CN106920925A - A kind of lithium iron phosphate positive material preparation method - Google Patents
A kind of lithium iron phosphate positive material preparation method Download PDFInfo
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- CN106920925A CN106920925A CN201510998804.XA CN201510998804A CN106920925A CN 106920925 A CN106920925 A CN 106920925A CN 201510998804 A CN201510998804 A CN 201510998804A CN 106920925 A CN106920925 A CN 106920925A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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Abstract
A kind of lithium iron phosphate positive material preparation method, comprises the following steps：Step 1, according to stoichiometric proportion 1:1:1 ratio weighs lithium carbonate, ammonium dihydrogen phosphate, ferrous oxalate respectively, carries out, with 350~450rpm rotating speed 6~10h of ball milling, being then vacuum dried 10~20h at 60~100 DEG C and obtaining ferric lithium phosphate precursor powder after adding absolute ethyl alcohol well mixed；Step 2, by ferric lithium phosphate precursor obtained in step 1 in the tube furnace of purity nitrogen atmosphere protection 350~450 DEG C of 4~6h of insulation, naturally cool to room temperature and obtain lithium iron phosphate positive material after being continuously heating to 600~800 DEG C of 6~10h of calcining；Step 3, weigh the LiFePO4 quality that step 1 is obtained 1wt.%~3wt.% copper foil and LiFePO4 quality 4wt.%~10wt.% sucrose be added to step 2 gained LiFePO 4 material in, washed with ethanol after 1~3h of ball milling, be centrifuged after dry, the lithium iron phosphate positive material of copper and carbon cladding jointly is obtained in the purity nitrogen atmosphere after 600~800 DEG C of 1~3h of calcining.
Description
【Technical field】
The present invention relates to technical field of lithium batteries, more particularly to a kind of lithium iron phosphate positive material preparation method.
【Background technology】
Developing rapidly for auto industry, has promoted the progress and development of the industries such as global machinery, the energy, traffic,
But fuel-engined vehicle is while promoting the well-being of mankind, exhaust emissions also causes severe contamination to human residential environment.
The requirement of environmental protection and energy shortage has driven the development of electric automobile (EV) and electrokinetic cell.Current electric motor car is deposited
Subject matter be the aspects such as price, continual mileage, power performance, and these problems all with battery skill
Art is closely related, and the research and development of battery technology and battery material will develop to it and play a decisive role, thus
Exploitation high-energy-density, cheap, safe and reliable positive electrode are found to electrical source of power lithium ion battery
Exploitation have very important significance.Current commercialized lithium ion anode material is mainly with LiFePO4
(LiFePO4), ternary material (nickel-cobalt-manganese ternary material NCM, nickel cobalt aluminium ternary material NCA) and manganese
Sour lithium (LiMn2O4) etc. based on, wherein lithium manganate battery cycle life is short and hot environment under cycle life more
Difference, and there is safety issue as electrokinetic cell in ternary material.LiFePO4 cost of material is low, and theory is held
Amount is big, has extended cycle life, and is the generally acknowledged most promising product of lithium battery.However, brilliant in LiFePO4
In body structure, because adjacent FeO6 octahedrons are connected by common summit, therefore, its electronic conductivity is low；
In addition, PO4 tetrahedrons are located between FeO6 octahedrons, this hinders the diffusion motion of Li+ to a certain extent；
Low electronic conductivity and low ion diffusion rates are not suitable for high current charge-discharge, limit LiFePO4 capacity
Play.
The shortcoming poor for the ion and electron conduction of LiFePO4, general method of modifying is carbon coating,
Material granule nanosizing and metal ion mixing etc., the high rate performance of battery are improved by above method, are changed
It is apt to its cyclical stability.Wherein nanosizing makes the poor processability of material, and doping vario-property technique is more complicated,
Need to be improved and develop.With it is most commonly used be carbon coating technology, the good conductivity and price of carbon material
It is cheap, while electrical conductivity is improved, moreover it is possible to suppress particle growth.The electrochemistry of carbon-coated LiFePO 4 for lithium ion batteries
The decentralization of energy and carbon source used, content and carbon has much relations.Traditional carbon coated majority is unformed
Carbon, itself pattern be especially distributed it is uncontrollable, while introducing of the carbon source as inert matter, can drop
The specific capacity of low electrode and the tap density of material.
【The content of the invention】
The technical problems to be solved by the invention be provide a kind of electronic conductivity that can improve material and from
Sub- conductivity, while particle growth can be suppressed, reduces the iron phosphate lithium positive pole material of the diffusion path of lithium ion
Preparation method for material.
