CN107093726A - A kind of method for improving lithium ion battery electrode material chemical property - Google Patents
A kind of method for improving lithium ion battery electrode material chemical property Download PDFInfo
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- CN107093726A CN107093726A CN201710301517.8A CN201710301517A CN107093726A CN 107093726 A CN107093726 A CN 107093726A CN 201710301517 A CN201710301517 A CN 201710301517A CN 107093726 A CN107093726 A CN 107093726A
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/02—Electrodes composed of, or comprising, active material
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Abstract
The invention discloses a kind of method for improving lithium ion battery electrode material chemical property, comprise the following steps：Surfactant is dissolved in deionized water；Various salt and auxiliary material are added in above-mentioned solution；Dried after being handled through correlation method, obtain presoma；Presoma is polished in pre-burning under low temperature；Grinding；It is calcined under high temperature, finally obtains corresponding electrode material；The electrode material of acquisition is as negative or positive electrode, for constituting lithium ion battery.The advantage of the invention is that：(1) chemical property of lithium ion battery material is significantly improved；(2) electrode material is prepared by surfactant, the dispersiveness and uniformity of material can be improved, so as to improve material and electrolyte contacts area, the transmission of shortening charge and discharge process intermediate ion and electric transmission path, the cycle performance and high rate performance and high temperature performance of electrode material are improved；(3) cost is low；(4) technique is simple, and equipment investment is few, and the cycle is shorter.
Description
Technical field
The present invention relates to field of chemical power source, more particularly to a kind of lithium ion battery electrode material chemical property that improves
Method.
Background technology
With the consumption of fossil fuel, the research to energy storage and converting apparatus increasingly causes the attention of people.Lithium
Ion battery because energy density is high, have extended cycle life, the low advantage of self-discharge rate and as most noticeable secondary electricity
Pond.However, the large scale equipment needed for electrokinetic cell and long-term energy storage requires that lithium ion battery possesses high rate capability, long-time surely
Qualitative energy and high-temperature behavior etc., these are all lithium ion battery development urgent problems to be solved.Solid sintering technology prepares electrode material
Material is easy to large-scale production, but material granule is easily reunited, and causes material electrochemical performance undesirable.Liquid phase method prepares electrode
Material can prepare the material that particle is uniform, specific surface area is big by changing condition, so as to increase contact of the material with electrolyte
The stability of area, reduction electronic resistance and ion resistance, raising material, so that the chemical property of material is significantly improved, and
It is easy to utilize and this method is with low cost.
Nano material because with larger surface can, it is more difficult be stabilized, easily occur spontaneous agglomeration lose it
Unique performance.In building-up process, the surface topography and size of nano-particle are influenceed by its local environment.Surface-active
Agent has unique amphiphilic structure, and its structure is divided into hydrophilic group and lipophilic group two parts, has good adsorptivity, easily form glue
Beam.Surfactant is mainly as the mechanism of the stable nano material of stabilizer：Electrostatic stabilization mechanism and steric hindrance mechanism.Table
These characteristics of face activating agent provide other synthesis path for the synthesis of nano-particle.On the one hand, surface-active is utilized
The characteristic (such as forming micella, reverse micelle, microemulsion) of agent provides template, micro emulsion method, hydro-thermal for the synthesis of nano-particle
The methods such as method, sol-gel, can preferably control the size of nano-particle；On the other hand, synthesized nanometer can preferably be reduced
The spontaneous agglomeration of particle, increases the stability of nano-particle.Meanwhile, surfactant is produced due to molecule dissymmetrical structure
Self-organizing behavior and reduction aqueous solution surface tension ability, the free energy of system can be reduced.
Therefore, it is badly in need of a kind of technique at present simple, easy to operate, reproducible, and is remarkably improved material electrochemical
The method of performance.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of technique is simple, easy to operate, repeatability
It is good, and the method for being remarkably improved the raising lithium ion battery electrode material chemical property of material electrochemical performance.
