CN115312843A - Se-doped solid electrolyte and preparation method and application thereof - Google Patents
Se-doped solid electrolyte and preparation method and application thereof 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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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a Se-doped solid electrolyte and a preparation method and application thereof, belonging to the field of electrochemical energy storage batteries. According to the invention, se element is doped in the sulfur-based solid electrolyte, so that the interface stability of the electrolyte is greatly improved, and the electrolyte has the function of a protective layer; after Se-doped solid electrolyte is coated on the surface of lithium cobaltate, a uniform coating layer can be formed on the surface of lithium cobaltate, the problem of oxygen loss of the lithium cobaltate during high-voltage circulation can be solved, and the coated lithium cobaltate can maintain good Li + The conductivity is also improved in specific capacity and cycle performance; the Se-doped solid electrolyte coated lithium cobaltate has the advantages of simple process, no need of complex treatment process, strong accessibility and direct application to the primary sintering and secondary sintering processes of lithium cobaltate.
Description
Technical Field
The invention relates to the field of electrochemical energy storage batteries, in particular to a Se-doped solid electrolyte and a preparation method and application thereof.
Background
Lithium Ion Batteries (LIBs) are the first energy storage system for portable electronic products and electric vehicles, and their development is still beyond the ever-increasing demand for high energy density batteries. Lithium cobaltate, as a positive electrode material of the rechargeable LIB, occupies a dominant position in 3C electronic equipment due to high tap density; however, lithium cobaltate in practical use only exerts 1/2 (about 140mAh g-1) of its theoretical capacity, which means that only half of the Li is present + Is separated from lithium cobaltate; although the energy density can be improved by more than 40% when lithium cobaltate is charged to a high voltage, when the lithium cobaltate is cycled under the high voltage, the oxygen ion redox pair participates in capacity contribution, and the high-voltage cycling lithium cobaltate is seriously oxygen-deprived due to the easy migration of high-oxidation-state oxygen ions, so that the irreversible phase change of a positive electrode material is caused to block the conduction of lithium ions, and the carbonate electrolyte is oxidatively decomposed, thereby the cycle life of the battery is rapidly shortened.
Strategies have been developed to address the issue of cell cycle life decay, including topography design, element doping, and cladding. Se is a special element with an anti-aging function in a human body, and can delay cell aging by capturing redundant oxygen ion free radicals in the metabolism process of the human body; by means of the unique characteristic of Se element for capturing oxygen ion free radicals, the problem of oxygen loss of lithium cobaltate during high-voltage circulation can be relieved through Se treatment; CN110668509A discloses that the preparation of Se-coated lithium cobaltate is blended and sintered with lithium cobaltate in the form of elementary Se, the process is simple, but the elementary Se forms SeO coating ion/Li in the subsequent sintering process + The conductivity is poor, in addition, the trace Se is coated in the lithium cobaltate in an island-like coating manner, and the exposed surface of the lithium cobaltate is still in direct contact with the electrolyte; these problems will beThe electrochemical polarization of the lithium cobaltate anode material is increased, so that the specific capacity of the material is reduced, and the cycling stability is reduced.
Thus, a uniform Se coating layer is formed on the surface of lithium cobaltate without reducing the ion/Li of lithium cobaltate + The conductivity of (2) is one of the difficulties in realizing stable cycling of lithium cobaltate at high voltage.
Disclosure of Invention
The present invention has been made to overcome the above-mentioned disadvantages of the prior art, and an object of the present invention is to provide a lithium ion secondary battery that can uniformly coat the surface of lithium cobaltate and can maintain the coated lithium cobaltate at a good quality + Se-doped solid electrolyte with conductivity, and a preparation method and application thereof.
In order to realize the purpose, the invention adopts the technical scheme that: se-doped solid electrolyte with chemical composition of Li 6+x P 1-x Se x S 5 X2 or Li 6+x P 1-x Se x S 5-2x X1 2x X2, wherein X is more than 0 and less than 1; the X1 is O or S, and the X2 is at least one of F, cl, br and I.
The Se-doped solid electrolyte provided by the invention enables the electrolyte to keep excellent ions/Li of the sulfur-based solid electrolyte by doping Se element in the sulfur-based solid electrolyte + The conductivity and the interface stability of the electrolyte are greatly improved by doping Se, and meanwhile, the sulfur-based solid electrolyte has the function of a protective layer, so that the stable circulation of lithium cobaltate under high voltage can be realized.
Another object of the present invention is to provide a method for preparing the Se-doped solid electrolyte, comprising the steps of: weighing the materials Li according to the stoichiometric ratio 2 S、SeX1、P 2 S 5 And pre-mixing with LiX2, and crushing the mixed material to obtain the Se-doped solid electrolyte.
