CN109167028A - A kind of regenerative preparation of lithium iron phosphate/carbon composite material - Google Patents
A kind of regenerative preparation of lithium iron phosphate/carbon composite material Download PDFInfo
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- 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
- 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
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The present invention relates to a kind of regenerative preparations of lithium iron phosphate/carbon composite material, its method and step includes: that the abnormal powder of oxidation will occur in LiFePO4 anaerobic sintering process to carry out airflow collision crushing, sufficiently broken agglomeration body and release liner surface layer indefinite form carbon；The oxidation and sinter powder of crushing is through the broken dispersion of ultrasonic vibration and is subject to air inducing cyclonic separation ambiguity carbon, obtains the abnormal LiFePO 4 material of oxidation；The LiFePO4 for weighing crushing and removing indefinite form carbon is mixed with carbon source, lithium salts, and to roller precompressed after high speed grinding, the regeneration of lithium iron phosphate/carbon composite material is realized in oxygen-free atmosphere sintering.The method of the present invention simple process, low energy consumption and reconstituted product function admirable, advantageously reduces the abnormal scrappage of LiFePO 4 material production process oxidation.
Description
Technical field
The present invention relates to battery material preparation technical field, especially a kind of regeneration system of lithium iron phosphate/carbon composite material
Preparation Method.
Background technique
The LiFePO4 of olivine-type structure is a kind of novel anode material for lithium-ion batteries, and theoretical capacity is
170mAh/g, to lithium platform voltage 3.5V or so.Strong covalent bond effect in LiFePO4 protect it can in charge and discharge process
The highly stable of crystal structure is held, therefore there is security performance more higher than other positive electrodes and longer recycling longevity
Life.Furthermore the space valence bond structure of LiFePO 4 material makes it have very strong thermodynamics and kinetics stability, under normal pressure
Air atmosphere in, be heated to 200 DEG C it is still relatively stable.Compared to other positive electrodes, the excellent safety of LiFePO4
Performance and excellent cyclical stability, so that the material has more wide application field and shows that its is outstanding rapidly
Competitive advantage.
The LiFePO4 production technology of current industrialization mostly uses ferric phosphate mix with lithium salts to add carbon source progress anaerobic
Calcine synthesizing iron lithium phosphate/carbon composite.The roller way kiln etc. that the equipment used in process of production mostly uses nitrogen to fill
Carry out anaerobic sintering.With the pursuit to capacity efficiency so that production equipment constantly increases lengthening, in actual use
Due to the generations exception leak source such as equipment fault, cause to enter a certain amount of air inside burner hearth, the material in high-temperature calcination stage because
Oxygen content increases and accelerates the loss of agraphitic carbon or even LiFePO 4 material aoxidizes, and iron ion valence state changes
Generate red ferric iron.Cause device fails that cannot stop in time since production equipment chases yield, causes high-volume
LiFePO 4 material oxidation is unqualified.
In existing public technology, mainly material is first carried out high-temperature oxydation then reduction treatment.Such as CN
A kind of reclaiming processing method of positive material of waste lithium iron phosphate of 102208706 A() consider waste lithium iron phosphate
Inside battery component is complex, and waste lithium iron phosphate battery is removed the positive electrode collected in refuse battery first and carries out height
The aerobic calcining of temperature removes anode additive, carbon and other substances, then adds lithium salts, carbon source etc. and carries out mixed grinding, finally
Mixed powder is placed in progress high-temperature calcination in non-oxidizing atmosphere.
Regeneration method is carried out extremely for material, and 102064366 A of CN gives similar treating method, will give up
LiFePO4 heat in air it is fully oxidized, carbon source mixing is then added and carried out in protective atmosphere high-temperature calcination it is cooling after
Taking-up obtains target product.
Above-mentioned existing method all uses high-temperature oxydation calcining removal of impurities to anode pole piece and abnormal LiFePO 4 material
The method of screening, then the powder of peroxidating adds lithium salts and carbon source progress anaerobic sintering and reducing to obtain target product, this undoubtedly gives
Material manufacturing process increases more non-controllable risks and improves material regeneration difficulty.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of regeneration of lithium iron phosphate/carbon composite material
Preparation method realizes the regeneration of abnormal oxidation lithium iron phosphate/carbon composite material during industrialization production, reduces LiFePO4 material
Expect scrappage, and reduces and occur burning and over reduction in material recovery process or the risks such as reduction is not thorough.
