CN110429277B - Preparation method of high-compaction high-rate lithium iron phosphate cathode material - Google Patents
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Abstract
The invention discloses a preparation method of a high-compaction high-rate lithium iron phosphate cathode material, which relates to the technical field of lithium ion battery cathode materials and comprises the following steps: taking the g-C of the laminar mesoporous graphite phase carbon nitride powder according to the mass ratio of 100: 4.5: 0.5-43N4PVP and carbohydrate are added into deionized water and dispersed to obtain dispersion liquid A; according to FePO4∶g‑C3N4Weighing FePO at a mass ratio of 50 to (0.8-1.5)4Adding the mixture into the dispersion liquid A, and dispersing to obtain dispersion liquid B; weighing a lithium source according to the stoichiometric ratio of Fe to Li of 1 to 1, adding the lithium source into the dispersion liquid B, and dispersing to obtain a dispersion liquid C; and (3) carrying out superfine grinding on the dispersion liquid C, carrying out spray drying, presintering and sintering in a protective atmosphere, and naturally cooling to obtain the dispersion liquid C. In the invention, g-C3N4The PVP is used as a layered template and a main carbon source, and the excellent dispersion property of PVP is utilized to perform shape regulation and modification in the lithium iron phosphate manufacturing process, so that the compaction and charge-discharge rate performance of the lithium iron phosphate anode material can be greatly improved.
Description
Technical Field
The invention relates to the technical field of lithium ion battery anode materials, in particular to a preparation method of a high-compaction high-rate lithium iron phosphate anode material.
Background
In recent years, as the influence of fossil energy on the global environment is increased, clean energy has been popularized and applied as a substitute. As a representative of clean energy, new energy batteries are gradually becoming the first choice for passenger cars, buses, and energy storage utilities. The lithium iron phosphate battery is a hotspot for current new energy battery research due to low price, high theoretical capacity (about 170mAh/g), stable working voltage, no toxicity, environmental protection, stable structure, good safety performance, good thermal stability and ultra-long cycle life. In terms of the currently developed lithium iron phosphate product, the material also has the defects of low ion conductivity, poor conductivity, low compaction density, poor low-temperature performance and the like, so that the problems of low energy density, poor processability and the like are caused, and the wide application of the material in power batteries is limited.
In order to solve the problems, related researchers improve the rate performance or compaction of the material by performing nanocrystallization treatment and carbon coating on the lithium iron phosphate material, but most of the lithium iron phosphate materials can only meet the single high rate or high compaction performance, the high compaction high rate cannot be achieved at the same time, and the problems of uneven carbon coating, poor machining performance and the like of the material exist. How to optimize the lithium iron phosphate process, the material has high rate performance and the compaction density is improved, which is a key research target at present.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of a high-compaction high-rate lithium iron phosphate anode material, which is characterized in that g-C is adopted3N4The layered template is used, a layered lithium iron phosphate finished product with uniform carbon coating is obtained by a layered template method, and the compaction and charge-discharge rate performance of the material can be greatly improved.
The invention provides a preparation method of a high-compaction high-rate lithium iron phosphate cathode material, which comprises the following steps of:
s1, taking g-C of laminar mesoporous graphite phase carbon nitride powder according to the mass ratio of 100: 4.5: 0.5-43N4Adding polyvinyl pyrrolidone (PVP) and saccharides into deionized water, and dispersing to obtain a dispersion liquid A;
s2 according to FePO4∶g-C3N4Weighing FePO at a mass ratio of 50 to (0.8-1.5)4Adding into the dispersion A, dispersing, and getting the dispersionSolution B;
s3, weighing a lithium source according to the stoichiometric ratio of Fe to Li of 1 to 1, adding the lithium source into the dispersion liquid B, and dispersing to obtain dispersion liquid C;
and S4, carrying out superfine grinding on the dispersion liquid C, carrying out spray drying to obtain a lithium iron phosphate precursor, presintering and sintering the precursor in a protective atmosphere, and naturally cooling to obtain the high-compaction high-rate performance lithium iron phosphate cathode material.
