CN112216874A - Preparation process of all-solid-state battery - Google Patents
Preparation process of all-solid-state battery Download PDFInfo
- Publication number
- CN112216874A CN112216874A CN202011090965.6A CN202011090965A CN112216874A CN 112216874 A CN112216874 A CN 112216874A CN 202011090965 A CN202011090965 A CN 202011090965A CN 112216874 A CN112216874 A CN 112216874A
- Authority
- CN
- China
- Prior art keywords
- solid
- electrolyte
- coating
- negative electrode
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
- H01M10/058—Construction or manufacture
-
- 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
-
- 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
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a preparation process of an all-solid-state battery, which comprises the following steps: s1: coating the molten electrolyte mixture on a negative electrode sheet to form a first electrolyte layer; s2: stacking a positive plate on the first electrolyte layer, applying a first pressure to press the positive plate, and coating the molten electrolyte mixture on the positive plate to form a second electrolyte layer; s3: stacking the other negative plate on the second electrolyte layer, and applying a second pressure for lamination; s4: repeating the operations of the steps S1 to S3 on the cathode sheets stacked in the step S3 for N times to obtain an all-solid-state battery, wherein N is an integer and is not less than 0; the electrolyte mixture is formed by mixing the following components in percentage by weight: 30-70% of PEO, 10-40% of LiTFSI, 4-10% of PEG, 4-10% of PVDF, 0-25% of oxide solid electrolyte and 0-25% of sulfide solid electrolyte. The electrolyte mixture is not easy to introduce moisture, the process flow control cost is reduced, and the prepared solid-state battery has low interface impedance and low internal resistance.
Description
Technical Field
The invention relates to the technical field of solid-state batteries, in particular to a preparation process of an all-solid-state battery.
Background
The solid-state battery has the characteristics of high energy density, high safety and the like, and is the development direction of future lithium batteries.
The existing manufacturing process of the anode and the cathode of the solid-state battery is carried out by using the traditional manufacturing process of the anode and the cathode of the liquid-state lithium battery, and only some changes are made on the formula. Compared with the conventional liquid lithium battery process, the solid electrolyte preparation process is added, that is, a simple diagram of a process route diagram of the conventional solid battery is shown in fig. 1.
Solid-state batteries face a number of technical difficulties at the present stage. For example, the interface impedance between the solid electrolyte and the electrode plate is high, which seriously affects the battery performance. At present, the published data shows that there are many documents that improve the interface performance of the solid-state battery. For example, 1) the interface fusion is promoted by heating and melting the surface of the solid electrolyte and the surface of the electrode by means of microwave, sound wave, ultrasonic wave and the like, so that the interface impedance of the battery is reduced; 2) a polyethylene oxide solution is injected between the electrode and the solid electrolyte to improve the interfacial properties.
However, the process route shown in fig. 1 still has the following disadvantages: 1) the electrolyte preparation is carried out by adopting a solvent dispersion mixing mode, the working procedure is complicated, multiple times of tank opening and feeding are needed, the viscosity is adjusted, the solid electrolyte is sensitive to moisture, the water is easily introduced by the mixing mode, and the control cost is high; 2) the solid electrolyte slurry is coated on one side of the positive electrode and the negative electrode in a coating process mode, and the other side of the positive electrode and the negative electrode is coated without the electrolyte, so that the interface impedance of the electrolyte-free side of the assembled battery is high, the performance of the battery is greatly influenced, and the improvement is limited although a clamp hot-pressing process is carried out in the follow-up process; 3) the whole battery manufacturing process flow increases the working procedure of coating the electrolyte on the pole piece, the management and control items are increased, and the process flow is relatively beneficial to the soft package battery, but cannot be used for the hard shell battery, has high limitation and cannot be used universally; 4) an interface treatment procedure for improving the interface of the solid battery is required to be added on the basis of manufacturing the solid battery, and the process is relatively complex.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the interface impedance of the battery is reduced by improving and simplifying the preparation process of the all-solid-state battery.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation process of an all-solid-state battery comprises the following steps:
s1: coating the molten electrolyte mixture on a negative electrode sheet to form a first electrolyte layer;
s2: stacking a positive plate on the first electrolyte layer, applying a first pressure to press the positive plate, and coating the molten electrolyte mixture on the positive plate to form a second electrolyte layer;
s3: stacking the other negative plate on the second electrolyte layer, and applying a second pressure for lamination;
s4: repeating the operations of the steps S1 to S3 on the cathode sheets stacked in the step S3 for N times to obtain an all-solid-state battery, wherein N is an integer and is not less than 0;
the electrolyte mixture is formed by mixing the following components in percentage by weight: 30-70% of polyethylene oxide, 10-40% of LiTFSI, 4-10% of polyethylene glycol, 4-10% of polyvinylidene fluoride, 0-25% of oxide solid electrolyte and 0-25% of sulfide solid electrolyte.
