CN114709471A - Preparation method of sulfide solid electrolyte - Google Patents
Preparation method of sulfide solid electrolyte Download PDFInfo
- Publication number
- CN114709471A CN114709471A CN202210318816.3A CN202210318816A CN114709471A CN 114709471 A CN114709471 A CN 114709471A CN 202210318816 A CN202210318816 A CN 202210318816A CN 114709471 A CN114709471 A CN 114709471A
- Authority
- CN
- China
- Prior art keywords
- solid electrolyte
- anhydrous
- electrolyte
- sulfide solid
- sulfide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—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
- H01M10/0562—Solid materials
Abstract
The invention relates to a preparation method of a sulfide solid electrolyte. Firstly, dissolving a raw material of the Geranite sulfide solid electrolyte in an ultra-dry solvent according to a certain proportion, and violently stirring to fully and uniformly mix the raw materials and react; after the reaction is finished, removing unreacted residual solid through centrifugation, collecting the solution and removing the solvent to obtain powder; and finally, placing the dried powder in a vacuum sealed quartz tube for sintering to obtain the silver germanite sulfide solid electrolyte. The preparation method solves the problems of high energy consumption, uneven mixing of the raw materials for preparing the sulfide electrolyte and the like caused by the traditional solid-state method, and can improve the conductivity of the prepared sulfide electrolyte.
Description
Technical Field
The invention belongs to the technical field of solid electrolytes, particularly relates to a preparation method of a sulfide solid electrolyte, and particularly relates to a preparation method of a liquid phase method for preparing a large amount of a silver germanite sulfide solid electrolyte.
Background
At present, lithium ion batteries are commercially available, but the traditional lithium ion batteries have obvious potential safety hazards due to the adoption of liquid electrolyte, for example, the liquid organic electrolyte is flammable, volatile and easy to corrode. In contrast, the solid electrolyte adopted by the all-solid-state battery is non-combustible and non-volatile, so that the safety of the battery is ensured, and the problem of short service life of the battery caused by the dryness of the liquid electrolyte in the battery circulation process can be avoided.
Among the developed solid electrolytes, sulfide solid electrolytes are promising solid electrolytes because of their high room-temperature conductivity and outstanding thermal stability in terms of solid batteries.
The common preparation method of the sulfide solid electrolyte is a high-energy mechanical ball milling method, but the ball milling method consumes time and energy, and the conductivity of the sulfide solid electrolyte is often low due to the fact that raw materials cannot be uniformly mixed. The solution method for preparing the sulfide solid electrolyte can ensure that the raw materials are in full contact reaction in a solvent to obtain more uniform solid electrolyte.
CN112768761A discloses a preparation method of a solid sulfide solid electrolyte, which comprises the steps of adding reaction raw materials into an ultra-dry organic solvent, adding the mixture into a high-pressure stirring kettle, heating for a certain time, cooling, stirring, filtering, washing the solvent, and drying to obtain solid sulfide electrolyte powder, wherein the conductivity of the sulfide solid electrolyte prepared by the method is lower than 1mS cm-1。
Compared with the sulfide solid electrolyte prepared by the method, the conductivity of the sulfide silver-germanium ore type sulfide prepared by the liquid phase method is high and reaches 7 mS-cm-1And is simple and easy to operate, and saves time.
Disclosure of Invention
The invention aims to provide a preparation method of a sulfide solid electrolyte aiming at the problems in the prior art. The invention aims to provide a method for preparing a solid electrolyte of a chalcogenide of Geranite type by a liquid phase method, which solves the problems of long time consumption and uneven material mixing of the traditional method by preparing the solid electrolyte by a solution method, improves the conductivity to a certain extent and can reach 7 mS.cm-1。
The purpose of the invention can be realized by the following scheme:
the invention provides a preparation method of a sulfide solid electrolyte, which comprises the following steps:
s1, mixing Li2S and P2S5Dispersing in super-dry organic solvent, and stirring at room temperature to react fully to obtain Li3PS4The suspension of (a);
s2, mixing Li2Dissolving S and LiX in a solvent to obtain a lithium solution;
s3, adding the lithium solution obtained in the step S2 into the suspension obtained in the step S1, and stirring to react to obtain a mixed solution;
s4, centrifugally separating the mixed solution obtained in the step S3, taking the upper clear solution for reduced pressure distillation, and carrying out vacuum drying on the distilled powder to obtain solid powder;
and S5, tabletting the solid powder obtained in the step S4, and heating, sintering and cooling the solid powder under a vacuum sealing environment to obtain the sulfide solid electrolyte.
