CN107123798A - A kind of preparation method of cladded type lithium iron phosphate positive material - Google Patents
A kind of preparation method of cladded type lithium iron phosphate positive material Download PDFInfo
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- CN107123798A CN107123798A CN201710345257.4A CN201710345257A CN107123798A CN 107123798 A CN107123798 A CN 107123798A CN 201710345257 A CN201710345257 A CN 201710345257A CN 107123798 A CN107123798 A CN 107123798A
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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
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- H—ELECTRICITY
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- 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 preparation method of cladded type lithium iron phosphate positive material, this method prepares lithium iron phosphate positive material using plasma high-temperature fusion technology, and uses the method for liquid phase coating to coat complete covering material thereon to improve electric conductivity.Methods described is simple to operation, cost is low, time-consuming short, and obtained LiFePO 4 material pattern rule is not reunited uniformly for highly spherical, composition, stable electrochemical property, with preferable electric conductivity and cycle performance, with higher specific capacity and longer service life.
Description
Technical field
The present invention relates to battery material field, and in particular to a kind of preparation method of cladded type lithium iron phosphate positive material.
Background technology
Lithium ion battery is new generation of green high-energy battery, with voltage is high, energy density is big, good cycle, is put certainly
The many merits such as electric small, memory-less effect, operating temperature range be wide, are widely used in phone, notebook computer, electric tool
Deng also being had a good application prospect in electric automobile, by it is believed that being 21 century significant high energy technology
Product.
Current commercialized lithium ion anode material is mainly with LiFePO4 (LiFePO4), ternary material (nickel cobalt manganese three
First material NCM, nickel cobalt aluminium ternary material NCA) and LiMn2O4 (LiMn2O4) etc. based on, wherein lithium manganate battery cycle life
Cycle life is worse under short and hot environment, and ternary material has safety issue as electrokinetic cell.Recently, LiFePO4
Anode material for lithium-ion batteries is due to its high discharge capacity, excellent security performance, and the advantages of good cycle performance
Become the focus studied now.
The synthetic method of current lithium ion battery anode material lithium iron phosphate mainly has high temperature solid phase synthesis, co-precipitation
Method, sol-gel process, Pechini methods etc..The wherein soft chemical method technique such as coprecipitation, sol-gel method, Pechini methods
Complexity, is difficult to realize industrialization.Therefore conventional synthesis process mainly uses high temperature solid phase synthesis.High temperature solid phase synthesis is
Lithium salts, ferrous salt and phosphorus compound are well mixed according to a certain percentage, one section is calcined at high temperature using inert gas shielding
LiFePO4 is made in time.Conventional lithium salts has lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate etc., and source of iron is then ferric phosphate,
Calcining heat is in the temperature of 600 DEG C~950 DEG C even more highs, and calcination time is 10~60h or so.High temperature solid phase synthesis is operated
And Process Route Planning is simple, technological parameter is easily controllable, and the material property of preparation is stable, it is easy to accomplish industrialization is extensive raw
Production.But, it is necessary to substantial amounts of inert protective gas when conventional high temperature solid phase synthesis prepares LiFePO4, inert gas cost compared with
It is high.
In addition, the ion and electron conduction of LiFePO4 are poor, it is general in the prior art to be received using carbon coating, material granule
The technologies such as riceization and metal ion mixing improve, and by above method can improve the high rate performance of battery, improve its and circulate
Stability.But nanosizing makes the poor processability of material, doping vario-property technique is more complicated, needs to be improved and develops.
The content of the invention
The present invention provides a kind of preparation method of cladded type lithium iron phosphate positive material, and methods described is simple to operation, into
This is low, time-consuming short, and obtained LiFePO 4 material pattern rule is not reunited uniformly for highly spherical, composition, chemical property is steady
It is fixed, with preferable electric conductivity and cycle performance, with higher specific capacity and longer service life.
