CN105226274B - A kind of preparation method of the scattered LiFePO4/graphene composite material of graphene uniform - Google Patents
A kind of preparation method of the scattered LiFePO4/graphene composite material of graphene uniform Download PDFInfo
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- CN105226274B CN105226274B CN201510391178.8A CN201510391178A CN105226274B CN 105226274 B CN105226274 B CN 105226274B CN 201510391178 A CN201510391178 A CN 201510391178A CN 105226274 B CN105226274 B CN 105226274B
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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
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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Abstract
A kind of preparation method of the LiFePO4/graphene composite material disperseed the present invention relates to graphene uniform, comprises the following steps：By ferric lithium phosphate precursor carry out it is pre-dispersed obtain slurry, adding chitosan dispersant to graphene with identical dispersant solution carries out that ultrasound is pre-dispersed to obtain graphene slurry.Extra-fine grinding admixed graphite alkene slurry and ferric lithium phosphate precursor slurry, realize that graphene slurry and ferric lithium phosphate precursor slurry are miscible, are dried by fast spraying, LiFePO4/graphene composite material is obtained after calcining again.Present invention process process is simple, it is easily achieved industrialized production, the LiFePO4 obtained/graphene composite material electrochemical performance, especially the powder resistance rate of material obtains effective reduction, polarization reduction, coulombic efficiency is obviously improved first, is with a wide range of applications in power lithium-ion battery field.
Description
Technical field
Prepared the present invention relates to electrochemical material and new energy field, more particularly to a kind of scattered phosphoric acid of graphene uniform
The preparation method of iron lithium/graphene composite material.
Background technology
With increasingly sharpening for energy crisis, new renewable resource is all being found in the whole world, renewable resource such as solar energy,
Wind energy, tide energy, geothermal energy etc. have the characteristics of region drinks timeliness.These resources are made full use of, it is necessary to intelligent grid
Or large-scale energy-storage system.Lithium ion battery has good application prospect as energy storage potential.On the other hand, petrochemical industry energy
The increasingly depleted in source forces people to develop hybrid electrically or pure electric vehicle, and its core component battery turns into research emphasis.
Lithium ion its higher energy density compared with other batteries, good security and longer service life and enjoy pro-gaze.
LiFePO 4 material is as anode material for lithium-ion batteries, with its abundant raw material, cheap, environmental protection, work
Make the advantages of voltage is moderate, heat endurance is good, cause the extensive concern of people.But the poorly conductive of LiFePO 4 material,
Lithium ion diffusion rate is slow, and lithium iron phosphate dynamic battery can not meet demand of the market to electric car high current charge-discharge.Graphite
Alkene, as a kind of new two-dimension nano materials, is the Two Dimensional Free state atomic crystal for the unique presence having now been found that.Graphene
Shown due to its special nanostructured and excellent physical and chemical performance in fields such as electronics, optics, catalysis, energy storage
Huge application potential.Field of lithium ion battery, Many researchers are by by grapheme material and existing battery material system
It is combined electric conductivity to lift electrode material etc..
Patent CN103855391A discloses fluorophosphoric acid iron lithium/graphene composite material and its preparation method and application.It is logical
Cross Fe source compound and phosphate compounds grinding prepares after precursor powder is calcined and obtains ferric phosphate, by ferric phosphate and oxidation stone
Ink, lithium fluoride, which pass through, obtains fluorophosphoric acid iron lithium/graphene composite material after ground and mixed, calcining.Patent CN103872287A is public
A kind of grapheme lithium iron phosphate battery anode composite material of cloth and preparation method thereof, is prepared first with high-temperature solid phase reaction method
Carbon-coated LiFePO 4 for lithium ion batteries positive electrode has been obtained, then by carbon-coated LiFePO 4 for lithium ion batteries material and grapheme material with alcohol or pure water
Ball milling is carried out for dispersant to disperse, cooling grinding obtains grapheme lithium iron phosphate anode composite wood after the drying of 60-120 degree
Material.Patent CN101562248A discloses a kind of compound lithium ion battery anode material lithium iron phosphate of graphene and its preparation side
Method.0.1-2.5% graphenes and graphene oxide by nano-grade lithium iron phosphate pure phase powder and LiFePO4 weight ratio is abundant
Mixed calcining or by iron content, lithium and phosphate radical according to certain mol proportion and by LiFePO4 weight than 0.5-5% graphene
Or the raw material of graphene oxide be sufficiently mixed after calcine.The characteristics of above-mentioned patent has one jointly, by graphene or oxidation stone
It is dry-mixed or add absolute ethyl alcohol, pure water polo that black alkene and LiFePO 4 material and ferric lithium phosphate precursor carry out simple ball milling
Mill mixing.Inherently there is the characteristics of being difficult to dispersed in dry powder ball milling.Have specific surface area big in view of graphene, it is easy to roll into a ball
Poly- the characteristics of, therefore common wet ball grinding is also difficult to disperse graphene well.