Preferably, in S1, the layered mesoporous graphite phase carbon nitride powder g-C3N4The thickness of (A) is 90-120 nm; preferably, g-C3N4The preparation of (a) was as follows: according to the weight ratio of 11.5: 1, dissolving urea and ammonium sulfate in ultrapure water according to the mass ratio, preparing a solution with the solid content of 55%, drying at 65-80 ℃ for 19-24h, sintering in a tube furnace at 600 ℃ for 5-8h to obtain a powder sample, and ultrasonically stripping the powder sample in the ultrapure water for 12h to obtain layered mesoporous graphite phase carbon nitride powder g-C3N4。
Preferably, in S1, the molecular weight of polyvinylpyrrolidone PVP is 8000-16000; preferably, the saccharide is one or more of glucose, fructose, galactose, sucrose, maltose and starch.
Preferably, in S1, dispersing for 30-50 min.
Preferably, in S2, the dispersion is 0.5-2 h.
Preferably, in S3, the lithium source is any one of lithium carbonate and lithium hydroxide or a mixture of the two.
Preferably, in S3, dispersing is carried out for 2-3.5 h.
Preferably, in S4, the particle size D50 of the dispersion C after ultrafine grinding is 300-400 nm.
Preferably, in S4, the protective atmosphere is one or more of high-purity nitrogen, high-purity helium, and high-purity argon.
Preferably, in S4, the pre-sintering is carried out at 460 ℃ of 330 ℃ for 3-5h, and the sintering is carried out at 790 ℃ of 680 ℃ for 8-14 h.
Has the advantages that: the invention provides a preparation method of a high-compaction high-rate lithium iron phosphate anode material, which is prepared from layered mesoporous graphite phase carbon nitride powder g-C3N4As a layered template, g-C is added by utilizing the excellent dispersing property of PVP3N4The iron phosphate particles and the saccharides are uniformly dispersed and coated on the surfaces of the iron phosphate particles, the particles are tightly combined together by controlling the superfine grinding granularity, an intercalation spherical precursor is formed during later drying granulation, the particle compactness is higher, the lithium iron phosphate can grow on the basis of a layered template to form a layered structure under low-temperature sintering, and g-C is formed along with the temperature transition3N4The template is decomposed and uniformly coated in a lithium iron phosphate layered structure in a carbon source form, and the lithium iron phosphate anode material obtained by the layered template method can greatly improve the compaction and charge-discharge rate performance of the material.
Drawings
Fig. 1 is an SEM image of a lithium iron phosphate material prepared in example 1 of the present invention;
fig. 2 is an SEM image of a lithium iron phosphate material prepared in a comparative example of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
(1) Dissolving urea and ammonium sulfate in ultrapure water according to the mass ratio of 11.5: 1 to prepare a solution with the solid content of 55%, drying at 70 ℃ for 20h to obtain a dried material, sintering the dried material in a 570 ℃ tubular furnace for 7h to obtain a powder sample, and ultrasonically stripping the powder sample in the ultrapure water for 12h to obtain the laminar mesoporous graphite phase carbon nitride powder (g-C) with the thickness of 100nm3N4);
(2) Weighing g-C in the step (1) according to the mass ratio of 100: 4.5: 13N4PVP with the relative molecular weight of 10000 and glucose are added into deionized water to be dispersed for 40min to obtain dispersion A;
(3) according to FePO4∶g-C3N4Weighing FePO at a mass ratio of 50: 14Adding the lithium source into the dispersion liquid A in the step (2) to disperse for 1h to obtain dispersion liquid B, then weighing the lithium source according to the stoichiometric ratio of Fe to Li of 1: 1, adding the lithium source into the dispersion liquid B to disperse for 2.5h to obtain dispersion liquid C;
(4) and (3) carrying out superfine grinding on the dispersion liquid C in the step (3) for 2h, wherein the ground granularity D50 is 380nm, carrying out spray drying to obtain a lithium iron phosphate precursor, presintering the precursor for 4h at 420 ℃ in a protective atmosphere, sintering for 12h at 710 ℃, and naturally cooling to obtain the high-compaction high-rate lithium iron phosphate cathode material.
FIG. 1 is an SEM image of lithium iron phosphate prepared in this example, which is clearly shown in g-C3N4The lithium iron phosphate material prepared by the template has a lamellar structure with uniformly distributed sizes, carbon is uniformly coated, and the surface of the material is free from amorphous carbon.