To achieve these goals, the present invention provides a kind of preparation method of cladded type lithium iron phosphate positive material, the party
Method comprises the following steps：
（1）Prepare LiFePO 4 material
According to iron：Lithium：Carbon geochemistry metering compares 1:1：（0.03-0.05）Ratio weigh lithium carbonate, ferric phosphate and starch respectively, plus
Enter and carry out, with 400-500rpm rotating speed ball milling 7-9h, being then dried in vacuo 12-16h at 80-90 DEG C after absolute ethyl alcohol is well mixed
Obtain ferric lithium phosphate precursor powder；
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage 20-
40kV, plasma electric arc current 500-1000A；
Frit reaction powder is spurted into cooling device with reducibility gas, particle crushed and screened after cooling, screening is obtained
Granular size be 5-10 microns of ball-type positive pole LiFePO 4 material；The wherein described nozzle diameter 2-5mm for being used to spray；
（2）Prepare covering liquid
Phosphate compounds are added in alcohols solvent, phosphate ester solution is obtained；
Aluminium salt is added in the phosphate ester solution, the aluminium salt is dissolved in the alcohols solvent, and is reacted with the phosphate compounds
To homogeneous settled solution, reaction temperature is 40-80 DEG C, and the reaction time is 2-5 hours；
Addition acidity regulator adjusts the pH value of the homogeneous settled solution to 6-7, and acidity regulator can be ammoniacal liquor, bicarbonate
One or more in ammonium, ammonium carbonate, ammonium acetate, pyridine and triethylamine, the total addition of the acidity regulator is according to N:
Al mol ratios are 1:1-6:1 weighs and obtains the covering liquid；
（3）Cladding
The lithium iron phosphate positive material is well mixed with the covering liquid, a solidliquid mixture is obtained；And
The solidliquid mixture is dried and sintered, the drying can naturally dry or heating, drying for normal temperature, as long as removing the mixing
Solvent in thing, the temperature of the heating, drying is preferably 60-100 DEG C.The sintering is carried out in atmosphere, makes the cladding
Organic group in predecessor is removed, and generates the clad.The sintering temperature is 450-750 DEG C, and sintering time is 5-8 hours,
Anode composite material is obtained, the anode composite material includes positive electrode active materials and is coated on the bag of the surface of positive electrode active material
Coating.
It is preferred that, the alcohols solvent is one or more kinds of in methanol, ethanol, propyl alcohol, n-butanol and isopropanol
Double solvents, the phosphate compounds formula can be AnP(O)(OH)m, wherein A is carbon corresponding with the alcohol solvent molecules
At least one of oxygen groups, i.e. methoxyl group, ethyoxyl, propoxyl group, butoxy and isopropoxy, n=1-3, m=0-2, m+n=3；
The mass ratio of phosphate compounds and alcohols solvent is 1:5-1:25.
It is preferred that, aluminium salt is the one or more in aluminium chloride, aluminum nitrate, aluminium isopropoxide and aluctyl.The alcohol is molten
Property the total addition of aluminium salt and alcohols solvent mass ratio be preferably 1:10-1:20.
It is preferred that, the step（1）In reducibility gas be the mixture of nitrogen and hydrogen, wherein hydrogen is in gaseous mixture
Percent by volume 1-3% in body.
The invention has the advantages that and remarkable result：
（1）The plasma high-temperature fusion technology that the present invention is used, is a kind of new technique developed in recent years, and principle is：
Introducing plasma working gas after vacuum system preset vacuum, in melt chamber and cooling chamber, (generally inert gas, lazy
Property gas be one or more in helium, neon and argon gas, the inert gas in melt chamber and cooling chamber can be it is same,
Can also be mixed gas), the inert gas plasma moment heating added between the two poles of the earth in voltage, melt chamber, temperature
Thousands of degree can be reached, the powder in addition feed appliance can be made to be rapidly reached molten condition, plasma high-speed motion, particle
Between can occur material under molten condition required for sharp impacts, in-time generatin, by be ejected come gas take out of
Melt chamber, is entered in cooling chamber, and required lithium iron phosphate positive material is obtained after cooling.This method can make LiFePO4 material
Material is formed in moment, and can form continuous production.
（2）Covering liquid in the present invention is a homogeneous settled solution, can be relatively easily equal on lithium iron phosphate particles surface
Clad is formed, each lithium iron phosphate particles surface is wrapped by layer cladding completely, further improves its electric conductivity and circulation
Stability.Therefore the lithium iron phosphate positive material that prepared by the present invention is put first when for lithium ion battery with higher
Electric reversible capacity and longer service life.
