CN106935840A - A kind of preparation method of tungsten coated LiFePO 4 for lithium ion batteries positive electrode - Google Patents
A kind of preparation method of tungsten coated LiFePO 4 for lithium ion batteries positive electrode Download PDFInfo
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- CN106935840A CN106935840A CN201710370271.XA CN201710370271A CN106935840A CN 106935840 A CN106935840 A CN 106935840A CN 201710370271 A CN201710370271 A CN 201710370271A CN 106935840 A CN106935840 A CN 106935840A
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The present invention relates to a kind of preparation method of tungsten coated LiFePO 4 for lithium ion batteries positive electrode, methods described is simple to operation, low cost, it is time-consuming short, one layer of equally distributed fast-ionic conductor clad is formed on positive electrode surface, using the effect of the characteristic and clad of fast-ionic conductor, circulation and the high rate performance of positive electrode are effectively improved.
Description
Technical field
The present invention relates to battery material field, and in particular to a kind of preparation method of tungsten coated LiFePO 4 for lithium ion batteries positive electrode.
Background technology
Lithium ion battery as the new renewable green energy resource of one kind, by its high-energy-density, high voltage, cycle life
The advantages of length, green non-pollution, widely should be obtained in miniaturized electronics (cell phone, notebook computer etc.)
With, and it is increasingly becoming one of topmost candidate's electrical source of power of electric automobile；In addition, in national defense and military fields, also contemplated land,
The equipment of many arm of the services such as sea, sky, day.With the development of science and technology we propose requirement higher to lithium ion battery, seek
High performance lithium ion battery is of great practical significance.Wherein, the performance of positive electrode turns into limiting lithium ion electricity
The key factor that pond performance is further lifted, seeks high performance anode material for lithium-ion batteries particularly significant.
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 due to its discharge capacity high, excellent security performance, and the advantages of good cycle performance
Become the focus of current research.
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 are
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
Time is obtained LiFePO4.Conventional lithium salts has lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate etc., and source of iron is then ferric phosphate,
In 600 DEG C of temperature of -950 DEG C of even more highs, calcination time is 10-60h or so to calcining heat.High temperature solid phase synthesis operate and
Process Route Planning is simple, and technological parameter is easily controllable, the strong mechanical property of preparation, it is easy to accomplish industrialization is extensive raw
Produce.But, it is necessary to substantial amounts of inert protective gas when the high temperature solid phase synthesis of routine prepare LiFePO4, inert gas cost compared with
It is high.
The ion and electron conduction of LiFePO4 are poor.Surface coating is to improve anode material for lithium-ion batteries deficiency at present
One of effective ways, clad can not only effectively suppress the side reaction between electrolyte and positive electrode, can also suppress material
Dissolving of middle transition metal etc., the cycle performance under the cyclical stability and high magnification of reinforcing material etc., are effectively improved material
Chemical property.
The content of the invention
The present invention provides a kind of preparation method of tungsten coated LiFePO 4 for lithium ion batteries positive electrode, and methods described is simple to operation, into
This is low, time-consuming short, one layer of equally distributed fast-ionic conductor clad is formed on positive electrode surface, using fast-ionic conductor
The effect of characteristic and clad, effectively improves circulation and the high rate performance of positive electrode.
To achieve these goals, the present invention provides a kind of preparation method of tungsten coated LiFePO 4 for lithium ion batteries positive electrode, 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 carries out, with 400-500rpm rotating speed ball milling 7-9h, being then vacuum dried 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 reducibility gas are spurted into cooling device, particle is 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 spraying；
（2）Prepare covering liquid
Tungstenic compound is dissolved in deionized water, is stirred well to and is completely dissolved, is well mixed；
（3）Cladding
In covering liquid, the above-mentioned ball-type positive pole LiFePO 4 material addition ball grinder that will be prepared, with turning for 300-500r/min
Fast ball milling mixing 4-6h, obtains mixed liquor；
After by the mixed liquor vacuum drying after mill, with the speed of 15 DEG C/min from room temperature to 480-620 DEG C, in 480-620
Constant temperature pre-burning 3-6h at DEG C, then be warming up to 850-900 DEG C with the speed of 10 DEG C/min, in calcining at constant temperature 8- at 850-900 DEG C
10h, is finally down to room temperature with the at the uniform velocity rate of temperature fall of 5 DEG C/min, after being fully ground, obtains tungsten coated LiFePO 4 for lithium ion batteries positive pole material
Material.
