CN110518250A - Plasticizing anode of high positive active material carrying capacity and preparation method thereof, solid state battery - Google Patents
Plasticizing anode of high positive active material carrying capacity and preparation method thereof, solid state battery Download PDFInfo
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- CN110518250A CN110518250A CN201910851102.7A CN201910851102A CN110518250A CN 110518250 A CN110518250 A CN 110518250A CN 201910851102 A CN201910851102 A CN 201910851102A CN 110518250 A CN110518250 A CN 110518250A
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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
- H01M4/13—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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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
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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
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Abstract
The invention discloses a kind of plasticizing of high positive active material carrying capacity anodes, including plus plate current-collecting body and the positive electrode active material layer being formed on plus plate current-collecting body, wherein, it is calculated in weight percent, it include the binder of 1wt%~15wt%, the conductive agent of 1wt%~10wt%, the lithium salts of 1wt%~10wt%, the plasticiser of 0.1wt%~40wt% and the positive active material of 50wt%~80wt% in the positive electrode active material layer.Solid state battery the invention also discloses the preparation method of the above plasticizing anode and comprising plasticizing anode.The energy density of battery can be improved in plasticizing anode provided by the invention, and improves the interface stability between anode and solid electrolyte, improves the cycle performance of solid state battery.
Description
Technical field
The invention belongs to the plasticizing of technical field of secondary batteries more particularly to a kind of high positive active material carrying capacity anode and
Preparation method, solid state battery.
Background technique
In recent years, in new-energy automobile field, the demand of lithium ion battery increases year by year.Lithium ion battery is generally adopted at present
Ionic conduction is carried out with liquid electrolyte, but organic electrolyte is easy to appear the accidents such as leakage, corroding electrode, combustion explosion,
There are biggish security risks.Solid state battery is a kind of battery using solid electrode and solid electrolyte.Solid state battery is general
Power density is lower, and energy density is higher, and power/weight is higher, therefore is the highly desirable battery of new-energy automobile.
Solid state battery is limited by the overall weight of battery at present, by that can reduce electricity with the anode of high active substance carrying capacity
Ratio shared by the quality such as the collector in pond, so that the accounting of positive active material is improved, it is close to improve the energy content of battery with this
Degree.However, since contact of the positive active material with solid electrolyte in solid state battery is only on very limited interface, very
Difficulty plays the advantage of high active substance carrying capacity anode, and the energy density of battery, cycle performance need to be further improved.
Summary of the invention
In view of the shortcomings of the prior art, it is positive that the present invention provides a kind of plasticizings of high positive active material carrying capacity,
To improve the energy density of battery, and improve the interface stability between anode and solid electrolyte, improves solid-state electricity
The cycle performance in pond.
For achieving the above object, present invention employs following technical solutions:
A kind of plasticizing anode of high positive active material carrying capacity, including plus plate current-collecting body and be formed on plus plate current-collecting body
Positive electrode active material layer, wherein it is calculated in weight percent, include in the positive electrode active material layer 1wt%~
The binder of 15wt%, the conductive agent of 1wt%~10wt%, 1wt%~10wt% lithium salts, 0.1wt%~40wt% modeling
The positive active material of agent and 50wt%~80wt%.
It preferably, include binder, the 2wt%~8wt% of 5wt%~10wt% in the positive electrode active material layer
Conductive agent, the lithium salts of 2wt%~8wt%, the plasticiser of 1wt%~30wt% and 55wt%~75wt% positive electrode active material
Matter.
Preferably, the plasticiser in ethylene carbonate, fluorinated ethylene carbonate, succinonitrile and ionic liquid at least
It is a kind of.
Preferably, the binder be selected from polyoxyethylene, Kynoar, butadiene-styrene rubber, styrene-acrylic emulsion, polyacrylonitrile and
At least one of sodium cellulose glycolate, the conductive agent in graphene, conductive black, acetylene black and carbon fiber extremely
Few one kind, the lithium salts are selected from lithium hexafluoro phosphate, bis trifluoromethyl sulfimide lithium, bis- (fluorine sulphonyl) imine lithiums, tetrafluoro boric acid
At least one of lithium, biethyl diacid lithium borate and LiODFB, the positive active material are selected from LiMn2O4, phosphoric acid
At least one of iron lithium, cobalt acid lithium, nickel cobalt manganese, nickel cobalt aluminium and lithium titanate.