Further, the electrolyte mixture was heated to a molten state under vacuum conditions of 165-200 ℃ with stirring.
Further, the revolution speed of stirring is 15-50rpm, the rotation speed of stirring is 1000-5000rpm, and the stirring and heating time is 1-6 h; after the complete melting, the electrolyte mixture is still kept for 1.5 to 2.5 hours at constant temperature under vacuum condition, so that the viscosity of the electrolyte mixture is kept in the range of 7000-40000 Pa-s for coating.
Further, before stirring and heating, the electrolyte mixture is dry-mixed for 1-6h under the vacuum condition that the revolution speed is 15-50rpm and the rotation speed is 1000-5000 rpm.
Or further, before stirring and heating, the electrolyte mixture is dry-mixed for 1-6h under vacuum by means of ball milling.
Further, coating the molten electrolyte mixture by means of doctor blade coating or extrusion coating, wherein the coating thickness of the first electrolyte layer is 10-20 μm, and the positive electrode sheets are stacked immediately after coating; the second electrolyte layer is coated to a thickness of 10 to 20 μm, and negative electrode sheets are stacked immediately after coating.
Further, the first pressure is 5-100N/cm2The first electrolyte layer is pressed to 6-18 mu m and is rapidly cooled immediately after the pressing is finished; the second pressure is 5-100N/cm2And the second electrolyte layer is pressed to 6-18 μm and rapidly cooled immediately after the pressing is completed.
Further, the negative plate is formed by coating negative slurry on a current collector and rolling the negative plate; the negative electrode slurry consists of a negative electrode solid component and an NMP solvent, and the solid content is 30-60%; the solid components of the negative electrode comprise the following components in percentage by weight: 80-95% of a negative electrode active material, 1-5% of LiTFSI, 0.5-3% of CNT, 1-5% of a nano-scale oxide solid electrolyte, 1-5% of SP and 2-5% of PVDF; the positive plate is formed by coating positive slurry on a current collector and rolling to prepare a sheet; the positive electrode slurry consists of positive electrode solid components and an NMP solvent, and the solid content is 30-60%; the solid components of the positive electrode comprise the following components in percentage by weight: 80-95% of positive active material, 1-5% of LiTFSI, 0.5-3% of CNT, 1-5% of nano-scale oxide solid electrolyte, 0-5% of PEO, 1-5% of SP and 2-5% of PVDF.
Further, the negative electrode active material is one of metal lithium foil, graphite and lithium titanate, and the positive electrode active material is one of NCM, NCA, LCO, LFP and LMO; the nanoscale oxide solid electrolyte is one or more of LLZTO, LZTO, NASICON and LLTO.
Further, in step S4, after the lamination is completed, the obtained all-solid-state battery is packaged, and finally subjected to capacity detection, voltage and internal resistance detection and self-discharge detection, and can be put into a warehouse after the detection is qualified.
