CN110233237A - A kind of combination electrode of all-solid lithium-ion battery and preparation method thereof - Google Patents
A kind of combination electrode of all-solid lithium-ion battery and preparation method thereof Download PDFInfo
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- CN110233237A CN110233237A CN201810189386.3A CN201810189386A CN110233237A CN 110233237 A CN110233237 A CN 110233237A CN 201810189386 A CN201810189386 A CN 201810189386A CN 110233237 A CN110233237 A CN 110233237A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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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Abstract
The present invention provides a kind of combination electrode material and preparation method thereof of all-solid lithium-ion battery, it include: electrode active material, nano solid electrolyte, conductive agent, it is characterised in that: the nano solid electrolyte and conductive agent are coated on to the surface of electrode active material using physically or chemically method for coating according to mass percent.The advantage of the invention is that not only can effectively solve the consistency problem between electrode material and electrolyte layer, but also the electric conductivity and other performances of primary electrode material will not be reduced.The method of the invention is easy to operate, low in cost, is suitble to industrialized production.
Description
Technical field
The present invention relates to New Solid batteries again, with specific dimensions, the active material of structure, conductive agent and solid electrolytic
Matter field.More particularly to a kind of combination electrode and preparation method thereof of all-solid lithium-ion battery.
Background technique
As lithium ion battery has been more and more widely used, safety is got growing concern for.Lithium from
In sub- battery, it is to cause lithium battery safety problem that solvent is inflammable in traditional electrolyte and it easily decomposes and generates imflammable gas
One of key factor, in order to thoroughly solve the problems, such as this, solid electrolyte becomes the research object of numerous scientific research institutions.Because using
Solid electrolyte can be to avoid flammable solvent be used, to substantially increase the security performance of conventional lithium ion battery.But
There is also some urgent problems for the application of solid electrolyte at present.
The technically interface compatibility of solid electrolyte being using obstacle with electrode active material.
Solid electrolyte is solved at present and the common method of electrode active material interface compatibility is in active material surface
Coating or deposition one layer of nanoscale dielectric property oxide (such as BaTiO3), lithium ion conductor (such as LiNbO3).The method can
The effect for reducing Charge-transfer resistance between active material and electrolyte is effectively played, so that the electrochemistry of battery greatly improved
Performance.
Patent (application number 201611021414.8) also provides the method for solid electrolyte cladding active material, the method
It combines using mechanical mixture with high temperature sintering to prepare the electrode active material for being coated with solid electrolyte.But due to solid
The electronic conductivity of state electrolyte is still much lower for conductive agent, is preparing pole piece using the composite material of the invention
When, because surface of active material has coated one layer of solid electrolyte to contact with conductive agent, and then pole piece can be seriously affected
Electronic conductivity.
The present invention using solid electrolyte and conductive agent mixing clad while control coating thickness, not only can be with
The consistency problem between electrode material and electrolyte layer is efficiently solved, on the other hand, mixes the conductive agent being added in clad
The electric conductivity between material granule can also effectively be improved.
Summary of the invention
The present invention is directed to the drawbacks of prior art, and the purpose of the present invention is to provide a kind of answering for all-solid lithium-ion battery
Composite electrode and proportionally that the preparation method of solid electrolyte and conductive agent jacketed electrode active material surface is solid to solve
The excessively high problem of state battery electrode interface impedance.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme:
A kind of combination electrode material of all-solid lithium-ion battery, comprising: electrode active material, nano solid electrolyte,
Conductive agent, it is characterised in that: using physically or chemically method for coating by the nano solid electrolyte and conductive agent according to quality
Percentage is coated on the surface of electrode active material.
