CN115636397A - Method for preparing sulfide electrolyte, sulfide electrolyte and application thereof - Google Patents
Method for preparing sulfide electrolyte, sulfide electrolyte and application thereof Download PDFInfo
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- CN115636397A CN115636397A CN202211271442.0A CN202211271442A CN115636397A CN 115636397 A CN115636397 A CN 115636397A CN 202211271442 A CN202211271442 A CN 202211271442A CN 115636397 A CN115636397 A CN 115636397A
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 55
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 29
- AYRZLUSHOXJGKY-UHFFFAOYSA-N [bis(sulfanylidene)-$l^{5}-arsanyl]sulfanyl-bis(sulfanylidene)-$l^{5}-arsane Chemical compound S=[As](=S)S[As](=S)=S AYRZLUSHOXJGKY-UHFFFAOYSA-N 0.000 claims abstract description 18
- CYQAYERJWZKYML-UHFFFAOYSA-N phosphorus pentasulfide Chemical compound S1P(S2)(=S)SP3(=S)SP1(=S)SP2(=S)S3 CYQAYERJWZKYML-UHFFFAOYSA-N 0.000 claims abstract description 18
- YIZVROFXIVWAAZ-UHFFFAOYSA-N germanium disulfide Chemical compound S=[Ge]=S YIZVROFXIVWAAZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007784 solid electrolyte Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 150000001875 compounds Chemical class 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 4
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011244 liquid electrolyte Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 101100468589 Arabidopsis thaliana RH30 gene Proteins 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the field of solid electrolytes, and discloses a method for preparing a sulfide electrolyte, the sulfide electrolyte and application thereof. The method comprises the following steps: (1) Mixing lithium sulfide, germanium disulfide, phosphorus pentasulfide and arsenic pentasulfide, and then grinding to obtain a mixture I; (2) Tabletting and molding the mixture I, and then heating to obtain the sulfide electrolyte; wherein the molar ratio of the phosphorus pentasulfide to the arsenic pentasulfide is 1-X: x is more than or equal to 0.01 and less than or equal to 0.5; based on the total molar usage of the phosphorus pentasulfide and the arsenic pentasulfide, the usage of the lithium sulfide is 300-700mol%, and the usage of the germanium disulfide is 60-170mol%. The sulfide electrolyte prepared by the method provided by the invention has high stability in air, high ionic conductivity, wide application prospect and commercial value.
Description
Technical Field
The invention relates to the field of solid electrolytes, in particular to a method for preparing a sulfide electrolyte, the sulfide electrolyte and application thereof.
Background
With the development of new energy electric vehicles, people have higher and higher requirements on energy density and safety of batteries, the traditional liquid batteries are difficult to meet the energy requirements of the new energy electric vehicles, and the safety cannot be guaranteed, so that the development of solid batteries is an inevitable trend.
Sulfide electrolytes have ion conductivity comparable to liquid electrolytes, but their safety is difficult to achieve with liquid electrolytes. Sulfide electrolytes have been a research hotspot of researchers due to their high ionic conductivity and safety.
However, the sulfide electrolyte is easily reacted with moisture in the air to generate H when exposed to the air 2 S，H 2 S is extremely toxic and produces H 2 The S process causes structural collapse of the electrolyte, resulting in a sharp drop in its ionic conductivity.
Therefore, it is of great significance to synthesize a sulfide electrolyte having excellent stability in air.
Disclosure of Invention
The object of the present invention is to provide a sulfide electrolyte having excellent stability in air and at the same time having a higher ionic conductivity.
In order to achieve the above object, a first aspect of the present invention provides a method for producing a sulfide electrolyte, the method comprising:
(1) Mixing lithium sulfide, germanium disulfide, phosphorus pentasulfide and arsenic pentasulfide, and then grinding to obtain a mixture I;
(2) Tabletting and forming the mixture I, and then heating under a protective atmosphere to obtain the sulfide electrolyte;
wherein the molar ratio of the phosphorus pentasulfide to the arsenic pentasulfide is 1-X: x is more than or equal to 0.01 and less than or equal to 0.5;
based on the total molar usage of the phosphorus pentasulfide and the arsenic pentasulfide, the usage of the lithium sulfide is 300-700mol%, and the usage of the germanium disulfide is 60-170mol%.
