CN108862230A - A kind of processing method of the ultra-fine powder material of LiFePO4 - Google Patents
A kind of processing method of the ultra-fine powder material of LiFePO4 Download PDFInfo
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- CN108862230A CN108862230A CN201811085446.3A CN201811085446A CN108862230A CN 108862230 A CN108862230 A CN 108862230A CN 201811085446 A CN201811085446 A CN 201811085446A CN 108862230 A CN108862230 A CN 108862230A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- 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
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of processing methods of the ultra-fine powder material of LiFePO4, and LiFePO4 fine powder is (1) put into rotary mixing machine, and carbon source binder solution is sprayed in rotary course, in mixing machine rotary course, form particle after powder and binder bonding；(2) moisture removal is removed into particle drying；(3) the particle after drying is put into sintering furnace and is sintered, calcined under nitrogen+vapor atmospheric condition, so that particle is sintered the LiFePO4 aggregate of bulky grain into again, the aggregate is by the broken LiFePO4 finished product for obtaining meeting Particle size requirements.The present invention is granulated again using the carbon source that can be cracked, become coarse aggregation after LiFePO4 fine powder sintering after granulation, the LiFePO4 finished product for meeting process system partial size can be fabricated to by subsequent pulverizing process, carbon content increases in order to prevent, and joined a small amount of water vapor absorption carbon conversion during the sintering process into carbon monoxide reduces carbon content.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries preparation field more particularly to a kind of ultra-fine powder materials of LiFePO4
Processing method.
Background technique
In anode material for lithium-ion batteries, LiFePO4 (LiFePO4) it is nontoxic with its, inexpensive, safety is good, resource is rich
The advantages that rich, receives significant attention, it is considered to be the preferred positive electrode of electric car, energy-accumulating power station lithium ion battery.
General lithium ion battery is all made of the techniques such as mixing, sintering, air-flow crushing, sieving.In air-flow crushing
In technique, in order to realize the broken of LiFePO 4 material, the general method using supersonic airstream head-on collision realizes the broken of particle.
Then the product of appropriate particle size is made up of classification, cyclonic separation.The fine powder for crossing broken generation is collected by dust arrester.It is logical
Often, the fine powder collected in dust arrester accounts for 20% of total amount or so, and high reaches 30%.The general partial size of fine powder is in 1um hereinafter, comparing table
Area is big, poor activity, and carbon content is high, and when for lithium ion battery processing, processing performance is very poor.Many LiFePO4 factories have
A large amount of fine powder inventory causes production cost substantial increase due to being difficult with.
LiFePO4 fine powder is typically all carbon-coated lithium iron phosphate particles.If addition common bond (such as butylbenzene
Rubber, carboxymethylcellulose sodium, Kynoar etc.) it is granulated, insulating layer can be generated between particle, increase battery system
Internal resistance.If the simple method for being granulated again thermal cracking by the way that sugar is added, can significantly improve carbon content, increase specific surface area.
With the rapid development of China's LiFePO4 industry, the processing of fine powder has become the task of top priority, becomes ferric phosphate
Lithium material manufacturer problem in the urgent need to address.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of carbon contents, and LiFePO4 low, that fine powder content is low is ultra-fine
The processing method of powder material.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that：A kind of ultra-fine powder material of LiFePO4
Processing method includes the following steps：
(1) LiFePO4 fine powder is put into rotary mixing machine, carbon source binder solution is sprayed in rotary course, mixed
In conjunction machine rotary course, particle is formed after powder and binder bonding；
(2) moisture removal is removed into particle drying；
(3) the particle after drying is put into sintering furnace and is sintered, calcined, made under nitrogen+vapor atmospheric condition
Particle sinters the LiFePO4 aggregate of bulky grain into again, and aggregate is by the broken LiFePO4 for obtaining meeting Particle size requirements
Finished product.
The carbon source binder is one of glucose, xylitol, polyethylene, polyvinyl butyral.
The solvent of the carbon source binder solution is water, ethyl alcohol or methanol.
The mass concentration of the carbon source binder solution is 1%-20%.
Ratio of the carbon source binder in the dry product mixed is 0.5%-10%, and percentage is quality percentage
Than.
The drying temperature that particle is dried in the step (2) is 80-150 DEG C.
The volume ratio of the nitrogen and vapor is 10:(0.1-10).
