CN119725497A - A doped graphite negative electrode material and its preparation method and application - Google Patents
A doped graphite negative electrode material and its preparation method and application Download PDFInfo
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Abstract
本发明公开了一种掺杂石墨负极材料及其制备方法和应用，属于可充电二次电池负极材料技术领域。掺杂石墨负极材料包括内核和内核外层的壳体；所述内核为元素掺杂的掺杂石墨二次颗粒；掺杂石墨二次颗粒的掺杂方式为固相掺杂或液相掺杂；所述壳体包括气相沉积形成的掺杂元素的碳包覆层；掺杂元素的总质量占掺杂石墨负极材料质量的0.5‑10%。本发明提供的掺杂石墨负极材料，对石墨二次颗粒内核及碳包覆层均进行了元素掺杂处理，利用元素掺杂改善石墨的微观结构，并形成活性位点缺陷，有助于电荷载体的扩散，提升材料动力学表现；同时扩大石墨层间距；碳包覆层隔绝石墨二次颗粒内核与电解液直接接触，全方位、多角度综合性的提升了掺杂石墨负极的快充性能。
The present invention discloses a doped graphite negative electrode material and a preparation method and application thereof, and belongs to the technical field of negative electrode materials for rechargeable secondary batteries. The doped graphite negative electrode material includes an inner core and a shell of an outer core layer; the inner core is an element-doped doped graphite secondary particle; the doping method of the doped graphite secondary particle is solid-phase doping or liquid-phase doping; the shell includes a carbon coating layer of doped elements formed by vapor deposition; the total mass of the doped elements accounts for 0.5-10% of the mass of the doped graphite negative electrode material. The doped graphite negative electrode material provided by the present invention performs element doping treatment on the inner core and the carbon coating layer of the graphite secondary particle, and improves the microstructure of the graphite by element doping, and forms active site defects, which is conducive to the diffusion of charge carriers and improves the kinetic performance of the material; at the same time, the graphite interlayer spacing is enlarged; the carbon coating layer isolates the inner core of the graphite secondary particle from direct contact with the electrolyte, and comprehensively improves the fast charging performance of the doped graphite negative electrode in all directions and from multiple angles.
Description
Technical Field
The invention relates to the technical field of rechargeable secondary battery anode materials, in particular to a graphite-doped anode material, a preparation method and application thereof.
Background
The method for improving the quick charge performance of the graphite mainly comprises the steps of 1) reducing the size, shortening the migration path of lithium ions, 2) making a porous structure, increasing the migration channel of the lithium ions, and simultaneously increasing the wettability of electrolyte, 3) coating a layer of soft carbon or hard carbon on the surface of the graphite, thereby improving quick charge, but simple carbon coating simultaneously causes deterioration of high-temperature performance, because the coated carbon layer is usually easier to react with electrolyte due to a secondary reaction with the amorphous structure, 4) element doping, and element doping effects can be summarized as points, namely, the first aspect of charging and discharging of the graphite is higher, and the risk of lithium precipitation is increased, and the method for improving the quick charge performance of the graphite mainly comprises the steps of 1) reducing the size, shortening the migration path of the lithium ions, 2) making a porous structure, increasing the interlayer spacing, and simultaneously increasing the wettability of the electrolyte, and 3) coating a layer of soft carbon or hard carbon on the surface of the graphite, thereby improving quick charge, but the simple carbon coating simultaneously causes deterioration of high-temperature performance, and the element doping effects of the coated carbon layer are more easily side-reacted with the electrolyte, and 4) element doping effects are summarized as the first aspect of the doping effect, and the change of the electron charge performance and the electron charge rate of the graphite are improved, and the shuttle material is more than the three-dimensional charge performance, and the electron charge performance is more than the conventional, and the factor is more than 35.
The patent CN116022781B mixes the carbon source precursor and the boron doped source and then heats the mixture in sections, and finally graphitizes the mixture to obtain the boron doped graphite anode material, so that the stability of the battery is ensured, and capacity and compaction and quick charge capacity are improved. The patent CN117342552A mixes raw coke and metal potassium, after temperature programming, heteroatom gas is introduced for doping, then graphitization energy storage is carried out, finally gas phase carbon cladding is carried out to obtain heteroatom doped porous graphite, the raw coke is subjected to layer expansion through potassium gasification, and a graphite cathode with large interlayer spacing is obtained after graphitization, so that the quick charging performance of the material is improved, the electronic conductivity is improved at the defect position of the raw coke through heteroatom doping, and the multiplying power performance is improved.
