CN113321485B - Preparation method of chalcogenide solid electrolyte - Google Patents
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Abstract
The invention discloses a method for using CS2A method for preparing sulfide solid electrolyte by combining wet ball milling and solid phase ball milling of raw materials and solvents. The invention uses low-cost Li2O2Or Li2O, P or P2O5、CS2And LiX (X is Cl, Br or I) is used as a raw material, so that high-price Li is avoided2S, preparing a solid electrolyte, namely CS by adopting a method of combining pressure reduction wet ball milling and solid phase ball milling2The prepared silver-germanium sulfide ore type solid electrolyte has high ionic conductivity and a wide electrochemical window, is applied to preparing all-solid batteries, and has high safety, high energy density and excellent cycling stability.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a chalcogenide solid electrolyte.
Background
With the increasing demand for energy storage systems with high energy density and high safety, the development of secondary all-solid-state battery technology has received much attention. The solid electrolyte with high ionic conductivity is used as a key component of the all-solid-state battery, so that the safety problem inherent in flammable organic electrolyte in the traditional lithium ion battery can be effectively solved, the battery packaging is simpler, more convenient and more efficient, and the energy density of a battery system is further improved.
Many super-ionic conductors have been considered as candidate materials for solid electrolytes of all-solid lithium batteries so far, and sulfide solid electrolytes and oxide solid electrolytes are most widely studied. Compared with oxide solid electrolyte, the sulfide solid electrolyte has lower synthesis temperature, low Young modulus, easier processing and densification, better interface contact with positive and negative electrode materials, 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。
At present, the main methods for preparing sulfide solid electrolytes are solid-phase methods and liquid-phase methods. The solid phase method is mainly a method of heat treatment after high-energy ball milling, raw materials are easy to adhere to the wall of a tank and the surface of a ball in the ball milling process, the raw materials are unevenly distributed, and an expected crystalline phase cannot be obtained. Liquid phase process due to P2S5And the raw materials are difficult to dissolve, the reaction time is long, and the ionic conductivity of the obtained solid electrolyte is generally low. How to directly and efficiently synthesize sulfide solid materials is still one of the difficulties in realizing the industrialization of all-solid batteries.
Disclosure of Invention
The invention mainly aims to overcome the defects of the prior art and provides a preparation method of a sulfide solid electrolyte by combining wet ball milling and solid phase ball milling. The invention uses low-cost Li2O2Or Li2O, P or P2O5、CS2And LiX (X is Cl, Br or I) as raw material, wherein CS2Serving both as raw material and as solvent for wet ball milling, to P or P2O5All have better solubility, have better dispersion effect on other raw materials in the wet ball milling process of the prior period, the raw materials are fully reacted, and the reaction product is mixed precursor and CO2A gas. Following CS2The wet ball milling is changed into solid-phase ball milling, and the mixed precursor undergoes an amorphization process in the solid-phase ball milling to form an initial solid electrolyte material. The initial solid electrolyte material can be sintered at low temperature to obtain the chalcogenide solid with high ionic conductivityA phase electrolyte.
In order to achieve the above object, the present invention provides a method for preparing a chalcogenide solid electrolyte, comprising the steps of:
(1) weighing Li according to the required stoichiometric ratio2O2Or Li2O, P or P2O5，CS2And lithium salt containing X, wherein X comprises one or more of Cl, Br and I;
(2) adding the raw materials in the step (1) into a ball milling tank, sealing the ball milling tank, and carrying out ball milling in a decompression state to obtain an initial solid electrolyte material which is uniformly mixed;
(3) and sintering the initial solid electrolyte material at low temperature under the protection of inert atmosphere, cooling, and grinding and screening to obtain the high-ionic-conductivity silver-germanium ore type solid electrolyte.
Preferably, the stoichiometric ratio in the step (1) is Li2O2:P:CS2LiX ═ 4-5:2:3-7:1-4 or Li2O:P2O5:CS2:LiX＝4-5:1:3-7:1-4。
Preferably, a dopant is further added in the step (2) for ball milling, wherein the dopant is P2S3、SiS2、GeS2、SnS2、As2S3、NiS、Sb2S3、Al2O3And ZnO.
Preferably, the ball milling pot in the step (2) is a ball milling pot with a gas valve capable of being vacuumized, and the material of the ball milling pot is any one of corundum, agate, zirconia and polytetrafluoroethylene.
Preferably, the degree of vacuum in the reduced pressure state in the step (2) is < -0.08 MPa.
Preferably, the ball milling in the step (2) is performed by adopting a mechanical ball milling mode, zirconia balls are added for assisting the ball milling, the ball-material ratio is 20-60:1, the ball milling rotation speed is 100-.
Preferably, in the step (2), the sealed ball milling tank is vacuumized once every 3 to 6 hours in the ball milling process, and the vacuum degree is less than-0.08 MPa.