To achieve the above object, the invention adopts the following technical scheme:
A kind of regenerative preparation of lithium iron phosphate/carbon composite material, comprising the following steps:
S1, the sintering powder that oxidation exception occurs during the sintering process for lithium iron phosphate/carbon composite material is collected, is filled with air-flow crushing
It sets and sintering powder is crushed, then classifying screen selects fine powder material；
S2, the fine powder material progress ultrasonic vibration that S1 is obtained is crushed, while by backfilling air inducing air-flow for powder conveying to whirlwind
In seperator, the separation of abnormal sintering LiFePO4 fine powder and its coated with carbon is realized；
S3, lithium, iron content in the abnormal sintering LiFePO4 fine powder of S2 separation are detected using elemental microanalysis method, by adding
Add lithium salts to make lithium in mixture, the molar ratio of ferro element is 1.1-1.2:1, be then added carbon source, dry stirring is uniformly mixed；
S4, the powder after being stirred is fully ground to rear precompressed, compacting is placed on the lower sintering of oxygen-free atmosphere protection, is regenerated
Lithium iron phosphate/carbon composite material.
Further, the air flow crushing device can select spiral jet pulverizer, fluidized bed to spray formula airflow milling, circulation pipe
Formula airflow milling, to spray formula airflow milling, one of target formula airflow milling.
Further, the material granularity of fine powder material described in S1 requires to be D50≤300nm, D100≤900nm.
Further, the cyclopneumatic separator is spiral cyclone；It is larger that specific gravity is collected by centrifugal sedimentation principle
LiFePO4 fine powder, realize the separation for being sintered abnormal LiFePO4 and indefinite form carbon.
Further, the elemental microanalysis method can use ICP Atomic Emission Spectral Analysis method or atomic absorption spectrography (AAS).
Further, the lithium salts is the eutectic point mixing lithium salts for adding lithium fluoride, and a mole accounting for the lithium fluoride is
1%-2%；Eutectic point mix lithium salts can for lithium hydroxide-lithium carbonate, lithium hydroxide-lithium chloride, lithium hydroxide-lithium nitrate,
Lithium nitrate-lithium chloride etc..
Further, the carbon source is 80% glucose of weight accounting and food grade sucrose, the wheat of weight accounting 20%
One of bud sugar, fructose are a variety of.
Further, the powder after being stirred in the S4 is ground 3-5 hours by high speed ball mill, then using to roller
Precompressed is 2mm to roller gap；Crucible filling calcining is carried out after compacting material again, this method is conducive to increase in material sintering process
Closeness of contact improves material in the compacted density of battery core coating end.
Further, the anaerobic sintering atmosphere is one of nitrogen, argon gas, helium or a variety of；Anaerobic is sintered flat-temperature zone
Temperature is 300-450 DEG C, keeps the temperature duration 4-7 hours.
Beneficial effects of the present invention are as follows: a kind of regeneration preparation side of lithium iron phosphate/carbon composite material provided by the invention
Method aoxidizes abnormal sintering powder using production process and carries out airflow collision crushing, agglomeration particle is fully open and break
Broken original sintered particles obtain LiFePO4 sintering fine powder, while the indefinite form carbon coated is also removed from powder body material surface layer.It is logical
Cross ultrasonic vibration and the screening of air inducing whirlwind, obtain the abnormal LiFePO 4 powder of the extremely low sintering of phosphorus content, for it is subsequent again
Packet carbon lays the foundation.
Aerobic high-temperature calcination is generallyd use in published technology except carbon, not only energy consumption is high, and material forms burning and by phosphorus
Sour iron lithium excessive oxidation, need more reducing agents carry out ferric iron backs and ferro element existed restore or restore it is halfway
Possibility greatly causes material property and loses and increase material quality risk.
