CN114031062B - Method for preparing pure lithium iron phosphate by high-temperature spray spiral pipe - Google Patents

Method for preparing pure lithium iron phosphate by high-temperature spray spiral pipe Download PDF

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CN114031062B
CN114031062B CN202111375144.1A CN202111375144A CN114031062B CN 114031062 B CN114031062 B CN 114031062B CN 202111375144 A CN202111375144 A CN 202111375144A CN 114031062 B CN114031062 B CN 114031062B
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temperature
iron phosphate
lithium iron
quartz tube
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CN114031062A (en
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李德
李源穿
陈永
韦雅庆
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Hainan University
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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
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • 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
    • 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
    • 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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Abstract

The invention relates to the technical field of pure lithium iron phosphate, in particular to a method for preparing pure lithium iron phosphate by a high-temperature spray spiral pipe, which comprises the following steps: s1, mixing a ferric nitrate solution, a lithium dihydrogen phosphate solution and a nitric acid solution, and atomizing the mixed solution to a micron level by using an ultrasonic atomizer to obtain atomized particles; and S2, enabling the atomized particles to sequentially enter a first quartz tube, a spiral tube and a second quartz tube by adopting argon, wherein the temperature of the first quartz tube is 720-780 ℃, the temperature of the spiral tube is 720-780 ℃, the temperature of the second quartz tube is 240-260 ℃, and a static collecting device is arranged in the second quartz tube, and a lithium iron phosphate precursor is collected by the static collecting device. The method has the advantages of low raw material cost and simple experimental operation, solves the problem of agglomeration of pure lithium iron phosphate, and is easy for large-scale production of lithium iron phosphate with good dispersibility.

Description

Method for preparing pure lithium iron phosphate by high-temperature spray spiral pipe
Technical Field
The invention relates to the technical field of pure lithium iron phosphate, in particular to a method for preparing pure lithium iron phosphate by a high-temperature spray spiral pipe.
Background
The pure lithium iron phosphate synthesized by the existing solid phase method has larger particles, unsatisfactory solid dispersion performance, smaller specific surface area, unfavorable desorption of lithium ions and increased diffusion distance of the lithium ions. The solid phase synthesis method has the advantages that the raw materials are not uniformly mixed, and the particles form local pressure in the grinding process, so that the raw materials are agglomerated to cause larger fired phase particles, unsatisfactory dispersing performance, smaller specific surface area, and unfavorable desorption and diffusion of lithium ions.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for preparing pure lithium iron phosphate by using a high-temperature spray spiral pipe.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing pure lithium iron phosphate by a high-temperature spray spiral pipe comprises the following steps:
s1, mixing an iron nitrate solution, a lithium dihydrogen phosphate solution and a nitric acid solution, and then atomizing the mixed solution to micron order by using an ultrasonic atomizer to obtain atomized particles;
s2, enabling the atomized particles to sequentially enter a first quartz tube, a spiral tube and a second quartz tube by adopting argon, wherein the temperature of the first quartz tube is 720-780 ℃, the temperature of the spiral tube is 720-780 ℃, the temperature of the second quartz tube is 240-260 ℃, and a static collecting device is arranged in the second quartz tube to collect a lithium iron phosphate precursor;
s3, sintering the lithium iron phosphate precursor in a third quartz tube, and introducing Ar and H 2 The temperature of the mixed gas is controlled to be 30 ℃ at the initial temperature, the heating time is 70-90 mm, the temperature is increased to 720-780 ℃, then the heat preservation time is 220-260min, and the mixed gas is naturally cooled to the room temperature after the heat preservation is finished, so that the pure lithium iron phosphate is obtained.
Preferably, the mass ratio of the ferric nitrate to the lithium dihydrogen phosphate to the nitric acid is (1.5-2): (1.5-2): 1.
preferably, the concentration of the ferric nitrate solution is 0.15-0.2mol/L, the concentration of the lithium dihydrogen phosphate solution is 0.15-0.2mol/L, and the concentration of the nitric acid solution is 0.5-1.5mol/L.