According to the technical scheme, the doping of the graphite anode material is lack of reasonable structural design, the doping process is not optimized, the doping uniformity is poor, and the quick charging performance of the material is improved.
Disclosure of Invention
The invention aims to provide a doped graphite anode material capable of improving the quick charge performance of a rechargeable secondary battery, and also aims to provide a preparation method of the doped graphite anode material with more reasonable and uniform doping, and further aims to provide an application of the doped graphite anode material.
The invention discloses a doped graphite anode material which is of a core-shell structure and comprises an inner core and a shell of an inner core outer layer, wherein the inner core is doped graphite secondary particles doped with elements, the doping mode of the doped graphite secondary particles is solid-phase doping or liquid-phase doping, the shell is a carbon coating layer formed by vapor deposition and provided with doping elements, and the total mass of the doped elements in the inner core and the shell accounts for 0.5-10% of the mass of the doped graphite anode material.
The doping element is one or more of N, B, P, S, F, O.
The outer layer doped carbon coating is vapor deposition coating, the coating is more compact and uniform, the direct contact between the inner core of the doped graphite secondary particle and the electrolyte can be well isolated, and side reactions with the electrolyte are reduced.
The doping source of the doped carbon coating layer is gas phase, so that the doping is more uniform. Solid phase doping can only rely on interparticle penetration and reaction, and vapor deposition doping is relatively more uniform than solid phase deposition doping.
Further, the total mass of the doping elements accounts for 2-5% of the mass of the doped graphite anode material.
The invention also provides a preparation method of the doped graphite anode material, which comprises the following steps:
s1, mixing a carbon-based material, a doping agent and a bonding carbon source to obtain a mixed material A;
s2, granulating and sintering the mixed material A, and graphitizing the granulated and sintered material at a high temperature to obtain a doped graphite core B;
s3, crushing and sieving the doped graphite core B;
and S4, introducing carbon source gas, doping source gas and carrier gas, and performing vapor deposition on a carbon coating layer doped with elements on the surface of the screened doped graphite core B to obtain the doped graphite anode material.
The element doping is completed in the graphitization and outer carbon coating processes, no extra step is needed, the cost is low, and the method is suitable for large-scale production.
Further, in the step S1, the carbon-based material includes any one of needle coke, petroleum coke and pitch coke, the dopant includes any one of urea, melamine, boron oxide, boric acid, boron nitride, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, phosphorus pentoxide, sodium sulfate, ammonium persulfate, thiourea, polytetrafluoroethylene, polyvinylidene fluoride, silicon tetrafluoride and hydrogen peroxide, and the bonding carbon source includes any one of pitch, resin and coal tar or a combination of at least two of them.
Simultaneously, different elements are doped, and the synergistic effect among the elements is utilized, so that the doping reaction is easier to carry out, and the doping effect is better.
Further, in the step S1, the mass ratio of the carbon-based material, the dopant and the binder carbon source is (10-25): (0.2-1.5): 1.
Mixing the carbon-based material, the doping agent and the bonding carbon source is solid-phase mixing or liquid-phase mixing, wherein the solid-phase mixing is carried out in a VC mixer, a kneader or a ball mill to obtain a mixed material A, the liquid-phase mixing is carried out by dispersing the material in an organic solvent, and the spray drying is carried out to obtain the mixed material A.
In the step S2, the granulating and sintering process is that in the protective gas atmosphere, the temperature is firstly kept at 200-350 ℃ for 1-3h, and then kept at 800-1000 ℃ for 2-5 h.
The primary graphite particles are bonded into secondary particles, compaction and low-temperature performance are improved, the granulation process firstly keeps the temperature at 200-350 ℃ to soften the bonded carbon source, the bonding effect is formed, and the carbonization at 800-1000 ℃ is to crack the carbon source into carbon.
Granulating by adopting a granulating kettle which is a horizontal granulating kettle or a vertical granulating kettle. High temperature graphitization is performed in an acheson furnace.
Further, in the step S2, the high-temperature graphitization treatment condition is that the temperature is 2800-3000 ℃ and the time is 12-24 hours.