Preferably, the stoichiometric ratio of the materials is Li 2 S:SeX1:P 2 S 5 LiX2= (5-6): (0-1): 2, and the inventor finds through experiments that the material can ensure enough Li under the stoichiometric ratio + The quantity of the conveying and the production can be controlledCost of Se doped solid state electrolyte.
Preferably, the materials are placed in a high-energy ball mill and are subjected to ball milling in an inert atmosphere, the high-energy ball milling is a crushing method combining a physical method and a chemical method, uniform dispersion and mixing of different components can be realized, the materials are fully mixed through the high-energy ball milling, not only can the chemical activation and crushing effects of the materials be realized, but also alloying action can be generated among the materials, so that a compact coating layer can be formed in the subsequent sintering process, and Li is improved + Electrical conductivity.
More preferably, the ball mass ratio of the ball mill is 15 to 1, and the inventor finds through experiments that the ball mass ratio in this range can maximize the mixing efficiency of the materials, and neither over-crushing phenomenon nor metal loss to the high-energy ball mill can occur.
More preferably, the inert atmosphere is nitrogen or argon.
More preferably, the ball milling media of the ball mill is zirconia.
Most preferably, the zirconia has a diameter of 5 15mm, and the inventors can use a ball milling medium with the diameter in combination with the hardness of the material to fully mill the material.
The invention also provides application of the Se-doped solid electrolyte in coating lithium cobaltate materials.
Preferably, the step of coating the Se-doped solid electrolyte with the lithium cobaltate material is as follows: and coating the Se-doped solid electrolyte and the lithium cobaltate material in an inert atmosphere, sintering at a low temperature in the inert atmosphere, cooling, and grinding and screening to obtain the lithium cobaltate material with the Se-doped solid electrolyte coating layer.
More preferably, the Se doped solid electrolyte comprises the following Se in the lithium cobaltate material in percentage by mass: se is more than 0 and less than or equal to 1 percent.
More preferably, the lithium cobaltate material includes at least one of cobalt carbonate, cobalt hydroxide, cobaltosic oxide, and lithium cobaltate.
Most preferably, the preparation method of the lithium cobaltate material comprises the following steps: uniformly mixing the raw materials, placing the mixture in a tube furnace, heating the mixture to 550-650 ℃ at the speed of 1-3 ℃/min, preserving heat for 1-3h, heating the mixture to 850-950 ℃ at the speed of 1-3 ℃/min, preserving heat for 9-11h, naturally cooling, and sieving the mixture by a pair of rollers to obtain a primary lithium cobaltate sintering product.
More preferably, the coating is performed by using a coating fusion machine.
Most preferably, the rotating speed of the coating fusion machine is 40-60Hz, the coating time is 2-8min, and the coating can be more fully performed under the coating parameters.
More preferably, the inert atmosphere during coating is nitrogen or argon.
More preferably, the process parameters of the low-temperature sintering are as follows: raising the temperature to 400-800 ℃ at a heating rate of 2-10 ℃/min, preserving the heat for 6-8h and then cooling.
The invention has the beneficial effects that: the invention provides a Se-doped solid electrolyte, which can greatly improve the interface stability of the electrolyte by doping Se element in a sulfur-based solid electrolyte, and simultaneously can ensure that the electrolyte has the function of a protective layer, so that the electrolyte can form a uniform coating layer on the surface of lithium cobaltate after being coated on the surface of the lithium cobaltate, and can also alleviate the problem of oxygen loss of the lithium cobaltate during high-voltage circulation, so that the coated lithium cobaltate can maintain good Li + The conductivity, specific capacity and cycle performance are also improved; the Se-doped solid electrolyte is coated on lithium cobaltate, the process is simple, a complex treatment process is not needed, the accessibility is strong, and the Se-doped solid electrolyte can be directly applied to the primary sintering and secondary sintering processes of lithium cobaltate.
Drawings
Fig. 1 is an SEM image of Se-doped solid electrolyte-coated lithium cobaltate in example 1.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
An example of a Se-doped solid electrolyte according to the present invention, preparation of a Se-doped solid electrolyte according to the present exampleThe method comprises the following steps: weighing Li according to a stoichiometric ratio of 5 2 S、Se、P 2 S 5 And LiCl solid powder, preliminarily premixing in a plastic package bag, pouring into a high-energy ball mill, stirring for 8 hours at the speed of 450rmp in the nitrogen atmosphere, and sieving to obtain the Se-doped solid electrolyte with the mass percent of 5%.