Preferably, in step (1), the mixing conditions at least satisfy: the stirring is carried out under the stirring condition, the rotating speed of the stirring is 300-350rpm, and the time is 20-80min.
Preferably, in step (1), the mixture I has an average particle diameter of 4 to 8 μm.
Preferably, in step (1), the conditions of the grinding treatment at least satisfy: the process is carried out in a ball mill, the rotating speed of the ball mill is 200-600rpm, and the time is 2-16h.
Preferably, in the step (2), the conditions for tablet forming at least satisfy: the pressure is 100-300MPa, the temperature is 20-30 ℃, and the time is 1-3min.
Preferably, in the step (2), the conditions of the heat treatment at least satisfy: the initial temperature is 20-30 ℃, the heating rate is 1-5 ℃/min, the termination temperature is 400-700 ℃, and the constant temperature time is 2-6h.
Preferably, the method further comprises: and carrying out temperature reduction treatment after the heating treatment to obtain the sulfide electrolyte.
Preferably, the condition of the temperature reduction treatment at least satisfies the following conditions: the initial temperature is 400-700 ℃, the cooling rate is 0.5-5 ℃/min, and the termination temperature is 30-80 ℃.
A second aspect of the invention provides a sulfide electrolyte produced by the method described in the first aspect.
A third aspect of the invention provides a use of the sulfide electrolyte described in the second aspect in a battery.
Compared with the prior art, the invention has at least the following advantages:
the method for preparing the sulfide electrolyte can synthesize the sulfide electrolyte in an atmosphere without filling inert gas, thereby simplifying the synthesis process of the sulfide electrolyte, reducing the synthesis cost and being beneficial to promoting the industrialization process.
The sulfide electrolyte prepared by the method provided by the invention has high stability in air, high ionic conductivity and wide application prospect.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
As previously described, a first aspect of the present invention provides a method of producing a sulfide electrolyte, the method comprising:
(1) Mixing lithium sulfide, germanium disulfide, phosphorus pentasulfide and arsenic pentasulfide, and then grinding to obtain a mixture I;
(2) Performing tabletting molding on the mixture I, and then performing heating treatment in a protective atmosphere to obtain the sulfide electrolyte;
wherein the molar ratio of the phosphorus pentasulfide to the arsenic pentasulfide is 1-X: x is more than or equal to 0.01 and less than or equal to 0.5;
based on the total molar usage of the phosphorus pentasulfide and the arsenic pentasulfide, the usage of the lithium sulfide is 300-700mol%, and the usage of the germanium disulfide is 60-170mol%.
Preferably, in step (1), the mixing conditions at least satisfy: the stirring is carried out under the stirring condition, the rotating speed of the stirring is 300-350rpm, and the time is 20-80min.
Preferably, in step (1), the mixture I has an average particle diameter of 4 to 8 μm.
In the present invention, the conditions of the grinding treatment are not particularly limited, and those skilled in the art can select the grinding treatment by combining the means known in the art, as long as the average particle size of the mixture I is 4 to 8 μm. However, in order to obtain a sulfide electrolyte with a lower amount of hydrogen sulfide gas generation, the present invention provides a preferred embodiment in which, in step (1), the conditions of the polishing treatment at least satisfy: the process is carried out in a ball mill, the rotating speed of the ball mill is 200-600rpm, and the time is 2-16h.
In the present invention, the kind of the ball mill is not particularly limited, and those skilled in the art can select the ball mill by combining technical means known in the art. Illustratively, the equipment for the milling process may be a high energy ball mill or the like.
Preferably, in the step (2), the conditions for tablet forming at least satisfy: the pressure is 100-300MPa, the temperature is 20-30 ℃, and the time is 1-3min.
It should be noted that the type of the tablet forming apparatus of the present invention is not particularly limited, and those skilled in the art can select the tablet forming apparatus by combining the technical means known in the art. Illustratively, the sheeting forming apparatus may be a YLJ-CIP-15 compact cold isostatic press or the like.
Preferably, in the step (2), the conditions of the heat treatment at least satisfy: the initial temperature is 20-30 deg.C, the heating rate is 1-5 deg.C/min, the final temperature is 400-700 deg.C, and the constant temperature time is 2-6h.