Example 2
(1) Dissolving urea and ammonium sulfate in ultrapure water according to the mass ratio of 11.5: 1 to prepare a solution with the solid content of 55%, drying at 70 ℃ for 20h to obtain a dried material, sintering the dried material in a 570 ℃ tubular furnace for 7h to obtain a powder sample, and ultrasonically stripping the powder sample in the ultrapure water for 12h to obtain the laminar mesoporous graphite phase carbon nitride powder (g-C) with the thickness of 100nm3N4);
(2) Weighing g-C in the step (1) according to the mass ratio of 100: 4.5: 0.53N4PVP with the relative molecular weight of 10000 and glucose are added into deionized water to be dispersed for 40min to obtain dispersion A;
(3) according to FePO4∶g-C3N4Weighing FePO at a mass ratio of 50: 14Adding the lithium source into the dispersion liquid A in the step (2) to disperse for 1h to obtain dispersion liquid B, then weighing the lithium source according to the stoichiometric ratio of Fe to Li of 1: 1, adding the lithium source into the dispersion liquid B to disperse for 2.5h to obtain dispersion liquid C;
(4) and (3) carrying out superfine grinding on the dispersion liquid C in the step (3) for 2h, wherein the ground granularity D50 is 380nm, carrying out spray drying to obtain a lithium iron phosphate precursor, presintering the precursor for 4h at 420 ℃ in a protective atmosphere, sintering for 12h at 710 ℃, and naturally cooling to obtain the high-compaction high-rate lithium iron phosphate cathode material.
Example 3
(1) Dissolving urea and ammonium sulfate in ultrapure water at a mass ratio of 11.5: 1 to obtain a solution with a solid content of 55%, drying at 70 deg.C for 20 hr to obtain a dried material, and dryingSintering the dried material in a 570 ℃ tubular furnace for 7h to obtain a powder sample, and ultrasonically stripping the powder sample in ultrapure water for 12h to obtain 100 nm-thick layered mesoporous graphite phase carbon nitride powder (g-C)3N4);
(2) Weighing g-C in the step (1) according to the mass ratio of 100: 4.5: 43N4PVP with the relative molecular weight of 10000 and glucose are added into deionized water to be dispersed for 40min to obtain dispersion A;
(3) according to FePO4∶g-C3N4Weighing FePO at a mass ratio of 50: 14Adding the lithium source into the dispersion liquid A in the step (2) to disperse for 1h to obtain dispersion liquid B, then weighing the lithium source according to the stoichiometric ratio of Fe to Li of 1: 1, adding the lithium source into the dispersion liquid B to disperse for 2.5h to obtain dispersion liquid C;
(4) and (3) carrying out superfine grinding on the dispersion liquid C in the step (3) for 2h, wherein the ground granularity D50 is 380nm, carrying out spray drying to obtain a lithium iron phosphate precursor, presintering the precursor for 4h at 420 ℃ in a protective atmosphere, sintering for 12h at 710 ℃, and naturally cooling to obtain the high-compaction high-rate lithium iron phosphate cathode material.
Example 4
(1) Dissolving urea and ammonium sulfate in ultrapure water according to the mass ratio of 11.5: 1 to prepare a solution with the solid content of 55%, drying at 65 ℃ for 19h to obtain a dried material, sintering the dried material in a 450 ℃ tube furnace for 5h to obtain a powder sample, and ultrasonically stripping the powder sample in the ultrapure water for 12h to obtain the laminated mesoporous graphite phase carbon nitride powder g-C with the thickness of 90nm3N4;
(2) Weighing g-C in the step (1) according to the mass ratio of 100: 4.5: 23N4PVP with the relative molecular weight of 8000 and glucose are added into deionized water to be dispersed for 30min, and dispersion liquid A is obtained;
(3) according to FePO4∶g-C3N4Weighing FePO at a mass ratio of 50: 0.84Adding the lithium source into the dispersion liquid A in the step (2) to disperse for 0.5h to obtain dispersion liquid B, weighing the lithium source according to the stoichiometric ratio of Fe to Li of 1: 1, adding the lithium source into the dispersion liquid B to disperse for 2h to obtain dispersion liquid C;
(4) and (3) carrying out superfine grinding on the dispersion liquid C in the step (3) for 1.5h, wherein the ground granularity D50 is 400nm, carrying out spray drying to obtain a lithium iron phosphate precursor, presintering the precursor at 330 ℃ for 3h in a protective atmosphere, sintering the precursor at 680 ℃ for 8h, and naturally cooling to obtain the high-compaction high-rate lithium iron phosphate cathode material.