Preferably, the low-temperature sintering in the step (3) is to raise the temperature to 150 ℃ and 400 ℃ at a temperature-raising rate of 5-40 ℃/min, and naturally cool the mixture after heat preservation for 1-3 hours.
Preferably, the grinding and screening in the step (3) is to screen the solid electrolyte powder by using a sieve with the size of 200-600 meshes after grinding by using an agate mortar.
Preferably, the weighing, ball milling, sintering and grinding and screening in the steps (1) to (3) are carried out under the protection of an inert atmosphere.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) the invention uses low-cost Li2O2Or Li2O, P or P2O5、CS2And LiX (X is Cl, Br or I) is used as a raw material, so that the use of a high-price raw material Li is avoided2S, the cost of industrial production of the chalcogenide-germanite solid electrolyte is greatly reduced;
(2) the invention adopts the method of wet ball milling at the early stage to prepare the mixed precursor and uses CS2Is both a raw material and a solvent for wet ball milling. CS2For P or P2O5All have better solubility, and avoid the traditional liquid phase method for preparing sulfide solid electrolyte with P2S5The problem of long time consumption caused by difficult dissolution; the reaction product of the wet ball milling is only CO except the target mixed precursor2And the melting point is low, so that the solvent is easy to remove, and the problems that the product is easy to contain impurities and the solvent is difficult to remove in the traditional liquid phase method are solved.
(3) According to the invention, solid-phase ball milling is carried out on the basis of wet ball milling in the later stage, and the raw materials are uniformly mixed in the wet ball milling process to generate a precursor, so that the problems of nonuniform material mixing and impure product crystalline phase in the traditional solid-phase method for preparing sulfide solid electrolyte are effectively avoided. The adopted solid phase ball milling can make the mixed precursor amorphized and densified to generate an initial solid electrolyte material, thereby effectively reducing CO2Escape sum CS2The structure is loosened due to volatilization, and the ion transmission rate in the material is accelerated.
(4) The initial solid electrolyte material prepared by the method can obtain the high ionic conductivity silver germanite type solid electrolyte without sintering treatment or only by low-temperature sintering in an inert atmosphere, thereby greatly reducing the energy consumption in the production process and being suitable for large-scale industrial production.
Drawings
Fig. 1 is an XRD pattern of the sulfide solid electrolyte powder prepared in example 1.
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 stoichiometric ratio of 5:2:6:22O2、P、CS2And LiCl, putting into a zirconia ball-milling tank with an air valve in sequence, adding zirconia balls with a ball-to-material ratio of 40:1, sealing the ball-milling tank and vacuumizing the ball-milling tank, wherein the vacuum degree is less than-0.09 MPa, then putting into a planetary ball mill for ball milling, the ball-milling rotation speed is 600r/min, the ball-milling is carried out for 12 hours, vacuumizing the ball-milling tank every 3 hours, and the vacuum degree is less than-0.09 MPa. Then taking out the initial electrolyte material, putting the initial electrolyte material in an electric furnace, heating to 200 ℃ at the speed of 15 ℃/min, preserving heat for 3 hours, naturally cooling, putting the initial electrolyte material in a mortar for grinding, and sieving the ground material with a 400-mesh sieve to obtain Li6PS5Cl solid electrolyte powder. Fig. 1 is an XRD spectrum of the solid electrolyte powder. And pressing the solid electrolyte 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 3.2X 10 at room temperature-3S cm-1。
Example 2:
weighing 2N pure reagent Li according to the stoichiometric ratio of 5:2:5:22O2、P、CS2And LiCl, sequentially putting into a zirconia ball-milling tank with an air valve, adding zirconia balls with a ball-to-material ratio of 30:1, sealing the ball-milling tank and vacuumizing the ball-milling tank, wherein the vacuum degree is lower than-0.09 MPa, then putting into a planetary ball mill for ball milling, the ball-milling rotation speed is 800r/min, the ball-milling is carried out for 15 hours, and pumping one ball into the ball-milling tank every 3 hoursSub-vacuum, the vacuum degree is less than-0.09 MPa. Then taking out the initial electrolyte material, putting the initial electrolyte material in an electric furnace, heating to 300 ℃ at the speed of 10 ℃/min, preserving heat for 3 hours, naturally cooling, putting the initial electrolyte material in a mortar for grinding, and sieving the ground material with a 400-mesh sieve to obtain Li6PS5Cl solid electrolyte powder. And pressing the solid electrolyte 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 3.5X 10 at room temperature-3S cm-1。
Example 3:
