CN110336017A - A kind of modified lithium manganate and its preparation method and application - Google Patents
A kind of modified lithium manganate and its preparation method and application Download PDFInfo
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- CN110336017A CN110336017A CN201910641783.4A CN201910641783A CN110336017A CN 110336017 A CN110336017 A CN 110336017A CN 201910641783 A CN201910641783 A CN 201910641783A CN 110336017 A CN110336017 A CN 110336017A
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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
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
- H01M4/604—Polymers containing aliphatic main chain polymers
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
- H01M4/606—Polymers containing aromatic main chain polymers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of modified lithium manganates and its preparation method and application, comprising the following steps: manganese presoma, lithium source are added to ball milling in ball mill and obtain mixture；Mixture is placed in tube furnace first low temperature presintering, then high temperature sintering, last cooled to room temperature, then is crushed, sieving obtains powder sample；Polyethyleneimine, polyaniline are dissolved in n,N-Dimethylformamide respectively, stirring forms mixed liquor；Powder sample stirring and ultrasound will be entered, then dried in a vacuum drying oven to get modified lithium manganate is arrived.The present invention introduces polyaniline with good conductivity on the surface of active material LiMn2O4, promotes the electric conductivity and circulating ratio of material.On LiMn2O4 surface, cladding polyethyleneimine can be reduced the contact area of material and electrolyte, inhibit the dissolution of transient metal Mn element in the electrolytic solution in manganate cathode material for lithium, to promote performance of lithium ion battery service life.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries and preparation method thereof more particularly to a kind of modified lithium manganate and its systems
Preparation Method and purposes.
Background technique
With the fast development of global economy and science and technology, the energy, environment, information become three big themes of social development,
Middle energy and environmental problem is by extensive concern all over the world.Lithium ion battery (LIBs) is as a kind of efficient green client
The energy is recycled.It has many advantages such as that operating voltage is high, specific energy is high, small in size, light-weight, the service life is long, wide
It is general to be used for the fields such as 3C, electric tool, model plane and new-energy automobile.Especially in new-energy automobile field, by the motorized of automobile
It is one of the revolutionary change of motor transport service instantly, in order to adapt to this change, lithium ion battery in a foreseeable future will
One of major technique selection as motorcar electric.With the lithium ion in portable electronic product and power grid storage battery market
Battery is compared, and electric car requires lithium ion battery to have higher service life and safety.
Positive electrode is one of the component part of most critical in LIBs, and the superiority and inferiority of performance directly constrains the property of LIBs
Energy.Currently, the LIBs positive electrode of the market mainstream has cobalt acid lithium, LiMn2O4, LiFePO4 and nickle cobalt lithium manganate.
LiMn2O4 is as positive electrode, and raw material sources are extensive and cost price is cheap, and security performance is fine, and environmental protection is without dirt
Dye.Cycle performance is good at normal temperature for it, and multiplying power discharging property is preferable, is very promising lithium electricity positive electrode.But it is high
Warm nature can be poor, and since the purity of raw material is low in technical grade production, technology controlling and process precision is poor to wait limitation, causes LiMn2O4 in height
Capacity attenuation is very fast under warm (55 DEG C), and cycle performance and storage performance are poor, limits its further development.To its defect
Optimizing research is carried out always, it may be said that if having grasped the key technology of its capacity attenuation, the cake of LiMn2O4 can also be made more
Greatly.Currently, the viewpoint of mainstream thinks, the main reason for capacity attenuation is dissolution, Jahn-Teller effect and the electrolyte of Mn
Decomposition under the high temperature conditions.In recent years, the main method for delaying performance of lithium ion battery to decay has: (1) in LiMn2O4 crystalline substance
Zwitterion substitution is carried out in lattice, such as introduces the elements such as Al, Mg, Zr, La, F, B, and to promote material lattice stability, (2) exist
Coating is carried out on active material or electrode, reduces the side reaction of active material and electrolyte；(3) electrolysis additive promotes electricity
Solve the stability of liquid.But the problem of above method dissolves transition metal in the electrolytic solution does not solve.
The present invention, not only can be bright by introducing the specific organic matter of adsorbable transition metal ions in surface of active material
The aobvious Mn element for reducing dissolution can then be deposited on the surface of cathode, cause the destruction of SEI film, and LIBs irreversible capacity subtracts
Few, cycle performance is significantly improved.