The content of the invention
The technical problem to be solved in the present invention is：A kind of scattered LiFePO4/graphene of graphene uniform is provided to be combined
The preparation method of material.
In order to solve the above-mentioned technical problem the present invention is adopted the following technical scheme that：
A kind of preparation method of the scattered LiFePO4/graphene composite material of graphene uniform, comprises the following steps：
(1) it is 0.5%~3.5% to weigh dispersant and be dissolved in deionized water and prepare dispersant according to dispersant mass fraction
Solution, according still further to mol ratio Li：Fe=(0.98~1.0 (2)：1 weighs phosphoric acid iron material and lithium source is added to dispersant solution
In, the solid content for controlling slurry is 25%~45%, is added in Ball-stirring mill, is ground stir process and obtains before LiFePO4
Drive somaplasm material；
(2) water soluble chitosan is weighed, is dissolved in the dispersant solution that dispersant mass fraction is 0.5%~3.5%, obtains
Chitosan dispersant blend solution is obtained, the wherein mass concentration of chitosan is 0.5%~2%, then weighs graphene powder addition
Into above-mentioned chitosan solution, the mass concentration for controlling graphene is 3%~5%, and graphene slurry is obtained after ultrasonic disperse
Material；
(3) the ferric lithium phosphate precursor slurry and graphene slurry in Ball-stirring mill are transferred in extra-fine grinding equipment
Row extra-fine grinding decentralized processing, the addition of graphene slurry is according to 0.5% that graphene content is theoretical LiFePO4 yield
~2% adds, after extra-fine grinding about 30min, and slurry spray drying obtains presoma；
(4) presoma of above-mentioned acquisition is placed in 350~500 DEG C of insulation 3h, 700~750 DEG C of guarantors under inert atmosphere protection
Warm 10h is to obtain LiFePO4/graphene composite material.
Preferably, the dispersant in step (1) is the combination of one or both of polyvinylpyrrolidone, polyvinyl alcohol,
Polyvinylpyrrolidone, the molecular weight of polyvinyl alcohol are 50000 to 80000.
Preferably, the lithium source in step (1) is one kind or at least two in lithium carbonate, lithium hydroxide, lithium acetate, lithium fluoride
The combination planted.
Preferably, the deacetylation of the chitosan in step (2) is 50%~60%, and the molecular weight of chitosan is 80000
~100000.
Preferably, the inert gas in step (4) is the one or more in helium, nitrogen and argon gas.
The beneficial effects of the invention are as follows：Present invention process process is simple, it is easy to accomplish industrialized production, the phosphoric acid obtained
The powder resistance rate of iron lithium/graphene composite material electrochemical performance, especially material obtains effective reduction, polarization drop
Low, coulombic efficiency is obviously improved first, is with a wide range of applications in power lithium-ion battery field.Before LiFePO4
Drive body progress is pre-dispersed to obtain slurry, adds chitosan dispersant progress ultrasound with identical dispersant solution to graphene and divides in advance
Dissipate and obtain graphene slurry.Extra-fine grinding admixed graphite alkene slurry and ferric lithium phosphate precursor slurry, realize graphene slurry again
It is miscible with ferric lithium phosphate precursor slurry, dried by fast spraying, LiFePO4/graphene composite material is obtained after calcining.
