CN113526565A - Method for rapidly synthesizing lithium cobaltate cathode material and application - Google Patents
Method for rapidly synthesizing lithium cobaltate cathode material and application Download PDFInfo
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- CN113526565A CN113526565A CN202110776680.6A CN202110776680A CN113526565A CN 113526565 A CN113526565 A CN 113526565A CN 202110776680 A CN202110776680 A CN 202110776680A CN 113526565 A CN113526565 A CN 113526565A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
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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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- 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
- H01M2004/028—Positive 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 method for quickly synthesizing a lithium cobaltate positive electrode material and application of the lithium cobaltate positive electrode material in preparation of a lithium ion battery. The precursor is subjected to rapid heating to generate the lithium cobaltate cathode material ultra-rapidly. The cobalt ions in the lithium cobaltate positive electrode material are positive trivalent, and the valence state of the cobalt ions is consistent with that of the lithium cobaltate positive electrode material synthesized by the traditional method. LiCoO of the present invention2The anode material has LiCoO synthesized by the traditional method2Comparable performance of the positive electrode material, without any modified LiCoO2The first coulombic efficiency of the positive electrode material is percent, the specific discharge capacity at the first time has mAh/g, the coulombic efficiency is still close to 100 percent when the positive electrode material is circulated for 300 circles at 1C, and the capacity retention rate within 100 circles is still about 90 percent.
Description
Technical Field
The invention relates to the field of lithium ion materials, in particular to a method for quickly synthesizing a lithium cobaltate positive electrode material and application of the lithium cobaltate positive electrode material in preparation of a lithium ion battery.
Background
At present, lithium cobalt oxide batteries are widely used in various electronic devices such as mobile phones and computers, wherein lithium cobalt oxide positive electrode materials account for a large proportion in the preparation and cost of the batteries, and with the continuous increase of the demand of people on the lithium cobalt oxide batteries, higher requirements are also put forward on the preparation process and production cost of the lithium cobalt oxide battery positive electrode materials.
Reducing the preparation period of the lithium cobaltate positive electrode material is one of the most important ways to reduce the production cost of the lithium cobaltate battery. However, the preparation period of the lithium cobaltate anode material in both laboratories and industries is generally more than ten hours at present, so that the preparation period of the lithium cobaltate battery anode material is long, much electric power and time are consumed during production, and the production cost of the lithium cobaltate battery is greatly improved.
Furthermore, the lithium cobaltate cathode material synthesized by the industrial method has a large particle size, which results in a small specific surface area and poor rate capability of the lithium cobaltate material.
Disclosure of Invention
The invention overcomes the defect of long production period in the existing preparation technology of the lithium cobaltate cathode material, and provides a method for quickly synthesizing the lithium cobaltate cathode material. The lithium cobaltate positive electrode material prepared by the invention has the performance which is almost the same as the lithium cobaltate positive electrode material synthesized by the traditional method (for example, the lithium cobaltate positive electrode material has the same hexagonal system layered structure, is beneficial to the extraction and the insertion of lithium ions, and the cobalt ions are trivalent positive and have the same valence state as the lithium cobaltate positive electrode material synthesized by the traditional method), such as the specific capacity of a battery, and the like, but the preparation time only needs dozens of seconds.
The invention also overcomes the defect that the lithium cobaltate anode material particles prepared by the traditional industrial technology are large, and compared with the lithium cobaltate anode material prepared by the existing industrial method, the lithium cobaltate anode material particles prepared by the invention are reduced by 3-5 times, and are expected to be widely applied to rate-type batteries.
The lithium cobaltate anode material rapidly synthesized by the method is granular, and when an electrochemical performance test is carried out, the first coulombic efficiency is 91% under the cut-off voltage of 4.6V, and the first discharge specific capacity is 200 mAh/g. Meanwhile, under the cut-off voltage of 4.3V, the coulomb efficiency of 100 cycles at 1C is still close to 100%, and the capacity retention rate within 100 cycles is still about 90%.
The purpose of the invention is realized by the following technical scheme:
a method for rapidly synthesizing a lithium cobaltate positive electrode material comprises the following steps: directly grinding 3-3.5 molar parts of lithium carbonate and 2 molar parts of cobaltosic oxide in a mortar until the lithium carbonate and the cobaltosic oxide are uniformly mixed to obtain a lithium cobaltate precursor; placing a lithium cobaltate precursor on an alumina ceramic wafer, wherein the alumina ceramic wafer is positioned on a carbon cloth with two ends connected to a direct-current power supply; electrifying and calcining twice, firstly calcining for the first time, grinding the primary calcined product, and then calcining for the second time to obtain the lithium cobaltate cathode material; the electrifying current for the first calcination is 11-13A, and the duration is 20-30 s; the electrifying current for the second calcination is 16-40A, and the duration is 20-80 s. The invention uniformly lays the powder on a thin alumina ceramic sheet with good thermal conductivity by twice calcination, and effectively avoids the contact reduction of carbon to cobalt.