Summary of the invention
In order to solve the above technical problems, the object of the present invention is to provide a kind of modified lithium manganate and preparation method thereof and using
On the way.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of modified lithium manganate, comprising the following steps:
(1) mixing: manganese presoma, lithium source are added to ball milling in ball mill and obtain mixture；
(2) it is sintered: mixture being placed in tube furnace first low temperature presintering, then high temperature sintering, last cooled to room temperature must be burnt
Tie sample；
(3) sintered sample is subjected to Mechanical Crushing, sieving obtains powder sample；
(4) polyethyleneimine, polyaniline are dissolved in n,N-Dimethylformamide respectively, stirring forms mixed liquor；
(5) powder sample by step (3) preparation is added in the mixed liquor of step (4) preparation, simultaneously ultrasound is stirred, then in vacuum
It is dried in drying box to get modified lithium manganate is arrived.
Further scheme, lithium source described in step (1), the additional amount of manganese presoma are to be according to the molar ratio of Li/Mn
2.0:1.0~1.10.
The revolving speed of ball mill described in step (1) is 200-600rpm, and Ball-milling Time 1-4h, ball-milling medium is polyurethane
Ball.
The temperature of low temperature presintering described in step (2) is 100 DEG C -450 DEG C, time 2-12h；The temperature of the high temperature sintering
Degree is 600 DEG C -900 DEG C, time 5-30h.
Mechanical crushing described in step (3) refers to flour mill or airslide disintegrating mill, revolving speed 200-500rpm, grinding time
For 60-200s；The sieve mesh number of the sieving is 120-375 mesh.
Polyethyleneimine described in step (4), polyaniline mass ratio be (0.5~4): 1, liquid-solid ratio in the mixed liquor
For 1:(1~9).
The mass ratio of powder sample described in step (5) and mixed liquor is 1:(1~20)；The temperature of the vacuum oven
For 80 DEG C -140 DEG C, drying time 5-20h.
The manganese presoma is at least one of Mn oxide, manganese hydroxide, manganese carbonate or manganese acetate.
The lithium source is at least one of lithium hydroxide, lithium carbonate, lithium nitrate, lithium acetate.
Second goal of the invention of the invention is to provide a kind of modified lithium manganate such as the preparation of above-mentioned preparation method.
Third goal of the invention of the invention is to provide the purposes of above-mentioned modified lithium manganate, and the modified lithium manganate is used as lithium
Ion battery positive electrode can promote performance of lithium ion battery service life.
Powder sample is put into be dissolved in N,N-dimethylformamide by polyethyleneimine, polyaniline by the present invention stirs shape
At in mixed liquor, polyethyleneimine can adsorb transition metal ions, inhibit transition metal element Mn element in the electrolytic solution
Dissolution；Polyaniline can make the electric conductivity of material get a promotion, while also promote its high rate performance.
The invention has the following advantages:
(1) present invention introduces polyaniline with good conductivity on the surface of active material LiMn2O4, and polyaniline leads to anion doped
(p-type doping) or cation doping (n-type doping), make the electric conductivity of material get a promotion, while also improving high rate performance.
(2) cladding polyethyleneimine in LiMn2O4 surface can be reduced the contact area of material and electrolyte, by hydrogen bond and divide
Between son active force come realize metal cation atomic level it is evenly dispersed, and then obtain perfect crystal morphology and excellent
Chemical property, adsorb the transient metal Mn element that dissolves out from manganate cathode material for lithium, inhibit in manganate cathode material for lithium
The dissolution of transient metal Mn element in the electrolytic solution, to promote performance of lithium ion battery service life.
(3) preparation method provided by the invention is easy to operate, and safe operation process is controllable, simple production process, Neng Goushi
Existing large-scale industrial production.
Specific embodiment
Performance test: being fabricated to 1500mAh soft bag lithium ionic cell for manganate cathode material for lithium prepared by each example respectively,
Charging and loop test are carried out in new prestige test macro.
Its concrete mode are as follows: prepared lithium manganate material is as positive-active material using in embodiment 1-3 and comparative example 1
Material mixes according to the ratio that mass ratio is 88:6:6 with acetylene black, PVDF, is dissolved in nmp solvent, is coated on after ball milling mixing
As anode on aluminium foil,；By graphite, conductive black, binder according to mass ratio be 91:3:6, be dissolved in deionized water,
Be coated on copper foil after wet-milling is stirred and be made into battery cathode sheet, then toasted, roll-in, slice, pole piece stepping, lamination,
Weldering and ear, heat-sealing, fluid injection, chemical conversion, partial volume, are finally tested.The charging/discharging voltage of volume test is 3.0V~4.2V, for the first time
Rate of charge is 0.2C, discharge-rate 0.2C.It is carried out in cycle performance test under room temperature (25 DEG C), charging/discharging voltage 3V
~4.2V.
Embodiment 1
A kind of preparation method of modified lithium manganate cathode material, includes the following steps.