Wherein used dispersant and chitosan not only play good dispersion effect to ferric lithium phosphate precursor, graphene, its
It is the carbon source of LiFePO 4 material preparation process.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram for LiFePO4/graphene composite material that embodiment 3 is obtained；
Fig. 2 is embodiment 3 and the ferric phosphate obtained in the LiFePO4/graphene composite material and comparative example of acquisition
Discharged under lithium/graphene composite material 0.2C multiplying powers curve comparison figure, wherein, a is LiFePO4/stone obtained in embodiment 3
Black alkene composite, b is LiFePO4/graphene composite material for obtaining in comparative example.
Specific embodiment
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Embodiment 1
(1) be 0.5% to weigh PVP and be dissolved in deionized water preparation PVP solution according to PVP mass fractions, according still further to mole
Compare Li：Fe=0.98：1 weighs appropriate phosphoric acid iron material and lithium carbonate is added in PVP solution, and the solid content for controlling slurry is
45%, it is added in Ball-stirring mill, is ground stir process and obtains ferric lithium phosphate precursor slurry.
(2) appropriate water soluble chitosan is weighed, is dissolved in the PVP solution that mass fraction is 0.5%, acquisition chitosan,
PVP blend solutions.Wherein the mass concentration of chitosan be 0.5%, then weigh appropriate graphene powder be added to above-mentioned shell gather
In sugar, PVP solution, the mass concentration for controlling graphene is 3%, and graphene slurry is obtained after ultrasonic disperse.
(3) the ferric lithium phosphate precursor slurry and graphene slurry in Ball-stirring mill are transferred in extra-fine grinding equipment
Row extra-fine grinding decentralized processing, the addition of graphene slurry is according to 0.5% that graphene content is theoretical LiFePO4 yield
Add.After extra-fine grinding about 30min, slurry spray drying obtains presoma.
(4) presoma of above-mentioned acquisition is placed in 350 degree of insulation 3h under inert atmosphere protection, 700 insulation 10h are to obtain phosphorus
Sour iron lithium/graphene composite material.
The powder resistance rate of the composite is 80 Ω ﹒ cm, and coulombic efficiency is 97.5% to button electrical testing first.
Embodiment 2
(1) be 1.5% to weigh PVA and be dissolved in deionized water and prepare PVA solution according to PVA mass fractions, according still further to mole
Compare Li：Fe=1.0：1 weighs appropriate phosphoric acid iron material and lithium hydroxide is added in PVA solution, controls the solid content of slurry
For 35%, it is added in Ball-stirring mill, is ground stir process and obtains ferric lithium phosphate precursor slurry.
(2) appropriate water soluble chitosan is weighed, is dissolved in the PVA solution that mass fraction is 1.5%, acquisition chitosan,
PVA blend solutions.Wherein the mass concentration of chitosan be 1.0%, then weigh appropriate graphene powder be added to above-mentioned shell gather
In sugar, PVA solution, the mass concentration for controlling graphene is 3.5%, and graphene slurry is obtained after ultrasonic disperse.
(3) the ferric lithium phosphate precursor slurry and graphene slurry in Ball-stirring mill are transferred in extra-fine grinding equipment
Row extra-fine grinding decentralized processing, the addition of graphene slurry is according to 1.5% that graphene content is theoretical LiFePO4 yield
Add.After extra-fine grinding about 30min, slurry spray drying obtains presoma.
(4) presoma of above-mentioned acquisition is placed in 400 degree of insulation 3h under inert atmosphere protection, 710 insulation 10h are to obtain phosphorus
Sour iron lithium/graphene composite material.
The powder resistance rate of the composite is 42.1 Ω ﹒ cm, and coulombic efficiency is 98.2% to button electrical testing first.
Embodiment 3
(1) be 2.0% to weigh PVP and be dissolved in deionized water preparation PVP solution according to PVP mass fractions, according still further to mole
Compare Li：Fe=1.01：1 weighs appropriate phosphoric acid iron material and lithium carbonate is added in PVP solution, and the solid content for controlling slurry is
40%, it is added in Ball-stirring mill, is ground stir process and obtains ferric lithium phosphate precursor slurry.
(2) appropriate water soluble chitosan is weighed, is dissolved in the PVP solution that mass fraction is 2.0%, acquisition chitosan,
PVP blend solutions.Wherein the mass concentration of chitosan be 1.5%, then weigh appropriate graphene powder be added to above-mentioned shell gather
In sugar, PVP solution, the mass concentration for controlling graphene is 4.5%, and graphene slurry is obtained after ultrasonic disperse.