Further, the combination electrode material is composite positive pole or composite negative pole material；The electrode activity material
Material is positive electrode active materials or negative electrode active material, the positive electrode active materials are as follows: the embedding lithium of stratiform lithium intercalation compound, spinel-type
One of compound, olivine-type lithium intercalation compound, rich lithium material, ternary material；
Layered lithium intercalation compound is LiAO2, one of A Co, Ni, Mn, preferably LiCoO2；The spinel-type
Lithium intercalation compound is LiMn2O4；The olivine-type lithium intercalation compound is LiDPO4, wherein D is one of Fe, Co, Ni, Mn,
It is preferred that LiFePO4；The richness lithium material is xLi2MnO3·(1-x)LiEO2, wherein E is Co, Fe, Ni1/2, Mn1/2One of,
0 < x < 1；The ternary material LiMxNiyCo1-x-yO2, wherein M is one of Mn, Al；(0 < x <, 1,0 < y <, 1,0 < x+
Y < 1)；The negative electrode active material be one of carbon-based material, alloy material, silicon substrate or tin class material, titanium based material or
It is several, the carbon-based material: graphite, amorphous carbon, carbonaceous mesophase spherules, graphitized carbon fibre；Titanium based material: lithium titanate.
Further, the size of electrode active material is 0.1-50 μm, and preferred size is 0.5-20 μm.
Further, the nano solid electrolyte is oxide-based solid electrolyte material or sulfide-based solid state electrolysis
Material, the further preferred nano solid electrolyte are NASICON type, Garnet type, Thio-LISICON type, Li2S-
P2S5And Li2S-SiS2One or more of；NASICON type nano solid electrolyte Li1+xAlxTi2-x(PO4)3, 0≤x < 1,
Garnet type nano solid electrolyte Li7-xLa3Zr2-xNxO12, one of N Nb, Al, Ta, 0≤x < 1, Thio-
LISICON type nano solid electrolyte Li10GeP2S12。
Further, the particle size of the nano solid electrolyte is 20~500nm, can be more preferably 50~
100nm。
Further, the conductive agent is granular conductive agent, fibrous conductive agent or sheets of conductive agent；The particle
Shape conductive agent is SP, acetylene black, Ketjen black；The threadiness conductive agent is SWCNT, MWCNT, VGCF, CNT；The sheet is led
Electric agent is graphene, KS6.
Further, the diameter of the SP is 30-40nm；The diameter of the VGCF is 50-500nm；The diameter of the CNT
For 5-20nm；The thickness 1-5nm of the graphene；The partial size of the KS6 is 1-5 μm.
A kind of method for coating of combination electrode material as mentioned, it is characterised in that: the method for coating is ball milling, colloidal sol
One of gel, co-precipitation and high temperature cladding process.
Further, the step of high temperature cladding process are as follows:
(1) electrode active material, solid electrolyte, conductive agent and the binder for weighing certain mass in proportion, are added to
In high temperature coating machine；
(2) solvent for weighing certain mass again is added in high temperature coating machine, opens stirring 0.5-2h, slurry is made；
(3) high temperature coating machine is warming up to 300-600 DEG C, keeps the temperature 1-6h, is cooled to room temperature and stops stirring, obtain forerunner
Body；
(4) under an inert atmosphere, to the persursor material of combination electrode in above-mentioned steps (3) in 500-800 DEG C of sintering 1-
10h obtains final combination electrode material.
Further, solvent described in step (1) be one of water, acetone, isooctane, ethyl alcohol, isopropanol etc. or
It is several.
Further, binder described in step (1) is polyvinyl alcohol, carboxymethyl cellulose, starch, dextrin, poly- second
One of glycol, polystyrene, polyacrylate, polyurethane, butyl rubber, vinyl acetate resin, acrylic resin are several
Kind.
Further, the solid-to-liquid ratio of combination electrode slurry described in step (2) is 40-80%.
Further, the solid-to-liquid ratio of combination electrode slurry is 50-60%.
Further, inert atmosphere described in step (4) is the one or more of nitrogen atmosphere, argon atmosphere.
Further, the mass ratio of the solid electrolyte, conductive agent, binder and electrode active material is respectively
0.1%~10%, 0.1%~10wt%, 0.1%~10%, further preferably 0.5%~5%, 0.5%~5%, 0.5%
~5%.
Further, combination electrode material coating thickness obtained is 10-150nm in step (3).