Preferably, the molar ratio of lithium carbonate to cobaltosic oxide is 3.5: 2.
the invention also relates to application of the lithium cobaltate positive electrode material synthesized by the method in preparation of a lithium cobaltate lithium ion battery.
The invention has the beneficial effects that: the lithium cobaltate cathode material with the size between dozens of nanometers and hundreds of nanometers is prepared by ultra-fast synthesis. The lithium cobaltate positive electrode material has the same hexagonal crystal system layered structure as the lithium cobaltate positive electrode material synthesized by the traditional method, is beneficial to the extraction and the insertion of lithium ions, and simultaneously, the valence state of the cobalt ions is positive trivalent as the same as that synthesized by the traditional method. The ultra-fast synthesized lithium cobaltate positive electrode material without any modification has the performance almost the same as the lithium cobaltate positive electrode material synthesized by the traditional method, the first coulombic efficiency is 91% under the cut-off voltage of 4.6V, and the first discharge specific capacity is 200 mAh/g. Meanwhile, under the cut-off voltage of 4.3V, the coulomb efficiency of 100 cycles at 1C is still close to 100%, and the capacity retention rate within 100 cycles is still about 90%.
The small-size lithium cobaltate cathode material is expected to be widely applied to rate-type batteries.
In conclusion, the research work provides a brand new method for rapidly synthesizing the lithium cobalt oxide lithium ion battery cathode material.
Drawings
FIG. 1 is a process for preparing LiCoO according to the present invention2An XRD pattern spectrum of the anode material;
FIG. 2 is LiCoO in the present invention2A Scanning Electron Microscope (SEM) image of the positive electrode material;
FIG. 3(a) is a schematic representation of the preparation of LiCoO according to the invention2A first charge-discharge curve of the material-assembled battery;
FIG. 3(b) is a schematic diagram of the preparation of LiCoO according to the present invention2Cycling curves and coulombic efficiency curves at 1C for the material assembled cells.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the following examples, the alumina ceramic chips were 2cm by 2cm in size and 0.65mm in thickness, and were obtained from Xinghua electronics of Foshan; the carbon cloth was 5cm by 2.5cm in size and was purchased from taiwan carbon technologies, inc.
Example 1
The method for ultra-fast synthesizing the lithium cobaltate cathode material comprises the following steps:
step 1, uniformly mixing 3.3mol of lithium carbonate and 2mol of cobaltosic oxide in a mortar, grinding the mixture to fine powder, namely a lithium cobaltate positive electrode material precursor, and then storing the lithium cobaltate precursor in a vacuum dryer.
Step 2, uniformly paving the lithium cobaltate positive electrode material precursor prepared in the step 1 on an alumina ceramic sheet (the paving mass is 0.05 g/cm)2) The alumina ceramic sheet is placed on a carbon cloth, the carbon cloth is connected to a direct current power supply, and the carbon cloth is electrified in an air atmosphere. Electrifying and calcining twice, electrifying current for primary calcining at 12A for 30s, grinding the primary calcined product, and calcining twiceAnd (3) carrying out secondary calcination with the electrifying current of 35A and the duration of 80s to obtain the lithium cobaltate cathode material.
As shown in fig. 1, the powder X-ray diffraction (XRD) pattern shows that the ultrafast prepared lithium cobaltate positive electrode material has a distinct two-pair bifurcation peak structure, which indicates that it has a good layered structure. With LiCoO2Compared with the standard PDF card, the diffraction peak of the ultrafast synthesized lithium cobaltate is consistent with that of the standard PDF card.
Ultra-fast synthesis of LiCoO2Morphology of the particles, ultra-fast synthesized LiCoO, as shown in FIG. 22The anode material is particles with the nanometer range from tens to hundreds.
To explore ultra-fast synthesized LiCoO2Electrochemical performance of the cathode material we further assembled the cell and tested the electrochemical performance, fig. 3(a) for the preparation of LiCoO2LiCoO of the first charge-discharge curve and charge-discharge platform of the battery assembled by the material2The first discharge specific capacity of a typical charge-discharge platform of the anode material is 200mAh/g, and the first coulombic efficiency can reach 91%, and fig. 3(b) shows that the LiCoO prepared by the method is2According to the cycle curve and the coulombic efficiency curve of the battery assembled by the material under 1C, the capacity retention rate is more than 90% after 100 cycles, the specific discharge capacity is increased after the first several cycles because the material is activated along with the charging and discharging, and the coulombic efficiency is still almost 100% after 100 cycles.
