CN111908437A - Preparation method of sulfide solid electrolyte - Google Patents
Preparation method of sulfide solid electrolyte Download PDFInfo
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- CN111908437A CN111908437A CN202010851445.6A CN202010851445A CN111908437A CN 111908437 A CN111908437 A CN 111908437A CN 202010851445 A CN202010851445 A CN 202010851445A CN 111908437 A CN111908437 A CN 111908437A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/14—Sulfur, selenium, or tellurium compounds of phosphorus
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- C01B25/08—Other phosphides
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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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- H01M2300/00—Electrolytes
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Abstract
The invention discloses a preparation method of a sulfide solid electrolyte, which comprises the following steps: (1) weighing Li according to the required stoichiometric ratio2S、P2S5And lithium salt containing X, wherein X comprises one or more of Cl, Br and I; (2) grinding and screening the uniformly mixed mixture to obtain a uniformly mixed precursor; (3) and placing the precursor in a ceramic vibration tank in microwave equipment for vibration and turnover, sintering for 10min-1h at the temperature of 150 ℃ and 400 ℃, and cooling to obtain the chalcogenide-germanite solid electrolyte containing Li, P, S and X elements. The method has the advantages of simple process, low sintering temperature, easy regulation and control of product components, and capability of obtaining the stable Geranite type cubic phase solid at room temperatureThe electrolyte can be applied to industrial mass production.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a sulfide solid electrolyte.
Background
With the rapid development of new energy technologies, the demand for secondary battery systems with high energy density and high safety is increasingly urgent. The commercial lithium ion battery mostly adopts liquid organic electrolyte, has inflammable and explosive properties, and has higher safety compared with solid electrolyte. Compared with the conventional liquid electrolyte lithium battery, the all-solid lithium secondary battery using the inorganic solid electrolyte theoretically has the following characteristics: (1) electrolyte leakage and combustion do not occur, and the safety is improved; (2) in all-solid batteries, the solid electrolyte has a dual function as a separator and an electrolyte; (3) compared with the traditional polymer diaphragm, the diaphragm has better mechanical strength and can ensure long-term operation; (4) side reactions between the solid electrolyte and the electrode are less; (5) the electrochemical window of solid electrolytes is wider than that of liquid organic electrolytes; (6) in solid-state electrolytes, the lithium ion transport number is very high, close to 1.
So far, among inorganic solid electrolytes, sulfide solid electrolytes and oxide solid electrolytes have been most widely studied. Compared with oxide solid electrolyte, the sulfide solid electrolyte has lower synthesis temperature, low hardness and better interface contact, higher ionic conductivity can be obtained after powder is cold-pressed into sheets, and the ionic conductivity of partial sulfide solid electrolyte exceeds that of commercial electrolyte and reaches 10-2S/cm. However, sulfide solid electrolytes still have the disadvantages of poor air stability and the like.
Disclosure of Invention
The invention mainly aims to overcome the defects of the prior art and provide a preparation method of a sulfide solid electrolyte.
In order to achieve the above object, the present invention provides a method for preparing a sulfide solid electrolyte, comprising the steps of:
(1) weighing Li according to the required stoichiometric ratio2S、P2S5And lithium salt containing X, wherein X comprises one or more of Cl, Br and I;
(2) grinding and screening the uniformly mixed mixture to obtain a uniformly mixed precursor;
(3) and placing the precursor in a ceramic vibration tank in microwave equipment for vibration and turnover, sintering for 10min-1h at the temperature of 150 ℃ and 400 ℃, and cooling to obtain the chalcogenide-germanite solid electrolyte containing Li, P, S and X elements.
Preferably, the stoichiometric ratio in the step (1) is Li2S:P2S5:LiX＝5:1:1-4。
Preferably, sulfide containing M is further added in the step (1) for mixing, M comprises at least one of Al, Si, Ge, As, Zn, Sn, Ni and Sb, and the step (2) correspondingly obtains Li6+xMxP1–xS5X is a solid electrolyte, wherein X is more than 0 and less than or equal to 0.6.
Preferably, the step (1) of mixing uniformly is performed by using a mechanical ball milling method, using a zirconia pot and zirconia balls, and performing ball milling at a ball milling rotation speed of 100-.
