CN109449414A - A kind of anode composite material of lithium ion battery and the all-solid-state battery containing the material - Google Patents
A kind of anode composite material of lithium ion battery and the all-solid-state battery containing the material Download PDFInfo
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- CN109449414A CN109449414A CN201811295790.5A CN201811295790A CN109449414A CN 109449414 A CN109449414 A CN 109449414A CN 201811295790 A CN201811295790 A CN 201811295790A CN 109449414 A CN109449414 A CN 109449414A
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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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- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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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 anode composite material of lithium ion battery, the material it is specific the preparation method is as follows: step 1: weigh suitable solid electrolyte and be dissolved in organic solvent, above-mentioned solution is added in suitable positive electrode, is put into after mixing evenly in high speed disperser in vacuum oven dry until solvent volatilization is complete；Step 2: obtained solid powder being calcined into certain time under atmosphere of inert gases, furnace cooling obtains the anode composite material of core-shell structure.Anode composite material prepared by the present invention has core-shell structure, positive electrode active materials are core, it is shell in its surface coated solid electrolyte, this core-shell structure can reduce directly contacting between positive electrode active materials and solid electrolyte, so as to improve the interface problem between anode and solid electrolyte, in addition, the solid electrolyte of shell can also reinforcing material ionic conductivity.
Description
Technical field
The invention belongs to lithium ion battery preparation field, be related to a kind of anode composite material of lithium ion battery and containing this just
The all-solid-state battery of pole composite material.
Background technique
Currently, commercialized lithium battery uses liquid organic electrolyte, the electrolyte and electrode material are in charge and discharge process
In be easy to happen side reaction, cause battery capacity irreversible decaying occur, while battery is during long service, organic liquid
Phenomena such as electrolyte will appear volatilization, dry up, reveal, influence battery life.On the other hand, traditional lithium battery is not available high energy
The lithium metal of metric density is as negative electrode material, in circulating battery, since metallic lithium surface current density and lithium ion are distributed not
Factors, the metal lithium electrode such as uniform dissolve repeatedly, deposit non-uniform hole and dendrite easy to form.Dendrite can pierce through diaphragm,
It reaches anode and causes a series of security risks such as battery short circuit, thermal runaway, Fire explosion.Liquid is replaced with solid electrolyte
Electrolyte is the fundamental way for obtaining the solid lithium battery of high-energy density, safety and long circulation life.All solid lithium electricity
Pond can improve safety and the service life of battery to avoid liquid electrolyte bring disutility.
Although all-solid lithium-ion battery shows clear superiority in various aspects, there are also in the urgent need to address simultaneously
The problem of: solid electrolyte ionic conductivity is relatively low, and interface impedance is big between solid electrolyte/electrode, and interface compatibility is poor, existing
The battery preparation cost in stage is higher etc..
Summary of the invention
The purpose of the present invention is to provide a kind of anode composite material of lithium ion battery and containing the anode composite material
All-solid-state battery, the anode composite material have core-shell structure, and positive electrode active materials are core, in its surface coated solid state electrolysis
Matter is shell, and this core-shell structure can reduce directly contacting between positive electrode active materials and solid electrolyte, so as to improve
Anode and solid electrolyte between interface problem, in addition, the solid electrolyte of shell can also reinforcing material ionic conductance
Rate, solves that existing solid electrolyte ionic conductivity is relatively low, and interface impedance is big between solid electrolyte/electrode, interface compatibility
It is poor, the higher problem of battery preparation cost at this stage.
The purpose of the present invention can be achieved through the following technical solutions:
Anode composite material of lithium ion battery, the material specific the preparation method is as follows:
It weighs suitable solid electrolyte to be dissolved in organic solvent, above-mentioned solution is added in suitable positive electrode, in height
It is put into after mixing evenly in vacuum oven dry in fast dispersion machine until solvent volatilization is complete；By obtained solid powder in inertia
Certain time is calcined under atmosphere, furnace cooling obtains the anode composite material of core-shell structure.