According to a preferred embodiment, the method further comprises: and carrying out temperature reduction treatment after the heating treatment to obtain the sulfide electrolyte.
Preferably, the condition of the temperature reduction treatment at least satisfies the following conditions: the initial temperature is 400-700 ℃, the cooling rate is 0.5-5 ℃/min, and the termination temperature is 30-80 ℃.
As mentioned previously, a second aspect of the present invention provides a sulfide electrolyte produced by the method described in the preceding first aspect.
As mentioned above, the third aspect of the present invention provides a use of the sulfide electrolyte described in the foregoing second aspect in a battery.
The present invention will be described in detail below by way of examples.
In the following examples, the room temperature means 25 ± 2 ℃ unless otherwise specified.
Example 1
(1) Stirring lithium sulfide (30 mmol), germanium disulfide (6 mmol), phosphorus pentasulfide (5.94 mmol) and arsenic pentasulfide (0.06 mmol) with average particle size of 10 mu m at the rotating speed of 320rpm for 20min, and adding into a high-energy ball mill for grinding treatment to obtain a mixture I with average particle size of 8 mu m;
wherein the rotating speed of the ball mill is 200rpm, and the time is 15h;
(2) Then putting the mixture I into a tablet press (model YLJ-CIP-15, manufacturer Shenzhenace crystal), and pressing the mixture I into a wafer with the diameter of 20mm at the pressure of 100 MPa; then placing the obtained wafer in a vacuum quartz tube, raising the temperature from room temperature to 560 ℃ at a constant speed within 3h, and preserving the heat for 6h at the temperature;
then the temperature is reduced to 30 ℃ at a constant speed within 3h to obtain the chemical formula of Li 10 Ge(P 0.99 As 0.01 ) 2 S 12 Sulfide electrolyte L1 of (1).
Example 2
(1) Stirring lithium sulfide (30 mmol), germanium disulfide (6 mmol), phosphorus pentasulfide (5.88 mmol) and arsenic pentasulfide (0.12 mmol) with average particle size of 10 mu m at the rotating speed of 320rpm for 30min, and adding into a high-energy ball mill for grinding treatment to obtain a mixture I with average particle size of 6 mu m;
wherein the rotating speed of the ball mill is 300rpm, and the time is 15h;
(2) Then putting the mixture I into a tablet press, and pressing the mixture I into a circular sheet with the diameter of 20mm at the pressure of 100 MPa; then placing the obtained wafer in a vacuum quartz tube, raising the temperature from room temperature to 560 ℃ at a constant speed within 3h, and preserving the heat for 6h at the temperature;
then the temperature is reduced to 40 ℃ at a constant speed within 3h to obtain the compound with the chemical formula of Li 10 Ge(P 0.98 As 0.02 ) 2 S 12 Sulfide electrolyte L2.
Example 3
(1) Stirring lithium sulfide (30 mmol), germanium disulfide (6 mmol), phosphorus pentasulfide (5.82 mmol) and arsenic pentasulfide (0.18 mmol) with average particle size of 10 mu m at the rotating speed of 320rpm for 60min, and adding into a high-energy ball mill for grinding treatment to obtain a mixture I with average particle size of 4 mu m;
wherein the rotating speed of the ball mill is 400rpm, and the time is 15h;
(2) Then putting the mixture I into a tablet press, and pressing the mixture I into a circular sheet with the diameter of 20mm at the pressure of 100 MPa; then placing the obtained wafer in a vacuum quartz tube, raising the temperature from room temperature to 560 ℃ at a constant speed within 3h, and preserving the heat for 6h at the temperature;
then the temperature is reduced to 50 ℃ at a constant speed within 3h to obtain the compound with the chemical formula of Li 10 Ge(P 0.97 As 0.03 ) 2 S 12 Sulfide electrolyte L3 of (1).