To achieve these goals, the present invention provides a kind of lithium iron phosphate positive material preparation method, including such as
Lower step：
Step 1, according to stoichiometric proportion 1:1:It is sub- that 1 ratio weighs lithium carbonate, ammonium dihydrogen phosphate, oxalic acid respectively
Iron, is carried out with 350~450rpm rotating speed 6~10h of ball milling, then 60~100 after adding absolute ethyl alcohol well mixed
DEG C vacuum drying 10~20h obtain ferric lithium phosphate precursor powder；
Step 2, by ferric lithium phosphate precursor obtained in step 1 in the tube furnace of purity nitrogen atmosphere protection
350~450 DEG C of 4~6h of insulation, naturally cool to room temperature and obtain phosphorus after being continuously heating to 600~800 DEG C of 6~10h of calcining
Sour iron lithium anode material；
Step 3, weigh the LiFePO4 quality that step 1 is obtained 1wt.%~3wt.% copper foil and ferric phosphate
The sucrose of the 4wt.%~10wt.% of lithium quality is added in the LiFePO 4 material of step 2 gained, 1~3h of ball milling
Washed with ethanol afterwards, be centrifuged after dry, obtain copper and carbon after 600~800 DEG C of 1~3h of calcining in the purity nitrogen atmosphere
The lithium iron phosphate positive material of common cladding.
The present invention uses sucrose and the common coated LiFePO 4 for lithium ion batteries of copper foil, is made in solid phase reaction using copper foil
The electrical conductivity of class graphite mould carbon, raising material is formed for the catalyst sucrose of chemical reaction, while rising into
Core effect, refiner material particle, and then improve the capacity and cycle performance of material.Other preparation process is simple,
Suitable for industrialized production.
【Brief description of the drawings】
The SEM of the copper foil that Fig. 1 is added by lithium iron phosphate positive material preparation method embodiment 2 of the present invention
Shape appearance figure.
Fig. 2 is LiFePO4/C (figures prepared by the contrast of lithium iron phosphate positive material preparation method embodiment 2 of the present invention
It is middle a) and lithium iron phosphate positive material preparation method embodiment 2 of the present invention prepare LiFePO4/Cu/C LiFePO4s
The SEM figures of positive electrode (b in figure).
Fig. 3 be LiFePO4/C prepared by lithium iron phosphate positive material preparation method embodiment 2 of the present invention contrast and
LiFePO4/Cu/C lithium iron phosphate positive materials are further made charging and discharging curve of the lithium battery under 0.2C multiplying powers
Figure
Fig. 4 is LiFePO4/C prepared by the contrast of lithium iron phosphate positive material preparation method embodiment 2 of the present invention
And LiFePO4/Cu/C lithium iron phosphate positive materials are further made circulation figure under lithium battery 0.2C multiplying powers.
【Specific embodiment】
In order that the purpose of the present invention, technical scheme and Advantageous Effects become apparent from understanding, below in conjunction with
The drawings and specific embodiments, the present invention will be described in further detail.It should be appreciated that this explanation
Specific embodiment described in book is not intended to limit the present invention just for the sake of explaining the present invention.
A kind of lithium iron phosphate positive material preparation method, comprises the following steps：
Step 1, according to stoichiometric proportion 1:1:It is sub- that 1 ratio weighs lithium carbonate, ammonium dihydrogen phosphate, oxalic acid respectively
Iron, adds absolute ethyl alcohol (absolute ethyl alcohol and lithium carbonate, ammonium dihydrogen phosphate, ferrous oxalate volume feed
1.5:1~2.2:1) carried out after being well mixed with 350~450rpm rotating speed 6~10h of ball milling, it is then true at 60~100 DEG C
Sky dries 10~20h and obtains ferric lithium phosphate precursor powder；
Step 2, by ferric lithium phosphate precursor obtained in step 1 in the tube furnace of purity nitrogen atmosphere protection
350~450 DEG C of 4~6h of insulation, naturally cool to room temperature and obtain phosphorus after being continuously heating to 600~800 DEG C of 6~10h of calcining
Sour iron lithium anode material；
Step 3, weigh the LiFePO4 quality that step 1 is obtained 1wt.%~3wt.% copper foil (wherein,
Copper foil must be added on a small quantity, it is to avoid it occurs side reaction with electrolyte under high pressure) and LiFePO4 quality
4wt.%~10wt.% sucrose be added to step 2 gained LiFePO 4 material in, use second after 1~3h of ball milling
Dried after alcohol washing, centrifugation, obtain copper after 600~800 DEG C of 1~3h of calcining in purity nitrogen atmosphere wraps jointly with carbon
The lithium iron phosphate positive material LiFePO4/Cu/C for covering.