Beneficial effects of the present invention:
Solid electrolyte and conductive agent proportionally can be coated on active electricity by the method that the present invention is coated by high temperature
The surface of pole material, while can control the thickness of clad, combination electrode is prepared.Solid electrolyte is coated on electrode
Material surface can efficiently solve the consistency problem between electrode material and electrolyte layer, on the other hand, mix in clad
The conductive agent of addition can also effectively improve the electric conductivity between material granule.What the method for this mass ratio was prepared answers
Composite electrode material can play the advantages of every kind of material, be finally reached good effect.
Detailed description of the invention
Fig. 1 is combination electrode material covered effect schematic diagram.
Fig. 2 is the NCM811 material (a) of the uncoated solid electrolyte in surface prepared by embodiment 1 and conductive agent and wraps
Cover the stereoscan photograph of the NCM811 material (b) of processing.
Fig. 3 is the solid state battery that is assembled into of composite material prepared by embodiment 1 and at without this patent surface cladding
Manage the EIS comparison diagram of the solid state battery of positive electrode material assembling.
Wherein: 1-NCM811 material, 2- solid electrolyte and conductive agent composition clad, 3- solid electrolyte particle,
4- conductive agent particle.
Specific embodiment
Combined with specific embodiments below to the preparation method of all-solid-state battery provided by the invention combination electrode carry out into
One step explanation.But the present invention is not limited in following embodiment.
Embodiment 1:
The solid electrolyte Li for being 50nm with partial size by the NCM811 that 9.5g partial size is 3um7La3Zr2O120.25g, partial size
It is added in high temperature coating machine for conductive agent SP0.2g and the 0.05g carboxymethyl cellulose of 30nm, adds 40mL water, open stirring
Then 1h is warming up to 500 DEG C of heat preservation 4h, obtain the combination electrode material forerunner that clad is 40nm after being naturally cooling to room temperature
Body.Then in a nitrogen atmosphere, final anode composite electrode material is obtained in 600 DEG C of sintering 4h.
The solid state battery that prepared composite material is assembled into is done into EIS test, and and is coated with without this patent surface
The solid state battery EIS test result comparison of positive electrode material assembling is handled, solid state battery made from this patent shows lower
Interface impedance, such as Fig. 3, it can be seen that impedance improves after cladding.
Embodiment 2:
By 9.5g partial size be 10 μm graphite and partial size be 80nm solid electrolyte Li10GeP2S120.30g, diameter are
Conductive agent CNT0.15g and the 0.05g polyvinyl alcohol of 10nm is added in high temperature coating machine, adds 50mL water, opens stirring 2h,
Then 400 DEG C of heat preservation 2h are warming up to, obtain the combination electrode material presoma that clad is 100nm after being naturally cooling to room temperature.
Then in a nitrogen atmosphere, final anode composite electrode material is obtained in 500 DEG C of sintering 4h.
Embodiment 3:
By 9.5g partial size be 10 μm NCA and partial size be 50nm solid electrolyte Li1.1Al0.1Ti1.9(PO4)30.30g、
Conductive agent VGCF0.15g and the 0.05g polyethylene glycol that diameter is 50nm is added in high temperature coating machine, adds 50mL water, opens
2h is stirred, 400 DEG C of heat preservation 3h are then warming up to, obtains the combination electrode material that clad is 100nm after being naturally cooling to room temperature
Presoma.Then in a nitrogen atmosphere, final anode composite electrode material is obtained in 600 DEG C of sintering 4h.
Embodiment 4:
By 9.5g partial size be 20 μm NCM811 and partial size be 50nm solid electrolyte Li1.1Al0.1Ti1.9(PO4)30.40g, conductive agent VGCF0.1g and the 0.1g polyethylene glycol that diameter is 50nm are added in high temperature coating machine, add 50mL water,
Stirring 2h is opened, 400 DEG C of heat preservation 4h are then warming up to, obtains the combination electrode that clad is 100nm after being naturally cooling to room temperature
Material precursor.Then under an argon atmosphere, final anode composite electrode material is obtained in 600 DEG C of sintering 4h.
Embodiment 5:
The SiO for being 5 μm by 9.5g partial sizexThe solid electrolyte Li that/C-material and partial size are 50nm2S-P2S5 0.4g、0.1g
Polyethylene glycol is added in high temperature coating machine, adds 50mL water, opens stirring 2h, is then warming up to 300 DEG C of heat preservation 3h, drops naturally
The combination electrode material presoma that clad is 60nm is obtained after warming to room temperature.Then in a nitrogen atmosphere, in 600 DEG C of sintering 4h
Obtain final anode composite electrode material.
Claims (17)
1. a kind of combination electrode material of all-solid lithium-ion battery, comprising: electrode active material, is led at nano solid electrolyte
Electric agent, it is characterised in that: using physically or chemically method for coating by the nano solid electrolyte and conductive agent according to quality hundred
Divide the surface than being coated on electrode active material.
2. combination electrode material as described in claim 1, it is characterised in that: the combination electrode material is composite positive pole
Or composite negative pole material；The electrode active material is positive electrode active materials or negative electrode active material, the positive electrode active materials
Are as follows: stratiform lithium intercalation compound, spinel-type lithium intercalation compound, olivine-type lithium intercalation compound, rich lithium material, in ternary material
It is a kind of；Layered lithium intercalation compound is LiAO2, one of A Co, Ni, Mn；The spinel-type lithium intercalation compound is
LiMn2O4；The olivine-type lithium intercalation compound is LiDPO4, wherein D is one of Fe, Co, Ni, Mn；The richness lithium material
For xLi2MnO3·(1-x)LiEO2, wherein E is Co, Fe, Ni1/2, Mn1/2One of, 0 < x < 1；The ternary material
LiMxNiyCo1-x-yO2, wherein M is one of Mn, Al, wherein 0 < x <, 1,0 < y <, 1,0 < x+y < 1；The negative electrode active
Material is one or more of carbon-based material, alloy material, silicon substrate or tin class material, titanium based material, the carbon-based material
Are as follows: graphite, amorphous carbon, carbonaceous mesophase spherules, graphitized carbon fibre；The titanium based material are as follows: lithium titanate.
3. combination electrode material as claimed in claim 2, it is characterised in that: the size of electrode active material is 0.5-20 μm.
4. combination electrode material as described in claim 1, it is characterised in that: the nano solid electrolyte be NASICON type,
Garnet type, Thio-LISICON type, Li2S-P2S5And Li2S-SiS2One or more of；NASICON type nano solid electricity
Solve matter Li1+xAlxTi2-x(PO4)3, 0≤x < 1, Garnet type nano solid electrolyte Li7-xLa3Zr2-xNxO12, N Nb, Al,
One of Ta, 0≤x < 1, Thio-LISICON type nano solid electrolyte Li10GeP2S12。
5. combination electrode material as claimed in claim 4, it is characterised in that: the particle size of the nano solid electrolyte is
50~100nm.
6. combination electrode material as described in claim 1, it is characterised in that: the conductive agent is granular conductive agent, fibre
Tie up shape conductive agent or sheets of conductive agent；The granular conductive agent is SP, acetylene black, Ketjen black；It is described threadiness conductive agent be
SWCNT,MWCNT,VGCF,CNT；The sheets of conductive agent is graphene, KS6.
7. combination electrode material as claimed in claim 6, it is characterised in that: the diameter of the SP is 30-40nm；The VGCF
Diameter be 50-500nm；The diameter of the CNT is 5-20nm；The thickness 1-5nm of the graphene；The partial size of the KS6 is
1-5μm。
8. a kind of method for coating of combination electrode material as described in claim 1, it is characterised in that: the method for coating is ball
One of mill, collosol and gel, co-precipitation and high temperature cladding process.
9. method for coating as claimed in claim 8, it is characterised in that: the step of the high temperature cladding process are as follows:
(1) electrode active material, solid electrolyte, conductive agent and the binder for weighing certain mass in proportion, are added to high temperature
In coating machine；
(2) solvent for weighing certain mass again is added in high temperature coating machine, opens stirring 0.5-2h, slurry is made；
(3) high temperature coating machine is warming up to 300-600 DEG C, keeps the temperature 1-6h, is cooled to room temperature and stops stirring, obtain presoma；
(4) under an inert atmosphere, to the persursor material of combination electrode in above-mentioned steps (3) in 500-800 DEG C of sintering 1-10h,
Obtain final combination electrode material.
