CN111106380A - A kind of preparation method of solid electrolyte with surface coating and solid electrolyte battery - Google Patents
A kind of preparation method of solid electrolyte with surface coating and solid electrolyte battery Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
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Abstract
The invention discloses a preparation method of a solid electrolyte with a surface coating, which comprises the steps of preparing a LLZO ceramic chip, preparing FS glue, forming the solid electrolyte and the like. Also provided is a solid electrolyte battery comprising the solid electrolyte prepared by the above method for preparing a solid electrolyte with a surface coating, and further comprising a positive electrode layer and a negative electrode layer disposed on both sides of the solid electrolyte. The solid electrolyte prepared by the method has the following advantages: firstly, the cubic phase structure of the LLZO is stabilized by doping the inorganic ceramic material with Ga and Nb elements, and the ionic conductivity is correspondingly improved. Secondly, the interface contact problem is effectively solved by coating the mixed fumed silica in the lithium ion electrolyte on two sides of the inorganic solid electrolyte, and the lithium ion conductivity of the electrolyte is ensured. The solid electrolyte of the solid electrolyte battery is prepared by the preparation method of the solid electrolyte with the surface coating, and has the advantages of small interface impedance, high lithium ion conductivity and the like.
Description
Technical Field
The invention relates to the field of solid electrolyte batteries, in particular to a preparation method of a solid electrolyte with a surface coating and a solid electrolyte battery.
Background
Among all energy conversion and storage systems, batteries are one of the most convenient devices for efficient energy utilization. With the development of lithium ion battery technology, lithium ion batteries have been widely used in the fields of 3C products, electric vehicles, and the like. At present, the lithium ion battery has the defects of low energy density, poor safety, short service life and the like.
When the negative electrode of the battery is changed to the metallic lithium, the metallic lithium has the lowest electrochemical potential (-3.04V) and the g is as high as 3861mAh-1The energy density of the battery can be greatly improved according to the specific capacity of the battery, but the battery also has the problem of lithium dendrite, which brings the risk of short circuit. Also, lithium metal has a large interfacial resistance when it comes into contact with an inorganic ceramic solid electrolyte. At the same time, the interface resistance between the cathode material and the inorganic ceramic solid electrolyte is also very large.
The ion conductivity of the tetragonal structure LLZO is much less than that of the cubic structure LLZO. In the cooling process of the LLZO without any element doping after high-temperature sintering, the cubic phase formed at high temperature is easy to recover to the tetragonal phase, so that the requirement of high lithium ion conductivity is not met.
Disclosure of Invention
In view of the above problems, the present invention provides a method for preparing a solid electrolyte with a surface coating, which aims to improve the interfacial resistance on the basis of increasing the lithium ion conductivity of the solid electrolyte, and provides a choice for commercializing the solid electrolyte, and also provides a solid electrolyte battery with low interfacial resistance and high lithium ion conductivity, and at least can solve one of the above problems.
According to one aspect of the present invention, there is provided a method of preparing a solid electrolyte having a surface coating, comprising the steps of:
s1, preparing the LLZO ceramic chip: according to a certain proportionRaw material Li was weighed in proportion2CO3、La2O3、ZrO2、Nb2O5And Ga2O3Mixing and carrying out first ball milling; tabletting the ball-milled precursor, performing primary sintering, crushing and sieving the ceramic chip subjected to primary sintering, performing secondary ball milling, tabletting the material subjected to secondary ball milling, and performing secondary sintering to obtain the LLZO ceramic chip;
s2, preparation of FS glue: uniformly mixing the fumed silica and the lithium ion electrolyte according to a certain mass ratio to obtain FS glue;
s3, formation of solid electrolyte: and coating the FS glue on two sides of the LLZO ceramic chip or immersing the LLZO ceramic chip into the FS glue to obtain the solid electrolyte with the surface coating.