Preferably, the plus plate current-collecting body be aluminium foil, the plus plate current-collecting body with a thickness of 1 μm~100 μm.
Preferably, the positive electrode active material layer is formed on one of surface of the plus plate current-collecting body either shape
At on the opposite surface of two in the plus plate current-collecting body.
It is plasticized positive preparation method the present invention also provides a kind of high positive active material carrying capacity as described above,
Include:
Binder, conductive agent, lithium salts, plasticiser and positive active material are provided according to scheduled mass ratio and are dissolved
In solvent, it is stirred to form anode sizing agent；
Plus plate current-collecting body is provided, the anode sizing agent is coated on the plus plate current-collecting body；
The plus plate current-collecting body for being coated with the anode sizing agent is dried, and obtains the plasticizing anode.
Preferably, the solvent is selected from N-Methyl pyrrolidone, dimethylformamide, n,N-Dimethylaniline and tricresyl phosphate
At least one of ethyl ester, the sum of the solvent and the binder, conductive agent, lithium salts, plasticiser and positive active material
Mass ratio be 1~3:1.
Preferably, the anode sizing agent be coated on plus plate current-collecting body on a thickness of 800 μm~1200 μm.
Another aspect of the present invention is to provide a kind of solid state battery comprising the anode layer that sets gradually, solid electrolyte
Layer and negative electrode layer, wherein the anode layer uses the plasticizing anode of high positive active material carrying capacity as described above.
The plasticizing anode of high positive active material carrying capacity provided in an embodiment of the present invention, is to improve positive electrode active material first
The accounting of matter improves battery energy density with this；It followed by joined plasticiser in anode, can be further improved solid
The energy density of state battery；In addition, anode and solid electrolyte can also be significantly improved after plasticiser is added in anode
Between interface stability, improve the cycle performance of solid state battery, while but also anode has superior mechanical strength.
Detailed description of the invention
Fig. 1 is the process flow chart of the preparation method of the plasticizing anode of the embodiment of the present invention；
Fig. 2 is the loop test curve graph of the battery sample 1 in the embodiment of the present invention 4；
Fig. 3 is the loop test curve graph of the battery sample 2 in the embodiment of the present invention 4；
Fig. 4 is the loop test curve graph of the battery sample 3 in the embodiment of the present invention 4；
Fig. 5 is the loop test curve graph of the battery sample 4 in the embodiment of the present invention 4.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, with reference to the accompanying drawing to specific reality of the invention
The mode of applying is described in detail.The example of these preferred embodiments is illustrated in the accompanying drawings.Shown in attached drawing and according to
The embodiments of the present invention of attached drawing description are only exemplary, and the present invention is not limited to these embodiments.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, in the accompanying drawings only
Show with closely related structure and/or processing step according to the solution of the present invention, and be omitted little with relationship of the present invention
Other details.
The embodiment of the present invention provides firstly a kind of plasticizing anode of high positive active material carrying capacity, the plasticizing anode packet
The positive electrode active material layer for including plus plate current-collecting body and being formed on plus plate current-collecting body, wherein it is calculated in weight percent, it is described
Include in positive electrode active material layer the binder of 1wt%~15wt%, the conductive agent of 1wt%~10wt%, 1wt%~
The positive active material of the lithium salts of 10wt%, the plasticiser of 0.1wt%~40wt% and 50wt%~80wt%.
Plasticizing anode as described above, the content of positive active material reach the ratio of 50wt%~80wt%, and its
In be also added into the plasticiser of 0.1wt%~40wt%: firstly, improving electricity by the accounting that improves positive active material with this
Pond energy density；Secondly, joined plasticiser in anode, the active material in anode can be made to form closer connect
Touching reduces the impedance in anode between active material, enables active material to reach higher utilization rate, there is higher specific volume
Amount, to improve the energy density of solid state battery；In addition, battery can also be being significantly improved just after plasticiser is added in anode
Interface stability between pole and solid electrolyte improves the cycle performance of solid state battery, but also anode is with more excellent
Mechanical strength.