weighing 2N pure reagent Li according to the stoichiometric ratio of 5:1:6:22O、P2O5、CS2And LiCl, putting into a zirconia ball-milling tank with an air valve in sequence, adding zirconia balls with a ball-to-material ratio of 40:1, sealing the ball-milling tank and vacuumizing the ball-milling tank, wherein the vacuum degree is less than-0.09 MPa, then putting into a planetary ball mill for ball milling, the ball-milling rotation speed is 600r/min, the ball-milling is carried out for 12 hours, vacuumizing the ball-milling tank every 3 hours, and the vacuum degree is less than-0.09 MPa. Then taking out the initial electrolyte material, putting the initial electrolyte material in an electric furnace, heating to 200 ℃ at the speed of 15 ℃/min, preserving heat for 3 hours, naturally cooling, putting the initial electrolyte material in a mortar for grinding, and sieving the ground material with a 400-mesh sieve to obtain Li6PS5Cl solid electrolyte powder. Fig. 1 is an XRD spectrum of the solid electrolyte powder. And pressing the solid electrolyte 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 1.3X 10 at room temperature-3S cm-1。
Example 4:
weighing 2N pure reagent Li according to the stoichiometric ratio of 5:1:5:22O、P2O5、CS2And LiCl, putting into a zirconia ball-milling tank with an air valve in sequence, adding zirconia balls with a ball-to-material ratio of 30:1, sealing the ball-milling tank and vacuumizing the ball-milling tank, wherein the vacuum degree is less than-0.09 MPa, then putting into a planetary ball mill for ball milling, the ball-milling rotation speed is 800r/min, the ball-milling is carried out for 15 hours, vacuumizing the ball-milling tank every 3 hours, and the vacuum degree is less than-0.09 MPa. Then taking out the initial electrolyte material, putting the initial electrolyte material into an electric furnace, raising the temperature to 300 ℃ at the speed of 10 ℃/min, and preserving the temperatureNaturally cooling for 3 hours, grinding in a mortar, and sieving with a 400-mesh sieve to obtain Li6PS5Cl solid electrolyte powder. And pressing the solid electrolyte 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 0.8X 10 at room temperature-3S cm-1。
Claims (5)
1. A preparation method of a AgGeranite sulfide solid electrolyte is characterized by comprising the following steps:
(1) weighing Li according to the required stoichiometric ratio2O2Or Li2O, P or P2O5，CS2And lithium salt containing X, wherein X comprises one or more of Cl, Br and I;
(2) adding the raw materials in the step (1) into a ball milling tank, sealing the ball milling tank, and performing ball milling in a decompression state to obtain an initial solid electrolyte material which is uniformly mixed;
(3) sintering the initial solid electrolyte material at low temperature under the protection of inert atmosphere, cooling, grinding and screening to obtain the high ionic conductivity Geranite type solid electrolyte, wherein,
the stoichiometric ratio in the step (1) is Li2O2:P:CS2LiX =4-5:2:3-7:1-4 or Li2O:P2O5:CS2LiX =4-5:1:3-7:1-4, the ball milling pot in the step (2) is a ball milling pot with an air valve capable of being vacuumized, and the material is any one of corundum, agate, zirconia and polytetrafluoroethylene; the vacuum degree of the decompression state in the step (2) is less than-0.08 MPa; vacuumizing the sealed ball milling tank once every 3-6 hours in the ball milling process in the step (2), wherein the vacuum degree is lower than-0.08 MPa; the low-temperature sintering in the step (3) is to raise the temperature to 150 ℃ and 400 ℃ at the temperature rise rate of 5-40 ℃/min, and naturally cool the mixture after heat preservation for 1-3 hours.
2. The method for producing a sulfide solid electrolyte according to claim 1Characterized in that a doping agent is also added in the step (2) for ball milling, wherein the doping agent is P2S3、SiS2、GeS2、SnS2、As2S3、NiS、Sb2S3、Al2O3And ZnO.
3. The method for preparing the sulfide solid electrolyte as claimed in claim 1, wherein the ball milling in the step (2) is performed by mechanical ball milling, zirconia balls are added to assist the ball milling, the ball-to-material ratio is 20-60:1, the ball milling rotation speed is 100-1200r/min, and the ball milling time is 6-60 hours.
4. The method for preparing the sulfide solid electrolyte according to claim 1, wherein the grinding and sieving in the step (3) is to screen the solid electrolyte powder by a sieve with the size of 200-600 meshes after grinding by an agate mortar.
5. The method according to claim 1, wherein the steps (1) to (3) of weighing, ball milling, sintering and grinding and screening are performed under an inert atmosphere.
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| CN114163240B (en) * | 2021-12-23 | 2022-09-09 | 湖南恩捷前沿新材料科技有限公司 | Efficient preparation method of sulfur halide compound solid electrolyte |
| CN114725490B (en) * | 2022-03-25 | 2023-11-07 | 广东马车动力科技有限公司 | Integrated sulfide solid electrolyte and preparation method and application thereof |
| 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 |
| CN115149095B (en) * | 2022-09-05 | 2023-06-27 | 中国科学院宁波材料技术与工程研究所 | High-purity sulfur silver germanium ore-phase sulfide solid electrolyte and preparation method thereof |
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