(3) the ferric lithium phosphate precursor slurry and graphene slurry in Ball-stirring mill are transferred in extra-fine grinding equipment
Row extra-fine grinding decentralized processing, the addition of graphene slurry is according to 1.5% that graphene content is theoretical LiFePO4 yield
Add.After extra-fine grinding about 30min, slurry spray drying obtains presoma.
(4) presoma of above-mentioned acquisition is placed in 450 degree of insulation 3h under inert atmosphere protection, 730 insulation 10h are to obtain phosphorus
Sour iron lithium/graphene composite material.
The powder resistance rate of the composite is 26.9 Ω ﹒ cm, and coulombic efficiency is 99.6% to button electrical testing first.
Embodiment 4
(1) be 3.5% to weigh PVA and be dissolved in deionized water and prepare PVA solution according to PVA mass fractions, according still further to mole
Compare Li：Fe=1.02：1 weighs appropriate phosphoric acid iron material and lithium hydroxide is added in PVA solution, controls the solid content of slurry
For 25%, it is added in Ball-stirring mill, is ground stir process and obtains ferric lithium phosphate precursor slurry.
(2) appropriate water soluble chitosan is weighed, is dissolved in the PVA solution that mass fraction is 3.5%, acquisition chitosan,
PVA blend solutions.Wherein the mass concentration of chitosan be 2%, then weigh appropriate graphene powder be added to above-mentioned chitosan,
In PVA solution, the mass concentration for controlling graphene is 5%, and graphene slurry is obtained after ultrasonic disperse.
(3) the ferric lithium phosphate precursor slurry and graphene slurry in Ball-stirring mill are transferred in extra-fine grinding equipment
Row extra-fine grinding decentralized processing, the addition of graphene slurry adds according to 2% that graphene content is theoretical LiFePO4 yield
Enter.After extra-fine grinding about 30min, slurry spray drying obtains presoma.
(4) presoma of above-mentioned acquisition is placed in 500 degree of insulation 3h under inert atmosphere protection, 750 insulation 10h are to obtain phosphorus
Sour iron lithium/graphene composite material.
The powder resistance rate of the composite is 35.7 Ω ﹒ cm, and coulombic efficiency is 98.9% to button electrical testing first.
Comparative example
(1) according to mol ratio Li：Fe=1.01：1 weighs in appropriate phosphoric acid iron material and lithium carbonate deionized water, control
The solid content of slurry is 40%, is added in Ball-stirring mill, is ground stir process and obtains ferric lithium phosphate precursor slurry.
(2) appropriate graphene powder is weighed according to 1.5% that graphene content is theoretical LiFePO4 yield, be added to
In ferric lithium phosphate precursor slurry.After extra-fine grinding about 30min, slurry spray drying obtains presoma.
(3) presoma of above-mentioned acquisition is placed in 450 degree of insulation 3h under inert atmosphere protection, 730 insulation 10h are to obtain phosphorus
Sour iron lithium/graphene composite material.
The powder resistance rate of the composite is 339.5 Ω ﹒ cm, and coulombic efficiency is 95.4% to button electrical testing first.
Button electricity makes and tested
Composite obtained in embodiment 3 and comparative example is assembled into 2016 type button cells and carries out charge and discharge
Electric performance test.According to quality than active material (positive electrode)：Acetylene black：Binding agent (PVDF)=80:10:10, add
NMP, prepares anode sizing agent, is evenly applied on aluminium foil obtain anode pole piece, uses metal lithium sheet for cathode pole piece,
1mol/L LiPF6Ethylene carbonate (EC)+dimethyl carbonate (DMC) (volume ratio is 1: 1) is dissolved in for electrolyte,
Celgard2300 films are barrier film, are assembled in argon gas glove box.Button electricity carries out discharge and recharge in 2.0V~4.0V voltage ranges
Test.From above-described embodiment and comparative example test result, the LiFePO4/graphite prepared using the method for the patent
Alkene composite has lower powder resistance rate and higher coulombic efficiency first.From Fig. 2 contrast first charge-discharge curve
, it is apparent that compared with comparative example, the composite button electrical testing that embodiment 3 is obtained has higher specific discharge capacity,
Higher coulombic efficiency first, smaller mean voltage difference illustrates that the composite has conductive network evenly, this with
Its graphene conductive network it is dispersed relevant.