Specific embodiment
Embodiment 1：
Step 1,0.05mol lithium carbonates, ammonium dihydrogen phosphate, ferrous oxalate are weighed respectively, add 30mL anhydrous
After terminating with 400rpm/min ball milling 6h, ball milling after ethanol is well mixed 12h is dried in 80 DEG C of vacuum drying chambers
Obtain ferric lithium phosphate precursor powder；
Step 2, ferric lithium phosphate precursor powder is placed in the tube furnace of purity nitrogen atmosphere protection, with 5 DEG C/min's
Heating rate is warming up to 350 DEG C, is incubated 4 hours, then is warming up to 650 DEG C with 5 DEG C/min, is incubated 10 hours,
Naturally cool to room temperature and obtain lithium iron phosphate positive material.
Step 3, weigh 0.11g copper foils and 1.1g sucrose is added in the lithium iron phosphate positive material of preparation, ball
Be well mixed for material by mill 1h；Then with washes of absolute alcohol 3 times and centrifugation, 10h is dried at 50 DEG C；
By dried powder in 600 DEG C of N2It is to obtain copper to be coated jointly with carbon that 2h is incubated in the tube furnace of atmosphere
Lithium iron phosphate positive material LiFePO4/Cu/C.
In order to compare needs, the phosphoric acid of pure carbon coating is also prepared for respectively under identical preparation condition and composition and ratio
Iron lithium anode material LiFePO4/C.
Embodiment 2：
Step 1,0.05mol lithium carbonates, ammonium dihydrogen phosphate, ferrous oxalate are weighed respectively, add 30mL anhydrous
After terminating with 400rpm/min ball milling 8h, ball milling after ethanol is well mixed 12h is dried in 80 DEG C of vacuum drying chambers
Obtain ferric lithium phosphate precursor powder；
Step 2, ferric lithium phosphate precursor powder is placed in the tube furnace of purity nitrogen atmosphere protection, with 5 DEG C/min's
Heating rate is warming up to 350 DEG C, is incubated 4 hours, then is warming up to 650 DEG C with 5 DEG C/min, is incubated 10 hours,
Naturally cool to room temperature and obtain lithium iron phosphate positive material.
Step 3, weigh 0.22g copper foils and 1.1g sucrose is added in the lithium iron phosphate positive material of preparation, ball
Be well mixed for material by mill 2h；Then with washes of absolute alcohol 3 times and centrifugation, 10h is dried at 50 DEG C；
By dried powder in 600 DEG C of N2It is to obtain copper to be coated jointly with carbon that 2h is incubated in the tube furnace of atmosphere
Lithium iron phosphate positive material LiFePO4/Cu/C.
In order to compare needs, the phosphoric acid of pure carbon coating is also prepared for respectively under identical preparation condition and composition and ratio
Iron lithium anode material LiFePO4/C.
Embodiment 3：
Step 1,0.05mol lithium carbonates, ammonium dihydrogen phosphate, ferrous oxalate are weighed respectively, add 30mL anhydrous
After terminating with 450rpm/min ball milling 6h, ball milling after ethanol is well mixed 12h is dried in 80 DEG C of vacuum drying chambers
Obtain ferric lithium phosphate precursor powder；
Step 2, ferric lithium phosphate precursor powder is placed in the tube furnace of purity nitrogen atmosphere protection, with 5 DEG C/min's
Heating rate is warming up to 350 DEG C, is incubated 4 hours, then is warming up to 650 DEG C with 5 DEG C/min, is incubated 10 hours,
It is cooled to room temperature and obtains lithium iron phosphate positive material.
Step 3, weigh 0.33g copper foils and 1.1g sucrose is added in the lithium iron phosphate positive material of preparation, ball
Be well mixed for material by mill 1h；Then with washes of absolute alcohol 3 times and centrifugation, 10h is dried at 50 DEG C；
By dried powder in 600 DEG C of N2It is to obtain copper to be coated jointly with carbon that 3h is incubated in the tube furnace of atmosphere
Lithium iron phosphate positive material LiFePO4/Cu/C.
In order to compare needs, the phosphoric acid of pure carbon coating is also prepared for respectively under identical preparation condition and composition and ratio
Iron lithium anode material LiFePO4/C.