10. method for coating as claimed in claim 9, it is characterised in that: solvent described in step (1) is water, acetone, different pungent
One or more of alkane, ethyl alcohol, isopropanol etc..
11. method for coating as claimed in claim 9, it is characterised in that: binder described in step (1) be polyvinyl alcohol,
Carboxymethyl cellulose, starch, dextrin, polyethylene glycol, polystyrene, polyacrylate, polyurethane, butyl rubber, vinyl acetate
One or more of resin, acrylic resin.
12. method for coating as claimed in claim 9, it is characterised in that: the solid-liquid of combination electrode slurry described in step (2)
Than for 40-80%.
13. method for coating as claimed in claim 12, it is characterised in that: the solid-to-liquid ratio of combination electrode slurry is 50-60%.
14. method for coating as claimed in claim 9, it is characterised in that: inert atmosphere described in step (4) be nitrogen atmosphere,
One or more of argon atmosphere.
15. method for coating as claimed in claim 9, it is characterised in that: the solid electrolyte, conductive agent, binder and electricity
The mass ratio of pole active material is respectively 0.1%~10%, 0.1%~10%, 0.1%~10%.
16. method for coating as claimed in claim 15, it is characterised in that: the solid electrolyte, conductive agent, binder and electricity
The mass ratio of pole active material is respectively 0.5%~5%, 0.5%~5%, 0.5%~5%.
17. method for coating as claimed in claim 9, it is characterised in that: combination electrode material clad obtained in step (3)
With a thickness of 10-150nm.
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| CN111326727A (en) * | 2020-03-09 | 2020-06-23 | 洛阳联创锂能科技有限公司 | Multi-component silicon-oxygen negative electrode material for lithium ion battery and preparation method thereof |
| CN111342017A (en) * | 2020-03-09 | 2020-06-26 | 洛阳联创锂能科技有限公司 | Multi-component silicon-oxygen negative electrode material for lithium ion battery and preparation method thereof |
| CN112002883A (en) * | 2020-08-25 | 2020-11-27 | 珠海冠宇动力电池有限公司 | Silicon-based composite material for negative electrode active material, negative electrode plate and lithium ion battery |
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| CN113206249A (en) * | 2021-04-19 | 2021-08-03 | 湖州金灿新能源科技有限公司 | Lithium battery silicon-oxygen composite negative electrode material with good electrochemical performance and preparation method thereof |
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| CN111342017A (en) * | 2020-03-09 | 2020-06-26 | 洛阳联创锂能科技有限公司 | Multi-component silicon-oxygen negative electrode material for lithium ion battery and preparation method thereof |
| CN112002883A (en) * | 2020-08-25 | 2020-11-27 | 珠海冠宇动力电池有限公司 | Silicon-based composite material for negative electrode active material, negative electrode plate and lithium ion battery |
| CN112164776A (en) * | 2020-09-16 | 2021-01-01 | 合肥国轩高科动力能源有限公司 | Composite coated all-solid-state battery positive electrode material, preparation method thereof and all-solid-state battery |
| CN114388748A (en) * | 2020-10-21 | 2022-04-22 | 深圳格林德能源集团有限公司 | Silicon-carbon cathode slurry and preparation process thereof |
| CN113206249A (en) * | 2021-04-19 | 2021-08-03 | 湖州金灿新能源科技有限公司 | Lithium battery silicon-oxygen composite negative electrode material with good electrochemical performance and preparation method thereof |
| CN113937291A (en) * | 2021-09-02 | 2022-01-14 | 深圳高能时代科技有限公司 | Electrode material for sulfide all-solid-state battery and preparation method thereof |
| WO2023071449A1 (en) * | 2021-10-27 | 2023-05-04 | 荆门市格林美新材料有限公司 | Method for coating nickel-cobalt-manganese ternary precursor with latp |
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Application publication date: 20190913 |