Example 5
(1) Dissolving urea and ammonium sulfate in ultrapure water according to the mass ratio of 11.5: 1 to prepare a solution with the solid content of 55%, drying the solution at 80 ℃ for 24 hours to obtain a dried material, sintering the dried material in a 600 ℃ tubular furnace for 8 hours to obtain a powder sample, and ultrasonically stripping the powder sample in the ultrapure water for 12 hours to obtain the layered mesoporous graphite phase carbon nitride powder g-C with the thickness of 120nm3N4;
(2) Weighing g-C in the step (1) according to the mass ratio of 100: 4.5: 3.53N4Adding PVP with a relative molecular weight of 16000 and glucose into deionized water, and dispersing for 50min to obtain dispersion A;
(3) according to FePO4∶g-C3N4Weighing FePO at a mass ratio of 50: 1.54Adding the lithium source into the dispersion liquid A in the step (2) for dispersing for 2h to obtain dispersion liquid B, then weighing the lithium source according to the stoichiometric ratio of Fe to Li of 1: 1, adding the lithium source into the dispersion liquid B for dispersing for 3.5h to obtain dispersion liquid C;
(4) and (3) carrying out superfine grinding on the dispersion liquid C in the step (3) for 3h, wherein the granularity D50 after grinding is 300nm, carrying out spray drying to obtain a lithium iron phosphate precursor, presintering the precursor at 460 ℃ for 5h in a protective atmosphere, sintering the precursor at 790 ℃ for 14h, and naturally cooling to obtain the lithium iron phosphate cathode material.
Comparative example
(1) Weighing glucose and PVP with the relative molecular weight of 10000 according to the mass ratio of 100: 4.5, adding into deionized water, and dispersing for 40min to obtain dispersion A;
(2) according to FePO4Weighing FePO at a mass ratio of glucose to glucose of 50: 14Adding the lithium source into the dispersion liquid A in the step (1) to disperse for 1h to obtain dispersion liquid B, then weighing the lithium source according to the stoichiometric ratio of Fe to Li of 1: 1, adding the lithium source into the dispersion liquid B to disperse for 2.5h to obtain dispersion liquid C;
(3) and (3) carrying out superfine grinding on the dispersion liquid C in the step (2) for 2h, wherein the ground particle size D50 is 380nm, carrying out spray drying to obtain a lithium iron phosphate precursor, presintering the precursor at 420 ℃ for 4h in a protective atmosphere, sintering at 710 ℃ for 12h, and naturally cooling to obtain the lithium iron phosphate cathode material.
Fig. 2 shows a SEM image corresponding to the lithium iron phosphate material prepared in the present comparative example, and it can be seen from the SEM image that the prepared lithium iron phosphate finished product has an irregular structure with hardened large and small particles, and many pores exist on the particle surface, which has a certain relationship with the low compacted density.
The lithium iron phosphate materials prepared in examples 1 to 3 of the present invention and comparative examples were tested for properties such as chargeability, compaction density, and the like, and the test results are shown in table 1.