The preparation method of Se-doped solid electrolyte coated lithium cobalt oxide described in this embodiment includes the following steps:
(1) Weighing 100g of cobaltosic oxide and 45.3g of lithium carbonate, uniformly mixing, placing in a tube furnace, heating to 600 ℃ at the speed of 2 ℃/min, preserving heat for 2h, heating to 900 ℃ at the speed of 2 ℃/min, preserving heat for 10h, naturally cooling, and sieving by a pair of rollers to obtain a pure-phase lithium cobaltate primary sintered product.
(2) Weighing 100g of the pure-phase lithium cobaltate primary sintered product obtained in the step (1) and 6g of Se-doped solid electrolyte, coating the product in a fusion coating machine at the frequency of 50Hz for 3min, placing the product in a tubular furnace filled with nitrogen, heating the product to 550 ℃ at the speed of 2 ℃/min, preserving the temperature for 10h, heating the product to 700 ℃ at the speed of 2 ℃/min, preserving the temperature for 10h, naturally cooling the product, and sieving the product by using a pair of rollers to complete coating of the Se-doped solid electrolyte on the lithium cobaltate, so as to obtain 0.3% by mass of high-voltage lithium cobaltate, wherein an SEM image of the high-voltage lithium cobaltate is shown in figure 1.
Example 2
This example only differs from example 1 in that: in the preparation method of the Se-doped solid electrolyte, seS is used 2 The remaining steps were in accordance with example 1, replacing Se.
Example 3
This example differs from example 1 only in that: in the preparation method of the Se-doped solid electrolyte, seO is used 2 The remaining steps were in accordance with example 1, replacing Se.
Example 4
This example differs from example 1 only in that: in the preparation method of the Se-doped solid electrolyte, li is weighed according to the stoichiometric ratio of 6 2 S、Se、P 2 S 5 And LiCl solid powder, the remaining procedure was in accordance with example 1.
Example 5
This example only differs from example 1 in that: in the preparation method of the Se-doped solid electrolyte, liCl is used for replacing LiF, and the other steps are consistent with those in example 1.
Example 6
This example only differs from example 1 in that: in the preparation method of the Se-doped solid electrolyte, liBr is replaced by LiCl, and the rest steps are consistent with those in example 1.
Example 7
This example differs from example 1 only in that: in the preparation method of the Se-doped solid electrolyte, liI is replaced by LiCl, and the rest steps are consistent with those in example 1.
Example 8
This example differs from example 1 only in that: in the preparation method of the Se-doped solid electrolyte, the mass of the weighed Se-doped solid electrolyte is 20g, and the rest steps are consistent with those of the example 1, so that the high-voltage lithium cobalt oxide with the Se mass percentage of 1% is prepared.
Comparative example 1
This comparative example differs from example 1 only in that: coating the lithium cobaltate primary sintered product with only elemental Se, and the mass of the elemental Se is 0.3g, to obtain Se-coated lithium cobaltate with the mass percent of 0.3 percent.
Comparative example 2
The comparative example only differs from example 1 in that: directly placing the primary sintered product of lithium cobaltate in a tubular furnace filled with nitrogen, heating to 300 ℃ at the speed of 2 ℃/min, preserving heat for 2h, heating to 700 ℃ at the speed of 2 ℃/min, preserving heat for 10h, naturally cooling, and sieving by a pair of rollers to obtain pure-phase lithium cobaltate.
Examples of effects
The lithium cobaltate materials of the above examples 1-2 and comparative examples 1-2 were prepared into electrode sheets, and electrochemical tests were performed on coin cells prepared using the lithium sheets as counter electrodes, and the results are shown in table 1 below.
Where CC and DC represent the first fully charged capacity and the first discharged capacity of the battery, respectively, and CE% represents the first effect, i.e., the ratio of the first fully charged capacity to the first discharged capacity of the battery.
TABLE 1
The result is shown in table 1, after the Se-doped sulfur-based solid electrolyte in examples 1 and 2 is coated on the surface of the lithium cobaltate material, the charge-discharge capacity and the cycle performance of the lithium cobaltate material are both obviously improved, and the cycle retention rate of example 1 reaches 86.6%, and the first effect reaches 94.6%; in contrast, in comparative example 1, only Se-coated lithium cobaltate is used, although the first full charge capacity is increased, the first discharge capacity is lower, so that the final first effect is only 91.7%, which is obviously lower than that in examples 1 and 2, and the cycle stability is lower than that in the examples; comparative example 2, because blank lithium cobaltate was used, the first charge capacity and the first discharge capacity were both significantly reduced, and the cycle stability was < 70%, which was only 67.1%.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. Se-doped solid electrolyte, characterized in that the chemical composition of the Se-doped solid electrolyte is Li 6+x P 1- x Se x S 5 X2 or Li 6+x P 1-x Se x S 5-2x X1 2x X2, wherein X is more than 0 and less than 1; the X1 is O or S, and the X2 is at least one of F, cl, br and I.
2. The method of preparing a Se-doped solid-state electrolyte according to claim 1, comprising the steps of: weighing material Li according to stoichiometric ratio 2 S、SeX1、P 2 S 5 And pre-mixing with LiX2, and crushing the mixed material to obtain the Se-doped solid electrolyte.
3. The method of claim 2 wherein the stoichiometric ratio of the materials is Li 2 S:SeX1:P 2 S 5 :LiX2＝(5-6):(0-1):2:1。
4. The method of claim 2 wherein the material is ball milled in a high energy ball mill.
5. The method of claim 4, wherein the ball-milled spheres have a mass ratio of 15 to 1.
6. Use of the Se-doped solid-state electrolyte of any of claims 1 to 5 for coating lithium cobaltate material.
7. The use of the Se-doped solid electrolyte as claimed in claim 6 for coating a lithium cobaltate material, wherein the step of coating the lithium cobaltate material with the Se-doped solid electrolyte comprises: and coating the Se-doped solid electrolyte and the lithium cobaltate material in an inert atmosphere, sintering in the inert atmosphere, cooling, grinding and screening to obtain the lithium cobaltate material with the Se-doped solid electrolyte coating layer.
8. The use of the Se-doped solid electrolyte of claim 6 for coating a lithium cobaltate material, wherein the Se-doped solid electrolyte comprises, in mass percent: se is more than 0 and less than or equal to 1 percent.
9. The use of the Se-doped solid electrolyte according to claim 6, wherein the lithium cobaltate material comprises at least one of cobalt carbonate, cobalt hydroxide, cobaltosic oxide, and lithium cobaltate.
10. The use of the Se-doped solid electrolyte of claim 7 for coating a lithium cobaltate material, wherein the sintering process parameters are: raising the temperature to 400-800 ℃ at the temperature raising rate of 2-10 ℃/min, preserving the temperature for 6-8h, and cooling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210996067.XA CN115312843A (en) | 2022-08-18 | 2022-08-18 | Se-doped solid electrolyte and preparation method and application thereof |
| PCT/CN2023/077433 WO2024036905A1 (en) | 2022-08-18 | 2023-02-21 | Se-doped solid electrolyte, and preparation method therefor and use thereof |
| FR2308768A FR3138973A1 (en) | 2022-08-18 | 2023-08-18 | Solid electrolyte doped with Se, its preparation process and its use |
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| WO2024036905A1 (en) * | 2022-08-18 | 2024-02-22 | 广东邦普循环科技有限公司 | Se-doped solid electrolyte, and preparation method therefor and use thereof |
| CN117996059A (en) * | 2024-04-07 | 2024-05-07 | 英德市科恒新能源科技有限公司 | Solid electrolyte coated lithium cobalt oxide positive electrode material and preparation method thereof |
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| JP3433173B2 (en) * | 2000-10-02 | 2003-08-04 | 大阪府 | Sulfide-based crystallized glass, solid electrolyte and all-solid secondary battery |
| WO2013073038A1 (en) * | 2011-11-17 | 2013-05-23 | トヨタ自動車株式会社 | Electrolyte-coated positive electrode active material particles, all-solid-state battery, and production method for electrolyte-coated positive electrode active material particles |
| CN103531841B (en) * | 2013-11-01 | 2016-03-02 | 中国科学院宁波材料技术与工程研究所 | Sulfide solid electrolyte and preparation method thereof and all solid lithium secondary battery |
| CN111430808B (en) * | 2020-03-23 | 2022-07-29 | 广东东邦科技有限公司 | Lithium-containing chalcogenide-germanite solid electrolyte with dopant and preparation method thereof |
| CN113321485B (en) * | 2021-05-28 | 2022-06-24 | 湖南恩捷前沿新材料科技有限公司 | Preparation method of chalcogenide solid electrolyte |
| CN113506911B (en) * | 2021-07-15 | 2024-03-08 | 山东威固新能源科技有限公司 | Sulfide solid electrolyte material, preparation method and application thereof, and all-solid-state lithium battery |
| CN115312843A (en) * | 2022-08-18 | 2022-11-08 | 广东邦普循环科技有限公司 | Se-doped solid electrolyte and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024036905A1 (en) * | 2022-08-18 | 2024-02-22 | 广东邦普循环科技有限公司 | Se-doped solid electrolyte, and preparation method therefor and use thereof |
| CN117996059A (en) * | 2024-04-07 | 2024-05-07 | 英德市科恒新能源科技有限公司 | Solid electrolyte coated lithium cobalt oxide positive electrode material and preparation method thereof |
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