Thus, the present invention provides a method for preparing a solid electrolyte with a surface coating, the solid electrolyte prepared by the method has the following advantages: firstly, the cubic phase structure of the LLZO is stabilized by doping the inorganic ceramic material with Ga and Nb elements, and the ionic conductivity is correspondingly improved. Secondly, the interface contact problem is effectively solved by coating the mixed fumed silica in the lithium ion electrolyte on two sides of the inorganic solid electrolyte, and the lithium ion conductivity of the electrolyte is ensured.
In some embodiments, in step S1, the sintering temperature of the first sintering is 900 to 950 ℃.
In some embodiments, in step S1, the sintering temperature of the second sintering is 1100 to 1230 ℃.
In some embodiments, in step S1, the first ball milling is performed at a rotation speed of 200-300 rpm for 12-36 h. Therefore, the components can be uniformly mixed.
In some embodiments, in step S1, the rotation speed of the second ball milling is 200-300 rpm for 8-16 h. Therefore, the components can be uniformly mixed.
In some embodiments, in step S2, the ratio is a molar ratio according to the molecular formula of each raw material.
In some embodiments, in step S2, the mass ratio of the fumed silica to the lithium ion electrolyte is 2% to 20%.
In some embodiments, in step S2, the lithium ion electrolyte is EC/DEC ═ 1:1, 1.0mol/L LiPF6The electrolyte of (1).
In some embodiments, in step S2, the fumed silica is vacuum-dried at 100-200 ℃ for 24-36 h before use. Thereby, moisture in the fumed silica can be removed.
According to another aspect of the present invention, there is also provided a solid electrolyte battery comprising a solid electrolyte prepared by the above method for preparing a solid electrolyte having a surface coating layer, and further comprising a positive electrode layer and a negative electrode layer disposed on both sides of the solid electrolyte.
Therefore, the solid electrolyte of the solid electrolyte battery is prepared by the preparation method of the solid electrolyte with the surface coating, so that the solid electrolyte battery has the advantages of small interface impedance, high lithium ion conductivity and the like.
The invention has the beneficial effects that:
according to the invention, the fumed silica gel is coated on two sides of the inorganic ceramic electrolyte sheet or surrounds the periphery of the inorganic ceramic electrolyte sheet, so that the interface impedance is greatly improved, Ga and Nb elements are doped in the LLZO ceramic sheet to enable the LLZO ceramic sheet to be stabilized in a cubic phase structure with higher conductivity, and the total lithium ion conductivity of the solid electrolyte is ensured.
Drawings
FIG. 1 is an XRD spectrum of Ga, Nb doped LLZO of the present invention;
FIG. 2 is a schematic structural view of a solid electrolyte having a surface coating layer according to example 1;
FIG. 3 is an AC impedance spectrum of a conventional solid-state electrolyte without a surface coating;
FIG. 4 is an AC impedance spectrum of a solid electrolyte battery of the present invention having a surface coating (lithium iron phosphate for the positive electrode and lithium for the negative electrode);
fig. 5 is a schematic structural view of a solid electrolyte having a surface coating layer of example 2.
Detailed Description
The invention is described in further detail below with reference to the figures and the specific embodiments.
Example 1
The target product of the inorganic ceramic sheet of the present embodiment is Li6.35Ga0.15La3Zr1.8Nb0.2O12。
The method for producing a solid electrolyte having a surface coating layer of the present embodiment includes the steps of:
s1, preparing the LLZO ceramic chip: li is weighed separately according to the stoichiometric ratio of this formula (i.e. 6.35:3:1.8:0.2:0.15)2CO3、La2O3、ZrO2、Nb2O5And Ga2O3The number of moles can be selected according to the size of the ball milling tank (1L ball milling tank can ball mill 0.02-0.1 mol). Wherein Li2CO3The excess is 5-20%. 5 raw materials are poured into a ball milling tank, and then isopropanol and ball milling beads are added for carrying out primary ball milling. The rotation speed of the first ball milling is 200-300 rpm, and the time is 12-36 h. After the first ball milling is completed, the solvent is dried to obtain white powder (i.e. precursor). And pressing the powder into a tablet by using a tablet pressing die every 2-6 g, wherein the pressure is 8-15 MPa. Then the mixture is moved into an alumina crucible for primary calcination, and the calcination condition is 900-950 ℃ annealing for 8-16 h. The material after the first calcination was crushed in a mortar and sieved using a standard 100 mesh sieve, and the powder obtained in this step was called a master powder. And (5) transferring the mother powder into a ball milling tank, and adding ball milling beads for secondary ball milling. The rotation speed of the second ball milling is 200-300 rpm, and the time is 8-16 h.