Preferably, the grinding and sieving in the step (2) is to sieve the mixture powder by using a sieve with the size of 300-600 meshes after grinding by using an agate mortar.
Preferably, the vibration frequency of the ceramic vibration tank in the step (3) is 10-30Hz, and the amplitude is 3-6 mm.
Preferably, the temperature in the step (3) is increased to 150 ℃ to 400 ℃ at a temperature increase rate of 5-40 ℃/min.
Preferably, the steps (1) to (3) are carried out under the protection of inert atmosphere, wherein the steps are weighing, uniformly mixing, grinding, screening and microwave sintering.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the invention adopts the microwave sintering technology to rapidly sinter at a lower temperature (150-400 ℃) within a short time (10min-1h), the raw materials are continuously vibrated and rolled in the ceramic vibration tank to reduce the agglomeration of the raw materials, and the obtained chalcogenide type solid electrolyte has uniform particle size, moderate crystallinity, freely adjustable components and stable existence at room temperature, not only has higher ionic conductivity, but also has ionic conductivity reaching 1.0 multiplied by 10 at normal temperature-4～1.0×10-2S/cm, good water resistance and oxidation resistance, simple and safe operation, excellent repeatability, suitability for industrial mass production, and capability of meeting the requirements of high output, high capacity and high safety when used as a solid electrolyte of an all-solid-state lithium secondary battery.
Drawings
FIG. 1 is a diagram showing a real object of a sulfide solid electrolyte powder obtained in example 1;
fig. 2 is a physical diagram of a sulfide solid electrolyte sheet obtained in example 1;
fig. 3 is an XRD pattern of the sulfide solid electrolyte powder prepared in example 1;
fig. 4 is a schematic structural diagram of the microwave heating apparatus used in step (3) of the present invention, in which 1 is a vibrator, 2 is a microwave heating chamber, 3 is a uniformly mixed precursor, and 4 is a ceramic vibration tank.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention.
Example 1:
weighing 2N pure reagent Li according to the required stoichiometric ratio2S、P2S5And LiCl, mixing, putting into a zirconia ball milling tank, adding zirconia balls for ball milling at the ball milling rotation speed of 300rpm for 6 hours, taking out, manually milling for 15 minutes by using a mortar, and screening by using a 300-mesh screen to obtain a uniformly mixed precursor. Placing the precursor in a ceramic vibration tank in a microwave device, vibrating and overturning, wherein the structural schematic diagram of the device is shown in FIG. 4, the vibration frequency is 10Hz, the amplitude is 5mm, heating to 150 ℃ at the speed of 30 ℃/min, preserving heat for 10min, and cooling to obtain Li6PS5A solid electrolyte powder of Cl, a schematic diagram of the solid electrolyte powder is shown in fig. 1. From XRD shown in figure 3, the solid electrolyte powder prepared by the method is a Geranite cubic phase, and has good crystal form and high purity. Pressing solid electrolyte powder under 200Mpa, maintaining pressure for 3min to obtain solid electrolyte sheet, and performing solid electrolysisPlease refer to fig. 2. The whole process is carried out under the protection of argon. The lithium cell conductivity of the solid electrolyte sheet was 6X 10 at room temperature-3S cm-1。
Example 2:
weighing 2N pure reagent Li according to the required stoichiometric ratio2S、P2S5And LiBr, mixing, putting into a zirconia ball milling tank, adding zirconia balls for ball milling at the ball milling rotation speed of 600rpm for 6 hours, taking out, manually milling for 15 minutes by using a mortar, and screening by using a 600-mesh screen to obtain a precursor which is uniformly mixed. Placing the precursor in a ceramic vibration tank in microwave equipment, vibrating and overturning at a vibration frequency of 20Hz and an amplitude of 5mm, heating to 300 ℃ at a speed of 10 ℃/min, preserving heat for 40min, and cooling to obtain Li6PS5Br solid electrolyte powder, pressing the obtained powder under 200Mpa, and maintaining the pressure for 3min to obtain the solid electrolyte sheet. The whole process is carried out under the protection of argon. The lithium cell conductivity of the solid electrolyte sheet was 4X 10 at room temperature-3S cm-1。