Preferably, the inner diameter of the first quartz tube is 4-5 times of the inner diameter of the spiral tube, and the length of the first quartz tube is 0.8-1.2 times of the length of the spiral tube; the inner diameter of the first quartz tube is 0.5-0.7 times of the inner diameter of the second quartz tube, and the length of the first quartz tube is 1.2-1.5 times of the length of the second quartz tube. Preferably, the inner diameter of the first quartz tube is 2.8cm, and the length of the first quartz tube is 44cm; the inner diameter of the spiral pipe is 0.6cm, the outer diameter is 0.8cm, the diameter of the outer ring is 3.0cm, and the length is 45cm; the inner diameter of the second quartz tube is 4.5cm, and the length of the second quartz tube is 35cm; the third quartz tube has an inner diameter of 4.5cm and a length of 50cm.
Preferably, the passing time of the argon gas through the first quartz tube, the spiral tube and the second quartz tube is 30 to 120s in total.
Preferably, ar and H are 2 In the mixed gas of (3), ar accounts for 95% of the total volume fraction, and H 2 Accounting for 5 percent of the total volume fraction.
Preferably, ar and H are 2 The air input of the mixed gas is 0.03-0.07L/min.
Preferably, in S2, argon gas is used to make the atomized particles enter the first quartz tube, the spiral tube and the second quartz tube in sequence, wherein the temperature of the first quartz tube is 750 ℃, the temperature of the spiral tube is 750 ℃, the temperature of the second quartz tube is 250 ℃, and the electrostatic collecting device is installed in the second quartz tube to collect the lithium iron phosphate precursor through the electrostatic collecting device.
Preferably, in S3, the lithium iron phosphate precursor is sintered in a third quartz tube, and Ar and H are introduced 2 The temperature of the mixed gas is set to be 30 ℃ as the initial temperature, the temperature rise time is 80mim, the temperature is raised to 750 ℃, then the temperature is kept for 240min, and after the temperature is over, the mixed gas is naturally cooled to the room temperature to obtain pure lithium iron phosphate.
Compared with the prior art, the invention has the beneficial effects that: the preparation method provided by the invention is simple in process and is beneficial to the performance research of pure lithium iron phosphate. Low raw material cost and simple experimental operation. Solves the agglomeration problem of pure lithium iron phosphate, and is easy to produce lithium iron phosphate with good dispersibility on a large scale.
Drawings
FIG. 1 is a scanning electron microscope image of pure lithium iron phosphate in example 3;
FIG. 2 is a scanning electron microscope image of pure lithium iron phosphate in a comparative example;
fig. 3 is an electrochemical performance test chart of pure lithium iron phosphate in example 3 and pure lithium iron phosphate in a comparative example;
fig. 4 is an XRD spectrum of pure lithium iron phosphate in example 3.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
A method for preparing pure lithium iron phosphate by a high-temperature spray spiral pipe comprises the following steps:
s1, mixing an iron nitrate solution, a lithium dihydrogen phosphate solution and a nitric acid solution, and then atomizing the mixed solution to micron order by using an ultrasonic atomizer to obtain atomized particles;
s2, enabling the atomized particles to sequentially enter a first quartz tube, a spiral tube and a second quartz tube by adopting argon, wherein the temperature of the first quartz tube is 720 ℃, the temperature of the spiral tube is 720 ℃, the temperature of the second quartz tube is 240 ℃, installing a static collecting device in the second quartz tube, and collecting a lithium iron phosphate precursor by the static collecting device;
s3, sintering the lithium iron phosphate precursor in a third quartz tube, and introducing Ar and H 2 The temperature of the mixed gas is set to be 30 ℃ as the initial temperature, the temperature rise time is 70 mm, the temperature is raised to 720 ℃, then the temperature is kept for 220min, and after the temperature is over, the mixed gas is naturally cooled to the room temperature to obtain the pure lithium iron phosphate.