And pressing the powder subjected to the secondary ball milling into slices with different shapes and sizes by using a tabletting mold according to the requirements of the shapes and sizes of the batteries. The pressure intensity is 8-15 MPa. 3-6 slices are preferred, a proper amount of mother powder is spread among the slices, and the slices are stacked together and moved into a magnesium oxide crucible for secondary calcination under the condition of annealing at 1100-1230 ℃ for 1-12 hours. Thus, the Ga and Nb doped LLZO ceramic sheet was completed, and the XRD pattern of the Ga and Nb doped LLZO ceramic sheet is shown in fig. 1.
S2, preparation of FS glue: before the FS is used, the FS is dried in vacuum for 24-36 hours at 100-200 ℃ to remove water. Lithium ion electrolyte (EC: DEC ═ 1:1, LiPF)61mol/L) and gas phase silica (FS) are mixed in a mortar according to the mass ratio of 5-30: 1, and are uniformly ground by a grinding rod for 15-30 min to obtain the FS glue.
S3, formation of solid electrolyte: the FS glue was evenly brushed on both sides of the LLZO ceramic sheet using a flat-head brush, and the solid electrolyte having a surface coating was prepared as shown in fig. 2.
According to another aspect of the present invention, there is also provided a solid electrolyte battery comprising a solid electrolyte prepared by the above method for preparing a solid electrolyte having a surface coating layer, and further comprising a positive electrode layer and a negative electrode layer disposed on both sides of the solid electrolyte.
The positive electrode layer of the present embodiment may be lithium iron phosphate (LiFePO)4LEP for short), the formation of the positive electrode layer can be realized by ball milling commercial lithium iron phosphate (LFP) to obtain nano-scale LFP, then dispersing the LFP into α -terpineol and ethyl cellulose solution to form flowing slurry, coating the prepared positive electrode slurry on one surface of the solid electrolyte, and drying to remove the dispersing agent to form the positive electrode layer.
The negative electrode layer of the present embodiment may be a metallic lithium sheet, and the formation of the negative electrode layer may be achieved by: and attaching a metal lithium sheet to the other surface of the solid electrolyte, heating to melt the metal lithium sheet, and pressurizing to tightly combine the metal lithium sheet in the molten state with the surface of the solid electrolyte.
The battery is assembled by the sequence of the negative electrode shell, the elastic sheet, the gasket, the negative electrode, the solid electrolyte and the positive electrode shell, and the battery structure of the solid electrolyte battery can be expressed as follows: LFP | | FS-LLZO-FS | | | Li (28 ℃).
As shown in fig. 3 and 4, in contrast, the solid-state electrolyte battery (LFP | | FS-LLZO-FS | | | Li) having the solid-state electrolyte with the surface coating layer has a greatly reduced interface resistance of the solid-state electrolyte battery of the present embodiment, compared to the conventional solid-state electrolyte battery (LFP | | LLZO | | Li).
Example 2
The steps of the method for preparing the solid electrolyte with the surface coating layer of the present example are substantially the same as those of example 1 except that: (1) in step S4 of the present embodiment, mixing of the lithium ion electrolyte and the fumed silica is performed in a beaker; (2) in step S5 of the present embodiment, the LLZO ceramic sheet obtained by the preparation method is immersed in the FS glue solution.
In the embodiment, a lithium ion electrolyte (EC: DEC 1:1, LiPF 61 mol/L) and FS are mixed in a beaker according to a mass ratio of 20-50: 1, and uniformly stirred by a magneton to form a transparent and slightly viscous liquid.