Table 1 chargingdensity data of lithium iron phosphate materials prepared in examples 1 to 3 and comparative example
As can be seen from Table 1, in example 1, the 0.2C initial discharge gram capacity is as high as 164.9mAh/g, the initial effect is 99%, the corresponding discharge gram capacities at 1C, 2C and 3C multiplying power are 152.3mAh/g, 149.1mAh/g and 141.9mAh/g, respectively, and the corresponding pole piece compaction density is 2.42 g/cc. Compared with the embodiment 1, the material has slightly reduced integral buckling performance by reducing the dosage of the glucose in the embodiment 2, the compacted density of the pole piece is 2.4g/cc, and the compacted density is slightly reduced compared with the embodiment 1. After the dosage of the glucose is increased in the example 3, the overall electric performance of the material is slightly reduced, but the first effect still reaches 98.9 percent, and the compaction density is also reduced to 2.37 g/cc. It is stated that excessive carbon coating does not necessarily improve the compaction performance and the electricity consumption of the material. Compared with examples 1-3, the lithium iron phosphate material prepared in the comparative example has poor overall buckling performance and low compaction, and the good carbon coating method and the material morphology play a crucial role in high-compaction high-rate performance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A preparation method of a carbon-coated lithium iron phosphate positive electrode material with high compaction and high rate performance is characterized by comprising the following steps:
s1, taking g-C of laminar mesoporous graphite phase carbon nitride powder according to the mass ratio of 100: 4.5: 0.5-43N4Adding polyvinyl pyrrolidone (PVP) and saccharides into deionized water, and dispersing to obtain a dispersion liquid A; in S1, layered mesoporous graphite phase carbon nitride powder g-C3N4The thickness of (A) is 90-120 nm;
s2 according to FePO4∶g-C3N4Weighing FePO at a mass ratio of 50 to (0.8-1.5)4Adding the mixture into the dispersion liquid A, and dispersing to obtain dispersion liquid B;
s3, weighing a lithium source according to the stoichiometric ratio of Fe to Li of 1 to 1, adding the lithium source into the dispersion liquid B, and dispersing to obtain dispersion liquid C;
s4, carrying out superfine grinding on the dispersion liquid C, carrying out spray drying to obtain a lithium iron phosphate precursor, and sintering the precursor for 12-14h at 460 ℃ and 790 ℃ under a protective atmosphere to obtain g-C3N4And (4) decomposing and naturally cooling to obtain the high-compaction high-rate performance carbon-coated lithium iron phosphate cathode material.
2. The method for preparing the carbon-coated lithium iron phosphate positive electrode material with high compaction and high rate capability according to claim 1, wherein g-C is3N4The preparation of (a) was as follows: according to the weight ratio of 11.5: 1, dissolving urea and ammonium sulfate in ultrapure water according to the mass ratio, preparing a solution with the solid content of 55%, drying at 65-80 ℃ for 19-24h, sintering in a tube furnace at 600 ℃ for 5-8h to obtain a powder sample, and ultrasonically stripping the powder sample in the ultrapure water for 12h to obtain layered mesoporous graphite phase carbon nitride powder g-C3N4。
3. The method for preparing the carbon-coated lithium iron phosphate positive electrode material with high compaction and high rate capability according to claim 1 or 2, wherein in S1, the molecular weight of polyvinylpyrrolidone PVP is 8000-16000; the saccharide is one or more of glucose, fructose, galactose, sucrose, maltose and starch.
4. The preparation method of the carbon-coated lithium iron phosphate positive electrode material with high compaction and high rate capability according to claim 1 or 2, wherein the carbon-coated lithium iron phosphate positive electrode material is dispersed in S1 for 30-50 min.
5. The preparation method of the carbon-coated lithium iron phosphate positive electrode material with high compaction and high rate capability according to claim 1 or 2, wherein the carbon-coated lithium iron phosphate positive electrode material is dispersed in S2 for 0.5-2 h.
6. The method for preparing the carbon-coated lithium iron phosphate positive electrode material with high compaction and high rate capability according to claim 1 or 2, wherein in S3, the lithium source is any one of lithium carbonate and lithium hydroxide or a mixture of the lithium carbonate and the lithium hydroxide.
7. The preparation method of the carbon-coated lithium iron phosphate positive electrode material with high compaction and high rate capability according to claim 1 or 2, wherein the carbon-coated lithium iron phosphate positive electrode material is dispersed in S3 for 2-3.5 h.
8. The method as claimed in claim 1 or 2, wherein in S4, the particle size D50 of the dispersion C after being subjected to ultrafine grinding is 300-400 nm.
9. The method for preparing the carbon-coated lithium iron phosphate positive electrode material with high compaction and high rate capability according to claim 1 or 2, wherein in S4, the protective atmosphere is one or more of high-purity nitrogen, high-purity helium and high-purity argon.
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CN109244395A (en) * | 2018-08-28 | 2019-01-18 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of situ Nitrogen Doping packet carbon lithium iron phosphate positive material |
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