Wherein the mass ratio of ferric nitrate, lithium dihydrogen phosphate and nitric acid is 3:3: and 2, wherein the concentration of the ferric nitrate solution is 0.15mol/L, the concentration of the lithium dihydrogen phosphate solution is 0.15mol/L, and the concentration of the nitric acid solution is 0.5mol/L.
The inner diameter of the first quartz tube is 2.4cm, and the length of the first quartz tube is 36cm; the inner diameter of the spiral pipe is 0.6cm, the outer diameter is 0.8cm, the diameter of the outer ring is 3.0cm, and the length is 45cm; the inner diameter of the second quartz tube is 4.8cm, and the length of the second quartz tube is 30cm; the third quartz tube has an inner diameter of 4.5cm and a length of 50cm.
The passing time of argon gas through the first quartz tube, the spiral tube and the second quartz tube was 30s in total.
Ar and H 2 In the mixed gas of (3), ar accounts for 95% of the total volume fraction, and H 2 5% of the total volume, ar and H 2 The intake air amount of the mixed gas (2) was 0.03L/min.
Example 2
A method for preparing pure lithium iron phosphate by a high-temperature spray spiral pipe comprises the following steps:
s1, mixing an iron nitrate solution, a lithium dihydrogen phosphate solution and a nitric acid solution, and then atomizing the mixed solution to micron order by using an ultrasonic atomizer to obtain atomized particles;
s2, enabling the atomized particles to sequentially enter a first quartz tube, a spiral tube and a second quartz tube by adopting argon, wherein the temperature of the first quartz tube is 780 ℃, the temperature of the spiral tube is 780 ℃, the temperature of the second quartz tube is 260 ℃, installing a static collecting device in the second quartz tube, and collecting a lithium iron phosphate precursor by the static collecting device;
s3, sintering the lithium iron phosphate precursor in a third quartz tube, and introducing Ar and H 2 The temperature of the mixed gas is controlled to be 30 ℃ at the initial temperature, the temperature rise time is 90 mm, the temperature is raised to 780 ℃, and then the temperature is kept for a whileAnd (4) naturally cooling to room temperature after 260min to obtain pure lithium iron phosphate.
Wherein the mass ratio of ferric nitrate, lithium dihydrogen phosphate and nitric acid is 2:2:1, wherein the concentration of the ferric nitrate solution is 0.2mol/L, the concentration of the lithium dihydrogen phosphate solution is 0.2mol/L, and the concentration of the nitric acid solution is 1.5mol/L.
The inner diameter of the first quartz tube is 3cm, and the length of the first quartz tube is 54cm; the inner diameter of the spiral pipe is 0.6cm, the outer diameter is 0.8cm, the diameter of the outer ring is 3.0cm, and the length is 45cm; the inner diameter of the second quartz tube is 4.3cm, and the length of the second quartz tube is 36cm; the third quartz tube has an inner diameter of 4.5cm and a length of 50cm.
The passing time of argon gas through the first quartz tube, the spiral tube and the second quartz tube was 120s in total.
Ar and H 2 In the mixed gas of (3), ar accounts for 95% of the total volume fraction, and H 2 5% of the total volume, ar and H 2 The intake air amount of the mixed gas of (3) is 0.07L/min.
Example 3
A method for preparing pure lithium iron phosphate by a high-temperature spray spiral pipe comprises the following steps:
s1, mixing a ferric nitrate solution, a lithium dihydrogen phosphate solution and a nitric acid solution, and atomizing the mixed solution to a micron level by using an ultrasonic atomizer to obtain atomized particles;
s2, enabling the atomized particles to sequentially enter a first quartz tube, a spiral tube and a second quartz tube by adopting argon, wherein the temperature of the first quartz tube is 750 ℃, the temperature of the spiral tube is 750 ℃, the temperature of the second quartz tube is 250 ℃, installing a static collecting device in the second quartz tube, and collecting a lithium iron phosphate precursor through the static collecting device;
s3, sintering the lithium iron phosphate precursor in a third quartz tube, and introducing Ar and H 2 The temperature of the mixed gas is controlled to be 30 ℃ at the initial temperature, the heating time is 80 mm, the temperature is increased to 750 ℃, then the heat preservation time is 240min, and after the heat preservation is finished, the mixed gas is naturally cooled to the room temperature to obtain the pure lithium iron phosphate.