The present invention is achieved by the following technical solutions：A kind of raising lithium ion battery electrode material chemical property
Method, comprises the following steps：
(1) surfactant is dissolved in deionized water；
(2) the various salt and auxiliary material of electrode material will be prepared, are maintained in the form of solid phase or the aqueous solution certain
Under the conditions of add step (1) solution in, formed solution；
(3) step (2) solution is dried after the processing of corresponding method, obtains presoma；
(4) it is the presoma after step (3) processing is polished in pre-burning under low temperature；
(5) sample after step (4) processing is ground；
(6) sample after step (5) processing is calcined at high temperature, finally obtains corresponding electrode material；
(7) electrode material for finally obtaining step (6) will be negative or positive electrode, for constituting lithium ion battery.
One of preferred embodiment as the present invention, surfactant includes anion surface active, sun in the step (1)
One or more in ionic surface active agent and nonionic surfactant.
One of preferred embodiment as the present invention, the various salt that electrode material is prepared in the step (2) are soluble lithium
Salt, soluble manganese salt, soluble cobalt, soluble nickel salt, soluble vanadium-containing compound, soluble ferric iron salt, Ti (OC4H9)4In
It is one or more；The soluble lithium salt is specially CH3COOLi·H2O、LiNO3、LiOH·H2O、Li2CO3In one kind or many
Kind；The soluble manganese salt is specially (CH3COO)2Mn·4H2O、MnSO4·H2O、Mn(NO3)2·H2One or more in O；
The soluble cobalt is specially (CH3COO)2Co·6H2O、CoSO4·7H2O、Co(NO3)2·H2One or more in O；Institute
It is specially (CH to state soluble nickel salt3COO)2Ni·4H2O、NiSO4·7H2O、Ni(NO3)2·6H2One or more in O；Institute
State soluble vanadium-containing compound specially NH4VO3、V2O5、NaVO3In one or more；The soluble ferric iron salt is specially
(CH3COO)2Fe、FeC2O4·2H2O、FePO4In one or more.
One of preferred embodiment as the present invention, auxiliary material is complexing agent or precipitating reagent in the step (2)；It is described
Complexing agent be specially 1,10- Phens, EDTA, dimercaprol dimercaptopropanol, Sodium Dimercapto Sulfonate, mercaptoethylmaine, TGA,
Thiocarbamide, ammonium fluoride, 8-hydroxyquinoline, cyanide, acetylacetone,2,4-pentanedione, citric acid, tartaric acid, oxalic acid, sulfosalicylic acid, three ethanol
One or more in amine, EGTA, ethylenediamine tetrapropionic acid, triethylenetetramine；The precipitating reagent is specially Na2CO3、NaHCO3、
NaOH、K2CO3、KHCO3、KOH、NH4One or more in OH.
Certain condition is maintained to include pH, temperature, raw material in one of preferred embodiment as the present invention, the step (2)
Rate of addition and atmosphere protection.
One of preferred embodiment as the present invention, corresponding method includes hydro-thermal method, sol-gel in the step (3)
Method, the precipitation method, Hydrolyze method, spray-on process, emulsion method, freeze-drying.
One of preferred embodiment as the present invention, being dried in the step (3) includes oven drying, vacuum drying, freezing
Dry and be spray-dried.
One of preferred embodiment as the present invention, pre-burning is in atmosphere tube type stove or Muffle under low temperature in the step (4)
250-600 DEG C of sintering 1-8h in stove；The 600-1200 in atmosphere tube type stove or Muffle furnace is roasted under step (6) high temperature
DEG C sintering 2-50h.
Obtained in one of preferred embodiment as the present invention, the step (7) after respective electrode material, with the electrode of preparation
Material is that negative or positive electrode, high-purity lithium piece are negative pole or positive pole, and the barrier film using microporous polypropylene membrane as battery is assembled into model
CR2032 tests battery, and button electricity is assembled into the glove box full of argon gas, electro-chemical test, test voltage scope is carried out
1.0-5.0V。
One of preferred embodiment as the present invention, the electro-chemical test is specially cycle performance, high rate performance and height
Warm performance test.