The solid electrolyte is 3LiBH4-LiI；
The organic solvent is N-Methyl pyrrolidone, N,N-dimethylformamide, N, N- diethylformamide, dimethyl
One or more of sulfoxide, tetrahydrofuran, acetone；
The positive electrode is nickle cobalt lithium manganate 523, nickle cobalt lithium manganate 622, nickle cobalt lithium manganate 811, LiFePO4, cobalt acid
One of lithium or LiMn2O4；
The mass ratio of the solid electrolyte and positive electrode is 1-15:100；
The protective atmosphere is one or more of nitrogen, argon gas, helium, neon；
The calcination temperature is 400-800 DEG C, calcination time 1-24h.
The specific preparation process of all-solid-state battery is as follows:
The first step prepares anode composite material；
Second step, the preparation of positive plate: weighing binder and dissolve in a solvent and stir evenly, and then addition is certain thereto
Anode composite material, the conductive agent of quality, and stirred evenly by high speed disperser, it adjusts solution viscosity and obtains anode sizing agent,
Anode sizing agent is coated on aluminium foil, obtains positive plate after drying, roll-in, cutting；
Third step, the preparation of positive composite pole piece: suitable binder is dissolved in solvent, then that solid electrolyte is molten
In above-mentioned solution, it is coated in the positive plate surface prepared in second step, coating thickness after mixing evenly by high speed disperser
It is 1-10 μm, obtains positive composite pole piece after dry；
4th step, negative electrode tab use existing negative electrode tab material；
The positive composite pole piece prepared in third step and the negative electrode tab prepared in the 4th step are passed through lamination respectively by the 5th step
Technique is assembled into the power soft-package battery of 5Ah, and after the battery after assembling is carried out chemical conversion treatment, multiplying power and circulation longevity are carried out to it
Life test.
Binder is Kynoar, polytetrafluoroethylene (PTFE), polyvinylpyrrolidone, polypropylene, poly- second in the second step
The one or more of alkene, polyurethane, polyamide, polyamidoimide；
Solvent is N-Methyl pyrrolidone, N,N-dimethylformamide, N, N- diethylformamide, two in the second step
One or more of methyl sulfoxide, tetrahydrofuran, acetone；
Conductive agent is one or more of acetylene black, carbon nanotube, Ketjen black in the second step；
Anode composite material in the second step, conductive agent, binder mass ratio be 94-85:1-15:3-4:2-3；
Anode sizing agent viscosity is 7000-9000cps in the second step；
Binder is Kynoar, polytetrafluoroethylene (PTFE), polyvinylpyrrolidone, polypropylene, poly- second in the third step
The one or more of alkene, polyurethane, polyamide, polyamidoimide；
The mass ratio of binder and solid electrolyte is 3-10:100 in the third step.
Beneficial effects of the present invention:
In all-solid-state battery prepared by the present invention, solid electrolyte and positive main material are sufficiently mixed and increase contact surface
Product, can be improved ionic conductivity；The cladding of the positive main material of solid state electrolysis confrontation, can reduce interface impedance to a certain extent.
Anode composite material prepared by the present invention has core-shell structure, and positive electrode active materials are core, surface coated at its
Solid electrolyte is shell, and this core-shell structure can reduce directly contacting between positive electrode active materials and solid electrolyte,
So as to improve the interface problem between anode and solid electrolyte.
The solid electrolyte for the shell that the present invention uses can also reinforcing material ionic conductivity.
Detailed description of the invention
In order to facilitate the understanding of those skilled in the art, the present invention will be further described below with reference to the drawings.
Fig. 1 is the SEM figure of anode composite material in the embodiment of the present invention 1；
Fig. 2 is the all-solid-state battery cycle performance figure prepared in the embodiment of the present invention 1 and comparative example 1.
Specific embodiment
Fig. 1 and Fig. 2 are please referred to, is described in detail in conjunction with following examples.
