CN113346076B - Surface modified graphite negative electrode material of lithium ion battery and preparation method thereof - Google Patents
Surface modified graphite negative electrode material of lithium ion battery and preparation method thereof Download PDFInfo
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- CN113346076B CN113346076B CN202110528798.7A CN202110528798A CN113346076B CN 113346076 B CN113346076 B CN 113346076B CN 202110528798 A CN202110528798 A CN 202110528798A CN 113346076 B CN113346076 B CN 113346076B
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
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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
- 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 surface modified graphite cathode material of a lithium ion battery and a preparation method thereof, wherein the graphite cathode material is prepared by the following steps: heating the graphite material to a certain temperature in an isolated mode, preserving heat for a period of time, adding the heated graphite into deionized water for rapid cooling, and filtering and drying the graphite material subjected to cooling treatment to obtain the surface modified material. The modified graphite material obtained by the method has better surface characteristics, the surface oxygen-containing groups are reduced, the micropore channels are increased, and the multiplying power charge-discharge performance and the first effect of the material are improved under the condition of ensuring that the charge capacity of the material is not changed. Because graphite material molecule is in active state under high temperature state, the surface stress that the quick cooling produced can make the outermost ink sheet face of material overcome the inter-laminar van der Waals' force and break away from the base member, nevertheless because the base member heat is higher, the ink sheet face that breaks away from can adsorb on the base member fast, forms the effect of normal position cladding, effectively improves material surface state, and this position vacancy becomes the micropore passageway after ink sheet face breaks away from original position simultaneously, is favorable to lithium ion to take off and inlays.
Description
Technical Field
The invention belongs to the field of preparation of lithium battery materials, and particularly relates to a lithium ion battery surface modified graphite negative electrode material and a preparation method thereof.
Background
Lithium ion batteries are increasingly used in human production and life, and include electronic products such as mobile phones, notebook computers and charge pal and electric automobiles, electric buses, serving trolleys and logistics vehicles, etc. all use the lithium ion batteries as power supplies. The negative electrode material is an important component of the lithium ion battery, and the performance of the negative electrode material has great influence on the performance of the lithium ion battery. The particle size, the true density, the morphology, the compacted density and the like of the negative electrode material have influence on the capacity, the multiplying power and the cycle performance of the lithium ion battery, and in order to enable the lithium ion battery to have higher energy density, better multiplying power performance and better cycle performance, the negative electrode material is increasingly modified in various aspects. In studies on modification of negative electrode materials, modification by adding silicon for increasing capacity, modification by surface oxidation for improving cycle performance, and modification of graphite surfaces including coating modification and redox modification have been studied.
The purpose of graphite surface modification is to improve the surface state and improve the material performance. Because some groups, impurities and micropores exist on the surface of the graphite, the surface smoothness is poor, the edges and corners are more, the capacity, the first effect, the multiplying power and the cycling stability of the lithium ion battery are greatly influenced, carbon coating or other modification treatment is carried out on the graphite, surface active sites are reduced, the surface smoothness of particles is improved, the edges and corners of the particles are modified, and the electrical property of the material is favorably improved.
Most of the current graphite surface modification aims at negative electrode materials with high specific surface area and poor morphology, the negative electrode materials with small specific surface area and regular morphology are difficult to further improve the surface performance of the materials, the problems cannot be solved by adopting a conventional coating mode, even the specific surface area can be increased, the particle morphology is influenced, and a counter effect is achieved.
Disclosure of Invention
Aiming at the problems, the invention provides a lithium ion battery surface modified graphite cathode material and a preparation method thereof, and the technical scheme adopted by the invention is as follows:
heating the graphite material to a certain temperature in an air isolation mode, preserving heat for a period of time, adding the heated graphite into deionized water for rapid cooling treatment, and filtering and drying the graphite material subjected to cooling treatment to obtain the surface modified material. The modified graphite material obtained by the method has good surface characteristics, the surface oxygen-containing groups are reduced, the micropore channels are increased, and the multiplying power charge-discharge performance and the first effect of the material are improved under the condition of ensuring that the charge capacity of the material is not changed. Because graphite material molecule is in active state under high temperature state, the surface stress that the quick cooling produced can make the outermost ink sheet face of material overcome the inter-laminar van der Waals' force and break away from the base member, nevertheless because the base member heat is higher, the ink sheet face that breaks away from can adsorb on the base member fast, forms the effect of normal position cladding, effectively improves material surface state, and this position vacancy becomes the micropore passageway after ink sheet face breaks away from original position simultaneously, is favorable to lithium ion to take off and inlays.
Preferably, the graphite heating process must be performed in an oxygen-isolated or inert gas atmosphere, and the inert gas may be argon, nitrogen or argon-nitrogen mixture.
Preferably, the heating temperature of the graphite is 1000 +/-200 ℃, and the heat preservation time is 0.5-3 h.
Preferably, the time from the high temperature state to the rapid cooling heat treatment of the graphite is 10 to 30S.
Preferably, the temperature of deionized water used for rapidly cooling the graphite is 0-100 ℃.
The invention has the beneficial effects that:
the graphite cathode material with the reduced specific surface area and the reduced surface active groups provides a beneficial mode for improving the surface state due to the small specific surface area, the fewer surface groups and the better appearance, and the method has the advantages of simple operation, fewer process steps and strong practicability.
Drawings
FIG. 1 is a schematic view of the surface of an untreated graphite particle;
FIG. 2 is a schematic view showing the state of the surface of graphite particles after being heated at a high temperature and rapidly cooled;
FIG. 3 is a plot of charging and discharging curves for untreated graphite material;
FIG. 4 is a graph showing charging and discharging curves of modified graphite material;
FIG. 5 is a comparative XRD pattern of the graphite material before and after modification;
FIG. 6 is a comparison graph of 10C-rate charge-discharge curves of the graphite material before and after modification;
FIG. 7 is a cyclic voltammogram of the graphite anode material before modification;
FIG. 8 is a cyclic voltammetry graph of a modified graphite anode material;
fig. 9 is a graph comparing infrared curves of the graphite anode material before and after modification.
Detailed Description
Example 1
The artificial graphite cathode material XC-7 is prepared by purifying, shaping and graphitizing coal-based coke, and has the specific surface area of 1.76m 2 (g), capacity of 330mAh/g, first effect of 92.5%, and compacted density of 1.37g/cm 3 Electrode sheetThe porosity is 31%, and the 10C charge-discharge capacity retention rate under a lithium iron system is 86.1%. Taking a certain amount of XC-7, putting the XC-7 into a test crucible, covering a crucible cover, filling coke particles at the edge of the outer surface of the cover, putting the XC-7 into a muffle furnace, isolating air, heating at the high temperature of 900 ℃, keeping the temperature for 1 hour, taking a certain amount of deionized water by using a glass beaker, wherein the amount of water needs to be completely immersed in graphite, controlling the water temperature to be 15 ℃, quickly taking out the crucible after heating, removing the coke particles at the periphery of the cover, opening the cover, quickly pouring the heated graphite into the deionized water, and quickly stirring to uniformly and quickly cool the graphite, wherein the whole operation time is controlled within 15 seconds. Filtering the cooled graphite water solution, taking the filtered graphite as XC-7S, placing the filtered graphite into a vacuum drying oven, drying at 150 ℃ for 12h, and performing physical property test after drying to obtain a specific surface area of 1.52m 2 The reversible capacity is 331mAh/g, the first effect is 92.8 percent, and the compaction density is 1.37g/cm 3 The porosity of the pole piece is 33%, and the 10C charge-discharge capacity retention rate under the lithium iron system is 88.3%. The specific surface area of the modified graphite anode material XC-7 is reduced by 0.24m 2 The porosity of the pole piece is increased by 2%, and the 10C charge-discharge rate performance is improved by 2.2%.
Example 2
The artificial graphite cathode material XC-7 is prepared by purifying, shaping and graphitizing coal-based coke, and has the specific surface area of 1.76m 2 (g), capacity of 330mAh/g, first effect of 92.5%, and compacted density of 1.37g/cm 3 The porosity of the pole piece is 31%, and the 10C charge-discharge capacity retention rate under a lithium iron system is 86.1%. Placing a certain amount of XC-7 into a test crucible, covering the crucible cover, filling coke particles on the outer edge of the cover, placing the cover into a muffle furnace, isolating air, heating at 1200 ℃ under the protection of nitrogen, keeping the temperature for 0.5 h, taking a certain amount of deionized water by using a glass beaker, adding the heated graphite into the deionized water, and rapidly stirring to uniformly and rapidly cool the graphite, wherein the whole operation time is controlled within 30 seconds. Filtering the cooled graphite water solution, taking the filtered graphite as XC-7S1, drying in a vacuum drying oven at 120 deg.C for 12h, and testing physical properties with specific surface area of 1.49m 2 Per g, 332mAh/g capacity, 93.1% first effectThe compacted density is 1.38g/cm 3 The porosity of the pole piece is 34%, and the retention rate of 10C charge-discharge capacity under a lithium iron system is 88.9%. The specific surface area of the modified graphite anode material XC-7 is reduced by 0.27m 2 The porosity of the pole piece is increased by 3%, and the 10C charge-discharge rate performance is improved by 2.9%.
Example 3
The artificial graphite cathode material XC-7 is prepared by purifying, shaping and graphitizing coal-based coke, and has the specific surface area of 1.76m 2 G, capacity of 330mAh/g, first effect of 92.5 percent and compacted density of 1.37g/cm 3 The porosity of the pole piece is 31%, and the charge-discharge capacity retention rate of 10C under a lithium iron system is 86.1%. Taking a certain amount of XC-7, putting the XC-7 into a test crucible, covering the crucible cover, filling coke particles on the outer edge of the cover, putting the cover into a muffle furnace, isolating air, heating at the high temperature of 800 ℃ under the protection of nitrogen, keeping the temperature for 3 hours, taking out the crucible quickly after the heating is finished, removing the coke particles on the periphery of the cover, opening the cover, pouring the heated graphite into deionized water quickly, stirring quickly, and cooling the graphite uniformly and quickly. Filtering the cooled graphite water solution, taking the filtered graphite as XC-7S2, placing the filtered graphite into a vacuum drying oven for drying at 120 ℃ for 12h, and performing physical property test after drying to obtain a specific surface area of 1.55m 2 Per g, capacity of 330mAh/g, first effect of 92.9%, and compacted density of 1.36g/cm 3 The porosity of the pole piece is 33.5%, and the charge-discharge capacity retention rate of 10C under a lithium iron system is 88.5%. The specific surface area of the modified graphite anode material XC-7 is reduced by 0.21m 2 The porosity of the pole piece is increased by 2.5 percent, and the charge-discharge rate performance of 10C is improved by 2.4 percent.
The negative electrode materials prepared in the above examples were assembled into a lithium ion battery, and electrochemical performance tests were performed, and the results are shown in the following table:
as can be seen from the particle size and tap density, the particle size and tap density before and after modification hardly changed, and as can be seen from the specific surface area, the ratio after modificationThe surface area is reduced by 0.21-0.27m 2 /g。
According to the electricity deduction data, the gram specific capacity is not improved after modification, and the first coulombic efficiency is improved by 0.2-0.6%.
As can be seen from the porosity data, the porosity after modification is increased by 2-3%, and the porosity test method comprises the following steps: taking 1cm 2 Weighing the negative pole piece, recording as m1, dripping sufficient amount of hexadecane, standing for 12h, sucking off excessive liquid by using oil absorption paper, weighing, recording as m2, and calculating the volume V of the sucked hexadecane Hole(s) ＝(m2-m1)/ρ Hexadecane (Hexadecane) The porosity n, n = V is the volume of the pores divided by the volume of the pole piece dressing Hole(s) /V Material 。
As can be seen from the 10C multiplying power charge-discharge data, the multiplying power is improved by 2.2-2.9% after modification.
As can be seen from the XRD contrast, XC-7 has a diffraction pattern substantially identical to that of XC-7S of the modified material, and has a strong (002) diffraction peak at 2 theta =26.4 degrees, which corresponds to
Indicating that they all have a complete graphite crystal structure.
As can be seen from the cyclic voltammetry curve, XC-7 and XC-7S both conform to the characteristics of a graphite CV curve, and the oxidation peak of XC-7S after modification is obviously enlarged, which indicates that modification treatment eliminates some irregular structures on the graphite surface, so that the graphite surface is more uniform, the irreversible capacity of the material is reduced, oxidation can form some nano channels on the graphite surface, the nano channels can only allow lithium ions to be reversibly inserted and removed, and solvated ions or solvent molecules cannot be inserted, thereby improving the reversible lithium storage capacity of the graphite material.
As can be seen from the infrared spectrogram, XC-7S of the modified material is 3436.50cm -1 The absorption peak disappears, and the surface hydroxyl functional groups are reduced, which shows that the modification improves the surface state of the material, reduces the surface functional groups of the material and is beneficial to improving the processing performance and the electrical performance of the material.