Preferably, described Tungstenic compound uses ammonium metatungstate, and described ammonium metatungstate is above-mentioned ball-type positive pole phosphoric acid
The 1wt%-3wt% of iron lithium material mass fraction.
Preferably, 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：
By introducing plasma working gas after vacuum system preset vacuum, in melt chamber and cooling chamber, (generally inert gas, lazy
Property gas be helium, neon and argon gas in one or more, the inert gas in melt chamber and cooling chamber can be it is same,
Can also be mixed gas), voltage is added between the two poles of the earth, the inert gas plasma moment in melt chamber heats up, 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 sharp impacts can occur, the material under molten condition required for in-time generatin is taken out of by the gas for being injected out
Melt chamber, is entered into 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 prodution.
（2）From Tungstenic compound to coat material in the present invention, with novelty, low cost, environment-friendly, clad
The side reaction between electrolyte and positive electrode can not only effectively be suppressed, dissolving of transition metal in material etc. can also be suppressed, had
Effect enhances cycle performance under the cyclical stability and high magnification of material etc..
Specific 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 vacuum dried 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 reducibility gas are spurted into cooling device, the reducibility gas are 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 spraying.
Tungstenic compound is dissolved in deionized water, is stirred well to and is completely dissolved, is well mixed, obtain covering liquid；Institute
The Tungstenic compound stated uses ammonium metatungstate, and described ammonium metatungstate is above-mentioned ball-type positive pole LiFePO 4 material mass fraction
1wt%.In covering liquid, the above-mentioned ball-type positive pole LiFePO 4 material addition ball grinder that will be prepared, with 300-500r/min's
Rotating speed ball milling mixing 4-6h, obtains mixed liquor.
After by the mixed liquor vacuum drying after mill, with the speed of 15 DEG C/min from room temperature to 480 DEG C, at 480 DEG C
Constant temperature pre-burning 3h, then be warming up to 850 DEG C with the speed of 10 DEG C/min, in calcining at constant temperature 8h at 850 DEG C, finally with 5 DEG C/min's
At the uniform velocity rate of temperature fall is down to room temperature, after being fully ground, obtains tungsten coated LiFePO 4 for lithium ion batteries positive electrode.
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 vacuum dried 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 reducibility gas are spurted into cooling device, the reducibility gas are 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 spraying.
Tungstenic compound is dissolved in deionized water, is stirred well to and is completely dissolved, is well mixed, obtain covering liquid；Institute
The Tungstenic compound stated uses ammonium metatungstate, and described ammonium metatungstate is above-mentioned ball-type positive pole LiFePO 4 material mass fraction
3wt%.In covering liquid, the above-mentioned ball-type positive pole LiFePO 4 material addition ball grinder that will be prepared, with the rotating speed of 500r/min
Ball milling mixing 6h, obtains mixed liquor.
After by the mixed liquor vacuum drying after mill, with the speed of 15 DEG C/min from room temperature to 620 DEG C, at 620 DEG C
Constant temperature pre-burning 6h, then be warming up to 900 DEG C with the speed of 10 DEG C/min, in calcining at constant temperature 10h at 900 DEG C, finally with 5 DEG C/min's
At the uniform velocity rate of temperature fall is down to room temperature, after being fully ground, obtains tungsten coated LiFePO 4 for lithium ion batteries positive electrode.
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, is made positive pole.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
Be packaged for battery 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 at being 25 DEG C in test temperature, after tested the material of the embodiment one and two
Compared with the product of comparative example, first charge-discharge reversible capacity improves 34-37%, and service life brings up to more than 15%.