Step (3) sintering condition is：500-800 DEG C of sintering, 0.5-12 hours.
The beneficial effects of the invention are as follows：The present invention is granulated again using the carbon source that can be cracked, the ferric phosphate after granulation
Become coarse aggregation after the sintering of lithium fine powder, the phosphorus for meeting process system partial size can be fabricated to by subsequent pulverizing process
Sour iron lithium finished product, carbon content increases in order to prevent, joined a small amount of water vapor absorption carbon conversion during the sintering process into an oxygen
Changing carbon reduces carbon content.
Specific embodiment
The present invention illustrates that detailed process and step of the invention, all operations and data are by following implementation
It is illustrative, it is not restrictive, this does not limit the scope of protection of the present invention.
The processing method of the ultra-fine powder material of LiFePO4 of the invention, includes the following steps：
(1) LiFePO4 fine powder is put into rotary mixing machine, carbon source binder solution is sprayed in rotary course, mixed
In conjunction machine rotary course, particle is formed after powder and binder bonding；
(2) moisture removal is removed into particle drying；
(3) the particle after drying is put into sintering furnace and is sintered, calcined, made under nitrogen+vapor atmospheric condition
Particle sinters the LiFePO4 aggregate of bulky grain into again, and aggregate is by the broken LiFePO4 for obtaining meeting Particle size requirements
Finished product.
The carbon source binder is one of glucose, xylitol, polyethylene, polyvinyl butyral.
The solvent of the carbon source binder solution is water, ethyl alcohol or methanol.
The mass concentration of the carbon source binder solution is 1-20%.
Ratio of the carbon source binder in the dry product mixed is 0.5-10%, and percentage is mass percent.
The drying temperature that particle is dried in the step (2) is 80-150 DEG C.
The volume ratio of the nitrogen and vapor is 10:(0.1-10).
Step (3) sintering condition is：500-800 DEG C of sintering, 0.5-12 hours.
The present invention is granulated again using the carbon source that can be cracked.Become coarse after LiFePO4 fine powder sintering after granulation
Aggregation, the LiFePO4 finished product for meeting process system partial size can be fabricated to by subsequent pulverizing process.In order to prevent
Carbon content increases, we joined a small amount of vapor during the sintering process.Vapor can pass through following routing cost carbon：
C+H2O→CO+H2
The carbon monoxide and hydrogen of generation can be rejected to outside furnace.It can reduce carbon by the introducing of vapor in this way and contain
Amount.It controls the ratio of vapor and is passed through the time, can effectively control the ratio of carbon content in product.
Embodiment 1
(1) 5g DEXTROSE ANHYDROUS is dissolved in 495g distilled water, the glucose solution that mass fraction is 1% is made.So
Afterwards by D50(average grain diameter) is that LiFePO4 fine powder (carbon content 2.5%) 995Kg of 0.85um is put into rotary mixing machine,
Above-mentioned glucose solution is sprayed in rotary course, 10 minutes sprayed.Continue rotation 2 hours after.LiFePO4 at this time
Fine powder is gradually adhesive into wet bulb due to snowball effect.
(2) in an oven by wet bulb, dried 2 hours by 80 DEG C, become dry bulb.Wherein binder is in the dry bulb mixed
Middle mass ratio is 0.5%.
(3) by dry bulb in atmosphere sintering furnace, the volume ratio for being continuously passed through nitrogen and vapor is 10:0.1 gaseous mixture
Body, heating sintering.Sintering schedule is 500 DEG C, 12 hours.
Sintered LiFePO 4 material is after air-flow crushing, D50(average grain diameter) is 1.8 microns, carbon content 2.2%.
Chemical property is constant.
Embodiment 2
(1) 50Kg xylitol is dissolved in 950Kg distilled water, the xylose alcohol solution that mass fraction is 5% is made.So
Afterwards by D50(average grain diameter) is that LiFePO4 fine powder (carbon content 1.85%) 950Kg of 0.6um is put into rotary mixing machine,
Above-mentioned xylose alcohol solution is sprayed in rotary course, 60 minutes sprayed.Continue rotation 5 hours after.LiFePO4 at this time
Fine powder is gradually adhesive into wet bulb.
(2) in an oven by wet bulb, dried 4 hours by 120 DEG C, become dry bulb.Wherein binder is in the dry bulb mixed
Middle mass ratio is 5%.
