h (20min, 40min and 1h), and growing purple MOF (ZIF-67) coated Co (CO) on carbon cloth after the reaction is finished3)0.5(OH)0.11H2O, the purple MOF (ZIF-67) coated Co (CO)3)0.5(OH)0.11H2O is denoted as Co (CO)3)0.5(OH)0.11H2O@ZIF-67。
In the prepared lithium ion battery cathode material, the MOF has a porous structure and is used for storing electrons; the carbon cloth has good conductive performance, is used as a substrate, is used for transmitting electrons and provides a conductive channel.
Co (CO) at different CVD times3)0.5(OH)0.11H2The rate performance graph of O @ ZIF-67 is shown in FIG. 4. As shown in FIG. 4, the optimal CVD time is 40 min.
Co (CO) prepared under hydrothermal condition of 100 ℃ for 8h3)0.5(OH)0.11H2The charge-discharge curve of O at 0.1C for the third cycle is shown in FIG. 1, and the charge-discharge curve is shown for Co (CO)3)0.5(OH)0.11H2Co (CO) prepared by performing chemical vapor deposition on O for 40min3)0.5(OH)0.11H2The charge-discharge curve of O @ ZIF-67 at 0.1C for the third cycle is shown in FIG. 2.
Comparing fig. 1 and fig. 2, it can be seen that: co (CO)3)0.5(OH)0.11H2The discharge area capacity of the third circle of O at 0.1 ℃ is 2.8mAh/cm-2，Co(CO3)0.5(OH)0.11H2The discharge area capacity of the third ring of O @ ZIF-67 at 0.1 ℃ is 3.25mAh/cm-2After the surface is coated with a layer of ZIF-67, the specific area capacity is increased by 0.45mAh/cm-2。
Co (CO) prepared under hydrothermal condition of 100 ℃ for 8h3)0.5(OH)0.11H2SEM image of O as shown in FIG. 5, the Co (CO)3)0.5(OH)0.11H2Co (CO) prepared by performing chemical vapor deposition on O for 40min3)0.5(OH)0.11H2An SEM image of O @ ZIF-67 is shown in FIG. 6, and a TEM image is shown in FIG. 7.
Comparing fig. 5 and fig. 6, it can be seen that: co (CO)3)0.5(OH)0.11H2The shape of O is a nano needle-shaped structure, and the shape of O is changed into a nano rod structure after the O is coated with a layer of ZIF-67.
As is evident from fig. 7: in Co (CO)3)0.5(OH)0.11H2The surface of the O is coated with a layer of ZIF-67.
According to the invention, the MOF material is directly synthesized by using a chemical vapor deposition method, although the obtained MOF material is non-conductive, the MOF material has a porous structure without annealing and calcining, the porous structure is favorable for permeation of electrolyte and lithium ion transmission, active sites of reaction are increased, and electrolyte is stored in the porous structure, so that lithium ions also enter the porous structure, and the lithium ions react with cobalt ions coated by the MOF in the porous structure, so that the effective area of the reaction of the lithium ions and the cobalt ions is increased, and the electrochemical performance of the lithium ion battery is improved.
In addition, the obtained MOF material does not need to be annealed and calcined, and the original morphology is maintained, so that the MOF material is not easy to agglomerate, and the adverse effect on the electrochemical performance of the lithium ion battery is reduced.
The conventional transition metal (such as cobalt) has large volume change in the charging/discharging process, so that the rate capability of the cathode material is reduced, and the cycle stability is deteriorated.
It should be noted that the above-mentioned embodiments do not limit the present invention in any way, and all technical solutions obtained by using equivalent alternatives or equivalent variations fall within the protection scope of the present invention.
Claims (6)
1. The preparation method of the lithium ion battery negative electrode material is characterized by comprising the following steps of:
step 1: pretreating the carbon cloth
Sequentially putting the carbon cloth into acetone, alcohol and deionized water for ultrasonic cleaning and drying;
step 2: synthesis of Co (CO) by hydrothermal method3)0.5(OH)0.11H2O
Mixing Co (No)3)2·6H20. Urea, NH4F, mixing with deionized water, stirring at room temperature to obtain a hydrothermal solution, transferring the hydrothermal solution into a liner of a hydrothermal kettle, putting the hydrothermal solution into the carbon cloth pretreated in the step 1, wherein the hydrothermal condition is 100 ℃ for 6-10 hours, and growing pink Co (CO) on the carbon cloth after the reaction is finished3)0.5(OH)0.11H2O, drying;
and step 3: synthesis of MOF-coated Co (CO) by chemical vapor deposition3)0.5(OH)0.11H2O material
Co (CO) to be grown on carbon cloth3)0.5(OH)0.11H2Placing O in a glass bottle, spreading organic ligand 2-methylimidazole at the bottom of the glass bottle, and placing 10Growing in an oven at 0 ℃ for 20 min-1 h, and growing purple MOF (Metal organic framework) coated Co (CO) on the carbon cloth after the reaction is finished3)0.5(OH)0.11H2O, as Co (CO)3)0.5(OH)0.11H2O@ZIF-67。
2. The preparation method of the lithium ion battery anode material according to claim 1, wherein in the step 1, the time of each ultrasonic cleaning is 30 min.
3. The preparation method of the lithium ion battery anode material according to claim 1, wherein the temperature of the oven in the steps 1 and 2 is 80 ℃.
4. The method for preparing the anode material for lithium ion batteries according to claim 1, wherein in step 2, Co (No)3)2·6H20. Urea and NH4The molar ratio of F is 2 mmol: 5 mmol: 5 mmol.
5. The preparation method of the negative electrode material for the lithium ion battery according to claim 1, wherein in the step 2, the stirring time is 20 min.
6. The lithium ion battery negative electrode material is characterized by being prepared by the preparation method of any one of claims 1 to 5, and the MOF material can have a porous structure without annealing and calcining the MOF material.
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Cited By (6)
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| CN111627720A (en) * | 2020-06-19 | 2020-09-04 | 太原理工大学 | Ni-doped composite electrode material and preparation method thereof |
| CN111916737A (en) * | 2020-08-11 | 2020-11-10 | 合肥工业大学 | Preparation method and application of porous carbon with one-dimensional core-shell structure |
| CN112259714A (en) * | 2020-09-29 | 2021-01-22 | 东莞东阳光科研发有限公司 | Solid-state battery composite electrode plate, preparation method thereof and solid-state battery comprising solid-state battery composite electrode plate |
| CN113097490A (en) * | 2021-04-02 | 2021-07-09 | 扬州大学 | Dodecahedral ZIF-67/Co3O4Composite material, preparation method and application thereof |
| CN113707846A (en) * | 2021-07-28 | 2021-11-26 | 福建师范大学 | MOF-derived modified carbon paper-based sodium metal negative electrode and preparation method thereof |
| WO2022102994A1 (en) * | 2020-11-10 | 2022-05-19 | 주식회사 엘지에너지솔루션 | Anode for all-solid-state battery and all-solid-state battery including same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022102994A1 (en) * | 2020-11-10 | 2022-05-19 | 주식회사 엘지에너지솔루션 | Anode for all-solid-state battery and all-solid-state battery including same |
| CN113097490A (en) * | 2021-04-02 | 2021-07-09 | 扬州大学 | Dodecahedral ZIF-67/Co3O4Composite material, preparation method and application thereof |
| CN113707846A (en) * | 2021-07-28 | 2021-11-26 | 福建师范大学 | MOF-derived modified carbon paper-based sodium metal negative electrode and preparation method thereof |
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Application publication date: 20200428 |