The invention has the beneficial effects that: the electrolyte mixture can be in a molten state only at a temperature higher than the boiling point of water, so that moisture is not easily introduced into the electrolyte mixture in the molten state, and the control cost of the process flow is reduced. When the electrolyte mixture is in a molten state, the positive plate and the negative plate are attached through the electrolyte mixture, so that the interface impedance among the positive plate, the negative plate and the electrolyte can be effectively reduced.
Drawings
The detailed structure of the invention is described in detail below with reference to the accompanying drawings
Fig. 1 is a process route diagram of a conventional solid-state battery;
fig. 2 is a general process scheme of a fabrication process for an all-solid-state battery of the present invention;
fig. 3 is a lamination flow chart of a manufacturing process of an all-solid battery according to the present invention.
Detailed Description
In the following examples, NCM is lithium nickel cobalt manganese oxide; NCA is nickel cobalt lithium aluminate; LCO is lithium cobaltate; LFP is lithium iron phosphate; LMO is lithium manganate; NASICON is a sodium ion conductor; LLZTO is a lithium lanthanum zirconium tantalum oxygen ion conductor; the LZTO is a lithium lanthanum zirconium oxygen ion conductor; LLTO is lanthanum lithium titanate; PVDF is polyvinylidene fluoride; NMP is N-methylpyrrolidone; SP is Super-P; PEO is polyethylene oxide; LiTFSI is lithium bis (trifluoromethanesulfonyl) imide; PEG is polyethylene glycol; CNTs are carbon nanotube conductive agents.
The present invention will be further described with reference to the accompanying drawings based on the detailed description of the technical contents, the structural features, and the objects and effects achieved by the present invention.
Example 1
Referring to fig. 2 and fig. 3, a process for manufacturing an all-solid battery includes the following steps:
s1: coating the molten electrolyte mixture on a negative electrode sheet to form a first electrolyte layer;
s2: stacking a positive plate on the first electrolyte layer, applying a first pressure to press the positive plate, and coating the molten electrolyte mixture on the positive plate to form a second electrolyte layer;
s3: stacking the other negative plate on the second electrolyte layer, and applying a second pressure for lamination;
s4: repeating the operations of the steps S1 to S3 on the cathode plates stacked in the step S3 for N times, packaging to obtain an all-solid-state battery, and finally performing capacity detection, voltage internal resistance detection and self-discharge detection to obtain qualified cathode plates which can be put into a warehouse; wherein N is an integer, and N is not less than 0;
the electrolyte mixture is formed by mixing the following components in percentage by weight: 30-70% of polyethylene oxide, 10-40% of LiTFSI, 4-10% of polyethylene glycol, 4-10% of polyvinylidene fluoride, 0-25% of oxide solid electrolyte and 0-25% of sulfide solid electrolyte.
The electrolyte mixture can be in a molten state only at a temperature higher than the boiling point of water, so that moisture is not easily introduced into the electrolyte mixture in the molten state, and the control cost of the process flow is reduced. When the electrolyte mixture is in a molten state, the positive plate and the negative plate are attached through the electrolyte mixture, so that the interface impedance among the positive plate, the negative plate and the electrolyte can be effectively reduced.
Example 2
On the basis of the above example 1, the electrolyte mixture is dry-mixed under the vacuum condition that the revolution speed is 15-50rpm and the rotation speed is 1000-; then under the vacuum condition that the revolution speed is kept between 15 and 50rpm and the autorotation speed is 1000-5000rpm, the temperature is increased to 165-200 ℃, the electrolyte mixture is stirred and heated to a molten state, and the stirring and heating time is 1 to 6 hours; and after the electrolyte mixture is completely melted, stopping stirring, and continuously standing for 1.5-2.5h at constant temperature under the vacuum condition. The electrolyte mixture was coated on the positive electrode sheet or the negative electrode sheet while the viscosity of the electrolyte mixture was maintained in the range of 7000-40000Pa · s.