Embodiment 1:
The preparation process of all-solid-state battery is as follows:
The preparation of anode composite material: the first step presses 3LiBH4- LiI claims with 523 mass ratio of nickle cobalt lithium manganate for 5:100
It takes, by 3LiBH4- LiI is dissolved in N-Methyl pyrrolidone, after being completely dissolved, nickle cobalt lithium manganate 523 is added, in high speed disperser
In be put into vacuum oven after mixing evenly it is dry until solvent volatilization completely, by obtained solid powder under argon atmosphere
500 DEG C, 6h is calcined, furnace cooling obtains the anode composite material of core-shell structure.
The preparation of positive plate: gained anode composite material in the first step and acetylene black, Kynoar are pressed matter by second step
Amount than be 94:3:3 weigh, then Kynoar is added in N-Methyl pyrrolidone and is dispersed, dispersion completely after according to
Secondary addition acetylene black and anode composite material, stir evenly, and adjusting slurry viscosity is 7500cps, and anode sizing agent is coated in aluminium
On foil, positive plate is obtained after drying, roll-in, cutting；
Third step, the preparation of positive composite pole piece: by Kynoar and 3LiBH4- LiI claims in mass ratio for 5:100
Amount, the Kynoar after weighing is dissolved in N-Methyl pyrrolidone, while by 3LiBH4- LiI is dissolved in above-mentioned solution, is passed through
High speed disperser is coated in the positive plate surface prepared in second step after mixing evenly, and coating thickness is 5 μm, obtains after dry
Positive composite pole piece；
4th step, negative electrode tab are commercial graphite pole piece.
Pole piece that third step and the 4th step obtain is assembled into the power Soft Roll of 5Ah by the 5th step by lamination process respectively
After the soft-package battery of preparation is then carried out chemical conversion treatment, multiplying power and cycle life test are carried out to it for battery.
Embodiment 2:
The preparation of anode composite material: the first step presses 3LiBH4- LiI and LiCoO2Mass ratio weighs for 8:100, will
3LiBH4- LiI is dissolved in tetrahydrofuran, and after being completely dissolved, LiCoO is added2, it is put into vacuum after mixing evenly in high speed disperser
It is dry until solvent volatilization completely, by obtained solid powder 500 DEG C under argon atmosphere, calcines 12h, furnace cooling in drying box
Obtain the anode composite material of core-shell structure；
The preparation of positive plate: gained anode composite material in the first step and Ketjen black, polytetrafluoroethylene (PTFE) are pressed matter by second step
Amount than be 92:5:3 weigh, then polytetrafluoroethylene (PTFE) is added in N-Methyl pyrrolidone and is dispersed, dispersion completely after according to
Secondary addition Ketjen black and anode composite material, stir evenly, and adjusting slurry viscosity is 8000cps, and anode sizing agent is coated in aluminium
On foil, positive plate is obtained after drying, roll-in, cutting；
The preparation of positive composite pole piece: third step presses polytetrafluoroethylene (PTFE) and 3LiBH4- LiI claims in mass ratio for 8:100
Amount, polytetrafluoroethylene (PTFE) is dissolved in tetrahydrofuran, then by 3LiBH4- LiI is dissolved in above-mentioned solution, is stirred by high speed disperser
Coated in the positive plate surface prepared in second step after mixing uniformly, coating thickness is 8 μm, it is dry after positive composite pole
Piece；
4th step, negative electrode tab are commercial graphite pole piece.
Pole piece that third step and third step obtain is assembled into the power Soft Roll of 5Ah by the 5th step by lamination process respectively
After the flexible-packed battery of assembling is then carried out chemical conversion treatment, multiplying power and cycle life test are carried out to it for battery.