Embodiment
Embodiment one
According to iron：Lithium：Carbon geochemistry metering compares 1:1：0.03 ratio weighs lithium carbonate, ferric phosphate and starch respectively, adds anhydrous
Carry out, with 400rpm rotating speed ball milling 7h, being then dried in vacuo 12h at 80 DEG C and obtaining ferric lithium phosphate precursor after ethanol is well mixed
Powder；Plasma-arc is imposed under reducing atmosphere to precursor, reaction powder is melted, plasma electric arc voltage 20kV,
Plasma electric arc current 1000A.
Frit reaction powder is spurted into cooling device with reducibility gas, the reducibility gas is nitrogen and hydrogen
Mixture, wherein percent by volume 1% of the hydrogen in mixed gas.Particle is crushed and screened after cooling, what screening was obtained
Granular size is 5 microns of ball-type positive pole LiFePO 4 material；The wherein described nozzle diameter 2mm for being used to spray.
Phosphate compounds are added in alcohols solvent, phosphate ester solution is obtained.It is preferred that, the alcohols solvent is first
One or more kinds of double solvents in alcohol, ethanol, propyl alcohol, n-butanol and isopropanol, the phosphate compounds formula
Can be AnP(O)(OH)m, wherein A is carbon oxygen groups corresponding with the alcohol solvent molecules, i.e. methoxyl group, ethyoxyl, the third oxygen
At least one of base, butoxy and isopropoxy, n=1-3, m=0-2, m+n=3；Phosphate compounds and alcohols solvent
Mass ratio is 1:5.
Aluminium salt is added in the phosphate ester solution, the aluminium salt is dissolved in the alcohols solvent, and anti-with the phosphate compounds
Homogeneous settled solution should be obtained, reaction temperature is 40 DEG C, and the reaction time is 2 hours；It is preferred that, aluminium salt is aluminium chloride, nitric acid
One or more in aluminium, aluminium isopropoxide and aluctyl.The total addition of the alcohol-soluble aluminium salt and alcohols solvent mass ratio
Preferably 1:10.
Addition acidity regulator adjusts the pH value of the homogeneous settled solution to 6-7, and acidity regulator can be ammoniacal liquor, carbon
One or more in sour hydrogen ammonium, ammonium carbonate, ammonium acetate, pyridine and triethylamine, the total addition of the acidity regulator is pressed
According to N:Al mol ratios are 1:1 weighs and obtains the covering liquid.
The lithium iron phosphate positive material is well mixed with the covering liquid, a solidliquid mixture is obtained；And consolidate this
Liquid mixture is dried and sintered, and the drying can naturally dry or heating, drying for normal temperature, as long as removing the solvent in the mixture
, the temperature of the heating, drying is preferably 60 DEG C.The sintering is carried out in atmosphere, is made organic in the cladding predecessor
Group is removed, and generates the clad.The sintering temperature is 450 DEG C, and sintering time is 5 hours, obtains anode composite material, this is just
Pole composite includes positive electrode active materials and is coated on the clad of the surface of positive electrode active material.
Embodiment two
According to iron：Lithium：Carbon geochemistry metering compares 1:1：0.05 ratio weighs lithium carbonate, ferric phosphate and starch respectively, adds anhydrous
Carry out, with 500rpm rotating speed ball milling 9h, being then dried in vacuo 16h at 80-90 DEG C and obtaining LiFePO4 forerunner after ethanol is well mixed
Body powder；Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage
40kV, plasma electric arc current 500A.
Frit reaction powder is spurted into cooling device with reducibility gas, the reducibility gas is nitrogen and hydrogen
Mixture, wherein percent by volume 3% of the hydrogen in mixed gas.Particle is crushed and screened after cooling, what screening was obtained
Granular size is 10 microns of ball-type positive pole LiFePO 4 material；The wherein described nozzle diameter 5mm for being used to spray.