And the present invention mixes the abnormal LiFePO 4 powder of the extremely low sintering of the phosphorus content being collected into lithium salts and carbon source, makes
Lithium salts is low melting point congruent melting salt, therefore the calcination temperature used is relatively low and calcination time is shorter, avoids material burning
And performance inactivates.Furthermore the powder after reasonable preparation eutectic lithium salt component, dry stirring are uniformly ground passes through to roller precompressed all
Being conducive to material, particle balling preparation is more regular during the sintering process.Material after regeneration has the electrical property with orthodox material shoulder to shoulder
Can, while when making battery core, anode pole piece has higher material compacted density, further increases the monomer energy of battery core
Density.
By the regenerated lithium iron phosphate/carbon composite material of the present invention be made using lithium piece as the CR2016 type button cell of cathode into
Row charge-discharge test, 0.2C first discharge specific capacity are 158-162mAh/g, coulombic efficiency 96-99%, 1C averaged discharge specific capacity
For 148-154mAh/g, 2C averaged discharge specific capacity is 137-143mAh/g, excellent electrical properties.
Detailed description of the invention
Fig. 1 is the SEM photograph of the regenerated lithium iron phosphate/carbon composite material of embodiment 1；Material is in real as can be seen from Figure 1
Heart spheric granules, pattern is relatively regular and fine powder gap is small, and molding of reuniting is preferable.
Fig. 2 is the XRD diagram of the regenerated lithium iron phosphate/carbon composite material of embodiment 1；It is of the invention compound as can be seen from Figure 2
Material purity with higher and preferable crystallinity.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below with reference to embodiment to the present invention
Technical solution in embodiment is clearly and completely described.Obviously, described embodiment is that a part of the invention is implemented
Example, rather than whole embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative labor
Every other embodiment obtained under the premise of dynamic, shall fall within the protection scope of the present invention.
CR2016 button battery is made in following each embodiments and the method for test material chemical property is as follows:
(1) lithium iron phosphate/carbon composite material obtained and binder Kynoar will the preparation of battery anode slice: be regenerated
(PVDF) sample is weighed with mass ratio 8:2.It dissolves, adds after binder and organic solvent N-Methyl pyrrolidone (NMP) are mixed
Enter the lithium iron phosphate/carbon composite material being fully ground and stir into slurry, is coated in carbon-coated aluminum foils surface, roll-in obtains electricity after drying
Pond positive plate.
(2) positive plate after roll-in: being struck out the positive plate of diameter 12mm by battery assembly, according to anode after correct amount
Piece composition converses lithium iron phosphate/carbon composite material effective mass.Use the positive plate, electrolyte, diameter 16mm prepared
The lithium piece of PE diaphragm, diameter 15mm, assembles button cell in glove box.
(3) performance test: the specific capacity test of battery uses the new prestige battery test system in Shenzhen, and test temperature is 25 DEG C,
0.2C, 1C, 2C charge-discharge magnification respectively carry out 10 loop tests.
The raw material collection step of each embodiment is as follows:
Oxygen content severely exceeds and excessive oxygen occurs in the burner hearth as caused by sintering kiln failure in collection producing line production process
The abnormal powder of micro- knot braised in soy sauce changed, only has 0.95% through carbon and sulfur analytical instrument test carbon content.Electric test method is detained by aforementioned CR2016
It measures material 0.2C specific discharge capacity and only has 125mAh/g, charging and discharging curve and with serious polarization phenomena.
Using air flow crushing device, (such as spiral jet pulverizer, fluidized bed are to spray formula airflow milling, circulating tube type airflow milling, right
Spray formula airflow milling, target formula airflow milling), LiFePO4 exception sintering feed progress compressed gas is crushed, the compressed gas pressure used >=
0.5MPa, smashed powder carry out screening collection through being classified motor, it is desirable that D50≤300nm, D100≤900nm.To collection
Fine powder material carry out ultrasonic vibration it is broken and with air inducing backfill air-flow by powder conveying to cyclopneumatic separator, by LiFePO 4 powder with
The indefinite form carbon of removing carries out separation screening and obtains the extremely low abnormal oxidation LiFePO4 fine powder of carbon content.
The cyclopneumatic separator is spiral cyclone；The biggish ferric phosphate of specific gravity is collected by centrifugal sedimentation principle
Lithium fine powder realizes the separation for being sintered abnormal LiFePO4 and indefinite form carbon.