It include the bonding of 5wt%~10wt% in more preferred technical solution, in the positive electrode active material layer
Agent, the conductive agent of 2wt%~8wt%, the lithium salts of 2wt%~8wt%, the plasticiser of 1wt%~30wt% and 55wt%~
The positive active material of 75wt%.
Wherein, the plasticiser in ethylene carbonate, fluorinated ethylene carbonate, succinonitrile and ionic liquid at least one
Kind.The binder is selected from polyoxyethylene, Kynoar, butadiene-styrene rubber, styrene-acrylic emulsion, polyacrylonitrile and hydroxymethyl cellulose
At least one of sodium.The conductive agent is selected from least one of graphene, conductive black, acetylene black and carbon fiber.It is described
Lithium salts is selected from lithium hexafluoro phosphate, bis trifluoromethyl sulfimide lithium, bis- (fluorine sulphonyl) imine lithiums, LiBF4, double ethanedioic acids
At least one of lithium borate and LiODFB.The positive active material is selected from LiMn2O4, LiFePO4, cobalt acid
At least one of lithium, nickel cobalt manganese, nickel cobalt aluminium and lithium titanate.It should be noted that material used in above each component is equal
For the material of commercially available acquisition.
In preferred technical solution, the plus plate current-collecting body be aluminium foil, the plus plate current-collecting body with a thickness of 1 μm~
100μm.Wherein, the positive electrode active material layer is formed on one of surface of the plus plate current-collecting body or is formed in
On two opposite surfaces of the plus plate current-collecting body.
Refering to fig. 1, the high positive active material carrying capacity plasticizing anode preparation method comprising steps of
S10, binder, conductive agent, lithium salts, plasticiser and positive active material are provided simultaneously according to scheduled mass ratio
It is dissolved in solvent, is stirred to form anode sizing agent.It is preferred that stirring 4h or more.
S20, plus plate current-collecting body is provided, the anode sizing agent is coated on the plus plate current-collecting body.
S30, the plus plate current-collecting body for being coated with the anode sizing agent are dried, and obtain the plasticizing anode.It is excellent
Selection of land, 50 DEG C~100 DEG C at a temperature of carry out drying drying process.
Wherein, the solvent is selected from N-Methyl pyrrolidone, dimethylformamide, n,N-Dimethylaniline and tricresyl phosphate second
At least one of ester.The sum of the solvent and the binder, conductive agent, lithium salts, plasticiser and positive active material
Mass ratio is 1~3:1, and preferred ratio is 2:1.
Preferably, the anode sizing agent be coated on plus plate current-collecting body on a thickness of 800 μm~1200 μm.
Embodiment 1
The preparation of the anode pole piece of high active substance carrying capacity using succinonitrile as plasticiser
One, by bis- (fluorine sulphonyl) imine lithiums of 7g LiFePO4,0.5g Kynoar, 0.5g conductive black, 0.5g and 2g
Succinonitrile is dissolved in 20g N-Methyl pyrrolidone, and 4h is mixed, obtains anode composite slurry.
Two, above-mentioned anode composite slurry is coated on a thickness of on 20 μm of aluminium foils, 1000 μm of coating thickness, then at 70 DEG C
At a temperature of dry, prepare anode pole piece.
Embodiment 2
The preparation of the anode pole piece of high active substance carrying capacity using ethylene carbonate as plasticiser
One, by bis- (fluorine sulphonyl) imine lithiums of 7g LiFePO4,0.5g Kynoar, 0.5g conductive black, 0.5g and 2g
Ethylene carbonate is dissolved in 20g N-Methyl pyrrolidone, and 4h is mixed, obtains anode composite slurry.
Two, above-mentioned anode composite slurry is coated on a thickness of on 20 μm of aluminium foils, 1000 μm of coating thickness, then at 50 DEG C
At a temperature of dry, prepare anode pole piece.