The embodiments of the present invention described above are not intended to limit the scope of the present invention.It is any in the present invention
Spirit and principle within the modifications, equivalent substitutions and improvements made etc., should be included in the claim protection model of the present invention
Within enclosing.
Claims (3)
1. a kind of preparation method of the scattered LiFePO4/graphene composite material of graphene uniform, it is characterised in that：Including with
Lower step：
(1) it is 0.5%~3.5% to weigh dispersant and be dissolved in deionized water that to prepare dispersant molten according to dispersant mass fraction
Liquid, according still further to mol ratio Li：Fe=(0.98~1.02)：1 weighs phosphoric acid iron material and lithium source is added in dispersant solution, control
The solid content of slurrying material is 25%~45%, is added in Ball-stirring mill, is ground stir process and obtains ferric lithium phosphate precursor
Slurry；
(2) water soluble chitosan is weighed, is dissolved in the dispersant solution that dispersant mass fraction is 0.5%~3.5%, obtains shell
Glycan dispersant blend solution, the wherein mass concentration of chitosan are 0.5%~2%, then weigh graphene powder and be added to
State in chitosan solution, the mass concentration for controlling graphene is 3%~5%, and graphene slurry is obtained after ultrasonic disperse；
(3) the ferric lithium phosphate precursor slurry and graphene slurry in Ball-stirring mill are transferred in extra-fine grinding equipment and surpassed
Fine lapping decentralized processing, the addition of graphene slurry is according to 0.5%~2% that graphene content is theoretical LiFePO4 yield
Add, after extra-fine grinding 30min, slurry spray drying obtains presoma；
(4) presoma of above-mentioned acquisition is placed in 350~500 DEG C of insulations 3h, 700~750 DEG C of insulation 10h under inert atmosphere protection
Obtain LiFePO4/graphene composite material；
Wherein, the dispersant in step (1) is the combination of one or both of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene
Pyrrolidones, the molecular weight of polyvinyl alcohol are 50000 to 80000；
The deacetylation of chitosan in step (2) is 50%~60%, and the molecular weight of chitosan is 80000~100000.
2. the preparation method of the scattered LiFePO4/graphene composite material of graphene uniform according to claim 1, its
It is characterised by：Lithium source in step (1) is one kind or at least two group in lithium carbonate, lithium hydroxide, lithium acetate, lithium fluoride
Close.
3. the preparation method of the scattered LiFePO4/graphene composite material of graphene uniform according to claim 1, its
It is characterised by：Inert gas in step (4) is the one or more in helium, nitrogen and argon gas.
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| CN106299360B (en) * | 2016-11-08 | 2019-01-29 | 浙江瑞邦科技有限公司 | A kind of LiFePO4/graphene composite material and its preparation method and application |
| CN106711447A (en) * | 2016-12-19 | 2017-05-24 | 重庆汉岳科技发展有限公司 | Preparation method of compound graphene lithium battery positive electrode material |
| CN107845792A (en) * | 2017-10-20 | 2018-03-27 | 深圳市毓丰新材料有限公司 | A kind of LiFePO4 with loose structure/graphene composite lithium ion battery positive electrode |
| CN108179627A (en) * | 2017-12-28 | 2018-06-19 | 泉州迪特工业产品设计有限公司 | A kind of graphene dress materials and its manufacturing method |
| CN108417801A (en) * | 2018-03-07 | 2018-08-17 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene In-situ reaction lithium iron phosphate positive material and preparation method thereof |
| CN110429277B (en) * | 2019-06-28 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Preparation method of high-compaction high-rate lithium iron phosphate cathode material |
| CN110176599A (en) * | 2019-07-10 | 2019-08-27 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene In-situ reaction lithium iron phosphate positive material and preparation method thereof |
| CN111293294B (en) * | 2020-02-22 | 2022-04-22 | 电子科技大学 | Method for synthesizing lithium iron phosphate/graphene composite material by template method in one step |
| CN112694078A (en) * | 2020-12-29 | 2021-04-23 | 陕西煤业化工技术研究院有限责任公司 | Graphene-coated lithium iron phosphate composite material and preparation method thereof |
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