Example 3:
weighing 2N pure reagent Li according to the required stoichiometric ratio2S、P2S5, LiCl and SiS2And after mixing, putting the mixture into a zirconia ball milling tank, adding zirconia balls for ball milling at the ball milling rotation speed of 800rpm for 8 hours, taking out the mixture, manually milling the mixture for 15 minutes by using a mortar, and screening the mixture by using a 300-mesh screen to obtain a precursor which is uniformly mixed. Placing the precursor in a ceramic vibration tank of a microwave device, vibrating and overturning at a vibration frequency of 20Hz and an amplitude of 5mm, heating to 300 ℃ at a speed of 15 ℃/min, preserving heat for 20min, and cooling to obtain Li5.4Si0.2PS5Cl solid electrolyte powder, pressing the obtained powder under the pressure of 200Mpa, and maintaining the pressure for 3min to obtain the solid electrolyte sheet. The whole process is carried out under the protection of argon. The lithium cell conductivity of the solid electrolyte sheet was 3.3X 10 at room temperature-3S cm-1。
Example 4:
weighing 2N pure reagent Li according to the required stoichiometric ratio2S、P2S5LiBr and GeS2And after mixing, putting the mixture into a zirconia ball milling tank, adding zirconia balls for ball milling at the ball milling rotation speed of 1000rpm for 16 hours, taking out the mixture, manually milling the mixture for 15 minutes by using a mortar, and screening the mixture by using a 400-mesh screen to obtain a precursor which is uniformly mixed. Placing the precursor in a ceramic vibration tank in microwave equipment, vibrating and overturning at a vibration frequency of 30Hz and an amplitude of 3mm, heating to 400 ℃ at a speed of 5 ℃/min, preserving heat for 30min, and cooling to obtain Li6.2P0.8Ge0.2S5Br solid electrolyte powder, pressing the obtained powder under 200Mpa, and maintaining the pressure for 3min to obtain the solid electrolyte sheet. The whole process is carried out under the protection of argon. The lithium cell conductivity of the solid electrolyte sheet was 8X 10 at room temperature-3S cm-1。
Claims (8)
1. A method for producing a sulfide solid electrolyte, comprising the steps of:
(1) weighing Li according to the required stoichiometric ratio2S、P2S5And lithium salt containing X, wherein X comprises one or more of Cl, Br and I;
(2) grinding and screening the uniformly mixed mixture to obtain a uniformly mixed precursor;
(3) and placing the precursor in a ceramic vibration tank in microwave equipment for vibration and turnover, sintering for 10min-1h at the temperature of 150 ℃ and 400 ℃, and cooling to obtain the chalcogenide-germanite solid electrolyte containing Li, P, S and X elements.
2. The method for producing a sulfide solid electrolyte according to claim 1, wherein the stoichiometric ratio in the step (1) is Li2S:P2S5:LiX＝5:1:1-4。
3. The method according to claim 1, wherein said step (1) further comprises adding a sulfide containing M comprising at least one of Al, Si, Ge, As, Zn, Sn, Ni, and Sb, and mixing, and said step (2) further comprises) Correspondingly obtain Li6+xMxP1–xS5X is a solid electrolyte, wherein X is more than 0 and less than or equal to 0.6.
4. The method for preparing the sulfide solid electrolyte as claimed in claim 1, wherein the step (1) of uniformly mixing is performed by mechanical ball milling using zirconia pot and zirconia balls at a ball milling speed of 100-1200rpm for 1-24 hours.
5. The method for producing a sulfide solid electrolyte according to any one of claims 1 to 4, wherein the grinding and sieving in step (2) is to sieve the mixture powder using a sieve having a size of 300-600 mesh after grinding with an agate mortar.
6. The production method of a sulfide solid electrolyte according to any one of claims 1 to 4, wherein the ceramic vibration cell in the step (3) has a vibration frequency of 10 to 30Hz and an amplitude of 3 to 6 mm.
7. The method for producing a sulfide solid electrolyte according to any one of claims 1 to 4, wherein the temperature is raised to 150 ℃ to 400 ℃ at a temperature raising rate of 5 to 40 ℃/min in the step (3).