Weigh respectively manganese presoma, battery-level lithium carbonate according to Li/Mn molar ratio be 2:1.05, be added in ball mill with
Revolving speed is 250rpm ball milling 1.5h, obtains mixture.Then by mixture in tube furnace with 400 DEG C of pre-burning 5h, then be warming up to
750 DEG C of sintering 20h, sintering atmosphere is air, cooled to room temperature；Again by sintered sample Mechanical Crushing after cooling, wherein
Mechanical revolving speed 300rpm, grinding time 180s, be sieved 200 mesh, obtains powder sample.
It is in mass ratio the N,N-dimethylformamide mixing that 1:10 is added to that mass fraction is 12% by above-mentioned powder sample
In liquid (the wherein mass ratio 2:1 of polyethyleneimine, polyaniline), simultaneously ultrasound 15min is stirred, mixed serum is formed.Then it will mix
It closes slurries to be placed in a vacuum drying oven, in 120 DEG C of dry 10h to get to modified lithium manganate cathode material.
Soft-package battery is made by test discovery in above-mentioned modified lithium manganate cathode material, discharge capacity is for the first time
115mAhg-1, capacity retention ratio 80% after recycling 500 times.
Embodiment 2
A kind of preparation method of modified lithium manganate cathode material, includes the following steps.
It is 2:1.065 that manganese presoma, battery-level lithium carbonate are weighed respectively according to Li/Mn molar ratio, is added in ball mill
Mixing, wherein the revolving speed of ball mill is 250rpm, and Ball-milling Time 2h obtains mixture.Then mixture is placed in tube furnace
With 350 DEG C of pre-burning 6h, then 760 DEG C of sintering 25h are warming up to, sintering atmosphere is air, cooled to room temperature, then will be after cooling
Sintered sample Mechanical Crushing, wherein mechanical revolving speed 300rpm, grinding time 180s, be sieved 200 mesh manually, obtains powder-like
Product.
It is in mass ratio the N that 1:10 is added to that mass fraction is 12%, N- dimethyl methyl by the powder sample after above-mentioned sieving
In amide mixed liquor (polyethyleneimine, polyaniline mass ratio 1:1), simultaneously ultrasound 15min is stirred, mixed serum is formed.Then will
Mixed serum is placed in a vacuum drying oven, 120 DEG C of dry 10h to get arrive modified lithium manganate cathode material.
Soft-package battery is made by test discovery in above-mentioned modified lithium manganate cathode material, discharge capacity is for the first time
108mAhg-1.Capacity retention ratio 80% after circulation 500 times.
Embodiment 3
A kind of preparation method of modified lithium manganate cathode material, includes the following steps.
It is 2:1.025 that manganese presoma, battery-level lithium carbonate are weighed respectively according to Li/Mn molar ratio, is added in ball mill
Mixing, rotational speed of ball-mill 250rpm, Ball-milling Time 2h obtain mixture.Then by mixture in tube furnace with 400 DEG C of pre-burnings
6h, then be warming up to 730 DEG C of sintering 18h, sintering atmosphere are air, cooled to room temperature, then by sintered sample machine after cooling
Tool is crushed revolving speed 300rpm, grinding time 150s, and be sieved 200 mesh manually, obtains powder sample.
It is in mass ratio the N that 1:10 is added to that mass fraction is 12%, N- dimethyl methyl by the powder sample after above-mentioned sieving
In amide mixed liquor (polyethyleneimine, polyaniline mass ratio 1:1), simultaneously ultrasound 15min is stirred, mixed serum is formed.Then will
Mixed serum is placed in a vacuum drying oven, 120 DEG C of dry 8h to get arrive modified lithium manganate cathode material.
Soft-package battery is made by test discovery in above-mentioned modified lithium manganate cathode material, discharge capacity is for the first time
106mAhg-1, circulation 500 times after capacity retention ratio 80%.
Comparative example 1
A kind of preparation method of modified lithium manganate cathode material, includes the following steps.
It is 2:1.025 that manganese presoma, battery-level lithium carbonate are weighed respectively according to Li/Mn molar ratio, is added in ball mill
Mixing, rotational speed of ball-mill 250rpm, Ball-milling Time 2h obtain mixture.Then by mixture in tube furnace with 400 DEG C of pre-burnings
6h, then be warming up to 730 DEG C of sintering 18h, sintering atmosphere are air, cooled to room temperature, then by sintered sample machine after cooling
Tool is crushed revolving speed 300rpm, grinding time 150s, and be sieved 200 mesh manually, obtains lithium manganate material.
Soft-package battery is made by test discovery, discharge capacity is 100mAhg-1 for the first time.Capacity is kept after circulation 500 times
Rate 45%.
Embodiment 4:
A kind of preparation method of modified lithium manganate cathode material, includes the following steps.