(3) by dry bulb in atmosphere sintering furnace, the volume ratio for being continuously passed through nitrogen and vapor is 10:2 mixed gas,
Heating sintering.Sintering schedule is 800 DEG C, 0.5 hour.
Sintered LiFePO 4 material is after air-flow crushing, D50(average grain diameter) is 1.55 microns, and carbon content is
1.60%.Chemical property is constant.
Embodiment 3
(1) 100Kg polyvinyl butyral is dissolved in 900Kg dehydrated alcohol, the poly- second that mass fraction is 10% is made
Enol butyral solution.Then by D50(average grain diameter) is that LiFePO4 fine powder (carbon content 2.23%) 900Kg of 0.4um is put
Enter rotary mixing machine, above-mentioned polyvinyl butyral solution is sprayed in rotary course, 30 minutes sprayed.Continue after pressing
Rotation 3 hours.LiFePO4 fine powder is gradually adhesive into wet bulb at this time.
(2) in an oven by wet bulb, dried 2 hours by 105 DEG C, become dry bulb.Wherein binder is in the dry bulb mixed
Middle mass ratio is 10%.
(3) by dry bulb in atmosphere sintering furnace, the volume ratio for being continuously passed through nitrogen and vapor is 10:1 mixed gas,
Heating sintering.Sintering schedule is 700 DEG C, 2 hours.Sintered LiFePO 4 material is after air-flow crushing, D50(average grain diameter)
It is 1.7 microns, carbon content 2.1%.Chemical property is constant.
Embodiment described above is merely to illustrate technical idea and feature of the invention, in the art its object is to make
Technical staff it will be appreciated that the contents of the present invention and implement accordingly, patent model of the invention only cannot be limited with the present embodiment
It encloses, i.e., same changes or modifications made by all disclosed spirit are still fallen in the scope of the patents of the invention.
Claims (8)
1. a kind of processing method of the ultra-fine powder material of LiFePO4, which is characterized in that include the following steps：
(1) LiFePO4 fine powder is put into rotary mixing machine, carbon source binder solution is sprayed in rotary course, in mixing machine
In rotary course, particle is formed after powder and binder bonding；
(2) moisture removal is removed into particle drying；
(3) the particle after drying is put into sintering furnace and is sintered, calcined under nitrogen+vapor atmospheric condition, make particle
Sinter the LiFePO4 aggregate of bulky grain into again, aggregate by the broken LiFePO4 for obtaining meeting Particle size requirements at
Product.
2. the processing method of the ultra-fine powder material of LiFePO4 according to claim 1, which is characterized in that the carbon source binder
For one of glucose, xylitol, polyethylene, polyvinyl butyral.
3. the processing method of the ultra-fine powder material of LiFePO4 according to claim 1, which is characterized in that the carbon source binder
The solvent of solution is water, ethyl alcohol or methanol.
4. the processing method of the ultra-fine powder material of LiFePO4 according to claim 1, which is characterized in that the carbon source binder
The mass concentration of solution is 1%-20%.
5. the processing method of the ultra-fine powder material of LiFePO4 according to claim 1, which is characterized in that the carbon source binder
Ratio in the dry product mixed is 0.5%-10%, and percentage is mass percent.
6. the processing method of the ultra-fine powder material of LiFePO4 according to claim 1, which is characterized in that in the step (2)
The drying temperature of particle drying is 80-150 DEG C.
7. the processing method of the ultra-fine powder material of LiFePO4 according to claim 1, which is characterized in that the nitrogen and water steam
The volume ratio of gas is 10:(0.1-10).
8. the processing method of the ultra-fine powder material of LiFePO4 according to claim 1, which is characterized in that the step (3) is burnt
Knot condition is：500-800 DEG C of sintering, 0.5-12 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811085446.3A CN108862230B (en) | 2018-09-18 | 2018-09-18 | Treatment method of lithium iron phosphate superfine powder material |
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| CN201811085446.3A CN108862230B (en) | 2018-09-18 | 2018-09-18 | Treatment method of lithium iron phosphate superfine powder material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112952097A (en) * | 2021-02-23 | 2021-06-11 | 贵州安达科技能源股份有限公司 | Lithium iron phosphate anode material and preparation method and application thereof |
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| CN112952097A (en) * | 2021-02-23 | 2021-06-11 | 贵州安达科技能源股份有限公司 | Lithium iron phosphate anode material and preparation method and application thereof |
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