8. The method for preparing a sulfide solid electrolyte according to any one of claims 1 to 4, wherein the weighing, the mixing, the grinding and screening, and the microwave sintering in the steps (1) to (3) are performed under the protection of an inert atmosphere.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112777632A (en) * | 2021-01-25 | 2021-05-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Sulfide lithium ion solid electrolyte and preparation method and application thereof |
| CN113363568A (en) * | 2021-06-29 | 2021-09-07 | 高能时代(佛山)新能源科技有限公司 | Method for preparing sulfide solid electrolyte with low cost and low energy consumption |
| CN113991167A (en) * | 2021-10-26 | 2022-01-28 | 西安交通大学 | Halide solid electrolyte material and preparation method and application thereof |
| CN114039087A (en) * | 2021-11-08 | 2022-02-11 | 厦门大学 | Sulfide solid electrolyte and application thereof |
| CN114400370A (en) * | 2022-01-21 | 2022-04-26 | 浙江大学山东工业技术研究院 | Fabric-reinforced sulfide solid electrolyte and dry preparation method and application thereof |
| CN114421003A (en) * | 2022-01-06 | 2022-04-29 | 北京科技大学 | Preparation method of sulfide solid electrolyte |
| CN114649567A (en) * | 2020-12-18 | 2022-06-21 | 恒大新能源技术(深圳)有限公司 | Composite solid electrolyte, composite solid electrolyte membrane, preparation method of composite solid electrolyte membrane and solid battery |
| CN114649562A (en) * | 2022-03-24 | 2022-06-21 | 上海屹锂新能源科技有限公司 | Preparation and application of IIA group element and double-halogen doped sulfide solid electrolyte |
| CN114709474A (en) * | 2022-04-28 | 2022-07-05 | 上海屹锂新能源科技有限公司 | Bismuth-doped silver germanite type sulfide solid electrolyte and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114649567A (en) * | 2020-12-18 | 2022-06-21 | 恒大新能源技术(深圳)有限公司 | Composite solid electrolyte, composite solid electrolyte membrane, preparation method of composite solid electrolyte membrane and solid battery |
| CN112777632A (en) * | 2021-01-25 | 2021-05-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Sulfide lithium ion solid electrolyte and preparation method and application thereof |
| CN113363568A (en) * | 2021-06-29 | 2021-09-07 | 高能时代(佛山)新能源科技有限公司 | Method for preparing sulfide solid electrolyte with low cost and low energy consumption |
| CN113991167A (en) * | 2021-10-26 | 2022-01-28 | 西安交通大学 | Halide solid electrolyte material and preparation method and application thereof |
| CN114039087A (en) * | 2021-11-08 | 2022-02-11 | 厦门大学 | Sulfide solid electrolyte and application thereof |
| CN114421003A (en) * | 2022-01-06 | 2022-04-29 | 北京科技大学 | Preparation method of sulfide solid electrolyte |
| CN114421003B (en) * | 2022-01-06 | 2024-03-22 | 北京科技大学 | Preparation method of sulfide solid electrolyte |
| CN114400370A (en) * | 2022-01-21 | 2022-04-26 | 浙江大学山东工业技术研究院 | Fabric-reinforced sulfide solid electrolyte and dry preparation method and application thereof |
| CN114400370B (en) * | 2022-01-21 | 2024-03-08 | 浙江大学山东工业技术研究院 | Fabric reinforced sulfide solid electrolyte, dry preparation method and application thereof |
| CN114649562A (en) * | 2022-03-24 | 2022-06-21 | 上海屹锂新能源科技有限公司 | Preparation and application of IIA group element and double-halogen doped sulfide solid electrolyte |
| CN114649562B (en) * | 2022-03-24 | 2023-08-08 | 上海屹锂新能源科技有限公司 | Preparation and application of IIA group element and dihalogen doped sulfide solid electrolyte |
| CN114709474A (en) * | 2022-04-28 | 2022-07-05 | 上海屹锂新能源科技有限公司 | Bismuth-doped silver germanite type sulfide solid electrolyte and preparation method thereof |
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