Embodiment 3
The preparation of the anode pole piece of high active substance carrying capacity using ionic liquid as plasticiser
One, by bis- (fluorine sulphonyl) imine lithiums of 7g LiFePO4,0.5g Kynoar, 0.5g conductive black, 0.5g and 2g
Ionic liquid is dissolved in 20g N-Methyl pyrrolidone, and 4h is mixed, obtains anode composite slurry.
Two, above-mentioned anode composite slurry is coated on a thickness of on 20 μm of aluminium foils, 1000 μm of coating thickness, then at 90 DEG C
At a temperature of dry, prepare anode pole piece.
Comparative example 1
The preparation of the anode pole piece of high active substance carrying capacity without plasticiser
One, bis- (fluorine sulphonyl) imine lithiums of 8g LiFePO4,1g Kynoar, 0.5g and 1g conductive black are dissolved in
In 20g N-Methyl pyrrolidone, 4h is mixed, obtains anode composite slurry.
Two, above-mentioned anode composite slurry is coated on a thickness of on 20 μm of aluminium foils, 1000 μm of coating thickness, then at 90 DEG C
At a temperature of dry, prepare anode pole piece.
Embodiment 4
Above embodiments 1-3 and comparative example 1 anode pole piece prepared are assembled respectively and form solid-state by the present embodiment
Then battery sample carries out electro-chemical test to solid state battery sample.It is specific as follows:
One, the preparation of cathode pole piece: high-purity lithium piece is cut into the disk of diameter 16mm, prepares cathode pole piece.It needs
Prepare 4 cathode pole pieces.
Two, the preparation of solid electrolyte
(1), bis- (fluorine sulphonyl) imine lithiums of 3g Kynoar, 2g, 15g dimethylformamide and 35g tetrahydrofuran is mixed
Close stirring 5h solid electrolyte slurry derived above.
(2), obtained solid electrolyte slurry is coated with, obtains solid electrolyte in 80 DEG C of baking 12h.
Three, the assembling of solid state battery
The cathode pole piece of acquisition made above, solid electrolyte and embodiment 1-3 and comparative example 1 are prepared just
Pole pole piece trimming is encapsulated as button cell at disk, using tablet press machine.Wherein, the anode pole piece of embodiment 1 corresponds to battery sample
Product 1, the anode pole piece of embodiment 2 correspond to battery sample 2, and the anode pole piece of embodiment 3 corresponds to battery sample 3, comparative example 1
Anode pole piece correspond to battery sample 4.
Circulating battery test, test are carried out to the above battery sample 1~4 using circulating battery system (blue electricity CT2001A)
Data are referring to following table 1 and attached drawing 2~5, wherein Fig. 2 corresponds to the test curve of battery sample 1, and Fig. 3 corresponds to battery sample
The test curve of product 2, Fig. 4 correspond to the test curve of battery sample 3, and Fig. 5 corresponds to the test curve of battery sample 4.
Table 1
| Project | Battery sample 1 | Battery sample 2 | Battery sample 3 | Battery sample 4 |
| Coulombic efficiency (%) | 95% | 96% | 92% | - |
| Specific capacity (mAh/g) | 110 | 105 | 55 | 0 |
From the data of table 1 and Fig. 2~5 as can be seen that battery sample 1~3 is (positive using high anode provided by the invention
The plasticizing anode of active material carrying capacity) 100 wheels circulation charge and discharge process can be carried out, (anode is using no plasticiser for battery sample 4
High positive active material carrying capacity anode) by 14 wheel cycle charge-discharges after, capacity is just reduced to 0.Wherein battery sample 1 and 2
Coulombic efficiency and specific capacity it is relatively high, by 100 wheel charge and discharge process also have 90% or more coulombic efficiency while,
Also there is higher capacity, illustrates that the anode of the high active substance carrying capacity of addition plasticiser can be obviously improved the circulation of battery
Performance can be further improved the energy density of battery, for power battery while keeping solid state battery security performance
Development has good facilitation.
The above is only the specific embodiment of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection scope of the application.