As an embodiment of the present invention, Li in step S12S and P2S5The molar ratio of the amounts used was 3: 1. The focus of this step is Li2S and P2S5Reaction in organic solvent to form Li3PS4The material can participate in the chemical reaction to obtain the final sulfide solid electrolyte, and the conductivity of the sulfide solid electrolyte is higher, and the crystallinity of the sulfide solid electrolyte is better.
As an embodiment of the present invention, Li in step S12S and P2S5The dispersing order is that the raw materials are mixed and then dispersed in the solvent or the raw materials are respectively dispersed in the solvent and then mixed.
As an embodiment of the present invention, the dispersion in step S1 is ultrasonic dispersion or agitation dispersion.
As an embodiment of the invention, the ultrasonic time of the ultrasonic dispersion is 10-15min, and the frequency is 20-25 kHz.
As an embodiment of the invention, the rotation speed of the stirring dispersion is 800-.
As an embodiment of the present invention, the steps S1, S2 are performed under a protective atmosphere. The protective atmosphere is argon.
As an embodiment of the present invention, the ultra-dry organic solvent in step S1 includes one or more of anhydrous Tetrahydrofuran (THF), anhydrous Ethylenediamine (EDA), Ethyl Propionate (EP), N-methylformamide (NMF), anhydrous acetonitrile, Ethyl Acetate (EA), 1, 2-Dimethylaminomethane (DME), THF-Ethanol.
As an embodiment of the present invention, Li in the suspension obtained in step S13PS4The mass fraction of (A) is 1% -1.5%.
As an embodiment of the present invention, the stirring time in step S1 is 10-12 h. Stirring was carried out for the purpose of thorough reaction, THF as solvent, Li2S and P2S5The chemical reaction is carried out in the solvent, and a complex is further formed with the solvent. Without stirring, the reaction was not complete.
As an embodiment of the present invention, Li is described in step S22The molar ratio of the S to the LiX is 1: 1.
as an embodiment of the present invention, the solvent in step S2 includes one of anhydrous acetone, anhydrous ethanol, anhydrous acetonitrile, and anhydrous methanol. Selecting a suitable solvent, and dissolving Li in the solvent2S and LiX are dissolved in corresponding solvents, and the liquid phase are in contact reaction, so that the reaction is more sufficient. If Li is directly incorporated2S and LiX are added into the reactant obtained from S1, and the two substances have no good compatibility with the solvent of S1, so that the two substances are prepared into a solution firstly and then added.
As an embodiment of the present invention, the mass fraction of the solute in the lithium solution obtained in step S2 is 3% to 4.7%.
As an embodiment of the present invention, the volume ratio of the lithium solution to the suspension in step S3 is 1:1 to 1: 3. The first step is the formation of a complex, which forms a suspension and is not a clear solution. Too little lithium solution is added and there is a possibility that it may not be completely contacted with the first step solution, so the amount of lithium solution should be at least consistent with the volume of the first step suspension.
As an embodiment of the present invention, the stirring speed in step S3 is 500-800rpm, and the time is 8-12 h.
As an embodiment of the present invention, the rotation speed of the centrifugal separation in step S4 is 5000-. The centrifugal separation is performed by a high-speed centrifuge.
As an embodiment of the present invention, the temperature of the vacuum drying in the step S4 is 140-200 ℃ and the time is 12-20 h. Further vacuum drying the solid powder to remove residual solvent
As an embodiment of the present invention, the pressure of the pellet in the step S5 is 200-300MPa.
As an embodiment of the present invention, the vacuum sealing environment in step S5 is specifically a sealed tube of quartz tube or glass tube, and the pressure of the sealed tube is less than 10-4Pa。
As an embodiment of the present invention, the sintering temperature in step S5 is 500-550 ℃ and the time is 6-10 h. Too high or too low a temperature and too long or too short a time may have some influence on the electrolyte, such as a decrease in conductivity and a deterioration in the crystallinity of the electrolyte.
As an embodiment of the present invention, the rate of temperature rise in step S5 is 0.5 to 1 ℃ min-1The cooling rate is 0.5-1 ℃ min-1. The sulfide solid electrolyte obtained by heating and cooling at 0.5-1 ℃ has the best quality. Temperature control is extremely important in the process of generating the sulfide electrolyte, improper temperature can be unfavorable for the crystal growth of the Geigranite electrolyte, and improper temperature control can generate amorphous crystal, so that the conductivity of the electrolyte is reduced rapidly.