The electrolyte mixture is mixed by adopting a dry mixing and melting vacuum stirring process, the melting temperature is higher than the boiling point of water, the whole process is vacuumized, the moisture of the electrolyte mixture is well controlled, and the method is simple. After dry blending, the electrolyte mixture is more readily melt isostatically, and the molten electrolyte mixture is uniform throughout.
Example 3
On the basis of the embodiment 1, the electrolyte mixture is firstly subjected to ball milling dry mixing under the vacuum condition for 1-6 h; then under the vacuum condition that the revolution speed is 15-50rpm and the rotation speed is 1000-5000rpm, the temperature is increased to 165-200 ℃, the electrolyte mixture is stirred and heated to a molten state, and the stirring and heating time is 1-6 h; and after the electrolyte mixture is completely melted, stopping stirring, and continuously standing for 1.5-2.5h at constant temperature under the vacuum condition. The electrolyte mixture was coated on the positive electrode sheet or the negative electrode sheet while the viscosity of the electrolyte mixture was maintained in the range of 7000-40000Pa · s.
The electrolyte mixture is mixed by adopting a dry mixing and melting vacuum stirring process, the melting temperature is higher than the boiling point of water, the whole process is vacuumized, the moisture of the electrolyte mixture is well controlled, and the method is simple. After dry blending, the electrolyte mixture is more readily melt isostatically, and the molten electrolyte mixture is uniform throughout.
Example 4
On the basis of the above examples, the molten electrolyte mixture was applied by blade coating or extrusion coating, the first electrolyte layer was applied to a thickness of 10 to 20 μm, and the positive electrode sheets were stacked immediately after the application; the second electrolyte layer is coated to a thickness of 10 to 20 μm, and negative electrode sheets are stacked immediately after coating. The first pressure is 5-100N/cm2The first electrolyte layer is pressed to 6-18 mu m and is rapidly cooled immediately after the pressing is finished; the second pressure is 5-100N/cm2And the second electrolyte layer is pressed to 6-18 μm and rapidly cooled immediately after the pressing is completed.
The extrusion scraper is adopted to coat the coating thickness of the control electrolyte mixture, full-automatic production can be well realized, the number of the large coating machines is reduced, the using area of a field is reduced, and the energy consumption in the production process is reduced. Before coating, the electrolyte mixture is in a vacuum environment and in a molten state, and moisture is not introduced.
Example 5
On the basis of the embodiment, the negative plate is formed by coating negative slurry on a current collector and rolling the negative plate; the negative electrode slurry consists of a negative electrode solid component and an NMP solvent, and the solid content is 30-60%; the solid components of the negative electrode comprise the following components in percentage by weight: 80-95% of a negative electrode active material, 1-5% of LiTFSI, 0.5-3% of CNT, 1-5% of a nano-scale oxide solid electrolyte, 1-5% of SP and 2-5% of PVDF; the positive plate is formed by coating positive slurry on a current collector and rolling to prepare a sheet; the positive electrode slurry consists of positive electrode solid components and an NMP solvent, and the solid content is 30-60%; the solid components of the positive electrode comprise the following components in percentage by weight: 80-95% of positive active material, 1-5% of LiTFSI, 0.5-3% of CNT, 1-5% of nano-scale oxide solid electrolyte, 0-5% of PEO, 1-5% of SP and 2-5% of PVDF. The negative active material is one of metal lithium foil, graphite and lithium titanate, and the positive active material is one of NCM, NCA, LCO, LFP and LMO; the nanoscale oxide solid electrolyte is one or more of LLZTO, LZTO, NASICON and LLTO.