It is 2:1 that manganese presoma, battery-level lithium carbonate are weighed respectively according to Li/Mn molar ratio, is added in ball mill to turn
Speed is 200rpm ball milling 4h, obtains mixture.Then by mixture in tube furnace with 100 DEG C of pre-burning 12h, then be warming up to 600
DEG C sintering 30h, sintering atmosphere is air, cooled to room temperature；Again by sintered sample Mechanical Crushing after cooling, wherein mechanical
Revolving speed 200rpm, grinding time 200s, be sieved 120 mesh, obtain powder sample.
It is in mass ratio the N,N-dimethylformamide mixing that 1:1 is added to that mass fraction is 10% by above-mentioned powder sample
In liquid (the wherein mass ratio 0.5:1 of polyethyleneimine, polyaniline), simultaneously ultrasound 15min is stirred, mixed serum is formed.Then will
Mixed serum is placed in a vacuum drying oven, 80 DEG C of dry 20h to get arrive modified lithium manganate cathode material.
Embodiment 5:
A kind of preparation method of modified lithium manganate cathode material, includes the following steps.
Weigh respectively manganese presoma, battery-level lithium carbonate according to Li/Mn molar ratio be 2:1.1, be added in ball mill with
Revolving speed is 600rpm ball milling 1h, obtains mixture.Then by mixture in tube furnace with 450 DEG C of pre-burning 2h, then be warming up to 900
DEG C sintering 5h, sintering atmosphere is air, cooled to room temperature；Again by sintered sample Mechanical Crushing after cooling, wherein mechanical
Revolving speed 500rpm, grinding time 60s, be sieved 375 mesh, obtain powder sample.
It is in mass ratio the N,N-dimethylformamide mixing that 1:20 is added to that mass fraction is 50% by above-mentioned powder sample
In liquid (the wherein mass ratio 4:1 of polyethyleneimine, polyaniline), simultaneously ultrasound 15min is stirred, mixed serum is formed.Then it will mix
It closes slurries to be placed in a vacuum drying oven, in 140 DEG C of dry 5h to get to modified lithium manganate cathode material.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of modified lithium manganate, it is characterised in that: the following steps are included:
(1) mixing: manganese presoma, lithium source are added to ball milling in ball mill and obtain mixture；
(2) it is sintered: mixture being placed in tube furnace first low temperature presintering, then high temperature sintering, last cooled to room temperature must be burnt
Tie sample；
(3) sintered sample is subjected to Mechanical Crushing, sieving obtains powder sample；
(4) polyethyleneimine, polyaniline are dissolved in n,N-Dimethylformamide respectively, stirring forms mixed liquor；
(5) powder sample by step (3) preparation is added in the mixed liquor of step (4) preparation, simultaneously ultrasound is stirred, then in vacuum
It is dried in drying box to get modified lithium manganate is arrived.
2. preparation method according to claim 1, it is characterised in that: the addition of lithium source, manganese presoma described in step (1)
It is 2.0:1.0~1.10 that amount, which is according to the molar ratio of Li/Mn,.
3. preparation method according to claim 1, it is characterised in that: the revolving speed of ball mill described in step (1) is 200-
600rpm, Ball-milling Time 1-4h, ball-milling medium are polyurethane ball.
4. preparation method according to claim 1, it is characterised in that: the temperature of low temperature presintering described in step (2) is 100
DEG C -450 DEG C, time 2-12h；The temperature of the high temperature sintering is 600 DEG C -900 DEG C, time 5-30h.
5. preparation method according to claim 1, it is characterised in that: described in step (3) mechanical crushing refer to flour mill or
Airslide disintegrating mill, revolving speed 200-500rpm, grinding time 60-200s；The sieve mesh number of the sieving is 120-375
Mesh.
6. preparation method according to claim 1, it is characterised in that: polyethyleneimine described in step (4), polyaniline
Mass ratio is (0.5~4): 1, liquid-solid ratio is 1:(1~9 in the mixed liquor).
7. preparation method according to claim 1, it is characterised in that: powder sample described in step (5) and mixed liquor
Mass ratio is 1:(1~20)；The temperature of the vacuum oven is 80 DEG C -140 DEG C, drying time 5-20h.
8. preparation method according to claim 1, it is characterised in that: the manganese presoma is Mn oxide, manganese hydroxide
At least one of object, manganese carbonate or manganese acetate；The lithium source is lithium hydroxide, in lithium carbonate, lithium nitrate, lithium acetate
It is at least one.
9. a kind of modified lithium manganate prepared such as any one of claim 1-8 preparation method.
10. the purposes of modified lithium manganate as claimed in claim 9, it is characterised in that: the modified lithium manganate is used as lithium ion
Cell positive material.
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| CN115196682A (en) * | 2022-07-13 | 2022-10-18 | 深圳中芯能科技有限公司 | Method for improving cycle life of lithium manganate |
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