Wherein the mass ratio of ferric nitrate, lithium dihydrogen phosphate and nitric acid is 5:5: and 3, wherein the concentration of the ferric nitrate solution is 0.17mol/L, the concentration of the lithium dihydrogen phosphate solution is 0.17mol/L, and the concentration of the nitric acid solution is 1mol/L.
The inner diameter of the first quartz tube is 2.8cm, and the length of the first quartz tube is 44cm; the inner diameter of the spiral pipe is 0.6cm, the outer diameter is 0.8cm, the diameter of the outer ring is 3.0cm, and the length is 45cm; the inner diameter of the second quartz tube is 4.5cm, and the length of the second quartz tube is 35cm; the inner diameter of the third quartz tube is 4.5cm, and the length of the third quartz tube is 50cm.
The passing time of argon gas through the first quartz tube, the spiral tube and the second quartz tube was 60s in total.
Ar and H 2 In the mixed gas of (3), ar accounts for 95% of the total volume fraction, and H 2 5% of the total volume, ar and H 2 The intake air amount of the mixed gas (2) was 0.05L/min.
Example 4
A method for preparing pure lithium iron phosphate by a high-temperature spray spiral pipe comprises the following steps:
s1, mixing a ferric nitrate solution, a lithium dihydrogen phosphate solution and a nitric acid solution, and atomizing the mixed solution to a micron level by using an ultrasonic atomizer to obtain atomized particles;
s2, enabling the atomized particles to sequentially enter a first quartz tube, a spiral tube and a second quartz tube by adopting argon, wherein the temperature of the first quartz tube is 720 ℃, the temperature of the spiral tube is 780 ℃, the temperature of the second quartz tube is 240 ℃, installing a static collecting device in the second quartz tube, and collecting a lithium iron phosphate precursor through the static collecting device;
s3, sintering the lithium iron phosphate precursor in a third quartz tube, and introducing Ar and H 2 The temperature of the mixed gas is controlled to be 30 ℃ at the initial temperature, the heating time is 70 mm, the temperature is increased to 720 ℃, then the heat preservation time is 240min, and after the heat preservation, the mixed gas is naturally cooled to the room temperature to obtain the pure lithium iron phosphate.
Wherein the mass ratio of ferric nitrate, lithium dihydrogen phosphate and nitric acid is 3:3:2, wherein the concentration of the ferric nitrate solution is 0.15mol/L, the concentration of the lithium dihydrogen phosphate solution is 0.15mol/L, and the concentration of the nitric acid solution is 1mol/L.
The inner diameter of the first quartz tube is 2.8cm, and the length of the first quartz tube is 44cm; the inner diameter of the spiral pipe is 0.6cm, the outer diameter is 0.8cm, the diameter of the outer ring is 3.0cm, and the length is 45cm; the inner diameter of the second quartz tube is 4.5cm, and the length of the second quartz tube is 35cm; the third quartz tube has an inner diameter of 4.5cm and a length of 50cm.
The passing time of argon gas through the first quartz tube, the spiral tube and the second quartz tube was 60s in total.
Ar and H 2 In the mixed gas of (3), ar accounts for 95% of the total volume fraction, and H 2 5 percent of the total volume fraction, ar and H 2 The intake air amount of the mixed gas of (2) was 0.7L/min.
Comparative example
The preparation method of pure lithium iron phosphate is different from the preparation method of the embodiment 3 in that: in the step 2, the atomized particles are directly sprayed and collected in a quartz tube at 350 ℃ by adopting argon, a spiral tube is not used, a static collecting device is arranged in the quartz tube, and a lithium iron phosphate precursor is collected by the static collecting device. The remaining steps were performed under the same conditions as in example 3 to obtain pure lithium iron phosphate.