To further illustrate the technical solution of the present invention, a solid-state battery with a specification of 60Ah was manufactured according to the following test examples and test descriptions, and the test results are shown in table 1:
60Ah solid-state battery (the battery core of which comprises 42 positive plates and 43 negative plates) manufacturing steps:
(1) preparing anode slurry: weighing the components in percentage by mass to obtain solid components of the anode: 90.0% NCM523, 2.0% lithium bistrifluoromethanesulfonylimide (LiTFSI), 1.0% carbon nanotube Conductor (CNT), 2.0% nanoscale oxide solid electrolyte (LLZTO), 1.0% SP, and 4% PVDF; adding an NMP solvent into the solid components of the positive electrode for dispersion to obtain positive electrode slurry with the solid content of 50.0%;
(2) preparing negative electrode slurry: weighing the components in percentage by mass to obtain solid components of the cathode: 90.0% graphite, 2.0% lithium bistrifluoromethanesulfonimide (LiTFSI), 1.0% carbon nanotube Conductor (CNT), 2.0% nanoscale oxide solid electrolyte (LLZTO), 1.0% SP, and 4% PVDF; adding an NMP solvent into the solid components of the negative electrode for dispersion to obtain negative electrode slurry with the solid content of 50%;
(3) coating: and respectively coating the positive electrode slurry and the negative electrode slurry on a current collector. When the coating is finished, the density of the positive electrode slurry coating on the surface of the current collector is 18.0mg/cm3The density of the negative electrode slurry coating on the surface of the current collector is 8.47mg/cm3The cathode excess ratio was 1.1;
(4) rolling and tabletting: according to the positive electrode compaction density of 3.2g/cm3Negative pole piece pressingThe solid density is 1.4g/cm3And rolling the positive electrode slurry coating and the negative electrode slurry coating to the designed thickness of the process respectively, and finally cutting to obtain a positive plate and a negative plate for later use. The size of the positive plate is 200.0 multiplied by 143.2mm, and the size of the negative plate is 202.0 multiplied by 145.2 mm.
(5) Preparing an electrolyte mixture according to the component content in the table 1, and dry-mixing for 4 hours under the conditions of revolution speed of 30rpm, rotation speed of 4000rpm and vacuum degree below-0.08 Mpa; keeping the revolution speed of 30rpm, the self-transferring speed of 4000rpm and the vacuum degree below-0.08 Mpa, heating the electrolyte mixture to the set heating temperature shown in the table 1, and stirring and heating for 4 hours; the stirring was stopped, and the mixture was allowed to stand at a constant vacuum condition of-0.08 MPa or less and a predetermined heating temperature shown in Table 1, and the viscosity of the electrolyte mixture was measured, and the results are shown in Table 1.
TABLE 1 test results of cell internal resistance
(6) Extruding and blade-coating the molten electrolyte mixture on a negative electrode sheet with a coating thickness of 18 μm by high pressure, stacking a positive electrode sheet, and applying a 90N/cm coating on the positive electrode sheet2The thickness of the first electrolyte layer is controlled to be 16 mu m, and the tolerance is controlled to be +/-2 mu m; rapidly cooling; coating an electrolyte mixture on the surface of the positive plate in a scraping mode, and controlling the thickness of the second electrolyte layer to be 18 microns; stacking another negative plate, and applying a 90N/cm negative plate face2The thickness of the second electrolyte layer is controlled to be 16 mu m, and the tolerance is controlled to be +/-2 mu m; and (6) rapidly cooling.
(7) The procedure of step (6) was repeated to design the number of stacked layers, and four solid-state batteries of test examples 1 to 4 were obtained after packaging, and the corresponding internal resistances of the batteries were measured, and the results are shown in table 1.
As can be seen from the data in table 1, the process of the present application can effectively reduce the interfacial impedance between the positive electrode sheet, the negative electrode sheet and the electrolyte in the solid-state battery, so as to reduce the internal resistance of the solid-state battery.
In conclusion, the preparation process of the all-solid-state battery provided by the invention can avoid the problem of introducing moisture in the electrolyte mixing stage; the interface impedance of the solid-state battery is reduced, the internal resistance of the battery is reduced, and the performance of the battery is improved; the battery is pressed in the process of assembling the stacked core, and is not limited to a soft-shell battery any more, and a hard-shell battery can also be used; compared with the traditional process, the process of coating the electrolyte on the positive plate and the negative plate respectively is reduced, the electrolyte mixture is coated and the electric core is assembled in the same process, the equipment integration can be realized, the input amount of the coating machine is reduced by 50%, and the equipment input cost, the site input cost and the energy consumption input cost are greatly reduced.