Further, in the step S4, the carbon source gas includes any one or a combination of at least two of acetylene, methane, propylene, acetone and natural gas, the doping source gas includes any one or a combination of at least two of ammonia, diborane, ding Pengwan, boron fluoride and phosphine, and the carrier gas includes any one of nitrogen, argon and helium.
In step S4, the flow ratio of the carbon source gas to the doping source gas to the carrier gas is 1 (0.2-2.5) (2-5), the vapor deposition temperature is 800-1000 ℃, and the treatment time is 2-6 h.
The invention also discloses application of the doped graphite anode material, and the doped graphite anode obtained by the preparation method is applied to manufacturing of rechargeable secondary batteries.
Rechargeable secondary batteries include lithium ion batteries, sodium ion batteries.
Mixing the doped graphite anode material, the conductive agent, the binder and the like, coating the mixture on a current collector, and processing to prepare the anode piece of the rechargeable secondary battery.
The doped graphite anode material provided by the invention adopts a twice doping mode to carry out element doping treatment on the graphite secondary particle inner core and the carbon coating layer, improves the microstructure of graphite by utilizing element doping, forms active site defects, is beneficial to the diffusion of charge carriers, improves the material dynamics performance, enlarges the graphite layer spacing, isolates the graphite secondary particle inner core from being in direct contact with electrolyte, and comprehensively improves the quick charge performance of the doped graphite anode in an all-around and multi-angle manner.
Drawings
FIG. 1 is a schematic structural diagram of a doped graphite anode material provided in example 1 of the present invention, wherein 1 is a nitrogen-doped carbon coating shell, 2 is a nitrogen-doped boron-doped graphite secondary particle core;
FIG. 2 is an SEM image of a doped graphite anode material prepared according to example 1 of the present invention;
Fig. 3 is a graph showing charge rate performance of the anode materials prepared in example 1 and comparative examples 1 to 3 according to the present invention.
Detailed Description
In order to make the technical scheme of the invention clearer, the invention is further described in detail below with reference to the attached drawings and specific embodiments.
The specific techniques or conditions are not identified in the examples and are described in the literature in this field or are carried out in accordance with the product specifications. All reagents or instrumentation are conventional products available for purchase by regular vendors, not noted to the manufacturer.
Example 1
The preparation method of the doped graphite anode material comprises the following steps:
s1, adding 2kg of needle coke, 150g of asphalt, 50g of melamine and 100g of boron oxide into a VC mixer, and mixing for 30min at 1000r/min to obtain a mixed material A.
S2, adding the mixed material A obtained in the step S1 into a horizontal granulating kettle, heating to 300 ℃ at 5 ℃ per min under the N 2 coating atmosphere, preserving heat for 2 hours, heating to 800 ℃ at 2 ℃ per min, preserving heat for 2 hours, naturally cooling to room temperature, transferring the granulated and sintered material into an Acheson graphitizing furnace, treating for 12 hours at 2800 ℃, graphitizing, and cooling to room temperature to obtain the doped graphite core B.
S3, crushing the doped graphite core B prepared in the step S2, and sieving the crushed doped graphite core B with a 200-mesh sieve.
And S4, placing the screened doped graphite core B in a CVD rotary furnace, firstly introducing argon for 1L/min to discharge air in the furnace, then heating to 800 ℃, adjusting the argon flow to 3L/min, introducing ammonia for 1L/min and acetylene gas for 1L/min, and treating for 4 hours to coat the doped graphite core B with a nitrogen-doped carbon layer to obtain the doped graphite anode material.
As shown in figure 1, the prepared graphite-doped anode material is provided with a nitrogen-and boron-doped graphite secondary particle core and a nitrogen-doped carbon coating layer shell.
The doped graphite anode material obtained in example 1 was subjected to Scanning Electron Microscope (SEM) examination to examine the microstructure thereof, and the result is shown in fig. 2. It can be seen from fig. 2 that the doped graphite anode material exhibits a granulated secondary structure.
Example 2
The preparation method of the doped graphite anode material comprises the following steps:
S1, adding 2kg of petroleum coke green coke, 200g of asphalt, 100g of boron oxide and 100g of ammonium dihydrogen phosphate into a VC mixer, and mixing at 1000r/min for 30min to obtain a mixed material A.