Example 4
(1) Stirring lithium sulfide (30 mmol), germanium disulfide (6 mmol), phosphorus pentasulfide (5.70 mmol) and arsenic pentasulfide (0.30 mmol) with average particle sizes of 10 mu m at the rotating speed of 320rpm for 70min, and then adding into a high-energy ball mill for grinding treatment to obtain a mixture I with the average particle size of 4 mu m;
wherein the rotation speed of the ball mill is 400rpm, and the time is 15h;
(2) Then putting the mixture I into a tablet press, and pressing the mixture I into a circular sheet with the diameter of 20mm at the pressure of 100 MPa; then placing the obtained wafer in a vacuum quartz tube, raising the temperature from room temperature to 560 ℃ at a constant speed within 3h, and preserving the heat for 6h at the temperature;
then the temperature is reduced to 50 ℃ at a constant speed within 3h to obtain the chemical formula of Li 10 Ge(P 0.95 As 0.05 ) 2 S 12 Sulfide electrolyte L4 of (1).
Example 5
(1) Stirring lithium sulfide (30 mmol), germanium disulfide (6 mmol), phosphorus pentasulfide (5.52 mmol) and arsenic pentasulfide (0.48 mmol) with average particle size of 10 mu m at the rotating speed of 320rpm for 80min, and adding into a high-energy ball mill for grinding treatment to obtain a mixture I with average particle size of 4 mu m;
wherein the rotation speed of the ball mill is 400rpm, and the time is 15h;
(2) Then putting the mixture I into a tablet press, and pressing the mixture I into a circular sheet with the diameter of 20mm at the pressure of 100 MPa; then placing the obtained wafer in a vacuum quartz tube, raising the temperature from room temperature to 560 ℃ at a constant speed within 3h, and preserving the heat for 6h at the temperature;
then the temperature is reduced at a constant speed within 3hTo 50 ℃ to obtain a compound of formula Li 10 Ge(P 0.92 As 0.08 ) 2 S 12 Sulfide electrolyte L5.
Example 6
This example was carried out in a similar manner to example 3, except that: the rotation speed of the ball mill was 600rpm for 10 hours to obtain a mixture I having an average particle diameter of 3 μm, and the remaining conditions were the same as in example 3 to prepare a mixture I having a chemical formula of Li 10 Ge(P 0.97 As 0.03 ) 2 S 12 Sulfide electrolyte L6.
Comparative example 1
This comparative example was carried out in a similar manner to example 3, except that:
the amount of lithium sulfide was 10mmol, and the other conditions were the same as in example 3, to prepare a compound of formula Li 10 Ge(P 0.97 As 0.03 ) 2 S 12 The sulfide electrolyte DL1.
Comparative example 2
This comparative example was carried out in a similar manner to example 3, except that:
the amount of germanium disulfide was 15mmol, and the other conditions were the same as in example 3, to prepare a compound of formula Li 10 Ge(P 0.97 As 0.03 ) 2 S 12 The sulfide electrolyte DL2.
Comparative example 3
This comparative example was carried out in a similar manner to example 3, except that:
phosphorus pentasulfide was used in an amount of 6.06mmol, and the other conditions were the same as in example 3, to prepare a compound represented by the formula Li 10 Ge(P 0.97 As 0.03 ) 2 S 12 The sulfide electrolyte DL3.
Comparative example 4
This comparative example was carried out in a similar manner to example 3, except that:
arsenic pentasulfide in an amount of 0.36mmol, prepared in the same manner as in example 3 under the same conditions as in example 3 to give a compound of the formula Li 10 Ge(P 0.97 As 0.03 ) 2 S 12 Sulfide electrolyte DL4 of (1).
Test example 1
The sulfide electrolytes prepared in the examples and the comparative examples were subjected to the following tests, and the specific detection results are shown in table 1:
(1) Hydrogen sulfide gas generation amount: sealing the weighed sulfide electrolyte in a glove box in argon atmosphere, transferring the sealed sulfide electrolyte to a constant temperature and humidity box with gloves, opening the seal after the temperature is stabilized at 25 ℃ and the humidity is stabilized at RH30%, placing the sealed sulfide electrolyte in a closable flask with the volume of 1000mL, standing for 24H, and using H 2 S detector (model HJ-4, manufactured by Sendai electric power) 2 S concentration, and calculating H 2 S gas generation amount.