Example 2
The method for ultra-fast synthesizing the lithium cobaltate cathode material comprises the following steps:
step 1, uniformly mixing 3.15mol of lithium carbonate and 2mol of cobaltosic oxide in a mortar, grinding the mixture to fine powder, namely a lithium cobaltate positive electrode material precursor, and then storing the lithium cobaltate precursor in a vacuum dryer.
Step 2, uniformly paving the lithium cobaltate positive electrode material precursor prepared in the step 1 on an alumina ceramic sheet (the paving mass is 0.05 g/cm)2) The alumina ceramic sheet is placed on a carbon cloth, the carbon cloth is connected to a direct current power supply, and the carbon cloth is electrified in an air atmosphere. The electrifying calcination is carried out twice, the electrifying current for one-time calcination is 11A, the duration is 20s, andand grinding the primary calcined product, and then carrying out secondary calcination, wherein the electrifying current of the secondary calcination is 16A, and the duration is 20s, so that the lithium cobaltate cathode material is obtained, and the size of the lithium cobaltate cathode material is below 200nm as shown by SEM.
XRD tests show that the lithium cobaltate obtained in the embodiment is consistent with the diffraction peak of the lithium cobaltate positive electrode material prepared by the traditional method, has a bifurcation peak, and shows that the lithium cobaltate has a good layered structure.
By using the test method in the same embodiment 1, it is determined that the first coulombic efficiency of the lithium cobaltate obtained in this embodiment can reach 90%, the capacity retention rate of the assembled battery is more than 90% after 100 cycles, and the coulombic efficiency is still almost 100% after 100 cycles.
Example 3
The method for ultra-fast synthesizing the lithium cobaltate cathode material comprises the following steps:
step 1, uniformly mixing 3mol of lithium carbonate and 2mol of cobaltosic oxide in a mortar, grinding the mixture to fine powder, namely a precursor of a lithium cobaltate positive electrode material, and then storing the precursor of the lithium cobaltate in a vacuum drier.
Step 2, uniformly paving the lithium cobaltate positive electrode material precursor prepared in the step 1 on an alumina ceramic sheet (the paving mass is 0.05 g/cm)2) The alumina ceramic sheet is placed on a carbon cloth, the carbon cloth is connected to a direct current power supply, and the carbon cloth is electrified in an air atmosphere. And (3) electrifying and calcining twice, wherein the electrifying current for primary calcination is 13A, the duration is 24s, then grinding the primary calcined product and then calcining twice, the electrifying current for secondary calcination is 40A, and the duration is 60s, so that the lithium cobaltate cathode material is obtained, and the size of the lithium cobaltate cathode material is shown by SEM (scanning electron microscope) to be below 200 nm.
XRD tests show that the lithium cobaltate obtained in the embodiment is consistent with the diffraction peak of the lithium cobaltate positive electrode material prepared by the traditional method, has a bifurcation peak, and shows that the lithium cobaltate has a good layered structure.
By using the test method in the same example 1, it is determined that the first coulombic efficiency of the lithium cobaltate obtained in this example can reach 89%, the capacity retention rate of the assembled battery is more than 90% around 100 cycles, and the coulombic efficiency of the assembled battery is still almost 100% after 100 cycles.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (3)
1. A method for rapidly synthesizing a lithium cobaltate positive electrode material is characterized by comprising the following steps: directly grinding 3-3.5 molar parts of lithium carbonate and 2 molar parts of cobaltosic oxide in a mortar until the lithium carbonate and the cobaltosic oxide are uniformly mixed to obtain a lithium cobaltate precursor; placing a lithium cobaltate precursor on an alumina ceramic wafer, wherein the alumina ceramic wafer is positioned on a carbon cloth with two ends connected to a direct-current power supply; electrifying and calcining twice, firstly calcining for the first time, grinding the primary calcined product, and then calcining for the second time to obtain the lithium cobaltate cathode material; the electrifying current for the first calcination is 11-13A, and the duration is 20-30 s; the electrifying current for the second calcination is 16-40A, and the duration is 20-80 s.
2. The method for rapidly preparing a lithium cobaltate positive electrode material according to claim 1, wherein the molar ratio of lithium carbonate to cobaltosic oxide is 3.5: 2.
3. the application of the lithium cobaltate positive electrode material synthesized by the method according to any one of claims 1 to 2 in preparing a lithium cobaltate lithium ion battery.
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