S2, adding the mixed material A obtained in the step S1 into a horizontal granulating kettle, heating to 280 ℃ at 5 ℃ per min under the atmosphere of N 2, preserving heat for 2 hours, heating to 800 ℃ at 2 ℃ per min, preserving heat for 2 hours, naturally cooling to room temperature, transferring the granulated and sintered material into an Acheson graphitizing furnace, treating for 12 hours at 3000 ℃, graphitizing, and cooling to room temperature to obtain the doped graphite core B.
S3, crushing the doped graphite core B prepared in the step S2, and sieving the crushed doped graphite core B with a 200-mesh sieve.
And S4, placing the screened doped graphite core B in a CVD rotary furnace, firstly introducing argon for 1L/min to discharge air in the furnace, then heating to 850 ℃, adjusting the argon flow to 3L/min, introducing ammonia for 1L/min, phosphine gas for 1L/min and acetylene gas for 1L/min, treating for 4 hours, and coating the doped graphite core B with a nitrogen and phosphorus co-doped carbon layer to obtain the doped graphite anode material.
Comparative example 1
The preparation process is the same as in example 1, except that in step S1, the nitrogen source melamine and the boron source boron oxide are not added during the mixing of the materials.
Comparative example 2
The preparation process is the same as in example 1, except that in step S4, the nitrogen source gas ammonia gas is not introduced when the carbon source and argon gas are introduced.
Comparative example 3
The preparation process is the same as in example 1, except that in step S1, the nitrogen source melamine and the boron source boron oxide are not added during material mixing, and in step S4, the nitrogen source gas ammonia is not introduced during carbon source and argon gas introduction.
Performance test:
The negative electrode materials prepared in examples 1-2 and comparative examples 1-3 were assembled into a type 2032 button cell for evaluation, and the specific scheme is that the negative electrode material, the conductive agent SP, the conductive agent VGCF and the binder LA136D were mixed according to the ratio of 75:5:10:10, water was used as a solvent, the mixture was made into a slurry, the slurry was coated on a copper foil, a counter electrode was a lithium sheet, a diaphragm was a Celgard2400 microporous polypropylene film, the charge and discharge cut-off voltage was 0.005-1.5V, the discharge rate was 0.1C constant current discharge to 0.005V, the discharge rate was 0.02C discharge to 0.005V, the charge rate was 0.1C charge to 1.5V, and the test structure was shown in Table 1.
Table 1 shows the buckling test results of examples 1-2 and comparative examples 1-3
| Material | First lithium intercalation capacity (mAh/g) | First lithium removal capacity (mAh/g) | First time efficiency (%) |
| Example 1 | 374.9 | 352.4 | 94 |
| Example 2 | 372.3 | 350.7 | 94.2 |
| Comparative example 1 | 371.7 | 347.5 | 93.5 |
| Comparative example 2 | 373.8 | 345 | 92.3 |
| Comparative example 3 | 372.5 | 342.7 | 92 |
As shown in Table 1, compared with comparative examples 1-3, the doped graphite anode materials prepared in examples 1-2 have higher reversible capacity and initial efficiency, and the fact that the two-time element doping has obvious improvement on lithium ion and electron transmission of the materials is proved, meanwhile, polarization is reduced, lithium storage sites are increased, capacity is improved, and comprehensive performance of the anode materials is improved greatly.
The button cells prepared in example 1 and comparative examples 1-3 were tested for rate performance by calibrating the constant current and constant voltage charging at 0.1C to 1.5V and constant current discharging at 0.1C to 0.005V for three weeks, then constant current charging at 0.5C to 1.5V and constant current discharging at 0.5C to 0.005V for three weeks, then constant current charging at 1C to 1.5V and constant current discharging at 1C to 0.005V for three weeks, then constant current charging at 2C to 1.5V and constant current discharging at 2C to 0.005V for three weeks, finally constant current charging at 3C to 1.5V and constant current discharging at 3C to 0.005V, and the retention rate at each charging rate was calculated to determine the rapid charging performance of different materials, and the results are shown in FIG. 3.
As shown in fig. 3, compared with comparative examples 1 to 3, the element doping before and after graphitization in example 1 can greatly improve the quick charge performance of the graphite material, the charge capacity at 2C and 3C is obviously improved, and the effect of single-side doping before graphitization or after graphitization is better than that of comparative examples 1 and 2.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
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