Phosphate compounds are added in alcohols solvent, phosphate ester solution is obtained.The alcohols solvent is isopropanol, the phosphorus
Acid esters compound formula can be AnP(O)(OH)m, wherein A is carbon oxygen groups corresponding with the alcohol solvent molecules, i.e. methoxy
At least one of base, ethyoxyl, propoxyl group, butoxy and isopropoxy, n=1-3, m=0-2, m+n=3；Phosphoric acid ester chemical combination
The mass ratio of thing and alcohols solvent is 1:25.
Aluminium salt is added in the phosphate ester solution, the aluminium salt is dissolved in the alcohols solvent, and anti-with the phosphate compounds
Homogeneous settled solution should be obtained, reaction temperature is 80 DEG C, and the reaction time is 5 hours；It is preferred that, aluminium salt is aluminium chloride, nitric acid
One or more in aluminium, aluminium isopropoxide and aluctyl.The total addition of the alcohol-soluble aluminium salt and alcohols solvent mass ratio
Preferably 1:20.
Addition acidity regulator adjusts the pH value of the homogeneous settled solution to 6-7, and acidity regulator can be ammoniacal liquor, carbon
One or more in sour hydrogen ammonium, ammonium carbonate, ammonium acetate, pyridine and triethylamine, the total addition of the acidity regulator is pressed
According to N:Al mol ratios are 6:1 weighs and obtains the covering liquid.
The lithium iron phosphate positive material is well mixed with the covering liquid, a solidliquid mixture is obtained；And consolidate this
Liquid mixture is dried and sintered, and the drying can naturally dry or heating, drying for normal temperature, as long as removing the solvent in the mixture
, the temperature of the heating, drying is preferably 100 DEG C.The sintering is carried out in atmosphere, makes having in the cladding predecessor
Machine group is removed, and generates the clad.The sintering temperature is 750 DEG C, and sintering time is 8 hours, obtains anode composite material, should
Anode composite material includes positive electrode active materials and is coated on the clad of the surface of positive electrode active material.
Comparative example
Commercially available lithium iron phosphate positive material.
Above-described embodiment one, two and comparative example products therefrom are used into NMP as solvent, by active material: SP: PVDF
Be configured to slurry that solid content be 70% at=90: 5: 5 is evenly applied on Al paper tinsels, and positive pole is made.Negative pole is from diameter 14mm's
Metal lithium sheet, electrolyte selects 1mol LiFP6 (EC：DMC：EMC=1:1:1, v/v), with negative electrode casing-shell fragment-pad-lithium
Battery is packaged by the order of piece-electrolyte-barrier film-positive plate-pad-anode cover, and whole process is all filled with argon
Completed in the glove box of gas.Electric performance test is carried out in the case where test temperature is 25 DEG C, after tested the material of the embodiment one and two
Compared with the product of comparative example, first charge-discharge reversible capacity improves 31-34%, and service life brings up to more than 25%.
Claims (4)
1. a kind of preparation method of cladded type lithium iron phosphate positive material, this method comprises the following steps：
（1）Prepare LiFePO 4 material
According to iron：Lithium：Carbon geochemistry metering compares 1:1：（0.03-0.05）Ratio weigh lithium carbonate, ferric phosphate and starch respectively, plus
Enter and carry out, with 400-500rpm rotating speed ball milling 7-9h, being then dried in vacuo 12-16h at 80-90 DEG C after absolute ethyl alcohol is well mixed
Obtain ferric lithium phosphate precursor powder；
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage 20-
40kV, plasma electric arc current 500-1000A；
Frit reaction powder is spurted into cooling device with reducibility gas, particle crushed and screened after cooling, screening is obtained
Granular size be 5-10 microns of ball-type positive pole LiFePO 4 material；The wherein described nozzle diameter 2-5mm for being used to spray；
（2）Prepare covering liquid
Phosphate compounds are added in alcohols solvent, phosphate ester solution is obtained；
Aluminium salt is added in the phosphate ester solution, the aluminium salt is dissolved in the alcohols solvent, and is reacted with the phosphate compounds
To homogeneous settled solution, reaction temperature is 40-80 DEG C, and the reaction time is 2-5 hours；
Addition acidity regulator adjusts the pH value of the homogeneous settled solution to 6-7, and acidity regulator can be ammoniacal liquor, bicarbonate
One or more in ammonium, ammonium carbonate, ammonium acetate, pyridine and triethylamine, the total addition of the acidity regulator is according to N:
Al mol ratios are 1:1-6:1 weighs and obtains the covering liquid；
（3）Cladding
The lithium iron phosphate positive material is well mixed with the covering liquid, a solidliquid mixture is obtained；And
The solidliquid mixture is dried and sintered, the drying can naturally dry or heating, drying for normal temperature, as long as removing the mixing
Solvent in thing, the temperature of the heating, drying is preferably 60-100 DEG C,
The sintering is carried out in atmosphere, is removed the organic group in the cladding predecessor, is generated the clad,
The sintering temperature is 450-750 DEG C, and sintering time is 5-8 hours, obtains anode composite material, the anode composite material bag
Include positive electrode active materials and be coated on the clad of the surface of positive electrode active material.