The first … … and the second … … are only used for name differentiation and do not represent how different the importance and position of the two are.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A preparation process of an all-solid-state battery is characterized by comprising the following steps:
s1: coating the molten electrolyte mixture on a negative electrode sheet to form a first electrolyte layer;
s2: stacking a positive plate on the first electrolyte layer, applying a first pressure to press the positive plate, and coating the molten electrolyte mixture on the positive plate to form a second electrolyte layer;
s3: stacking the other negative plate on the second electrolyte layer, and applying a second pressure for lamination;
s4: repeating the operations of the steps S1 to S3 on the cathode sheets stacked in the step S3 for N times to obtain an all-solid-state battery, wherein N is an integer and is not less than 0;
the electrolyte mixture is formed by mixing the following components in percentage by weight: 30-70% of polyethylene oxide, 10-40% of LiTFSI, 4-10% of polyethylene glycol, 4-10% of polyvinylidene fluoride, 0-25% of oxide solid electrolyte and 0-25% of sulfide solid electrolyte.
2. The process for preparing an all-solid battery according to claim 1, wherein the electrolyte mixture is stirred and heated to a molten state under vacuum conditions of 165-200 ℃.
3. The process for preparing an all-solid battery according to claim 2, wherein the revolution speed of the stirring is 15-50rpm, the rotation speed of the stirring is 1000-5000rpm, and the time for stirring and heating is 1-6 h; after the complete melting, the electrolyte mixture is still kept for 1.5 to 2.5 hours at constant temperature under vacuum condition, so that the viscosity of the electrolyte mixture is kept in the range of 7000-40000 Pa-s for coating.
4. The process for preparing an all-solid battery according to claim 3, wherein the electrolyte mixture is dry-blended under vacuum conditions of revolution speed of 15-50rpm and rotation speed of 1000-5000rpm for 1-6 hours before stirring and heating.
5. The process for preparing an all-solid battery according to claim 3, wherein the electrolyte mixture is dry-blended under vacuum for 1-6 hours by means of ball milling before being heated with stirring.
6. The process for producing an all-solid battery according to any one of claims 1 to 5, wherein the coating of the molten electrolyte mixture is carried out by blade coating or extrusion coating, the first electrolyte layer is coated to a thickness of 10 to 20 μm, and the positive electrode sheets are stacked immediately after the coating; the second electrolyte layer is coated to a thickness of 10 to 20 μm, and negative electrode sheets are stacked immediately after coating.
7. The process for preparing an all-solid battery according to claim 6, wherein the first pressure is 5 to 100N/cm2The first electrolyte layer is pressed to 6-18 μm, and after the pressing is completedImmediately and rapidly cooling; the second pressure is 5-100N/cm2And the second electrolyte layer is pressed to 6-18 μm and rapidly cooled immediately after the pressing is completed.
8. The process for producing an all-solid battery according to claim 1, wherein the negative electrode sheet is formed by roll-pressing a negative electrode slurry coated on a current collector; the negative electrode slurry consists of a negative electrode solid component and an NMP solvent, and the solid content is 30-60%; the solid components of the negative electrode comprise the following components in percentage by weight: 80-95% of a negative electrode active material, 1-5% of LiTFSI, 0.5-3% of CNT, 1-5% of a nano-scale oxide solid electrolyte, 1-5% of SP and 2-5% of PVDF; the positive plate is formed by coating positive slurry on a current collector and rolling to prepare a sheet; the positive electrode slurry consists of positive electrode solid components and an NMP solvent, and the solid content is 30-60%; the solid components of the positive electrode comprise the following components in percentage by weight: 80-95% of positive active material, 1-5% of LiTFSI, 0.5-3% of CNT, 1-5% of nano-scale oxide solid electrolyte, 0-5% of PEO, 1-5% of SP and 2-5% of PVDF.