(2) Ionic conductivity: measuring the thickness d of the obtained sulfide electrolyte wafer by using a micrometer, respectively placing a piece of carbon-coated copper foil (the carbon end faces to the sulfide electrolyte) at two ends of the sulfide electrolyte wafer to be used as a blocking electrode, placing the blocking electrode into a conductivity test kit, pressurizing to 60Mpa, applying 5mV direct current voltage after connecting an electrochemical workstation, testing in a frequency range of 10mHz to 100kHz by using an alternating current impedance method, and calculating the ionic conductivity sigma; σ = d/Re × S; wherein, the first and the second end of the pipe are connected with each other,
re represents the impedance (ohm) of the measured sample body, and is obtained by intersection points of a semicircular arc and an oblique line in an electrochemical impedance spectrogram;
s represents the effective area (cm) of the electrode 2 )。
TABLE 1
| Example numbering | Hydrogen sulfide gas Generation amount (cm) 3 /g) | Ion conductivity (S/cm) |
| Example 1 | 0.46 | 0.90×10 -2 |
| Example 2 | 0.38 | 1.20×10 -2 |
| Example 3 | 0.27 | 1.60×10 -2 |
| Example 4 | 0.16 | 1.70×10 -2 |
| Example 5 | 0.05 | 0.15×10 -2 |
| Example 6 | 0.29 | 1.59×10 -2 |
| Comparative example 1 | 0.25 | 0.63×10 -2 |
| Comparative example 2 | 0.29 | 1.58×10 -2 |
| Comparative example 3 | 0.28 | 1.59×10 -2 |
| Comparative example 4 | 0.32 | 1.57×10 -2 |
As can be seen from the results in Table 1, the sulfide electrolyte prepared by the method provided by the invention has good stability in air (the generation amount of hydrogen sulfide gas is small and is as low as 0.05 cm) 3 /g) and simultaneously has higher ionic conductivity which is as high as 1.70 multiplied by 10 -2 S/cm。
Therefore, the sulfide electrolyte provided by the invention has wide application prospect and commercial value.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method of preparing a sulfide electrolyte, the method comprising:
(1) Mixing lithium sulfide, germanium disulfide, phosphorus pentasulfide and arsenic pentasulfide, and then grinding to obtain a mixture I;
(2) Tabletting and forming the mixture I, and then heating to obtain the sulfide electrolyte;
wherein the molar ratio of the phosphorus pentasulfide to the arsenic pentasulfide is 1-X: x is more than or equal to 0.01 and less than or equal to 0.5;
based on the total molar amount of the phosphorus pentasulfide and the arsenic pentasulfide, the amount of the lithium sulfide is 300-700mol%, and the amount of the germanium disulfide is 60-170mol%.
2. The method according to claim 1, wherein in step (1), the mixing condition at least satisfies: the stirring is carried out under the stirring condition, the rotating speed of the stirring is 300-350rpm, and the time is 20-80min.
3. The process according to claim 1 or 2, wherein in step (1), the mixture I has an average particle size of 4 to 8 μm.
4. A method according to any one of claims 1 to 3, wherein in step (1), the conditions of the grinding treatment are at least: the process is carried out in a ball mill, the rotating speed of the ball mill is 200-600rpm, and the time is 2-16h.
5. The method according to any one of claims 1 to 4, wherein in the step (2), the conditions for the tablet molding are at least satisfied: the pressure is 100-300MPa, the temperature is 20-30 ℃, and the time is 1-3min.
6. The method according to any one of claims 1 to 5, wherein in step (2), the conditions of the heat treatment are at least satisfied: the initial temperature is 20-30 deg.C, the heating rate is 1-5 deg.C/min, the final temperature is 400-700 deg.C, and the constant temperature time is 2-6h.
7. The method of any one of claims 1-6, further comprising: and carrying out temperature reduction treatment after the heating treatment to obtain the sulfide electrolyte.
8. The method according to claim 7, wherein the condition of the temperature reduction treatment at least satisfies the following conditions: the initial temperature is 400-700 deg.C, the cooling rate is 0.5-5 deg.C/min, and the final temperature is 30-80 deg.C.
9. A sulfide electrolyte prepared by the method of any one of claims 1 to 8.
10. Use of the sulfide electrolyte of claim 9 in a battery.
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