In embodiments 1 to 4 of the present invention, first, an ultrasonic atomizer is used to atomize a mixed solution to a micron level, to obtain atomized particles: so that the raw materials are uniformly mixed to generate micron-sized particles. Then, using a first quartz tube for 720-780 ℃ high-temperature treatment: the atomized gas is quickly dried to form independent small particles, and a large amount of particles are prevented from agglomerating. Further, using a spiral pipe for high-temperature treatment at 720-780 ℃: the time of the small particles in high temperature is prolonged, so that the particles are fully dried, the spiral pipe enables the particles to generate more collisions, the particles are convenient to shape, and the particle size is nano-scale. And then, using a second quartz tube for temperature reduction and temperature treatment at 240-260 ℃, installing a static collecting device in the second quartz tube, and collecting the lithium iron phosphate precursor through the static collecting device. Finally, sintering the lithium iron phosphate precursor in a third quartz tube, and introducing Ar and H 2 The temperature of the mixed gas is controlled to be 30 ℃ at the initial temperature, the heating time is 70-90 mm, the temperature is increased to 720-780 ℃, then the heat preservation time is 220-260min, and the mixed gas is naturally cooled to the room temperature after the heat preservation is finished, so that the pure lithium iron phosphate is obtained.
FIG. 1 is a scanning electron microscope characterization of a sample of example 3, and FIG. 2 is a scanning electron microscope characterization of a comparative example, and it can be seen from a comparison between FIG. 1 and FIG. 2 that the obtained product of the present invention is nano-sized particles, and has the characteristics of uniform particles, no agglomeration, and good dispersibility.
FIG. 3 is a comparison graph of electrochemical performance test results of example 3 (750 ℃) and comparative example (350 ℃), and it can be shown from FIG. 3 that the electrochemical performance of the product is effectively improved by the lithium iron phosphate precursor prepared by high temperature, spraying and spiral tube.
As can be seen from fig. 4, the XRD pattern of example 3 is identical to that of the standard PDF card, indicating that the product is pure lithium iron phosphate.
The preparation method provided by the invention is simple in process and is beneficial to the performance research of pure lithium iron phosphate. Low raw material cost and simple experimental operation. Solves the agglomeration problem of pure lithium iron phosphate, and is easy to produce lithium iron phosphate with good dispersibility on a large scale.
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 method for preparing pure lithium iron phosphate by using a high-temperature spray spiral pipe is characterized by comprising the following steps:
s1, mixing a ferric nitrate solution, a lithium dihydrogen phosphate solution and a nitric acid solution, and atomizing the mixed solution to a micron level by using an ultrasonic atomizer to obtain atomized particles;
s2, enabling atomized particles to sequentially enter a first quartz tube, a spiral tube and a second quartz tube by adopting argon, wherein the temperature of the first quartz tube is 720-780 ℃, the temperature of the spiral tube is 720-780 ℃, the temperature of the second quartz tube is 240-260 ℃, a static collecting device is arranged in the second quartz tube, and a lithium iron phosphate precursor is collected by the static collecting device, the inner diameter of the first quartz tube is 4-5 times of the inner diameter of the spiral tube, and the length of the first quartz tube is 0.8-1.2 times of that of the spiral tube; the inner diameter of the first quartz tube is 0.5-0.7 times of the inner diameter of the second quartz tube, and the length of the first quartz tube is 1.2-1.5 times of the length of the second quartz tube;
s3, sintering the lithium iron phosphate precursor in a third quartz tube, and introducing Ar and H 2 Mixed gas of (2)And the temperature is prepared to be 30 ℃ at the initial temperature, the heating time is 70-90 mm, the temperature is increased to 720-780 ℃, then the heat preservation time is 220-260min, and after the heat preservation is finished, the pure lithium iron phosphate is naturally cooled to the room temperature.
2. The method for preparing pure lithium iron phosphate by using the high-temperature spraying spiral tube as claimed in claim 1, wherein the mass ratio of the ferric nitrate to the lithium dihydrogen phosphate to the nitric acid is (1.5-2): (1.5-2): 1.