And soaking the obtained LLZO ceramic wafer in the solution for 1-10 min, and clamping to obtain the solid electrolyte with the FS glue layer, wherein the structure of the solid electrolyte with the surface coating is shown in figure 5.
The invention provides a preparation method of a solid electrolyte with a surface coating, wherein the solid electrolyte prepared by the method adopts garnet type Lithium Lanthanum Zirconium Oxide (LLZO) as a matrix, and Fumed Silica (FS) is dissolved in liquid lithium ion electrolyte to form FS glue as a modification layer of the LLZO. Wherein, LLZO adopts a binary doping strategy to stabilize the cubic phase and increase the density thereof, thereby improving the ionic conductivity thereof. FS glue is coated on two sides of the LLZO, so that the interface impedance of the LLZO is greatly reduced. The solid electrolyte effectively solves the interface problem of the inorganic ceramic solid electrolyte and has high lithium ion conductivity.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method of preparing a solid electrolyte having a surface coating, comprising the steps of:
s1, preparing the LLZO ceramic chip: weighing raw material Li according to a certain proportion2CO3、La2O3、ZrO2、Nb2O5And Ga2O3Mixing and carrying out first ball milling; tabletting the ball-milled precursor, performing primary sintering, crushing and sieving the ceramic chip subjected to primary sintering, performing secondary ball milling, tabletting the material subjected to secondary ball milling, and performing secondary sintering to obtain the LLZO ceramic chip;
s2, preparation of FS glue: uniformly mixing the fumed silica and the lithium ion electrolyte according to a certain mass ratio to obtain FS glue;
s3, formation of solid electrolyte: and coating the FS glue on two sides of the LLZO ceramic chip or immersing the LLZO ceramic chip into the FS glue to obtain the solid electrolyte with the surface coating.
2. The method for preparing a solid electrolyte with a surface coating according to claim 1, wherein in step S1, the sintering temperature of the first sintering is 900-950 ℃.
3. The method for preparing a solid electrolyte with a surface coating according to claim 1, wherein in step S1, the sintering temperature of the second sintering is 1100-1230 ℃.
4. The method for preparing the solid electrolyte with the surface coating according to claim 1, wherein in step S1, the rotation speed of the first ball milling is 200-300 rpm for 12-36 h.
5. The method for preparing the solid electrolyte with the surface coating according to claim 1, wherein in step S1, the rotation speed of the second ball milling is 200-300 rpm for 8-16 h.
6. The method of claim 1, wherein the ratio in step S2 is a molar ratio according to a molecular formula of each raw material.
7. The method for preparing a solid electrolyte with a surface coating according to claim 1, wherein in step S2, the mass ratio of the fumed silica to the lithium ion electrolyte is 2% to 20%.
8. The method of claim 1, wherein in step S2, the li-ion electrolyte solution is EC/DEC ═ 1:1, 1.0mol/L LiPF6The electrolyte of (1).
9. The method for preparing the solid electrolyte with the surface coating according to claim 1, wherein the fumed silica is dried in vacuum at 100-200 ℃ for 24-36 h before use in step S2.
10. A solid electrolyte battery comprising the solid electrolyte prepared by the method for preparing a solid electrolyte with a surface coating according to any one of claims 1 to 9, characterized by further comprising a positive electrode layer and a negative electrode layer disposed on both sides of the solid electrolyte.
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Cited By (3)
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| CN113991170A (en) * | 2021-10-15 | 2022-01-28 | 深圳大学 | All-solid-state battery |
| WO2025010699A1 (en) * | 2023-07-13 | 2025-01-16 | 广东邦普循环科技有限公司 | Solid electrolyte containing lithium iron phosphate coating layer and preparation method thereof |
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Effective date of registration: 20250324 Address after: No. 11-5-11, Section 2, Lingang Road, Jialing District, Nanchong City, Sichuan Province, 637901 Patentee after: Sichuan Zhihui New Energy Co.,Ltd. Country or region after: China Address before: 510000 Building 516, South China Normal University, Panyu District, Guangzhou City, Guangdong Province, China Patentee before: SOUTH CHINA NORMAL University Country or region before: China |