The preparation of positive plate and the assembling of button cell and test
Lithium iron phosphate positive material LiFePO4/Cu/C with present invention synthesis is active material, and Super-P is to lead
Electrode, segregation PVF (PVDF) is binding agent, successively according to 80:10:10 ratio and N- crassitudes
Ketone (NMP) mixes and obtains slurry after grinding.Slurry is coated in current collector aluminum foil, 120 DEG C of dryings of vacuum
12h, punching is obtained the positive pole disk of a diameter of 10mm.
Test Selection of Battery CR2032 button cells, negative pole selects the metal lithium sheet of diameter 14mm, electrolyte choosing
With 1mol LiFP6 (EC：DMC：EMC=1:1:1, v/v), with negative electrode casing-shell fragment-pad-lithium piece
Be packaged for battery by the order of-electrolyte-barrier film-positive plate-pad-anode cover, and whole process is all
Completed in the glove box filled with argon gas.
Test equipment selects new prestige Neware BTS test systems (the test system of Shenzhen Xin Wei Electronics Co., Ltd.s
System, in other embodiments, it is also possible to other test systems commonly used using those skilled in the art), fill
Discharge cut-off voltage 1.8~4.5V of scope, 25 DEG C of test temperature records the discharge capacity first of battery.
The resistivity value of the different positive electrodes obtained by the embodiment of the present invention：Surveyed with solid conductivity measurement
LiFePO 4 material before and after examination cladding, from data it can be seen that as the addition resistivity of copper foil substantially drops
Low, when addition is 2wt.%, resistivity is minimum；Resistivity has declined when addition increases to 3wt.%.
Table 1
The SEM shape appearance figures of the copper foil that Fig. 1 is added by the embodiment of the present invention 2：It can be seen that copper foil is presented
Irregular lamellar structure, with radius-thickness ratio higher, can be very good to be dispersed in around lithium iron phosphate particles.
Fig. 2 is that LiFePO4/C the and LiFePO4/Cu/C LiFePO4s prepared by the embodiment of the present invention 2 are compound just
The SEM figures of pole material：It can be seen that the more uniform cloth of positive electrode LiFePO4/C particles point, grain size
500nm or so (a in figure)；Sample LiFePO4/Cu/C particles are smaller and distribution uniform, and particle diameter is in 200nm
Left and right (b in figure), while not finding copper foil, illustrates to divide well by copper foil after ball milling and calcining
It is dispersed in around lithium iron phosphate particles, has refined the particle of positive electrode；Less particle shortens lithium ion
Diffusion path, improves the lithium ion and electron mobility of LiFePO4 bulk material, and then improves the appearance of material
Amount and cycle performance.
Fig. 3 is LiFePO4/C the and LiFePO4/Cu/C iron phosphate lithium positive pole materials prepared by the embodiment of the present invention 2
Charging and discharging curve figure under material 0.2C multiplying powers：As can be seen from the figure LiFePO4/Cu/C LiFePO4s are compound just
Pole material has specific capacity higher compared with the LiFePO4/C positive electrodes of pure carbon coating under 0.2C, point
Wei not 157mAh/g, 141mAh/g.
LiFePO4/C and LiFePO4/Cu/C iron lithium phosphate compound anodes prepared by Fig. 4 embodiment of the present invention 2
Cycle performance curve under material 0.2C multiplying powers：Copper foil and carbon are coated jointly as seen from the figure
LiFePO4/Cu/C materials have capacity and cyclical stability higher than the LiFePO4/C materials of pure carbon coating,
It is that 92%, LiFePO4/Cu/C, 300 capability retentions of circulation are that LiFePO4/C circulates 300 capability retentions
95%, LiFePO4/Cu/C material attenuation rate are low, cyclical stability is more preferable.It can be seen that, LiFePO4/Cu/C is multiple
Close lithium iron phosphate positive material has potential application value on electrokinetic cell and energy-storage battery application.
Present invention aim to overcome that the existing defect of LiFePO4, there is provided one kind improves material conductivity, carries
Rise the method that capacity improves circulation.The present invention uses sucrose and the common coated LiFePO 4 for lithium ion batteries of copper foil, using copper
Thin slice forms class graphite mould carbon, improves material in solid phase reaction as the catalyst sucrose of chemical reaction
Electrical conductivity, while rise nucleation, refiner material particle, and then improve material capacity and cycle performance.
Other preparation process is simple, it is adaptable to industrialized production.
The present invention is not restricted to described in specification and implementation method, therefore for the people of familiar field
Additional advantage and modification are easily achieved for member, therefore are limited without departing substantially from claim and equivalency range
In the case of the spirit and scope of fixed universal, the present invention is not limited to specific details, representational
Equipment and shown here as with description examples shown.