3. the method for preparing pure lithium iron phosphate by using the high-temperature spraying spiral tube as claimed in claim 1, wherein the concentration of the ferric nitrate solution is 0.15-0.2mol/L, the concentration of the lithium dihydrogen phosphate solution is 0.15-0.2mol/L, and the concentration of the nitric acid solution is 0.5-1.5mol/L.
4. The method for preparing pure lithium iron phosphate by using the spiral pipe for high-temperature spraying as claimed in claim 1, wherein the first quartz tube has an inner diameter of 2.8cm and a length of 44cm; the inner diameter of the spiral pipe is 0.6cm, the outer diameter is 0.8cm, the diameter of the outer ring is 3.0cm, and the length is 45cm; the inner diameter of the second quartz tube is 4.5cm, and the length of the second quartz tube is 35cm; the third quartz tube has an inner diameter of 4.5cm and a length of 50cm.
5. The method for preparing pure lithium iron phosphate by using the high-temperature spray spiral pipe as claimed in claim 1, wherein the passing time of the argon gas in the first quartz pipe, the spiral pipe and the second quartz pipe is 30-120s in total.
6. The method for preparing pure lithium iron phosphate by using the high-temperature spray spiral tube as claimed in claim 1, wherein Ar and H are added 2 In the mixed gas of (3), ar accounts for 95% of the total volume fraction, and H 2 Accounting for 5 percent of the total volume fraction.
7. The method for preparing pure lithium iron phosphate by using the high-temperature spray spiral tube as claimed in claim 1, wherein Ar and H are added 2 The air input of the mixed gas is 0.03-0.07L/min.
8. The method for preparing pure lithium iron phosphate by using the high-temperature spray spiral pipe according to claim 1, wherein in the step S2, the atomized particles sequentially enter the first quartz pipe, the spiral pipe and the second quartz pipe by using argon, wherein the temperature of the first quartz pipe is 750 ℃, the temperature of the spiral pipe is 750 ℃, the temperature of the second quartz pipe is 250 ℃, the static collecting device is arranged in the second quartz pipe, and the lithium iron phosphate precursor is collected by the static collecting device.
9. The method for preparing pure lithium iron phosphate by using the high-temperature spray spiral pipe according to claim 1, wherein in S3, the lithium iron phosphate precursor is sintered in a third quartz pipe, ar and H are introduced into the third quartz pipe 2 The temperature of the mixed gas is controlled to be 30 ℃ at the initial temperature, the heating time is 80 mm, the temperature is increased to 750 ℃, then the heat preservation time is 240min, and after the heat preservation is finished, the mixed gas is naturally cooled to the room temperature to obtain the pure lithium iron phosphate.
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Citations (1)

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Publication number Priority date Publication date Assignee Title
CN102082266A (en) * 2010-12-28 2011-06-01 陕西科技大学 Solid-phase preparation method of composite coated lithium iron phosphate anode material

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JP2011086524A (en) * 2009-10-16 2011-04-28 Univ Of Fukui Method of manufacturing positive electrode active material of lithium ion secondary battery
JP2011096394A (en) * 2009-10-27 2011-05-12 Univ Of Fukui Manufacturing method for positive electrode active material of lithium ion secondary battery
CN105336929B (en) * 2015-10-15 2017-11-10 福建师范大学 A kind of method that atomization prepares spherical carbon-coated LiFePO 4 for lithium ion batteries positive electrode
CN107275635A (en) * 2017-06-28 2017-10-20 福建师范大学 A kind of ultrasonic atomizatio preparation method of the spherical tertiary cathode material of porous hollow
CN108390025B (en) * 2018-01-16 2020-11-06 湖南国盛石墨科技有限公司 Graphene-coated carbon/sulfur composite material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN102082266A (en) * 2010-12-28 2011-06-01 陕西科技大学 Solid-phase preparation method of composite coated lithium iron phosphate anode material

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