CN107221657A - A kind of preparation method of three-dimensional carbon composite lithium ion battery material - Google Patents
A kind of preparation method of three-dimensional carbon composite lithium ion battery material Download PDFInfo
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- CN107221657A CN107221657A CN201710435662.5A CN201710435662A CN107221657A CN 107221657 A CN107221657 A CN 107221657A CN 201710435662 A CN201710435662 A CN 201710435662A CN 107221657 A CN107221657 A CN 107221657A
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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
- H01M4/362—Composites
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- 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
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- 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 three-dimensional carbon composite lithium ion battery material, methods described is simple to operation, cost is low, it is time-consuming short, coated using the stratum level hole carbon material of three-dimensional structure, active component capacity is improved with meso-hole structure, and three-dimensional structure can effectively improve the scattering and permeating of electrolyte, electronic and ionic efficiency of transmission is improved, circulation and the high rate performance of positive electrode is effectively improved.
Description
Technical field
The present invention relates to battery material field, and in particular to a kind of preparation method of three-dimensional carbon composite lithium ion battery material.
Background technology
New energy industry is that the current whole world improves an important development direction of energy shortage and environmental protection.Lithium-ion electric
Pond is due to high operating voltage, and memory-less effect, self discharge is small, energy density is big and the advantage that has extended cycle life, by
To extensive concern.Current lithium ion battery mainly develops towards high-energy-density, low production cost, high safety direction.
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 of -950 DEG C of even more highs, and calcination time is 10-60h or so.High temperature solid phase synthesis operate and
Process Route Planning is simple, and 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.
The ion and electron conduction of LiFePO4 are poor.Surface coating is that current improvement anode material for lithium-ion batteries is not enough
One of effective ways, clad can not only effectively suppress the side reaction between electrolyte and positive electrode, can also suppress material
Cycle performance under dissolving of middle transition metal etc., the cyclical stability and high magnification of reinforcing material etc., is effectively improved material
Chemical property.
The content of the invention
The present invention provides a kind of preparation method of three-dimensional carbon composite lithium ion battery material, and methods described is simple to operation, cost
It is low, it is time-consuming short, coated using the stratum level hole carbon material of three-dimensional structure, active component appearance is improved with meso-hole structure
Amount, and three-dimensional structure can effectively improve the scattering and permeating of electrolyte, improve electronic and ionic efficiency of transmission, effectively improve positive pole
The circulation of material and high rate performance.
To achieve these goals, the present invention provides a kind of preparation method of three-dimensional carbon composite lithium ion battery material, this method
Comprise 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 three-dimensional flower-shaped carbon material
Potassium hydroxide and zinc acetate progress hydro-thermal reaction soluble in water are obtained to the matter of flower shape zinc oxide, potassium hydroxide and zinc acetate
Amount is than being 3:(2-4)；
Flower shape zinc oxide, mesoporous pore creating material are mixed in water into then addition trishydroxymethylaminomethane and dopamine hydrochloride to enter
Row mixing coating reaction, product suction filtration is then dried, solid product is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction
One, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine hydrochloride are 10:(3-
5):(2-3):(2-4)；
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, three hydroxyls are then sequentially added
Aminomethane and dopamine hydrochloride carry out mixing coating reaction, on the basis of the meso-hole structure that solid product one is constructed
One layer of microcellular structure is coated, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide template is removed with acid, is obtained
Three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate potassium, three
The mass ratio of hydroxymethyl aminomethane and dopamine hydrochloride is 10:(1-2):(4-5):(9-11)；
（3）Compound coating
The three-dimensional flower-shaped carbon material of gained and the LiFePO 4 material are combined, compound condition is：Under a nitrogen atmosphere, plus
Heat is incubated 20-24h, then purged to 150-200 DEG C, removes the LiFePO 4 material being not filled by into duct, three-dimensional carbon bag
Cover lithium iron phosphate positive material.
It is preferred that, the step（2）In, hydrothermal temperature is 80-90 DEG C, and the reaction time is 30-50min, described mixed
The temperature for closing coating reaction is 25-40 DEG C, and the time is 6-8h.
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）The present invention is coated using the stratum level hole carbon material of three-dimensional structure, and activity is improved with meso-hole structure
Composition capacity, and three-dimensional structure can effectively improve the scattering and permeating of electrolyte, improve electronic and ionic efficiency of transmission, be effectively improved
The circulation of positive electrode and high rate performance.
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.
Potassium hydroxide and the zinc acetate hydro-thermal reaction soluble in water that carries out are obtained into flower shape zinc oxide, potassium hydroxide and zinc acetate
Mass ratio be 3:2；Hydrothermal temperature is 80 DEG C, and the reaction time is 30min.