Claims (10)
1. a kind of plasticizing anode of high positive active material carrying capacity, including plus plate current-collecting body and is formed on plus plate current-collecting body
Positive electrode active material layer, which is characterized in that it is calculated in weight percent, include in the positive electrode active material layer 1wt%~
The binder of 15wt%, the conductive agent of 1wt%~10wt%, 1wt%~10wt% lithium salts, 0.1wt%~40wt% modeling
The positive active material of agent and 50wt%~80wt%.
2. the plasticizing anode of high positive active material carrying capacity according to claim 1, which is characterized in that the positive-active
Include in material layer the binder of 5wt%~10wt%, the conductive agent of 2wt%~8wt%, 2wt%~8wt% lithium salts,
The plasticiser of 1wt%~30wt% and the positive active material of 55wt%~75wt%.
3. the plasticizing anode of high positive active material carrying capacity according to claim 1 or 2, which is characterized in that the plasticizing
Agent is selected from least one of ethylene carbonate, fluorinated ethylene carbonate, succinonitrile and ionic liquid.
4. the plasticizing anode of high positive active material carrying capacity according to claim 3, which is characterized in that the binder choosing
At least one of selfpolyoxyethylene, Kynoar, butadiene-styrene rubber, styrene-acrylic emulsion, polyacrylonitrile and sodium cellulose glycolate,
The conductive agent is selected from least one of graphene, conductive black, acetylene black and carbon fiber, and the lithium salts is selected from hexafluorophosphoric acid
Lithium, bis trifluoromethyl sulfimide lithium, bis- (fluorine sulphonyl) imine lithiums, LiBF4, biethyl diacid lithium borate and oxalic acid difluoro
At least one of lithium borate, the positive active material be selected from LiMn2O4, LiFePO4, cobalt acid lithium, nickel cobalt manganese, nickel cobalt aluminium and
At least one of lithium titanate.
5. the plasticizing anode of high positive active material carrying capacity according to claim 3, which is characterized in that the anode collection
Body is aluminium foil, the plus plate current-collecting body with a thickness of 1 μm~100 μm.
6. the plasticizing anode of high positive active material carrying capacity according to claim 3, which is characterized in that the positive-active
Material layer is formed on one of surface of the plus plate current-collecting body or is formed in two phases of the plus plate current-collecting body
Pair surface on.
7. a kind of preparation method of the plasticizing anode of high positive active material carrying capacity as described in claim 1-6 is any, special
Sign is, comprising:
Binder, conductive agent, lithium salts, plasticiser and positive active material are provided according to scheduled mass ratio and are dissolved in molten
In agent, it is stirred to form anode sizing agent；
Plus plate current-collecting body is provided, the anode sizing agent is coated on the plus plate current-collecting body；
The plus plate current-collecting body for being coated with the anode sizing agent is dried, and obtains the plasticizing anode.
8. the preparation method of the plasticizing anode of high positive active material carrying capacity according to claim 7, which is characterized in that institute
It states solvent and is selected from least one of N-Methyl pyrrolidone, dimethylformamide, n,N-Dimethylaniline and triethyl phosphate,
The mass ratio of the sum of the solvent and the binder, conductive agent, lithium salts, plasticiser and positive active material is 1~3:1.
9. the preparation method of the plasticizing anode of high positive active material carrying capacity according to claim 7, which is characterized in that institute
State anode sizing agent coated on plus plate current-collecting body with a thickness of 800 μm~1200 μm.
10. a kind of solid state battery, including positive plate, solid-state electrolyte layer and the negative electrode tab set gradually, which is characterized in that described
Positive plate is positive using the plasticizing of high positive active material carrying capacity as claimed in claim 1.
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| CN112133923B (en) * | 2020-09-30 | 2022-05-03 | 蜂巢能源科技有限公司 | Positive electrode material layer suitable for semi-solid battery, preparation method thereof, positive plate and semi-solid battery |
| CN114069024A (en) * | 2021-11-15 | 2022-02-18 | 惠州亿纬锂能股份有限公司 | 3D printing solid-state battery and preparation method and application thereof |
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