Claims (7)
1. Surface modified graphite negative electrode material of lithium ion batteryThe material is prepared by modifying a graphite negative electrode material, and the graphite negative electrode material has a specific surface area of 1.3-2.0 m 2 G, compacted density of 1.3-1.45 g/cm 3 Particle size and distribution D10 of 6.5-7.5 μm, D50 of 14-16 μm, D90 of 27-30 μm, XRD diffractogram having a strong (002) diffraction peak at 2 theta =26.4 DEG, D002=3.354 ANG, and infrared spectrogram at 3436.50cm -1 Has an absorption peak, and is characterized in that:
insulating air from the graphite cathode material, heating the graphite cathode material to a certain temperature, preserving heat for a period of time, adding the heated graphite cathode material into deionized water for rapid cooling treatment, and filtering and drying the cooled graphite cathode material to obtain a surface modified graphite cathode material; the heating temperature of the negative electrode material is 1000 +/-200 ℃, and the heat preservation time is 0.5 to 3h; the time from the high-temperature state to the rapid cooling heat treatment of the negative electrode material is 10 to 30S; rapidly cooling the cathode material by using deionized water at the temperature of 0-100 ℃;
the infrared spectrogram of the surface modified graphite cathode material is 3436.50cm -1 No absorption peak, and the modified surface hydroxyl functional group is reduced; the specific surface area of the surface modified graphite negative electrode material is reduced by 0.21-0.27m 2 /g。
2. The lithium ion battery surface modified graphite negative electrode material of claim 1, characterized in that: the CV curve oxidation peak of the surface modified graphite cathode material is larger than that of the graphite cathode material.
3. The lithium ion battery surface modified graphite negative electrode material of claim 1, characterized in that: the porosity of the negative electrode material pole piece is increased by at least 2%, and the 10C discharge rate is improved by at least 2.2%.
4. The surface-modified graphite negative electrode material of the lithium ion battery according to any one of claims 1 to 3, characterized in that: the initial coulombic efficiency of the surface modified graphite negative electrode material is improved by at least 0.3%.
5. The preparation method of the surface modified graphite negative electrode material of the lithium ion battery of any one of claims 1 to 4, which is characterized by comprising the following steps: isolating the graphite cathode material from air, heating to a certain temperature, preserving heat for a period of time, adding the heated graphite cathode material into deionized water for rapid cooling treatment, filtering and drying the cooled graphite cathode material to obtain a surface modified graphite cathode material;
the heating temperature of the negative electrode material is 1000 +/-200 ℃, and the heat preservation time is 0.5 to 3h; the time from the high-temperature state to the rapid cooling heat treatment of the negative electrode material is 10 to 30S; and (3) rapidly cooling the cathode material by using deionized water at the temperature of 0-100 ℃.
6. The lithium ion battery surface modified graphite negative electrode material and the preparation method thereof according to claim 5 are characterized in that: the heating process of the graphite cathode material must be carried out in an oxygen-isolated environment.
7. The lithium ion battery surface modified graphite negative electrode material and the preparation method thereof according to claim 6 are characterized in that: the heating process of the graphite cathode material must be carried out in an inert gas protection environment.
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| JP2004111110A (en) * | 2002-09-13 | 2004-04-08 | Kansai Coke & Chem Co Ltd | Manufacturing method of electrode material for secondary battery |
| CN107720745A (en) * | 2017-09-05 | 2018-02-23 | 河南易成新能源股份有限公司 | Graphite cathode material heat-treatment furnace cooling system and cooling means |
| CN111864203A (en) * | 2019-04-28 | 2020-10-30 | 中国科学院上海硅酸盐研究所 | High-capacitance lithium-carbon negative electrode material and preparation method and application thereof |
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| WO2006003849A1 (en) * | 2004-06-30 | 2006-01-12 | Mitsubishi Chemical Corporation | Negative electrode material for lithium secondary battery, method for producing same, negative electrode for lithium secondary battery using same and lithium secondary battery |
| CN102569753A (en) * | 2010-12-10 | 2012-07-11 | 新乡远东电子科技有限公司 | Carbon negative electrode material for lithium-ion secondary battery for power application and preparation method thereof |
| CN105702945B (en) * | 2016-03-02 | 2018-08-28 | 华南师范大学 | Liquid phase in-situ reducing-cold quenching preparation method and applications of composite negative pole material |
| US11369929B2 (en) * | 2017-06-22 | 2022-06-28 | University Of Maryland, College Park | Nanoparticles and systems and methods for synthesizing nanoparticles through thermal shock |
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| JP2004111110A (en) * | 2002-09-13 | 2004-04-08 | Kansai Coke & Chem Co Ltd | Manufacturing method of electrode material for secondary battery |
| CN107720745A (en) * | 2017-09-05 | 2018-02-23 | 河南易成新能源股份有限公司 | Graphite cathode material heat-treatment furnace cooling system and cooling means |
| CN111864203A (en) * | 2019-04-28 | 2020-10-30 | 中国科学院上海硅酸盐研究所 | High-capacitance lithium-carbon negative electrode material and preparation method and application thereof |
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