9. The process for preparing an all-solid battery according to claim 8, wherein the negative active material is one of metallic lithium foil, graphite and lithium titanate, and the positive active material is one of NCM, NCA, LCO, LFP and LMO; the nanoscale oxide solid electrolyte is one or more of LLZTO, LZTO, NASICON and LLTO.
10. The process of claim 1, wherein in step S4, the obtained all-solid-state battery is packaged after lamination, and finally subjected to capacity detection, internal resistance voltage detection and self-discharge detection, and can be put into storage after passing detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011090965.6A CN112216874B (en) | 2020-10-13 | 2020-10-13 | Preparation process of all-solid-state battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011090965.6A CN112216874B (en) | 2020-10-13 | 2020-10-13 | Preparation process of all-solid-state battery |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112216874A true CN112216874A (en) | 2021-01-12 |
| CN112216874B CN112216874B (en) | 2022-03-04 |
Family
ID=74053878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011090965.6A Active CN112216874B (en) | 2020-10-13 | 2020-10-13 | Preparation process of all-solid-state battery |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112216874B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113013475A (en) * | 2021-02-25 | 2021-06-22 | 深圳吉阳智能科技有限公司 | Laminated cell production process, laminated cell production system and laminated cell |
| CN113611819A (en) * | 2021-07-30 | 2021-11-05 | 蜂巢能源科技(无锡)有限公司 | All-solid-state battery and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1412884A (en) * | 2001-09-11 | 2003-04-23 | 株式会社Skc | Lithium ion polymer cell and its mfg. method |
| US20070099080A1 (en) * | 2005-10-28 | 2007-05-03 | Pickett David F Jr | Thermal battery with reduced operational temperature |
| CN103730684A (en) * | 2014-01-15 | 2014-04-16 | 广东亿纬赛恩斯新能源系统有限公司 | High-safety all-solid-state lithium ion battery and production method thereof |
| CN106299467A (en) * | 2016-09-13 | 2017-01-04 | 清华大学 | Composite solid electrolyte and flexible all-solid-state battery and preparation method, wearable electronic |
| CN106450394A (en) * | 2016-11-24 | 2017-02-22 | 东莞理工学院 | PVDF-PEO solid composite polymer electrolyte and preparation method thereof |
| CN109698319A (en) * | 2018-12-28 | 2019-04-30 | 蜂巢能源科技有限公司 | Cathode of solid state battery and preparation method thereof and solid state electrode |
| CN109860720A (en) * | 2019-01-30 | 2019-06-07 | 浙江锋锂新能源科技有限公司 | A kind of preparation method and solid state battery of composite electrolyte layer |
| CN111244537A (en) * | 2020-02-24 | 2020-06-05 | 南方科技大学 | Composite solid electrolyte, solid battery and preparation method thereof |
| CN111653823A (en) * | 2020-06-16 | 2020-09-11 | 南京邮电大学 | All-solid-state composite electrolyte based on glass fiber vertical array structure and preparation method thereof |
-
2020
- 2020-10-13 CN CN202011090965.6A patent/CN112216874B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1412884A (en) * | 2001-09-11 | 2003-04-23 | 株式会社Skc | Lithium ion polymer cell and its mfg. method |
| US20070099080A1 (en) * | 2005-10-28 | 2007-05-03 | Pickett David F Jr | Thermal battery with reduced operational temperature |
| CN103730684A (en) * | 2014-01-15 | 2014-04-16 | 广东亿纬赛恩斯新能源系统有限公司 | High-safety all-solid-state lithium ion battery and production method thereof |
| CN106299467A (en) * | 2016-09-13 | 2017-01-04 | 清华大学 | Composite solid electrolyte and flexible all-solid-state battery and preparation method, wearable electronic |
| CN106450394A (en) * | 2016-11-24 | 2017-02-22 | 东莞理工学院 | PVDF-PEO solid composite polymer electrolyte and preparation method thereof |
| CN109698319A (en) * | 2018-12-28 | 2019-04-30 | 蜂巢能源科技有限公司 | Cathode of solid state battery and preparation method thereof and solid state electrode |