The extremely low abnormal oxidation LiFePO4 fine powder of carbon content is collected, (ICP atomic emissions can be used through elemental microanalysis method
Spectra methods or atomic absorption spectrography (AAS)) detection after obtain lithium in the powder, iron molar ratio be 0.97:1, show excessive
Slight lithium loss has occurred in oxidation process, needs to add corresponding Li source compound during subsequent regeneration.
Embodiment 1
It accurately weighs and screens the extremely low abnormal oxidation LiFePO4 fine powder raw material sample of obtained carbon content by broken apart
Lithium hydroxide-lithium carbonate eutectic point mixing lithium salts and lithium fluoride is added in 100g, and mole accounting of lithium fluoride is 1%, adjusts sample
Lithium, iron molar ratio are 1.1:1 in product, add 8g glucose and 2g food grade sucrose dry stirring is uniformly mixed, then will mix
It closes powder and grinds 5h in high speed ball mill, by milled sample through collecting, in nitrogen after to roller precompressed (being 2mm to roller gap)
It is warming up to after 300 DEG C in protective atmosphere with 5 DEG C/min heating rate and keeps the temperature 7h, material temperature, which is cooled to room temperature, can be obtained regeneration
Lithium iron phosphate/carbon composite material.It detects to obtain carbon content to be 1.35% through carbon and sulfur analytical instrument, material tap density is 1.0g/
cm3, battery core anode pole piece compacted density can reach 2.4g/cm3, greatly improve the capacity of single battery core.
By the regenerated lithium iron phosphate/carbon composite material of embodiment 1 by assembling button-shaped half-cell in 0.2C, 1C, 2C times
Charge and discharge under rate, test result are as follows: the corresponding specific discharge capacity of 0.2C, 1C, 2C multiplying power be followed successively by 161mAh/g, 150mAh/g,
141mAh/g illustrates regenerated composite material specific capacity with higher and high rate performance.
Embodiment 2
It accurately weighs and screens the extremely low abnormal oxidation LiFePO4 fine powder raw material sample of obtained carbon content by broken apart
Lithium hydroxide-lithium nitrate eutectic point mixing lithium salts and lithium fluoride is added in 100g, and mole accounting of lithium fluoride is 1.5%, adjusts
Lithium, iron molar ratio are 1.15:1 in sample, add 8g glucose and 2g maltose dry stirring is uniformly mixed, then will mixing
Powder grinds 3h in high speed ball mill, by milled sample through collecting, protects after to roller precompressed (being 2mm to roller gap) in helium
Be warming up to after 450 DEG C with 5 DEG C/min heating rate in shield atmosphere and keep the temperature 4h, material temperature be cooled to room temperature can be obtained it is regenerated
Lithium iron phosphate/carbon composite material.It detects to obtain carbon content to be 1.5% through carbon and sulfur analytical instrument, material tap density is 0.9g/cm3,
Battery core anode pole piece compacted density can reach 2.35g/cm3, greatly improve the capacity of single battery core.
Electrical property point is carried out to lithium iron phosphate/carbon composite material obtained by the present embodiment by the identical test mode of embodiment 1
Analysis, electric performance test result are as follows: the corresponding specific discharge capacity of 0.2C, 1C, 2C multiplying power be followed successively by 158mAh/g, 148mAh/g,
138mAh/g illustrates regenerated composite material specific capacity with higher and high rate performance.
Embodiment 3
It accurately weighs and screens the extremely low abnormal oxidation LiFePO4 fine powder raw material sample of obtained carbon content by broken apart
Lithium hydroxide-lithium chloride eutectic point mixing lithium salts and lithium fluoride is added in 100g, and mole accounting of lithium fluoride is 2%, adjusts sample
Lithium, iron molar ratio are 1.2:1 in product, add 8g glucose and 2g fructose dry stirring is uniformly mixed, then by mixed-powder
3h is ground in high speed ball mill, by milled sample through collecting, protects gas in argon gas after to roller precompressed (being 2mm to roller gap)
It is warming up to after 450 DEG C in atmosphere with 5 DEG C/min heating rate and keeps the temperature 7h, material temperature, which is cooled to room temperature, can be obtained regenerated phosphoric acid
Iron lithium/carbon composite material.It detects to obtain carbon content to be 1.38% through carbon and sulfur analytical instrument, material tap density is 1.03g/cm3, electricity
Core anode pole piece compacted density can reach 2.38g/cm3, greatly improve the capacity of single battery core.
Electrical property point is carried out to lithium iron phosphate/carbon composite material obtained by the present embodiment by the identical test mode of embodiment 1
Analysis, electric performance test result are as follows: the corresponding specific discharge capacity of 0.2C, 1C, 2C multiplying power be followed successively by 160mAh/g, 149mAh/g,
140mAh/g illustrates regenerated composite material specific capacity with higher and high rate performance.
Embodiment 4
It accurately weighs and screens the extremely low abnormal oxidation LiFePO4 fine powder raw material sample of obtained carbon content by broken apart
Lithium nitrate-lithium chloride eutectic point mixing lithium salts and lithium fluoride is added in 100g, and mole accounting of lithium fluoride is 1%, adjusts sample
Middle lithium, iron molar ratio are 1.15:1, add 8g glucose and 2g maltose dry stirring is uniformly mixed, then by mixed-powder
4h is ground in high speed ball mill, by milled sample through collecting, in nitrogen protection gas after to roller precompressed (being 2mm to roller gap)
It is warming up to after 450 DEG C in atmosphere with 5 DEG C/min heating rate and keeps the temperature 6h, material temperature, which is cooled to room temperature, can be obtained regenerated phosphoric acid
Iron lithium/carbon composite material.It detects to obtain carbon content to be 1.45% through carbon and sulfur analytical instrument, material tap density is 1.0g/cm3, battery core
Anode pole piece compacted density can reach 2.39g/cm3, greatly improve the capacity of single battery core.
Electrical property point is carried out to lithium iron phosphate/carbon composite material obtained by the present embodiment by the identical test mode of embodiment 1
Analysis, electric performance test result are as follows: the corresponding specific discharge capacity of 0.2C, 1C, 2C multiplying power be followed successively by 160mAh/g, 152mAh/g,
142mAh/g illustrates regenerated composite material specific capacity with higher and high rate performance.
Comparative example 1
The lithium iron phosphate/carbon composite material of normal production preparation is taken to carry out performance evaluation by the identical test mode of embodiment 1,
Carbon content is 1.45%, and material tap density is 0.91g/cm3, battery core compacted density is 2.23g/cm3, electric performance test result
Are as follows: the corresponding specific capacity of 0.2C, 1C, 2C multiplying power is followed successively by 160mAh/g, 148mAh/g, 137mAh/g, which meets phosphoric acid
Iron lithium material industry volumetric(al) standards, while also belonging to performance preferably LiFePO 4 material.
Comparative example 2
This comparative example prepares lithium iron phosphate/carbon composite wood using wet grinding when carrying out lithium salts, raw material and carbon source and mixing
Material.It accurately weighs first and screens the extremely low abnormal oxidation LiFePO4 fine powder raw material sample of obtained carbon content by broken apart
Lithium hydroxide-lithium carbonate eutectic point mixing lithium salts and lithium fluoride is added in product 100g, and mole accounting of lithium fluoride is 1%, adjusts
Lithium, iron molar ratio are 1.1:1 in sample, add 8g glucose and 2g food grade sucrose, are subsequently poured into and fill dehydrated alcohol
High speed ball milling mixing 5h is carried out in ball grinder.Ball milling mixing sample drying, grinding, to roller precompressed (to roller gap be 2mm) after
It is warming up to after 300 DEG C in nitrogen protection atmosphere with 5 DEG C/min heating rate and keeps the temperature 7h, material temperature, which is cooled to room temperature, to be obtained
To regenerated lithium iron phosphate/carbon composite material.It detects to obtain carbon content to be 1.4% through carbon and sulfur analytical instrument, material tap density is
0.93g/cm3, battery core anode pole piece compacted density can reach 2.25g/cm3。
Electrical property point is carried out to lithium iron phosphate/carbon composite material obtained by this comparative example by the identical test mode of embodiment 1
Analysis, electric performance test result are as follows: the corresponding specific discharge capacity of 0.2C, 1C, 2C multiplying power be followed successively by 142mAh/g, 134mAh/g,
121mAh/g illustrates to be more advantageous to raising material using dry stirring ground and mixed in lithium iron phosphate/carbon composite material regenerative process
The performance of material.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (9)
1. a kind of regenerative preparation of lithium iron phosphate/carbon composite material, which comprises the following steps:
S1, the sintering powder that oxidation exception occurs during the sintering process for lithium iron phosphate/carbon composite material is collected, is filled with air-flow crushing
It sets and sintering powder is crushed, then classifying screen selects fine powder material；
S2, the fine powder material progress ultrasonic vibration that S1 is obtained is crushed, while by backfilling air inducing air-flow for powder conveying to whirlwind
In seperator, the separation of abnormal sintering LiFePO4 fine powder and its coated with carbon is realized；
S3, lithium, iron content in the abnormal sintering LiFePO4 fine powder of S2 separation are detected using elemental microanalysis method, by adding
Add lithium salts to make lithium in mixture, the molar ratio of ferro element is 1.1-1.2:1, be then added carbon source, dry stirring is uniformly mixed；
S4, the powder after being stirred is fully ground to rear precompressed, compacting is placed on the lower sintering of oxygen-free atmosphere protection, is regenerated
Lithium iron phosphate/carbon composite material.
2. a kind of regenerative preparation of lithium iron phosphate/carbon composite material according to claim 1, it is characterised in that: institute
State air flow crushing device can select spiral jet pulverizer, fluidized bed to spray formula airflow milling, circulating tube type airflow milling, to spray formula gas
One of stream mill, target formula airflow milling.
3. a kind of regenerative preparation of lithium iron phosphate/carbon composite material according to claim 1, it is characterised in that: S1
Described in fine powder material material granularity require be D50≤300nm, D100≤900nm.
4. a kind of regenerative preparation of lithium iron phosphate/carbon composite material according to claim 1, it is characterised in that: institute
Stating cyclopneumatic separator is spiral cyclone.
5. a kind of regenerative preparation of lithium iron phosphate/carbon composite material according to claim 1, it is characterised in that: institute
ICP Atomic Emission Spectral Analysis method or atomic absorption spectrography (AAS) can be used by stating elemental microanalysis method.
6. a kind of regenerative preparation of lithium iron phosphate/carbon composite material according to claim 1, it is characterised in that: institute
Stating lithium salts is the eutectic point mixing lithium salts for adding lithium fluoride, and mole accounting of the lithium fluoride is 1%-2%.
7. a kind of regenerative preparation of lithium iron phosphate/carbon composite material according to claim 1, it is characterised in that: institute
State one of the food grade sucrose, maltose, fructose of 80% glucose that carbon source is weight accounting and weight accounting 20%
Or it is a variety of.
8. a kind of regenerative preparation of lithium iron phosphate/carbon composite material according to claim 1, it is characterised in that: institute
It states the powder after being stirred in S4 to grind 3-5 hours by high speed ball mill, then using to roller precompressed, is to roller gap
2mm。
9. according to a kind of regenerative preparation of lithium iron phosphate/carbon composite material described in claim 1, it is characterised in that: described
Anaerobic sintering atmosphere is one of nitrogen, argon gas, helium or a variety of；It is 300-450 DEG C that anaerobic, which is sintered flat-temperature zone temperature, heat preservation
Duration 4-7 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111017901A (en) * | 2019-12-11 | 2020-04-17 | 合肥国轩电池材料有限公司 | Method for recycling abnormal materials in preparation of lithium iron phosphate positive electrode material |
| CN112614979A (en) * | 2020-12-17 | 2021-04-06 | 华中科技大学 | Secondary carbon-coated lithium iron phosphate and preparation method thereof |
| CN113582153A (en) * | 2021-09-30 | 2021-11-02 | 中南大学 | Waste lithium iron phosphate cathode material for repairing and regenerating and repairing and regenerating method thereof |
| CN113594460A (en) * | 2021-07-26 | 2021-11-02 | 山东精工电子科技有限公司 | Method for preparing lithium iron phosphate composite material by high-temperature kneading |
| CN116443840A (en) * | 2023-03-28 | 2023-07-18 | 合肥国轩高科动力能源有限公司 | Lithium iron phosphate positive electrode material and preparation method thereof |
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