Claims (3)
1. a kind of preparation method of tungsten coated LiFePO 4 for lithium ion batteries positive electrode, the 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 carries out, with 400-500rpm rotating speed ball milling 7-9h, being then vacuum dried 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 reducibility gas are spurted into cooling device, particle is 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 spraying；
（2）Prepare covering liquid
Tungstenic compound is dissolved in deionized water, is stirred well to and is completely dissolved, is well mixed；
（3）Cladding
In covering liquid, the above-mentioned ball-type positive pole LiFePO 4 material addition ball grinder that will be prepared, with turning for 300-500r/min
Fast ball milling mixing 4-6h, obtains mixed liquor；
After by the mixed liquor vacuum drying after mill, with the speed of 15 DEG C/min from room temperature to 480-620 DEG C, in 480-620
Constant temperature pre-burning 3-6h at DEG C, then be warming up to 850-900 DEG C with the speed of 10 DEG C/min, in calcining at constant temperature 8- at 850-900 DEG C
10h, is finally down to room temperature with the at the uniform velocity rate of temperature fall of 5 DEG C/min, after being fully ground, obtains tungsten coated LiFePO 4 for lithium ion batteries positive pole material
Material.
2. the method for claim 1, it is characterised in that described Tungstenic compound uses ammonium metatungstate, and described is inclined
Ammonium tungstate is the 1wt%-3wt% of above-mentioned ball-type positive pole LiFePO 4 material mass fraction.
3. method as claimed in claim 1 or 2, it is characterised in that the step（1）In reducibility gas be nitrogen and hydrogen
The percent by volume 1-3% of the mixture of gas, wherein hydrogen in mixed gas.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107895788A (en) * | 2017-11-23 | 2018-04-10 | 绵阳师范学院 | A kind of conducting metal oxide modifies LiFePO4The preparation method of positive electrode |
| CN108288704A (en) * | 2018-02-05 | 2018-07-17 | 邳州易萨新型材料有限公司 | A kind of preparation method of anode material of lithium battery |
| CN111900401A (en) * | 2020-07-24 | 2020-11-06 | 贵州梅岭电源有限公司 | Method for coating positive electrode material of lithium battery by using tungsten oxide and nitrogen-doped carbon composite |
| CN112786859A (en) * | 2021-01-22 | 2021-05-11 | 合肥国轩高科动力能源有限公司 | Preparation method of tantalum-doped/porous metal nanoparticle-coated modified lithium iron phosphate material |
| CN115732647A (en) * | 2021-08-30 | 2023-03-03 | 中国科学院化学研究所 | Low-alkalinity high-lattice-stability coated modified cathode material and preparation method and application thereof |
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| CN101604747A (en) * | 2009-07-07 | 2009-12-16 | 刘强 | The preparation method of lithium iron phosphate positive material |
| CN103618065A (en) * | 2013-11-20 | 2014-03-05 | 浙江南都电源动力股份有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN105742592A (en) * | 2016-03-02 | 2016-07-06 | 合肥国轩高科动力能源有限公司 | W/W2Preparation method of C/Action Carbon coated lithium ion battery anode material |
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| CN101428781A (en) * | 2008-12-08 | 2009-05-13 | 广州丰江电池新技术有限公司 | Conglobation type nanostructured lithium iron phosphate anode material and method for producing the same |
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| CN105742592A (en) * | 2016-03-02 | 2016-07-06 | 合肥国轩高科动力能源有限公司 | W/W2Preparation method of C/Action Carbon coated lithium ion battery anode material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107895788A (en) * | 2017-11-23 | 2018-04-10 | 绵阳师范学院 | A kind of conducting metal oxide modifies LiFePO4The preparation method of positive electrode |
| CN108288704A (en) * | 2018-02-05 | 2018-07-17 | 邳州易萨新型材料有限公司 | A kind of preparation method of anode material of lithium battery |
| CN111900401A (en) * | 2020-07-24 | 2020-11-06 | 贵州梅岭电源有限公司 | Method for coating positive electrode material of lithium battery by using tungsten oxide and nitrogen-doped carbon composite |
| CN111900401B (en) * | 2020-07-24 | 2022-02-22 | 贵州梅岭电源有限公司 | Method for coating positive electrode material of lithium battery by using tungsten oxide and nitrogen-doped carbon composite |
| CN112786859A (en) * | 2021-01-22 | 2021-05-11 | 合肥国轩高科动力能源有限公司 | Preparation method of tantalum-doped/porous metal nanoparticle-coated modified lithium iron phosphate material |
| CN115732647A (en) * | 2021-08-30 | 2023-03-03 | 中国科学院化学研究所 | Low-alkalinity high-lattice-stability coated modified cathode material and preparation method and application thereof |
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Application publication date: 20170707 |