The advantage of the present invention compared with prior art is：
(1) chemical property of lithium ion battery material is improved by surfactant, and effect is notable；
(2) electrode material is prepared by surfactant, it is possible to increase the dispersiveness and uniformity of material, so as to improve material
Material and electrolyte contacts area, the transmission of shortening charge and discharge process intermediate ion and electric transmission path, improve the circulation of electrode material
Performance and high rate performance and high temperature performance；
(3) surfactant selected is cheap and easy to get, and cost is low；
(4) technique is simple, and equipment investment is few, and the cycle is shorter, beneficial to cost and heavy industrialization is reduced, with universality
And replicability.
Brief description of the drawings
Fig. 1 is a kind of LVP electrode materials of the method for raising lithium ion battery electrode material chemical property in embodiment 1
X-ray diffraction (XRD) result figure of material；
Fig. 2 is a kind of LVP electrode materials of the method for raising lithium ion battery electrode material chemical property in embodiment 1
The SEM electron-microscope scanning figures of material；
Fig. 3 is a kind of LVP electrode materials of the method for raising lithium ion battery electrode material chemical property in embodiment 1
The high rate performance test result figure of material.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment 1
A kind of method of raising lithium ion battery electrode material chemical property of the present embodiment, comprises the following steps：
(1) neopelex (SDBS) is dissolved in deionized water；
(2) NH of electrode material will be prepared4VO3、CH3COOLi·H2O、NH4H2PO4And complexing agent citric acid, with solid phase or
(pH, temperature, the rate of addition and atmosphere protection of raw material) addition step (1) is molten under certain condition for the form maintenance of person's aqueous solution
In liquid, solution is formed；
(3) step (2) solution is done in 60 DEG C of heating water bath stirrings until being formed and being transferred to after colloidal sol shape in 120 DEG C of baking ovens
It is dry, obtain presoma；
(4) presoma obtained step (3) is polished in 5%H2/N2In atmosphere tube type stove after 350 DEG C of sintering 5h certainly
So it is cooled to room temperature；
(5) sample after step (4) processing is ground；
(6) by the sample after step (5) processing in 5%H2/N2750 DEG C of sintering 10h, finally obtain phase in atmosphere tube type stove
Electrode material LVP (the Li answered3V2(PO4)3), its material composition is characterized by X-ray diffraction (XRD) test, sees Fig. 1 (not add
It is contrast to enter SDBS LVP), its pattern is characterized by the test of SEM electron-microscope scannings, Fig. 2 is seen；
(7) electrode material for finally obtaining step (6) will be negative pole as positive pole, high-purity lithium piece, with polypropylene microporous
Film is the barrier film of battery, using Super P as conductive agent, using PVdF as binding agent, slurry is tuned into by solvent of NMP, with 1mol/L
LiPF6/EC+DEC(LiPF6/ EC and DEC volume ratio is 1:1) it is electrolyte, is assembled into model CR2032 test batteries,
Button electricity is assembled into the glove box full of argon gas, electro-chemical test, i.e. cycle performance, high rate performance and high and low temperature is carried out
It can test, test voltage scope 2.4-4.3V, wherein, Fig. 3 is then its high rate performance test result figure (not add SDBS
LVP is contrast).
Embodiment 2
A kind of method of raising lithium ion battery electrode material chemical property of the present embodiment, comprises the following steps：
(1) cetyl trimethylammonium bromide (CTAB) is dissolved in deionized water；
(2) CH of electrode material will be prepared3COOLi·H2O、(CH3COO)2Mn·4H2O、(CH3COO)2Ni·4H2O and auxiliary
Help raw material ammonia water, in the form of solid phase or the aqueous solution maintain under certain condition (pH, temperature, raw material rate of addition it is gentle
Atmosphere is protected) add in step (1) solution, form solution；
(3) step (2) solution is transferred in hydrothermal reaction kettle, reacting 24h at 180 DEG C obtains colloidal sol, then at 70 DEG C of water-baths
Evaporation, is then transferred to 120 DEG C of dryings in baking oven, obtains presoma；
(4) the polished 250 DEG C of sintering 1h in Muffle furnace of presoma obtained step (3)；
(5) sample after step (4) processing is ground；
(6) sample after step (5) processing is sintered into 2h for 600 DEG C in Muffle furnace, finally obtains corresponding electrode material；
(7) electrode material for finally obtaining step (6) will be negative pole as positive pole, high-purity lithium piece, with polypropylene microporous
Film is assembled into model CR2032 test batteries for the barrier film of battery, and button electricity is assembled into the glove box full of argon gas, is entered
Row electro-chemical test (cycle performance, high rate performance and high temperature performance test), test voltage scope 3.0-4.5V.
Embodiment 3
A kind of method of raising lithium ion battery electrode material chemical property of the present embodiment, comprises the following steps：
(1) polyvinyl alcohol (PVA) and cetyl trimethylammonium bromide (CTAB) are dissolved in deionized water；
(2) CH of electrode material will be prepared3COOLi·H2O、(CH3COO)2Co·6H2O and precipitating reagent Na2CO3Each self-dissolving
Each solution is added dropwise in the solution of step (1) by solution simultaneously under continuous stirring in deionized water, and pH is kept with ammoniacal liquor regulation
=10,10h is persistently stirred after completion of dropwise addition, rear filtering is cleaned with deionized water, obtains sediment；
(3) gained sediment in step (2) is transferred in vacuum drying oven and be dried in vacuo, obtain presoma；
(4) presoma obtained step (3) is polished in 10%H2/N2600 DEG C of sintering 8h in atmosphere tube type stove；
(5) sample after step (4) processing is ground；
(6) by the sample after step (5) processing in 10%H2/N21200 DEG C of sintering 50h, final acquisition in atmosphere tube type stove
Corresponding electrode material；
(7) electrode material for finally obtaining step (6) will be positive pole as negative pole, high-purity lithium piece, with polypropylene microporous
Film is assembled into model CR2032 test batteries for the barrier film of battery, and button electricity is assembled into the glove box full of argon gas, is entered
Row electro-chemical test (cycle performance, high rate performance and high temperature performance test), test voltage scope 2.4-4.3V.
Embodiment 4
A kind of method of raising lithium ion battery electrode material chemical property of the present embodiment, comprises the following steps：
(1) cetyl trimethylammonium bromide (CTAB) is dissolved in deionized water；
(2) (Ti (OC of electrode material will be prepared4H9)4)、CH3COOLi·H2O and complexing agent citric acid, with solid phase or
The form of the aqueous solution maintains (pH, temperature, the rate of addition and atmosphere protection of raw material) addition step (1) solution under certain condition
In, form solution；
(3) step (2) solution is transferred in pneumatic spray drying device and is spray-dried, transferred in baking oven and dry,
Obtain presoma；
(4) presoma obtained step (3) is polished in N2350 DEG C of sintering 6h in atmosphere tube type stove；
(5) sample after step (4) processing is ground；
(6) by the sample after step (5) processing in N2700 DEG C of sintering 10h, the final corresponding electricity of acquisition in atmosphere tube type stove
Pole material；
(7) electrode material for finally obtaining step (6) will be as negative pole, high-purity lithium piece positive pole, with microporous polypropylene membrane
Model CR2032 test batteries are assembled into for the barrier film of battery, button electricity is assembled into the glove box full of argon gas, is carried out
Electro-chemical test (cycle performance, high rate performance and high temperature performance test), test voltage scope 1.0-3.0V.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of method for improving lithium ion battery electrode material chemical property, it is characterised in that comprise the following steps：
(1) surfactant is dissolved in deionized water；
(2) the various salt and auxiliary material of electrode material will be prepared, certain condition is maintained in the form of solid phase or the aqueous solution
In lower addition step (1) solution, solution is formed；
(3) step (2) solution is dried after the processing of corresponding method, obtains presoma；
(4) it is the presoma after step (3) processing is polished in pre-burning under low temperature；
(5) sample after step (4) processing is ground；
(6) sample after step (5) processing is calcined at high temperature, finally obtains corresponding electrode material；
(7) electrode material for finally obtaining step (6) is as negative or positive electrode, for constituting lithium ion battery.
2. the method according to claim 1 for improving lithium ion battery electrode material chemical property, it is characterised in that institute
Stating surfactant in step (1) is included in anion surface active, cationic surfactant and nonionic surfactant
One or more.