| CN109860720A (en) * | 2019-01-30 | 2019-06-07 | 浙江锋锂新能源科技有限公司 | A kind of preparation method and solid state battery of composite electrolyte layer |
| CN111244537A (en) * | 2020-02-24 | 2020-06-05 | 南方科技大学 | Composite solid electrolyte, solid battery and preparation method thereof |
| CN111653823A (en) * | 2020-06-16 | 2020-09-11 | 南京邮电大学 | All-solid-state composite electrolyte based on glass fiber vertical array structure and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113013475A (en) * | 2021-02-25 | 2021-06-22 | 深圳吉阳智能科技有限公司 | Laminated cell production process, laminated cell production system and laminated cell |
| CN113611819A (en) * | 2021-07-30 | 2021-11-05 | 蜂巢能源科技(无锡)有限公司 | All-solid-state battery and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112216874B (en) | 2022-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Cao et al. | Processing strategies to improve cell-level energy density of metal sulfide electrolyte-based all-solid-state Li metal batteries and beyond | |
| CN108963327B (en) | Inorganic filler composite PEO solid electrolyte material, preparation method and all-solid-state battery | |
| CN110581311B (en) | Composite solid electrolyte membrane, preparation method thereof and solid battery | |
| Li et al. | A promising composite solid electrolyte incorporating LLZO into PEO/PVDF matrix for all-solid-state lithium-ion batteries | |
| CN112670483B (en) | Positive plate, positive polar plate and solid-state battery | |
| CN108232286B (en) | Preparation method of composite positive electrode added with polymer and application of composite positive electrode in solid-state battery | |
| CN108232156B (en) | Silicon-carbon composite cathode for solid-state battery and preparation method thereof | |
| CN107093764A (en) | Anode mixture, positive pole and all-solid-state lithium-ion secondary battery and their manufacture method | |
| CN111834662B (en) | Interface functional layer, preparation method thereof and lithium ion battery | |
| CN109904514A (en) | Two-layer compound solid electrolyte and its preparation method and application | |
| CN112216874B (en) | Preparation process of all-solid-state battery | |
| JP7336692B2 (en) | Solid electrolyte and battery using the same | |
| CN107317009B (en) | Method for manufacturing sulfur-containing anode and method for manufacturing solid lithium battery comprising sulfur-containing anode | |
| CN107017387A (en) | It is a kind of for composite positive pole of solid lithium ion battery and preparation method thereof | |
| JP7286072B2 (en) | Polymer-Ceramic Composite Electrolyte Membrane | |
| CN113851609B (en) | Silicon-based negative electrode plate, preparation method thereof and all-solid-state lithium ion battery | |
| CN112652815B (en) | Low-internal-resistance all-solid-state battery and preparation method thereof | |
| CN115917819A (en) | Solid electrolyte composition, method for producing solid electrolyte sheet, and method for producing battery | |
| CN110957534A (en) | Solid electrolyte membrane, method for producing same, and solid battery | |
| CN110931852A (en) | Composite solid electrolyte, method for preparing same, and lithium secondary solid battery comprising same | |
| CN114512708A (en) | Preparation method and application of lithium ion composite solid electrolyte | |
| CN114050271A (en) | Positive active material with core-shell structure, preparation method thereof and all-solid-state lithium battery containing positive active material | |
| Qi et al. | A Review on Engineering Design for Enhancing Interfacial Contact in Solid-State Lithium–Sulfur Batteries | |
| Li et al. | Lithiophilic interface guided transient infiltration of molten lithium for stable 3D composite lithium anodes | |
| CN110676515B (en) | Preparation method of low-temperature high-energy-density lithium ion battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |