CN115810709A - Positive pole piece, preparation method and solid-state battery - Google Patents
Positive pole piece, preparation method and solid-state battery Download PDFInfo
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- CN115810709A CN115810709A CN202211621364.2A CN202211621364A CN115810709A CN 115810709 A CN115810709 A CN 115810709A CN 202211621364 A CN202211621364 A CN 202211621364A CN 115810709 A CN115810709 A CN 115810709A
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Abstract
The invention provides a positive pole piece, a preparation method and a solid-state battery, wherein the preparation method comprises the following steps: stirring a positive electrode active material, a solid electrolyte, a binder, a conductive agent, a lithium salt and an organic solvent to prepare slurry, wherein the ratio of the average particle size of the positive electrode active material to the average particle size of the solid electrolyte is A, and A is more than or equal to 4 and less than or equal to 140; coating the slurry on an aluminum foil to prepare an electrode material pole piece, and drying the electrode material pole piece, wherein the drying temperature is higher than the melting point of lithium salt and lower than the decomposition temperature of the lithium salt; and heating and rolling the cooled electrode material pole piece to form a positive pole piece, wherein the hot pressing temperature is higher than the melting point of the lithium salt and lower than the decomposition temperature of the lithium salt. The lithium salt is melted into fluid in the drying and heating rolling processes and dispersed in gaps among various component particles, so that the contact area between solids is increased, and the molten lithium salt can repair small-particle solid electrolyte with defects.
Description
Technical Field
The invention relates to the technical field of solid-state batteries, in particular to a positive pole piece, a preparation method and a solid-state battery.
Background
The solid-state battery adopts non-flammable solid-state battery electrolyte to replace flammable organic liquid electrolyte, so that the safety of a battery system is greatly improved, the high-energy anode and cathode can be better adapted, the weight of the system is reduced, and the synchronous improvement of energy density is realized. The solid electrolyte is a solid-phase material, and compared with a liquid electrolyte, the wettability of the solid electrolyte is very poor, and because solid electrolyte particles cannot be in close contact with positive active material particles, lithium ions diffused through a contact surface are short of sufficient diffusion channels.
In order to alleviate the above problems, a method of reducing the particle size of solid electrolyte particles is currently adopted to increase the contact area between the solid electrolyte and the positive electrode active material particles, but in the process of reducing the particle size of the solid electrolyte, the solid electrolyte particles have defects such as "fracture", "crack", and the like, which cause the ionic conductivity of the solid electrolyte itself to be reduced, and the diffusion efficiency of lithium ions in the solid electrolyte is greatly reduced, which finally affects the electrochemical performance of the solid battery.
In view of the above problems, no effective solution has been proposed.
Disclosure of Invention
The invention mainly aims to provide a positive pole piece, a preparation method and a solid-state battery, and aims to solve the technical problem of increasing the contact surface between solid electrolyte particles and positive active material particles.
In order to achieve the above object, according to an aspect of the present invention, there is provided a method for manufacturing a positive electrode sheet, the method comprising the steps of: step S1: stirring a positive electrode active material, a solid electrolyte, a binder, a conductive agent, a lithium salt and an organic solvent to prepare slurry, wherein the ratio of the average particle size of the positive electrode active material to the average particle size of the solid electrolyte is A, and A is more than or equal to 4 and less than or equal to 140; step S2: coating the slurry on an aluminum foil to prepare an electrode material pole piece, and drying the electrode material pole piece, wherein the drying temperature is higher than the melting point of lithium salt and lower than the decomposition temperature of the lithium salt; and step S3: and heating and rolling the cooled electrode material pole piece to form the positive pole piece, wherein the hot pressing temperature is higher than the melting point of the lithium salt and lower than the decomposition temperature of the lithium salt.
Further, the dew point temperature of the environment in which step S1 is located is less than-40 ℃.
Further, the dew point temperature of the environment in which step S2 is located is less than-40 ℃.
Furthermore, when the electrode material pole piece is dried, nitrogen is filled into the environment where the electrode material pole piece is located.
Further, the lithium salt is lithium bis (fluorosulfonyl) imide.
Further, the solid electrolyte is a sulfide.
Further, in step S1, the mass ratio of the solid electrolyte to all the raw materials is B, the mass ratio of the lithium salt to all the raw materials is C, wherein B is more than or equal to 70% and less than or equal to 95%, and C is more than or equal to 0.1% and less than or equal to 1%.
Further, the average particle diameter of the solid electrolyte is D1, wherein D1 is more than or equal to 1.5 mu m and less than or equal to 2.5 mu m.
According to another aspect of the invention, the invention provides a positive pole piece, and the positive pole piece is prepared by the preparation method of the positive pole piece.
According to another aspect of the invention, a solid-state battery is provided, which comprises a positive pole piece, wherein the positive pole piece is prepared by the preparation method of the positive pole piece.
By applying the technical scheme of the invention, the ratio of the average particle size of the anode active material to the average particle size of the solid electrolyte is A, A is more than or equal to 4 and less than or equal to 140, namely the anode active material and the solid electrolyte material adopt a preparation method with matched sizes, the contact area of the anode active material and the solid electrolyte is increased, and thus the diffusion path of lithium ions is increased. When the pole piece of the pole material is dried, the drying temperature is higher than the melting point of the lithium salt and lower than the decomposition temperature of the lithium salt, so that the lithium salt is melted into fluid in the drying and heating rolling processes and is dispersed in gaps among various component particles, the contact area between the solid and the solid is increased, and the diffusion path of lithium ions is supplemented. Meanwhile, the molten lithium salt can repair the defective small-particle solid electrolyte, so that the ionic conductivity of the solid electrolyte is improved, and the electrochemical performance of the solid battery is further improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic flow chart of an embodiment of a method for preparing a positive electrode sheet according to the present invention;
fig. 2 shows a schematic composition diagram of the positive electrode sheet.
Detailed Description
It should be noted that, in the present application, the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the accompanying drawings are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those illustrated or otherwise described herein. Moreover, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
Exemplary embodiments according to the present application will now be described in more detail with reference to the accompanying drawings. These exemplary embodiments may, however, be embodied in many different forms and should not be construed as limited to only the embodiments set forth herein. It is to be understood that these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the exemplary embodiments to those skilled in the art, in the drawings, it is possible to enlarge the thicknesses of layers and regions for clarity, and the same devices are denoted by the same reference numerals, and thus the description thereof will be omitted.
Referring to fig. 1 to 2, according to an embodiment of the present application, a method for manufacturing a positive electrode sheet is provided.
Specifically, as shown in fig. 1, the preparation method of the positive electrode sheet includes the following steps:
step S1: stirring a positive electrode active material, a solid electrolyte, a binder, a conductive agent, a lithium salt and an organic solvent to prepare slurry, wherein the ratio of the average particle size of the positive electrode active material to the average particle size of the solid electrolyte is A, and A is more than or equal to 4 and less than or equal to 140. Wherein, preferably, 1.5. Ltoreq. A.ltoreq.10. The components are mixed at one time, so that the preparation time is shortened.
In step S1, the raw materials such as the positive electrode active material, the solid electrolyte, the binder, the conductive agent, and the lithium salt need to be weighed in a predetermined ratio before the stirring. Wherein the mass ratio of the solid electrolyte to all the raw materials is B, the mass ratio of the lithium salt to all the raw materials is C, wherein B is more than or equal to 70% and less than or equal to 95%, and C is more than or equal to 0.1% and less than or equal to 1%.
The positive active material is any one or more of a lithium cobaltate material, a lithium iron phosphate material, a lithium manganate material, a lithium iron manganese phosphate material and a lithium-rich manganese material.
The solid electrolyte may be a sulfide, an oxide, a polymer, a halide, or the like, and in this embodiment, the solid electrolyte is a sulfide, such as a binary sulfide (Li) 2 S-P 2 S 5 ，Li 2 S-SiS 2 ，Li 2 S-GeS 2 ，Li 2 S-B 2 S 3 ) And ternary sulfides (Li) 2 S-MeS 2 -P, li-P-S-Cl, li-P-S-Br, li-P-S), etc., further, the solid electrolyte is Li 6 PS 5 Cl, the conductivity of sulfides is higher than oxides, polymers, and halides. The solid electrolyte has an average particle diameter D1, wherein D1 is 0.1 μm. Ltoreq.D 1. Ltoreq.10 μm, preferably 1.5 μm. Ltoreq.D 1. Ltoreq.2.5. Mu.m.
The lithium salt is difluoride sulfonyl imide lithium salt (LiTFSI), the melting point temperature of the difluoride sulfonyl imide lithium salt is [124 ℃,128 ℃), the decomposition temperature of the difluoride sulfonyl imide lithium salt is greater than 200 ℃, namely the melting point temperature of the difluoride sulfonyl imide lithium salt is lower, the difference between the melting point temperature of the difluoride sulfonyl imide lithium salt and the decomposition temperature of the difluoride sulfonyl imide lithium salt is larger, in the step S2 and the step S3, the drying temperature and the hot pressing temperature are easy to control, high temperature is not needed, the cooling time is shortened, and the preparation time of the whole preparation process is further shortened.
Wherein the organic solvent can be one or more of n-butane, n-pentane, isopentane, n-hexane, n-heptane, isooctane, cyclopentane, cyclohexane, methylcyclopentane, methylcyclohexane, decalin, bicyclononane, tricyclodecane, benzene, toluene and xylene.
Step S2: and coating the slurry on an aluminum foil to prepare an electrode material pole piece, and drying the electrode material pole piece, wherein the drying temperature is higher than the melting point of the lithium salt and lower than the decomposition temperature of the lithium salt.
It is noted that the drying temperature is T1, T1 is more than or equal to 80 ℃ and less than or equal to 180 ℃, and preferably the drying temperature is 150 ℃. The drying time is t, and t is more than or equal to 1h and less than or equal to 24h. The lithium salt is melted under the influence of drying temperature, and is dispersed in gaps among particles of various components in the pole piece mixture, and meanwhile, the melted lithium salt further compensates and repairs small-particle solid electrolyte with certain defects.
And step S3: and heating and rolling the cooled electrode material pole piece to form the positive pole piece, wherein the hot pressing temperature is higher than the melting point of the lithium salt and lower than the decomposition temperature of the lithium salt.
It is noted that the hot pressing temperature is T2, T2 is more than 120 ℃ and less than 180 ℃, and preferably, the hot pressing temperature is 160 ℃. In the rolling process, the thickness of the pole piece is reduced, and the molten lithium salt is further dispersed in gaps among the components of the pole piece, so that the density of the pole piece is improved.
In the process from the step S1 to the step S2, the ratio of the average particle size of the positive electrode active material to the average particle size of the solid electrolyte is A, and A is more than or equal to 4 and less than or equal to 140, namely the positive electrode active material and the solid electrolyte material adopt a preparation method with matched sizes, so that the contact area of the positive electrode active material and the solid electrolyte is increased, and the diffusion path of lithium ions is increased. When the pole piece of the pole material is dried, the drying temperature is higher than the melting point of the lithium salt and lower than the decomposition temperature of the lithium salt, so that the lithium salt is melted into fluid in the drying and heating rolling processes and is dispersed in gaps among various component particles, the contact area between the solid and the solid is increased, and the diffusion path of lithium ions is supplemented. Meanwhile, the molten lithium salt can repair the defective small-particle solid electrolyte, so that the ionic conductivity of the solid electrolyte is improved, and the electrochemical performance of the solid battery is further improved.
The dew point temperature of the environment in which the step S1 is positioned is less than minus 40 ℃, namely, the step S1 is carried out in a dry environment, so that the sulfide in the mixture is prevented from generating chemical reaction with the moisture in the air.
The dew point temperature of the environment in which the step S2 is positioned is less than minus 40 ℃, namely the step S1 is carried out in a dry environment, and the sulfide in the mixture is prevented from generating chemical reaction with the moisture in the air.
In the step S2, when the electrode material pole piece is dried, nitrogen is filled into the environment where the electrode material pole piece is located. In the drying process, nitrogen is used as protective gas, so that chemical reaction between sulfides in the electrode material pole piece and water vapor is avoided.
The preparation method of the positive electrode plate is further described by the following specific examples and comparative examples:
example 1
Step S10: 78g of LiNi, a positive electrode active material, was weighed 0.8 Co 0.1 Mn 0.1 O 2 18g of a solid electrolyte material Li having an average particle diameter of 2.5 μm 6 PS 5 Cl,2g of SBS (styrene-butadiene-styrene block copolymer) binder material, 1.5g of VGCF (vapor grown carbon fiber) conductive material, and 0.5g of lithium salt LiFSI (lithium bis-fluorosulfonylimide).
Step S20: the weighed raw materials were put into 80ml of xylene solvent and mixed with stirring. Specifically, under the environment that the dew point temperature is less than minus 40 ℃, the positive electrode slurry is obtained after the stirrer continuously stirs for 5 hours at a uniform speed of 300 rpm.
Step S30: and uniformly coating the slurry on an aluminum foil current collector, and drying in an oven at 150 ℃ for 12 hours. The dew point temperature of the environment where the pole piece is located is kept to be less than-40 ℃ in the drying process, or nitrogen is filled in the environment for protection. And after the organic solvent in the pole piece is completely evaporated, cooling the pole piece to room temperature and taking out the pole piece from the oven.
Step S40: and (3) putting the dried pole piece into a roller press with a heating function for rolling, wherein the heating temperature is 160 ℃.
The preparation conditions in the examples and comparative examples are shown in table 1:
TABLE 1
Examples 2 to 10
The synthesis conditions were the same as in example 1, except that the average particle size of the solid electrolyte material was different, the added weight of the LiFSI material was different, the drying temperature and drying time of the electrode sheet were different, and the hot-pressing temperature of the electrode sheet was different.
Comparative examples 1 to 3
The synthesis conditions were the same as in example 1, except that no LiFSI material was added, the drying temperature and drying time of the electrode sheet were different, and the hot-pressing temperature of the electrode sheet was different.
Performance detection
1. Simulated battery assembly
Mixing the positive pole piece and Li 6 PS 5 And assembling the Cl electrode layer and the Li-In alloy negative electrode into the all-solid-state secondary battery.
2. Interface impedance, charge and discharge capacity and rate capability test
And putting the assembled all-solid-state secondary battery into a pressurizing outer sleeve capable of maintaining pressure, and carrying out battery impedance test at the pressure of 300Mpa and the test frequency of 3.5MHz-0.1Hz. And then the all-solid-state secondary battery is subjected to a charge-discharge test by adopting a current density of 20mA/g, and the cut-off voltage is 1.9-3.7V. After one-time charge and discharge cycle, the current density is increased to 200mA/g for carrying out a multiplying power performance test, and the ratio of the specific discharge capacity obtained under the condition of 200mA/g to the specific discharge capacity obtained under the condition of 20mA/g is the multiplying power capacity retention rate.
The test results are shown in table 2:
TABLE 2
According to the test results shown in table 2, it can be seen that the positive electrode sheet obtained by the preparation method of the present invention has low interface impedance, and excellent charge and discharge capacity and rate capability.
Example 11
According to another specific embodiment of the invention, a positive pole piece is provided, and the positive pole piece is prepared by the preparation method of the positive pole piece in the embodiment.
Example 12
According to another specific embodiment of the present invention, a solid-state battery is provided, which includes a positive electrode plate, and the positive electrode plate is prepared by the preparation method of the positive electrode plate in the foregoing embodiment.
For ease of description, spatially relative terms such as "over 8230," "upper surface," "above," and the like may be used herein to describe the spatial positional relationship of one device or feature to other devices or features as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary terms "at 8230; \8230; above" may include both orientations "at 8230; \8230; above" and "at 8230; \8230; below". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
In addition to the foregoing, it should be appreciated that reference throughout this specification to "one embodiment," "another embodiment," "an embodiment," or the like, means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment described generally in this application. The appearances of the same phrase in various places in the specification are not necessarily all referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the scope of the invention to effect such feature, structure, or characteristic in connection with other embodiments.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a positive pole piece is characterized by comprising the following steps:
step S1: stirring a positive electrode active material, a solid electrolyte, a binder, a conductive agent, a lithium salt and an organic solvent to prepare slurry, wherein the ratio of the average particle size of the positive electrode active material to the average particle size of the solid electrolyte is A, and A is more than or equal to 4 and less than or equal to 140;
step S2: coating the slurry on an aluminum foil to prepare an electrode material pole piece, and drying the electrode material pole piece, wherein the drying temperature is higher than the melting point of the lithium salt and lower than the decomposition temperature of the lithium salt;
and step S3: and heating and rolling the cooled electrode material pole piece to form a positive pole piece, wherein the hot pressing temperature is higher than the melting point of the lithium salt and lower than the decomposition temperature of the lithium salt.
2. The method for preparing the positive pole piece according to claim 1, wherein the dew point temperature of the environment in which the step S1 is performed is less than-40 ℃.
3. The method for preparing the positive electrode plate according to claim 1, wherein the dew point temperature of the environment in which the step S2 is performed is less than-40 ℃.
4. The method for preparing the positive electrode plate according to claim 1, wherein nitrogen is filled into an environment where the electrode material plate is located when the electrode material plate is dried.
5. The method for preparing the positive electrode plate according to claim 1, wherein the lithium salt is a lithium bis-fluorosulfonylimide.
6. The method for manufacturing a positive electrode sheet according to claim 1, wherein the solid electrolyte is a sulfide.
7. The method for preparing the positive electrode sheet according to claim 1, wherein in the step S1, the mass ratio of the solid electrolyte to all the raw materials is B, and the mass ratio of the lithium salt to all the raw materials is C, wherein B is 70% to 95%, and C is 0.1% to 1%.
8. The method for preparing the positive electrode plate according to claim 1, wherein the solid electrolyte has an average particle size of D1, wherein D1 is greater than or equal to 1.5 μm and less than or equal to 2.5 μm.
9. A positive pole piece, which is characterized in that the positive pole piece is prepared by the preparation method of the positive pole piece according to any one of claims 1 to 8.
10. A solid-state battery comprises a positive pole piece, and is characterized in that the positive pole piece is prepared by the preparation method of the positive pole piece in any one of claims 1 to 8.
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| CN118040074A (en) * | 2024-04-11 | 2024-05-14 | 蜂巢能源科技股份有限公司 | Semi-solid lithium ion battery and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118040074A (en) * | 2024-04-11 | 2024-05-14 | 蜂巢能源科技股份有限公司 | Semi-solid lithium ion battery and preparation method thereof |
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