Embodiment 3
The preparation of anode composite material: the first step presses 3LiBH4- LiI and LiFePO4Mass ratio weighs for 15:100, will
3LiBH4- LiI is dissolved in tetrahydrofuran, and after being completely dissolved, LiFePO is added4, it is put into vacuum after mixing evenly in high speed disperser
It is dry until solvent volatilization completely, by 800 DEG C under nitrogen atmosphere of obtained solid powder, calcines 1h, furnace cooling in drying box
Obtain the anode composite material of core-shell structure；
The preparation of positive plate: the anode composite material of first step preparation and Ketjen black, polytetrafluoroethylene (PTFE) are pressed matter by second step
Amount than be 92:5:3 weigh, then polytetrafluoroethylene (PTFE) is added in N-Methyl pyrrolidone and is dispersed, dispersion completely after according to
Secondary addition Ketjen black and anode composite material, stir evenly, and adjusting slurry viscosity is 8500cps, and anode sizing agent is coated in aluminium
On foil, positive plate is obtained after drying, roll-in, cutting；
The preparation of positive composite pole piece: third step presses polytetrafluoroethylene (PTFE) and 3LiBH4- LiI claims in mass ratio for 8:100
Amount, polytetrafluoroethylene (PTFE) is dissolved in tetrahydrofuran, then by 3LiBH4- LiI is dissolved in above-mentioned solution, is stirred by high speed disperser
Coated in the positive plate surface prepared in second step after mixing uniformly, coating thickness is 10 μm, it is dry after positive composite pole
Piece；
4th step, negative electrode tab are commercial graphite pole piece；
Pole piece that third step and the 4th step obtain is assembled into the power Soft Roll of 5Ah by the 5th step by lamination process respectively
Battery, while by after the battery progress chemical conversion treatment after assembling, multiplying power and cycle life test are carried out to it.
Comparative example 1
The first step, the preparation of positive plate: being 94:3 by nickle cobalt lithium manganate 523 and acetylene black, Kynoar in mass ratio:
3 weigh, and then Kynoar is added in N-Methyl pyrrolidone and is dispersed, and sequentially add acetylene after dispersion completely
Black and anode composite material, stirs evenly, and adjusting slurry viscosity is 7500cps, anode sizing agent is coated on aluminium foil, through drying
Positive plate is obtained after dry, roll-in, cutting；
The preparation of positive composite pole piece: second step presses Kynoar and 3LiBH4- LiI claims in mass ratio for 5:100
Amount, Kynoar is dissolved in N-Methyl pyrrolidone, then by 3LiBH4- LiI is dissolved in above-mentioned solution, passes through high speed point
Scattered machine coats the positive plate surface prepared in the first step after mixing evenly, and coating thickness is 5 μm, obtains after dry positive multiple
Close pole piece；
Third step, negative electrode tab are commercial graphite pole piece；
4th step, the power that pole piece obtained in second step and third step is assembled into 5Ah by lamination process respectively are soft
Packet battery, while by after the progress chemical conversion treatment of the battery of assembling, multiplying power and cycle life test are carried out to it.
Cycle performance test is carried out to embodiment 1 and comparative example 1, it is specific that test results are shown in figure 2, as shown in Figure 2, packet
The positive ternary material obtained after solid electrolyte is covered compared with uncoated positive ternary material, capacity retention is higher, and
And after circulation 100 times, coats the positive ternary material capacity retention obtained after solid electrolyte and remains to reach 95% or more,
And uncoated positive ternary material retention only has 90% or so, it follows that using positive electrode active materials as core, on its surface
The solid electrolyte of cladding is shell, and this core-shell structure can reduce direct between positive electrode active materials and solid electrolyte
Contact, so as to improve the interface problem between anode and solid electrolyte, in addition, the solid electrolyte of shell can also strengthening material
The ionic conductivity of material, it is relatively low to solve existing solid electrolyte ionic conductivity, interface impedance between solid electrolyte/electrode
Greatly, interface compatibility is poor, the higher problem of battery preparation cost at this stage.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (10)
1. a kind of anode composite material of lithium ion battery, which is characterized in that the material specific the preparation method is as follows:
Step 1: it weighs suitable solid electrolyte and is dissolved in organic solvent, above-mentioned solution is added in suitable positive electrode,
It is put into after mixing evenly in vacuum oven dry in high speed disperser until solvent volatilization is complete；
Step 2: obtained solid powder being calcined into certain time under atmosphere of inert gases, furnace cooling is obtaining core-shell structure just
Pole composite material.
2. a kind of anode composite material of lithium ion battery according to claim 1, which is characterized in that solid electrolyte is
3LiBH4-LiI；Organic solvent is N-Methyl pyrrolidone, N,N-dimethylformamide, N, N- diethylformamide, dimethyl
One or more of sulfoxide, tetrahydrofuran, acetone；Positive electrode is nickle cobalt lithium manganate 523, nickle cobalt lithium manganate 622, nickel cobalt manganese
One of sour lithium 811, LiFePO4, cobalt acid lithium or LiMn2O4；Protective atmosphere is nitrogen, argon gas, helium, one in neon
Kind is several.