2. the method as described in claim 1, it is characterised in that the alcohols solvent is methanol, ethanol, propyl alcohol, n-butanol and different
One or more kinds of double solvents in propyl alcohol, the phosphate compounds formula can be AnP(O)(OH)m, wherein A is
In carbon oxygen groups corresponding with the alcohol solvent molecules, i.e. methoxyl group, ethyoxyl, propoxyl group, butoxy and isopropoxy extremely
Few one kind, n=1-3, m=0-2, m+n=3；The mass ratio of phosphate compounds and alcohols solvent is 1:5-1:25.
3. the method as described in claim 1, it is characterised in that aluminium salt is in aluminium chloride, aluminum nitrate, aluminium isopropoxide and aluctyl
One or more,
The total addition of the alcohol-soluble aluminium salt and alcohols solvent mass ratio are preferably 1:10-1:20.
4. the method as described in claim 1-3 is any, it is characterised in that the step（1）In reducibility gas be nitrogen
With the mixture of hydrogen, wherein percent by volume 1-3% of the hydrogen in mixed gas.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114373892A (en) * | 2021-12-22 | 2022-04-19 | 中国科学院化学研究所 | Method for controllably constructing phosphate coating layer and application thereof |
| CN115832236A (en) * | 2022-03-25 | 2023-03-21 | 宁德时代新能源科技股份有限公司 | Lithium iron phosphate positive electrode material, preparation method thereof, positive electrode plate, lithium ion battery, battery module, battery pack and electric device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103515590A (en) * | 2013-09-23 | 2014-01-15 | 北京鼎能开源电池科技股份有限公司 | Preparation method of ternary anode material of lithium ion battery |
| CN105720256A (en) * | 2016-04-13 | 2016-06-29 | 杨仲英 | Preparation method for lithium iron phosphate positive electrode material |
| CN105742605A (en) * | 2016-04-13 | 2016-07-06 | 杨仲英 | Preparation method for coating type lithium manganate composite positive electrode material |
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2017
- 2017-05-16 CN CN201710345257.4A patent/CN107123798A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103515590A (en) * | 2013-09-23 | 2014-01-15 | 北京鼎能开源电池科技股份有限公司 | Preparation method of ternary anode material of lithium ion battery |
| CN105720256A (en) * | 2016-04-13 | 2016-06-29 | 杨仲英 | Preparation method for lithium iron phosphate positive electrode material |
| CN105742605A (en) * | 2016-04-13 | 2016-07-06 | 杨仲英 | Preparation method for coating type lithium manganate composite positive electrode material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114373892A (en) * | 2021-12-22 | 2022-04-19 | 中国科学院化学研究所 | Method for controllably constructing phosphate coating layer and application thereof |
| CN114373892B (en) * | 2021-12-22 | 2023-12-26 | 中国科学院化学研究所 | Method for controllably constructing phosphate coating and application thereof |
| CN115832236A (en) * | 2022-03-25 | 2023-03-21 | 宁德时代新能源科技股份有限公司 | Lithium iron phosphate positive electrode material, preparation method thereof, positive electrode plate, lithium ion battery, battery module, battery pack and electric device |
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