Flower shape zinc oxide, mesoporous pore creating material are mixed in water and then added trishydroxymethylaminomethane and dopamine hydrochloric acid
Salt carries out mixing coating reaction, then dries product suction filtration, solid is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction
Product one, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine hydrochloride are 10:
3:2:2；The temperature of the mixing coating reaction is 25 DEG C, and the time is 6h.
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, then sequentially added
Trishydroxymethylaminomethane and dopamine hydrochloride carry out mixing coating reaction, the base for the meso-hole structure constructed in solid product one
One layer of microcellular structure is coated on plinth, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide mould is removed with acid
Plate, obtains the three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate
The mass ratio of potassium, trishydroxymethylaminomethane and dopamine hydrochloride is 10:1:4:9.
The three-dimensional flower-shaped carbon material of gained and the LiFePO 4 material are combined, compound condition is：In condition of nitrogen gas
Under, 150 DEG C are heated to, 20h is incubated, is then purged, the LiFePO 4 material being not filled by into duct, three-dimensional carbon coating is removed
Lithium iron phosphate positive 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.
Potassium hydroxide and the zinc acetate hydro-thermal reaction soluble in water that carries out are obtained into flower shape zinc oxide, potassium hydroxide and zinc acetate
Mass ratio be 3:4；Hydrothermal temperature is 90 DEG C, and the reaction time is 50min.
Flower shape zinc oxide, mesoporous pore creating material are mixed in water and then added trishydroxymethylaminomethane and dopamine hydrochloric acid
Salt carries out mixing coating reaction, then dries product suction filtration, solid is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction
Product one, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine hydrochloride are 10:
5:3:4；The temperature of the mixing coating reaction is 40 DEG C, and the time is 8h.
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, then sequentially added
Trishydroxymethylaminomethane and dopamine hydrochloride carry out mixing coating reaction, the base for the meso-hole structure constructed in solid product one
One layer of microcellular structure is coated on plinth, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide mould is removed with acid
Plate, obtains the three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate
The mass ratio of potassium, trishydroxymethylaminomethane and dopamine hydrochloride is 10:2:5:11.
The three-dimensional flower-shaped carbon material of gained and the LiFePO 4 material are combined, compound condition is：In condition of nitrogen gas
Under, 200 DEG C are heated to, 24h is incubated, is then purged, the LiFePO 4 material being not filled by into duct, three-dimensional carbon coating is removed
Lithium iron phosphate positive 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 24-27%, and service life brings up to more than 20%.
Claims (2)
1. a kind of preparation method of three-dimensional carbon composite lithium ion battery 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 three-dimensional flower-shaped carbon material
Potassium hydroxide and zinc acetate progress hydro-thermal reaction soluble in water are obtained to the matter of flower shape zinc oxide, potassium hydroxide and zinc acetate
Amount is than being 3:(2-4)；
Flower shape zinc oxide, mesoporous pore creating material are mixed in water into then addition trishydroxymethylaminomethane and dopamine hydrochloride to enter
Row mixing coating reaction, product suction filtration is then dried, solid product is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction
One, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine hydrochloride are 10:(3-
5):(2-3):(2-4)；
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, three hydroxyls are then sequentially added
Aminomethane and dopamine hydrochloride carry out mixing coating reaction, on the basis of the meso-hole structure that solid product one is constructed
One layer of microcellular structure is coated, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide template is removed with acid, is obtained
Three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate potassium, three
The mass ratio of hydroxymethyl aminomethane and dopamine hydrochloride is 10:(1-2):(4-5):(9-11)；
（3）Compound coating
The three-dimensional flower-shaped carbon material of gained and the LiFePO 4 material are combined, compound condition is：Under a nitrogen atmosphere, plus
Heat is incubated 20-24h, then purged to 150-200 DEG C, removes the LiFePO 4 material being not filled by into duct, three-dimensional carbon bag
Cover lithium iron phosphate positive material.
2. the method as described in claim 1, it is characterised in that the step（2）In, hydrothermal temperature is 80-90 DEG C, instead
It is 30-50min between seasonable, the temperature of the mixing coating reaction is 25-40 DEG C, and the time is 6-8h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101604747A (en) * | 2009-07-07 | 2009-12-16 | 刘强 | The preparation method of lithium iron phosphate positive material |
| 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 |
| CN106654231A (en) * | 2017-01-23 | 2017-05-10 | 武汉理工大学 | Anode material for lithium sulfur batteries and method for preparing anode material |
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2017
- 2017-06-11 CN CN201710435662.5A patent/CN107221657A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101604747A (en) * | 2009-07-07 | 2009-12-16 | 刘强 | The preparation method of lithium iron phosphate positive material |
| 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 |
| CN106654231A (en) * | 2017-01-23 | 2017-05-10 | 武汉理工大学 | Anode material for lithium sulfur batteries and method for preparing anode material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20170929 |