3. a kind of anode composite material of lithium ion battery according to claim 1, which is characterized in that the solid electrolyte
Mass ratio with positive electrode is 1-15:100.
4. a kind of anode composite material of lithium ion battery according to claim 1, which is characterized in that the calcination temperature is
400-800 DEG C, calcination time 1-24h.
5. a kind of all-solid-state battery, which is characterized in that contain the lithium ion battery prepared in claim 1 in the all-solid-state battery
Anode composite material.
6. a kind of all-solid-state battery according to claim 5, which is characterized in that the specific preparation process of the all-solid-state battery
It is as follows:
The first step prepares anode composite material；
Second step, the preparation of positive plate: weighing binder and dissolve in a solvent and stir evenly, and then adds certain mass thereto
Anode composite material, conductive agent, and stirred evenly by high speed disperser, adjust solution viscosity and obtain anode sizing agent, will just
Pole slurry is coated on aluminium foil, obtains positive plate after drying, roll-in, cutting；
Third step, the preparation of positive composite pole piece: suitable binder is dissolved in solvent, is then dissolved in solid electrolyte
It states in solution, is coated in the positive plate surface prepared in second step, coating thickness 1- after mixing evenly by high speed disperser
10 μm, positive composite pole piece is obtained after dry；
4th step, negative electrode tab use existing negative electrode tab material；
The positive composite pole piece prepared in third step and the negative electrode tab prepared in the 4th step are passed through lamination process respectively by the 5th step
It is assembled into the power soft-package battery of 5Ah, after the battery after assembling is carried out chemical conversion treatment, multiplying power is carried out to it and cycle life is surveyed
Examination.
7. a kind of all-solid-state battery according to claim 6, which is characterized in that binder is to gather inclined fluorine in the second step
One kind of ethylene, polytetrafluoroethylene (PTFE), polyvinylpyrrolidone, polypropylene, polyethylene, polyurethane, polyamide, polyamidoimide
Or it is several；Solvent is N-Methyl pyrrolidone, N,N-dimethylformamide, N, N- diethylformamide, dimethyl sulfoxide, tetrahydro
One or more of furans, acetone；Conductive agent is one or more of acetylene black, carbon nanotube, Ketjen black.
8. a kind of all-solid-state battery according to claim 6, which is characterized in that anode composite material, conduction in second step
Agent, binder mass ratio be 94-85:1-15:3-4:2-3.
9. a kind of all-solid-state battery according to claim 6, which is characterized in that anode sizing agent viscosity is in second step
7000-9000cps。
10. a kind of all-solid-state battery according to claim 6, which is characterized in that binder is polyvinylidene fluoride in third step
Alkene, polytetrafluoroethylene (PTFE), polyvinylpyrrolidone, polypropylene, polyethylene, polyurethane, polyamide, polyamidoimide one kind or
It is several；Wherein the mass ratio of binder and solid electrolyte is 3-10:100 in third step.
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| CN109950616A (en) * | 2019-03-13 | 2019-06-28 | 江西星盈科技有限公司 | Lacking oxygen solid electrolyte and positive electrode and positive plate and lithium ion battery and preparation process |
| CN111490243A (en) * | 2020-05-25 | 2020-08-04 | 蜂巢能源科技有限公司 | Composite positive electrode material for lithium ion battery, preparation method and application thereof |
| CN111509293A (en) * | 2020-04-15 | 2020-08-07 | 国联汽车动力电池研究院有限责任公司 | Method for reducing grain boundary impedance and interface impedance of oxide electrolyte |
| CN111934004A (en) * | 2020-08-19 | 2020-11-13 | 清陶（昆山）能源发展有限公司 | Lithium manganate/solid electrolyte composite material and preparation method and application thereof |
| CN112310354A (en) * | 2019-07-29 | 2021-02-02 | 北京卫蓝新能源科技有限公司 | Lithium battery composite positive electrode material and preparation method thereof |
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