Claims (5)
1. a kind of lithium iron phosphate positive material preparation method, comprises the following steps：
Step 1, according to stoichiometric proportion 1:1:It is sub- that 1 ratio weighs lithium carbonate, ammonium dihydrogen phosphate, oxalic acid respectively
Iron, is carried out with 350~450rpm rotating speed 6~10h of ball milling, then 60~100 after adding absolute ethyl alcohol well mixed
DEG C vacuum drying 10~20h obtain ferric lithium phosphate precursor powder；
Step 2, by ferric lithium phosphate precursor obtained in step 1 in the tube furnace of purity nitrogen atmosphere protection
350~450 DEG C of 4~6h of insulation, naturally cool to room temperature and obtain phosphorus after being continuously heating to 600~800 DEG C of 6~10h of calcining
Sour iron lithium anode material；
Step 3, weigh the LiFePO4 quality that step 1 is obtained 1wt.%~3wt.% copper foil and ferric phosphate
The sucrose of the 4wt.%~10wt.% of lithium quality is added in the LiFePO 4 material of step 2 gained, 1~3h of ball milling
Washed with ethanol afterwards, be centrifuged after dry, obtain copper and carbon after 600~800 DEG C of 1~3h of calcining in the purity nitrogen atmosphere
The lithium iron phosphate positive material of common cladding.
2. lithium iron phosphate positive material preparation method as claimed in claim 1, it is characterised in that：In step 1
With 400rpm/min ball milling 6h, ball milling dries 12h after terminating in 80 DEG C of vacuum drying chambers.
3. lithium iron phosphate positive material preparation method as claimed in claim 1, it is characterised in that：Step 2
In be warming up to 350 DEG C with the heating rate of 5 DEG C/min, be incubated 4 hours, then 650 are warming up to 5 DEG C/min
DEG C, it is incubated 10 hours.
4. lithium iron phosphate positive material preparation method as claimed in claim 1, it is characterised in that：Step 3
Be well mixed for material by middle ball milling 1h；Then with washes of absolute alcohol 3 times and centrifugation, in 50 DEG C of dryings
10h；By dried powder in 600 DEG C of N22h is incubated in the tube furnace of atmosphere.
5. lithium iron phosphate positive material preparation method as claimed in claim 1, it is characterised in that：Step 1
Middle absolute ethyl alcohol and lithium carbonate, ammonium dihydrogen phosphate, ferrous oxalate volume feed 1.5:1~2.2:1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107946572A (en) * | 2017-11-20 | 2018-04-20 | 广西师范大学 | A kind of novel metal elemental copper/lithium iron phosphate/carbon composite material and its preparation method and application |
| CN110600744A (en) * | 2019-07-18 | 2019-12-20 | 桑顿新能源科技(长沙)有限公司 | Carbon-coated lithium iron phosphate material, preparation method and lithium ion battery anode material |
| CN114122361A (en) * | 2021-11-25 | 2022-03-01 | 天能帅福得能源股份有限公司 | Preparation method of lithium ion battery using modified lithium iron phosphate |
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| CN1649188A (en) * | 2004-12-17 | 2005-08-03 | 清华大学 | Method for preparing metal Ni, Cu, coated LiFePo4 powder |
| CN1649189A (en) * | 2004-12-29 | 2005-08-03 | 浙江大学 | Method for preparing carbon coated lithium ferrous phosphate composite material including metal conductive agent |
| CN101339988A (en) * | 2008-06-25 | 2009-01-07 | 中国地质大学（武汉） | Positive electrode material of lithium ion cell and its preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107946572A (en) * | 2017-11-20 | 2018-04-20 | 广西师范大学 | A kind of novel metal elemental copper/lithium iron phosphate/carbon composite material and its preparation method and application |
| CN107946572B (en) * | 2017-11-20 | 2020-05-15 | 广西师范大学 | Metal elemental copper/lithium iron phosphate/carbon composite material and preparation method and application thereof |
| CN110600744A (en) * | 2019-07-18 | 2019-12-20 | 桑顿新能源科技(长沙)有限公司 | Carbon-coated lithium iron phosphate material, preparation method and lithium ion battery anode material |
| CN114122361A (en) * | 2021-11-25 | 2022-03-01 | 天能帅福得能源股份有限公司 | Preparation method of lithium ion battery using modified lithium iron phosphate |
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Application publication date: 20170704 |