3. the method according to claim 1 for improving lithium ion battery electrode material chemical property, it is characterised in that institute
State prepared in step (2) the various salt of electrode material for soluble lithium salt, soluble manganese salt, soluble cobalt, soluble nickel salt,
Soluble vanadium-containing compound, soluble ferric iron salt, Ti (OC4H9)4In one or more；The soluble lithium salt is specially
CH3COOLi·H2O、LiNO3、LiOH·H2O、Li2CO3In one or more；The soluble manganese salt is specially (CH3COO)2Mn·4H2O、MnSO4·H2O、Mn(NO3)2·H2One or more in O；The soluble cobalt is specially (CH3COO)2Co·6H2O、CoSO4·7H2O、Co(NO3)2·H2One or more in O；The soluble nickel salt is specially (CH3COO)2Ni·4H2O、NiSO4·7H2O、Ni(NO3)2·6H2One or more in O；The soluble vanadium-containing compound is specially
NH4VO3、V2O5、NaVO3In one or more；The soluble ferric iron salt is specially (CH3COO)2Fe、FeC2O4·2H2O、
FePO4In one or more.
4. the method according to claim 1 for improving lithium ion battery electrode material chemical property, it is characterised in that institute
It is complexing agent or precipitating reagent to state auxiliary material in step (2)；The complexing agent is specially 1,10- Phens, EDTA, two mercaptos
Base propyl alcohol, Sodium Dimercapto Sulfonate, mercaptoethylmaine, TGA, thiocarbamide, ammonium fluoride, 8-hydroxyquinoline, cyanide, acetyl
In acetone, citric acid, tartaric acid, oxalic acid, sulfosalicylic acid, triethanolamine, EGTA, ethylenediamine tetrapropionic acid, triethylenetetramine
It is one or more of；The precipitating reagent is specially Na2CO3、NaHCO3、NaOH、K2CO3、KHCO3、KOH、NH4One kind or several in OH
Kind.
5. the method according to claim 1 for improving lithium ion battery electrode material chemical property, it is characterised in that institute
Stating the condition for remaining certain in step (2) includes pH, temperature, the rate of addition and atmosphere protection of raw material.
6. the method according to claim 1 for improving lithium ion battery electrode material chemical property, it is characterised in that institute
Stating corresponding method in step (3) includes hydro-thermal method, sol-gel process, the precipitation method, Hydrolyze method, spray-on process, emulsion method, freezing
Seasoning.
7. the method according to claim 1 for improving lithium ion battery electrode material chemical property, it is characterised in that institute
Stating to dry in step (3) includes oven drying, vacuum drying, freeze-drying and is spray-dried.
8. the method according to claim 1 for improving lithium ion battery electrode material chemical property, it is characterised in that institute
It is the 250-600 DEG C of sintering 1-8h in atmosphere tube type stove or Muffle furnace to state in step (4) pre-burning under low temperature；In the step (6)
The 600-1200 DEG C of sintering 2-50h in atmosphere tube type stove or Muffle furnace is roasted under high temperature.
9. the method according to claim 1 for improving lithium ion battery electrode material chemical property, it is characterised in that institute
State in step (7) and obtain after respective electrode material, by negative or positive electrode of the electrode material of preparation, high-purity lithium piece be negative pole or just
Pole, the barrier film using microporous polypropylene membrane as battery is assembled into model CR2032 test batteries, in the glove box full of argon gas
Button electricity is assembled into, electro-chemical test, test voltage scope 1.0-5.0V is carried out.
10. the method according to claim 9 for improving lithium ion battery electrode material chemical property, it is characterised in that
The electro-chemical test is specially cycle performance, high rate performance and high temperature performance test.
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| CN108550796A (en) * | 2018-04-12 | 2018-09-18 | 上海空间电源研究所 | Closed lithium-oxygen battery lithia-fluorocarbons anode pole piece and preparation method thereof |
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| CN115440971A (en) * | 2021-06-04 | 2022-12-06 | 河北大学 | Lithium ion battery anode material and doping method thereof |
| CN118026284A (en) * | 2024-02-06 | 2024-05-14 | 西安工业大学 | Lithium-rich manganese-based positive electrode material with excellent low-temperature performance and preparation method thereof |
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