Compared with the prior art, the invention has the following advantages:
(1) the sulfide solid electrolyte is prepared by adopting a solution method reaction. The solution method is used for reaction, so that the reaction time can be shortened, the raw materials react in the solution, the contact reaction can be better carried out, the mixing is uniform, and the more uniform electrolyte can be obtained.
(2) The sulfide solid electrolyte is prepared by a solution method, and compared with other liquid phase methods, the conductivity of the obtained solid electrolyte is higher.
(3) The sulfide solid electrolyte is prepared by a solution method, and compared with other liquid phase methods, the obtained solid electrolyte has good crystallinity.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 shows a Geranite-type electrolyte Li prepared in example 16PS5X-ray diffraction pattern of Cl;
FIG. 2 is an impedance diagram of the electrolyte prepared in example 1;
FIG. 3 is a charge and discharge graph of the electrolyte prepared in example 1;
fig. 4 is a charge and discharge graph of the electrolyte prepared in comparative example 4.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The following examples, which are set forth to provide a detailed description of the invention and a detailed description of the operation, will help those skilled in the art to further understand the present invention. It should be noted that the scope of the present invention is not limited to the following embodiments, and that several modifications and improvements made on the premise of the idea of the present invention belong to the scope of the present invention.
Example 1
This example provides a sulfide solid electrolyte Li6PS5The preparation method of Cl comprises the following specific steps:
(1) weighing Li according to a molar ratio of 3:1 in a glove box under an argon atmosphere2S and P2S5Fully grinding in an agate mortar, and uniformly and ultrasonically dispersing in ultra-dry tetrahydrofuran, wherein the ultrasonic time is 10min, and the frequency is 25 kHz.
(2) Stirring the mixture obtained in the step (1) at room temperature for 10h under the protection of no water and no oxygen to obtain Li with the mass fraction of 1%3PS43THF/THF suspension.
(3) In a glove box filled with argon, the molar ratio of 1:1 weighing Li2S and LiCl are dissolved in anhydrous acetone to prepare a solution with the mass fraction of 3%.
(4) Adding the solution obtained in the step (3) into the suspension obtained in the step (2), wherein the volume ratio is 1: 1. the suspension was stirred overnight at room temperature at a rate of 500rpm for 10 hours and centrifuged at 5000rpm for 10min to give a clear solution.
(5) And (4) distilling the clear solution obtained in the step (4) under reduced pressure to obtain solid powder, then drying in vacuum to remove the solvent, and drying the obtained solid powder in a vacuum oven to remove the residual solvent at the temperature of 140 ℃ for 12 hours.
(6) Tabletting the dried powder under 200MPa, and vacuum sealing in quartz tube under vacuum sealing pressure of less than 10-4Pa。
(7) And (3) sintering the sealed glass tube in a muffle furnace at 550 ℃ for 6 h. The heating and cooling rates are both 0.5 ℃ and min-1。
The prepared chalcogenide-germanite electrolyte Li6PS5The X-ray diffraction pattern of Cl is shown in figure 1; the impedance diagram is shown in fig. 2; the charge-discharge curve is shown in fig. 3.
Example 2
This example provides a sulfide solid electrolyte Li6PS5The preparation method of Br comprises the following specific steps:
(1) weighing Li in a molar ratio of 3:1 in a glove box under argon atmosphere2S and P2S5Fully grinding in an agate mortar, and uniformly and ultrasonically dispersing in ultra-dry tetrahydrofuran, wherein the ultrasonic time is 10min, and the frequency is 25 kHz.
(2) Stirring the mixture obtained in the step (1) at room temperature for 10h under the protection of no water and no oxygen to obtain Li with the mass fraction of 1%3PS43THF/THF suspension.
(3) In a glove box filled with argon, the molar ratio of 1:1 weighing Li2S and LiBr are dissolved in anhydrous acetone to prepare a solution with the mass fraction of 4.2%.
(4) Adding the solution obtained in the step (3) into the suspension obtained in the step (2). The volume ratio is 1: the suspension was stirred at room temperature overnight at 500rpm for 10h and centrifuged to give a clear solution. The centrifugation speed was 5000rpm and the time was 10 min.
(5) And (4) carrying out reduced pressure distillation on the clear solution obtained in the step (4) to obtain solid powder, and drying the obtained solid powder in a vacuum oven at the temperature of 140 ℃ for 20 hours to remove residual solvent.
(6) Tabletting the dried powder under the conditions of 200-300MPa, vacuum sealing in a quartz tube, and sealing the tube under vacuum<10-4pa。
(7) And (3) sintering the sealed quartz tube in a muffle furnace at 550 ℃ for 6 h. The heating and cooling rates are both 0.5 ℃ and min-1。
Example 3
This example provides a sulfide solid electrolyte Li6PS5The preparation method of I comprises the following specific steps:
weighing Li according to a molar ratio of 3:1 in a glove box under an argon atmosphere2S and P2S5Ground well in an agate mortar and dispersed uniformly in ultra dry tetrahydrofuran ultrasonically. The ultrasonic treatment time is 10min, and the frequency is 25 kHz.
(2) Stirring the mixture obtained in the step (1) at room temperature for 10h under the protection of no water and no oxygen to obtain Li with the mass fraction of 1%3PS43THF/THF suspension.
(3) In a glove box filled with argon, the molar ratio of 1:1 weighing Li2S and LiI are dissolved in anhydrous acetone to prepare a solution with the mass fraction of 3.74%.
(4) Adding the solution obtained in the step (3) to the suspension obtained in the step (2). The suspension was stirred overnight at room temperature at 500rpm for 10h at a volume ratio of 1: 1. The clear solution was obtained by centrifugation. The centrifugation rate was 5000rpm for 10 min.
(5) And (4) carrying out reduced pressure distillation on the clear solution obtained in the step (4) to obtain solid powder, and drying the obtained solid powder in a vacuum oven at the temperature of 140 ℃ for 20 hours to remove residual solvent.
(6) The dried powder was pressed into tablets under the conditions of 300-500MPa and vacuum-sealed in a quartz tube.
(7) And sintering the sealed quartz tube in a muffle furnace at 550 ℃ for 6 hours. The heating and cooling rates are both 0.5 ℃ and min-1。
Example 4
This example provides a sulfide solid electrolyte Li6PS5The preparation method of Cl comprises the following specific steps:
(1) weighing Li according to a molar ratio of 3:1 in a glove box under an argon atmosphere2S and P2S5Fully grinding in an agate mortar, and uniformly and ultrasonically dispersing in ultra-dry tetrahydrofuran, wherein the ultrasonic time is 10min, and the frequency is 25 kHz.
(2) Stirring the mixture obtained in the step (1) at room temperature for 10h under the protection of no water and no oxygen to obtain Li with the mass fraction of 1%3PS43THF/THF suspension.
(3) In a glove box filled with argon, the molar ratio of 1:1 weighing Li2S and LiCl are dissolved in anhydrous acetone to prepare a solution with the mass fraction of 3%.
(4) Adding the solution obtained in the step (3) into the suspension obtained in the step (2), wherein the volume ratio is 1: 1. the suspension was stirred overnight at room temperature at a rate of 500rpm for 10 hours and centrifuged at 5000rpm for 10min to give a clear solution.
(5) And (4) distilling the clear solution obtained in the step (4) under reduced pressure to obtain solid powder, then drying in vacuum to remove the solvent, and drying the obtained solid powder in a vacuum oven to remove the residual solvent at the temperature of 140 ℃ for 12 hours.
(6) Tabletting the dried powder under 200MPa, and vacuum sealing in quartz tube under vacuum sealing pressure of less than 10-4Pa。
(7) And (3) sintering the sealed glass tube in a muffle furnace at 550 ℃ for 6 h. The heating and cooling rates are both 5 ℃ and min-1。
Comparative example 1
This comparative example provides a vulcanizationThe preparation method of the solid electrolyte basically has the same specific steps as the example 1, and only the difference is that Li2The feeding molar ratio of S to LiCl is 2:3 to obtain Li5.8PS4.8Cl1.2。
Comparative example 2
This comparative example provides a method of preparing a sulfide solid electrolyte, which comprises substantially the same steps as in example 1, except that Li is used2The feeding molar ratio of S to LiBr is 3:7, and Li is obtained5.6PS4.6Br1.4。
Comparative example 3
This comparative example provides a method of preparing a sulfide solid electrolyte, which comprises substantially the same steps as in example 1, except that Li is used2The feeding molar ratio of S to LiI is 1:3 to obtain Li5.5PS4.5I1.5。
Comparative example 4
This comparative example provides a method of preparing a sulfide solid electrolyte, the specific steps being substantially the same as those of example 1, except that: weighing Li according to a molar ratio of 3:1:12S、P2S5And directly mixing and fully grinding LiCl, and then sintering.
Mixing Li2S、P2S5LiX is directly mixed, sealed and calcined, and the obtained product has no difference in chemical composition. However, the direct mixing calcination is a ball milling method, but the raw materials obtained by ball milling are sintered again to prepare the sulfide electrolyte with large and uneven particles. The sulfide solid electrolyte prepared by the method has more uniform and sufficient reaction and smaller particles because of chemical reaction in the ultra-dry organic solvent.
The charge and discharge curves of the prepared electrolyte are shown in fig. 4.
Comparative example 5
This comparative example provides a method of preparing a sulfide solid electrolyte, the specific steps being substantially the same as those of example 1, except that: the sintering temperature was 450 ℃.
Comparative example 6
This comparative example provides a method of preparing a sulfide solid electrolyte, the specific steps being substantially the same as those of example 1, except that: the sintering temperature was 600 ℃.
And (3) performance testing:
conductivity test results List
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. A method for producing a sulfide solid electrolyte, comprising the steps of:
s1, mixing Li2S and P2S5Dispersing in super-dry organic solvent, and stirring at room temperature to react fully to obtain Li3PS4A suspension;
s2, mixing Li2Dissolving S and LiX in a solvent to obtain a lithium solution, wherein X comprises one of Cl, Br and I;
s3, adding the lithium solution obtained in the step S2 into the suspension obtained in the step S1, and stirring to react to obtain a mixed solution;
s4, centrifugally separating the mixed solution obtained in the step S3, taking the upper clear solution for reduced pressure distillation, and carrying out vacuum drying on the distilled powder to obtain solid powder;
and S5, tabletting the solid powder obtained in the step S4, heating and sintering the solid powder in a vacuum sealing environment, and cooling the solid powder to obtain the sulfide solid electrolyte.
2. The method of claim 1, wherein Li in step S12S and P2S5The molar ratio of the amounts used was 3: 1.
3. The method for preparing the compound of claim 1, wherein the ultra-dry organic solvent in step S1 comprises one or more of anhydrous tetrahydrofuran, anhydrous ethylenediamine, ethyl propionate, N-methylformamide, anhydrous acetonitrile, ethyl acetate, 1, 2-dimethylaminomethane and THF-Ethanol.
4. The method of claim 1, wherein the suspension obtained in step S1 contains Li3PS4The mass fraction of (A) is 1-1.5%.
5. The method of claim 1, wherein the Li in step S22The molar ratio of the S to the LiX is 1: 1.
6. the method of claim 1, wherein the solvent in step S2 is one of anhydrous acetone, anhydrous ethanol, anhydrous acetonitrile, and anhydrous methanol.
7. The method according to claim 1, wherein the lithium solution obtained in step S2 contains Li2The mass fraction of S and LiX is 3% -4.7%.
8. The method of claim 1, wherein the volume ratio of the lithium solution to the suspension in step S3 is 1:1 to 1: 3.
9. The method as claimed in claim 1, wherein the sintering temperature in step S5 is 500-550 ℃ for 6-10 h.
10. The method of claim 1, wherein the temperature is raised in step S5 at a rate of 0.5-1 ℃. min-1The cooling rate is 0.5-1 ℃ min-1。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210318816.3A CN114709471A (en) | 2022-03-29 | 2022-03-29 | Preparation method of sulfide solid electrolyte |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210318816.3A CN114709471A (en) | 2022-03-29 | 2022-03-29 | Preparation method of sulfide solid electrolyte |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114709471A true CN114709471A (en) | 2022-07-05 |
Family
ID=82170694
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210318816.3A Pending CN114709471A (en) | 2022-03-29 | 2022-03-29 | Preparation method of sulfide solid electrolyte |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114709471A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103500853A (en) * | 2013-10-08 | 2014-01-08 | 中国科学院宁波材料技术与工程研究所 | Sulfide electrolyte material and preparation method thereof |
| CN110165293A (en) * | 2019-05-28 | 2019-08-23 | 浙江锋锂新能源科技有限公司 | A kind of preparation method of sulfide solid electrolyte |
| CN110444806A (en) * | 2019-08-06 | 2019-11-12 | 深圳大学 | A kind of sulfide solid electrolyte precursor solution and its preparation method and application |
| WO2020153973A1 (en) * | 2019-01-25 | 2020-07-30 | Solid Power, Inc. | Solid electrolyte material synthesis method |
| CN112397775A (en) * | 2020-10-27 | 2021-02-23 | 广东东邦科技有限公司 | Li3PS4 solid electrolyte, solid mixed electrolyte, all-solid lithium-sulfur battery and preparation method thereof |
| CN113508089A (en) * | 2019-03-05 | 2021-10-15 | 三菱瓦斯化学株式会社 | Method for producing sulfide-based solid electrolyte |
-
2022
- 2022-03-29 CN CN202210318816.3A patent/CN114709471A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103500853A (en) * | 2013-10-08 | 2014-01-08 | 中国科学院宁波材料技术与工程研究所 | Sulfide electrolyte material and preparation method thereof |
| WO2020153973A1 (en) * | 2019-01-25 | 2020-07-30 | Solid Power, Inc. | Solid electrolyte material synthesis method |
| CN113508089A (en) * | 2019-03-05 | 2021-10-15 | 三菱瓦斯化学株式会社 | Method for producing sulfide-based solid electrolyte |
| CN110165293A (en) * | 2019-05-28 | 2019-08-23 | 浙江锋锂新能源科技有限公司 | A kind of preparation method of sulfide solid electrolyte |
| CN110444806A (en) * | 2019-08-06 | 2019-11-12 | 深圳大学 | A kind of sulfide solid electrolyte precursor solution and its preparation method and application |
| CN112397775A (en) * | 2020-10-27 | 2021-02-23 | 广东东邦科技有限公司 | Li3PS4 solid electrolyte, solid mixed electrolyte, all-solid lithium-sulfur battery and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6017789B2 (en) | Cathode material for lithium ion battery to which nickel / cobalt / manganese multielements are added and method for producing the same | |
| CN108232308A (en) | The manufacturing method of sulfide solid electrolyte | |
| JP2012517675A5 (en) | ||
| JP5467264B2 (en) | Method for producing electrode material for non-aqueous electrolyte secondary battery, electrode material for non-aqueous electrolyte secondary battery, and non-aqueous electrolyte secondary battery using the electrode material | |
| CN105098228A (en) | Sulfide solid electrolyte material and preparation method thereof | |
| CN109755540B (en) | Lithium-sulfur battery positive electrode material and preparation method thereof | |
| CN105789581A (en) | Production method for high-capacity long-cycle lithium-rich type-622 ternary positive electrode material | |
| JP2016185903A (en) | Manufacturing method of lithium manganese composite oxide | |
| CN103187556B (en) | Lithium ion battery and its negative material, preparation method | |
| CN108878962A (en) | A kind of sulfide solid electrolyte and preparation method thereof | |
| WO2023217260A1 (en) | Sulfide solid state electrolyte, as well as preparation method therefor and use thereof | |
| KR20180074071A (en) | Method for manufacturing lithium oxide, and method for manufacturing lithium nickel oxide | |
| CN106207128A (en) | A kind of Zr (OH)4the preparation method of cladding nickel cobalt aluminum tertiary cathode material | |
| CN114956020A (en) | Li 3 Preparation method of P crystal powder and Li 3 P crystal powder and application thereof | |
| CN103474653A (en) | Preparation method for lithium iron phosphate | |
| CN111934004B (en) | Lithium manganate/solid electrolyte composite material and preparation method and application thereof | |
| CN103825013B (en) | The method of high temperature modification LiMn2O4 produced by a kind of mangano-manganic oxide | |
| Ding et al. | High performance of Pb-doped Li4Ti5O12 as an anode material for lithium ion batteries | |
| CN112768684A (en) | Sodium-ion battery layered positive electrode material with excellent performance and method for improving electrochemical performance of sodium-ion battery layered positive electrode material by expanding interlayer spacing | |
| CN114709471A (en) | Preparation method of sulfide solid electrolyte | |
| CN102531057B (en) | Method for preparing lithium vanadate as cathode material of lithium ion battery | |
| CN114314668A (en) | Manganese-based ternary positive electrode material of sodium-ion battery and preparation method | |
| CN102698626B (en) | Multifunctional mixer and method for synthesizing lithium titanate anode material | |
| CN108400295B (en) | Silver-coated spinel-type LiMn2O4Material and method for the production thereof | |
| CN110994008A (en) | Preparation method of liquid-phase synthesized sulfide solid electrolyte |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |