CN113363568B - Method for preparing sulfide solid electrolyte - Google Patents

Method for preparing sulfide solid electrolyte Download PDF

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Publication number
CN113363568B
CN113363568B CN202110730538.8A CN202110730538A CN113363568B CN 113363568 B CN113363568 B CN 113363568B CN 202110730538 A CN202110730538 A CN 202110730538A CN 113363568 B CN113363568 B CN 113363568B
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ball milling
solid electrolyte
sulfide solid
mixture
preparing
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CN113363568A (en
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刘延成
林坚业
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High Energy Era Zhuhai New Energy Technology Co ltd
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Shenzhen High Energy Times Technology Co ltd
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    • 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
    • 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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • 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 discloses a method for preparing sulfide solid electrolyte with low cost and low energy consumption. The method comprises the following steps: mixing Li3N, P or P3N5S to obtain a mixture; or, adding Li3N, P or P3N5Mixing S and LiX to obtain a mixture, wherein X is one or more of Cl, Br and I; and (3) carrying out high-energy ball milling on the mixture, and grinding and screening to obtain the sulfide solid electrolyte. The method uses Li3N replaces the traditional raw material Li2S, greatly reduces the production cost, and simultaneously Li3The N and other raw materials have extremely strong reactivity and release a large amount of heat in the solid-phase high-energy ball milling process, a ball milling reaction product does not need secondary sintering, a sulfide solid electrolyte is prepared in one step, the prepared electrolyte has high ionic conductivity and a wide electrochemical window, and the electrolyte is applied to preparation of an all-solid battery.

Description

Method for preparing sulfide solid electrolyte
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for preparing a sulfide solid electrolyte with low cost and low energy consumption.
Background
With the increasing demand for high energy density, high safety energy storage systems, lithium ion batteries based on conventional combustible electrolytes have presented significant challenges. The all-solid-state battery technology uses non-flammable solid electrolyte to replace the traditional liquid electrolyte, so that the safety performance of the all-solid-state battery is greatly improved, and the research on the all-solid-state electrolyte is widely concerned all over the world at present.
Up to now, three kinds of solid electrolytes, namely polymer, oxide and sulfide, have been mainstream. Among them, the sulfide solid electrolyte is considered as a favorable competitor in the all-solid lithium battery because of its extremely strong processability and extremely high ion conductivity. 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 10-2 S/cm（Kamaya et al. “A lithium superionic conductor”,2011 Nature materials, Volume 10,Pages 682-686）。
At present, Li is mainly used for preparing sulfide solid electrolyte2S and P2S5Etc. as source materials, but Li2S and P2S5The stability in the air is poor, the preparation is difficult, the cost is high, and the method is not suitable for large-scale industrial production. And the current mainstream methods all need secondary sintering of the electrolyte, increase energy consumption and are not in line with environmental protection development. How to develop a large-scale high-efficiency preparation method of the sulfide solid electrolyte is still a difficulty of the current process production.
Accordingly, the prior art remains to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a method for preparing a sulfide solid electrolyte with low cost and low energy consumption, and aims to solve the problem that the existing method for preparing a sulfide solid electrolyte adopts high-price Li2S and P2S5And the like, which leads to a problem of high production cost.
The technical scheme of the invention is as follows:
a method for preparing a sulfide solid electrolyte with low cost and low energy consumption, wherein the method comprises the following steps:
mixing Li3N, P or P3N5S to obtain a mixture; or, adding Li3N, P or P3N5Mixing S and LiX to obtain a mixture, wherein X is one or more of Cl, Br and I;
and carrying out high-energy ball milling on the mixture, and grinding and screening the mixture after ball milling to obtain the sulfide solid electrolyte.
Optionally, the step of subjecting the mixture to high-energy ball milling specifically includes:
placing the mixture in a ball milling tank, and sealing the ball milling tank in a positive pressure state;
and placing the sealed ball milling tank in a ball mill for high-energy ball milling.
Optionally, the sulfide solid electrolyte is Li3PS4、Li4P2S6Or Li7-xPS6-xXxWherein x is more than or equal to 0 and less than or equal to 2.
Alternatively, the ratio by stoichiometric ratio (1-3): (1-2): (4-7) adding Li3N, P, S mixing;
or, according to the stoichiometric ratio of (1-3) to (0.3-0.7) to (4-7), adding Li3N、P3N5And S are mixed.
Optionally, the high-energy ball milling is carried out with the aid of zirconia balls, the diameter of each zirconia ball is 5-15mm, and the mass ratio of balls to materials is 15-70: 1.
Optionally, the material of the ball milling pot is any one of corundum, agate, zirconia and polytetrafluoroethylene.
Optionally, the relative atmospheric pressure of the positive pressure state is >0.01 MPa.
Optionally, the high-energy ball milling is performed by planetary mechanical ball milling, the rotation speed of the high-energy ball milling is 400-1200 r/min, and the time of the high-energy ball milling is 4-80 h.
Optionally, the ball milling tank is a ball milling tank with a pressure reducing valve, and in the high-energy ball milling process, when the air pressure in the ball milling tank is greater than 2atm, the pressure reducing valve of the ball milling tank automatically releases pressure.
Optionally, the particle size of the sulfide solid electrolyte obtained after the grinding and screening is 10-75 μm.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the invention provides a method for quickly preparing a high-crystallinity sulfide solid electrolyte with low cost and low energy consumption. In particular with lower-priced Li3N, P or P3N5S, LiX (X is Cl, Br or I) and the like as raw materials, and expensive Li is not needed2S、P2S5Etc. while Li3N and other raw materials have extremely strong reactivity in the process of solid-phase high-energy ball milling, can release a large amount of heat to directly promote the ball-milling intermediate product to generate crystalline state transformation to generate the target crystalline state sulfide solid electrolyte, namely the ball-milling reaction product does not need secondary sintering and can be prepared into sulfide solid in one stepAnd (5) preparing a finished product of the electrolyte. The prepared sulfide solid electrolyte has higher ionic conductivity and wider electrochemical window, and is applied to preparing an all-solid battery, so that the prepared all-solid battery has high safety, high energy density and excellent cycling stability. The method has the advantages of low price of used raw materials, simple and efficient synthetic route, no need of secondary sintering of products, great reduction of production time and production cost, and suitability for large-scale industrial production of sulfide solid electrolytes.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a sulfide solid electrolyte with low cost and low energy consumption according to an embodiment of the invention.
FIG. 2 shows the measurement of Li at room temperature in example 13PS4XRD powder diffractogram of solid electrolyte powder.
FIG. 3 shows the measurement of Li at room temperature in example 26PS5XRD powder diffractogram of Cl solid electrolyte powder.
FIG. 4 shows the measurement of Li at room temperature in example 35.5PS4.5Cl1.5XRD powder diffractogram of solid electrolyte powder.
FIG. 5 shows Li test at room temperature in example 45.5PS4.5Cl0.75 Br0.75XRD powder diffractogram of solid electrolyte powder.
FIG. 6 shows Li test at room temperature in example 55.5PS4.5Cl0.75Br0.5I0.25XRD powder diffractogram of solid electrolyte powder.
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.
Fig. 1 is a schematic flow chart of a method for preparing a sulfide solid electrolyte with low cost and low energy consumption according to an embodiment of the invention, as shown in fig. 1, the method comprises the following steps:
s1, mixing Li3N, P or P3N5S to obtain a mixture; or, adding Li3N, P or P3N5Mixing S and LiX to obtain a mixture, wherein X is one or more of Cl, Br and I;
and S2, carrying out high-energy ball milling on the mixture, and carrying out grinding and screening after ball milling to obtain the sulfide solid electrolyte.
The Li source used in this example is Li3N, P the source is elemental P or P3N5The material is prepared by the following steps that S is used as a simple substance, LiX (X is one or more of Cl, Br and I) is used as an auxiliary source, and a sulfide solid electrolyte finished product is directly prepared in one step by a solid phase high energy ball milling method. This example uses Li as the method3N is Li source to replace traditional raw material Li2S, not only greatly reduces the production cost, but also Li3N and other raw materials have strong reactivity in the process of solid-phase high-energy ball milling, for example, P source is P simple substance, 2 Li3N + 8 S + 2 P → 2 Li3PS4 + N2The calculated enthalpy of reaction is Δ Hcalculated = -1482 kJ mol-1Therefore, the reaction process can release a large amount of heat. Meanwhile, nitrogen volatilizes along with the reaction, so that the reaction is rapidly carried out in the forward direction to continuously generate energy, the ball-milling intermediate product is promoted to generate crystalline state transformation, and the target crystalline state sulfide solid electrolyte is generated, namely the ball-milling reaction product does not need secondary sintering, and a sulfide solid electrolyte finished product can be prepared in one step. The prepared sulfide solid electrolyte has higher ionic conductivity and wider electrochemical window, and is applied to preparing an all-solid battery, so that the prepared all-solid battery has high safety, high energy density and excellent cycling stability.
The method has the advantages of low price of used raw materials, simple and efficient synthetic route, no need of secondary sintering, great reduction of production time and production cost, and suitability for large-scale industrial production of sulfide solid electrolytes.
In one embodiment, the sulfide solid state electrolyte may be Li3PS4、Li4P2S6Or Li7-xPS6-xXxWherein x is more than or equal to 0 and less than or equal to 2.
In step S1, in one embodiment, the ratio of (1-3): (1-2): (4-7) adding Li3N, P, S and adding LiX, wherein X is one or more of Cl, Br and I;
or, according to the stoichiometric ratio of (1-3) to (0.3-0.7) to (4-7), adding Li3N、P3N5And S, and LiX is added into the mixture, wherein X is one or more of Cl, Br and I.
In step S2, in one embodiment, the step of subjecting the mixture to high energy ball milling specifically includes:
placing the mixture in a ball milling tank, and sealing the ball milling tank in a positive pressure state;
and placing the sealed ball milling tank in a ball mill for high-energy ball milling.
In one embodiment, the relative atmospheric pressure of the positive pressure state is >0.01 MPa to ensure that air does not enter the ball mill jar during transfer.
In one embodiment, the ball milling is carried out by adopting planetary mechanical ball milling, the rotating speed of the ball milling is 400-1200 r/min, the ball milling time is 4-80 h, and the ball milling can ensure that the collision between materials is more violent and the strong reaction can occur.
In one embodiment, the high energy ball milling is performed with the aid of zirconia balls, i.e., zirconia balls are added to the milling pot to aid in the ball milling. Furthermore, the diameter of the zirconia ball is 5-15mm, and the mass ratio of the ball material (namely the mass ratio of the zirconia ball to the mixture) is 15-70: 1.
In one embodiment, the ball mill tank is a ball mill tank with a pressure relief valve. In the high-energy ball milling process, when the air pressure in the ball milling tank is more than 2atm, the pressure reducing valve of the ball milling tank automatically releases pressure.
In one embodiment, the material of the ball mill pot is any one of corundum, agate, zirconia, polytetrafluoroethylene, and the like.
In one embodiment, the step of grinding and screening after ball milling specifically comprises: grinding for a certain time, and then sieving the ground powder to obtain the sulfide solid electrolyte with proper granularity.
In one embodiment, the particle size of the sulfide solid state electrolyte obtained after the milling and sieving is 10-75 μm, such as 10-25 μm.
In one embodiment, step S2 is performed under an inert gas environment. Further, the inert gas includes, but is not limited to, Ar, N2。
The invention is further illustrated by the following specific examples.
Example 1:
weighing 2N pure reagent Li according to the stoichiometric ratio of 1:1:43N, P powder and S powder are put into a zirconia ball milling tank with an automatic pressure reducing valve, zirconia balls with the diameter of 10mm are added, and the material ball ratio is 1: 20. and packaging the ball milling tank, and filling inert gas argon to ensure that the relative pressure in the ball milling tank is more than 0.01 MPa. And (4) placing the ball milling tank after the packaging in a planetary ball mill for ball milling for 10 hours at the rotating speed of 400 r/min. Cooling the ball milling tank, and then carrying out ball milling on the sulfide solid electrolyte Li produced by the ball milling3PS4Grinding and sieving with 400 mesh sieve to obtain Li with particle size less than 40 μm3PS4And (5) obtaining a solid electrolyte finished product. Fig. 2 is an XRD spectrum of the solid electrolyte powder. Pressing solid electrolyte powder under 200MPa, maintaining the pressure for 5min to obtain solid electrolyte sheet with lithium ion conductivity of 0.75 × 10 at room temperature-3S cm-1. The whole process is carried out under the protection of argon.
Example 2:
weighing 2N pure reagent Li according to the stoichiometric ratio of 2:1:5:13N, P powder, S powder and LiCl, putting the powder, the S powder and the LiCl into a zirconia ball-milling tank with an automatic pressure reducing valve, adding zirconia balls with the diameter of 12mm, and mixing the materials according to a ball ratio of 1: 40. and packaging the ball milling tank, and filling inert gas argon to ensure that the relative pressure in the ball milling tank is more than 0.01 MPa. And (4) placing the ball milling tank after the packaging in a planetary ball mill for ball milling for 15 h, wherein the rotating speed is 800 r/min. After the ball milling tank is cooled, the balls are put into the ball milling tankSulfide solid electrolyte Li produced by grinding6PS5Cl is ground and sieved by a 300-mesh sieve to obtain Li with the granularity of less than 40 mu m6PS5And (5) preparing a Cl solid electrolyte finished product. Fig. 3 is an XRD spectrum of the solid electrolyte powder. Pressing solid electrolyte powder under 200MPa, maintaining the pressure for 5min to obtain solid electrolyte sheet with lithium ion conductivity of 3.8 × 10 at room temperature-3S cm-1. The whole process is carried out under the protection of argon.
Example 3:
weighing 2N pure reagent Li according to the stoichiometric ratio of 1.83:0.3:4.5:1.53N、P3N5S powder and LiCl are put into a zirconia ball-milling tank with an automatic pressure reducing valve, zirconia balls with the diameter of 10mm are added, and the material ball ratio is 1: 40. and packaging the ball milling tank, and filling inert gas argon to ensure that the relative pressure in the ball milling tank is more than 0.01 MPa. And (4) placing the ball milling tank after the packaging in a planetary ball mill for ball milling for 12 hours at the rotating speed of 900 r/min. Cooling the ball milling tank, and then carrying out ball milling on sulfide solid electrolyte Li5.5PS4.5Cl1.5Grinding and sieving with 300 mesh sieve to obtain Li with particle size less than 50 μm5.5PS4.5Cl1.5And (5) obtaining a solid electrolyte finished product. Fig. 4 is an XRD spectrum of the solid electrolyte powder. Pressing solid electrolyte powder under 200MPa, maintaining the pressure for 5min to obtain solid electrolyte sheet with lithium ion conductivity of 10.5 × 10 at room temperature-3S cm-1. The whole process is carried out under the protection of argon.
Example 4:
2N pure reagent Li is weighed according to the stoichiometric ratio of 1.83:0.3:4.5:0.75:0.753N、P3N5S powder, LiCl and LiBr are put into a zirconia ball-milling tank with an automatic pressure reducing valve, zirconia balls with the diameter of 15mm are added, and the material ball ratio is 1: 40. and packaging the ball milling tank, and filling inert gas argon to ensure that the relative pressure in the ball milling tank is more than 0.01 MPa. And (4) placing the ball milling tank after the packaging in a planetary ball mill for ball milling for 20 hours at the rotating speed of 1200 r/min. Cooling the ball milling tank, and then carrying out ball milling on sulfide solid electrolyte Li5.5PS4.5Cl0.75Br0.75Grinding and sieving with 300 mesh sieve to obtain Li with particle size less than 50 μm5.5PS4.5Cl0.75Br0.75And (5) obtaining a solid electrolyte finished product. Fig. 5 is an XRD spectrum of the solid electrolyte powder. Pressing solid electrolyte powder under 200MPa, maintaining the pressure for 5min to obtain solid electrolyte sheet with lithium ion conductivity of 9.8 × 10 at room temperature-3S cm-1. The whole process is carried out under the protection of argon.
Example 5:
weighing 2N pure reagent Li according to the stoichiometric ratio of 1.83:1:4.5:0.75:0.5:0.253N, P powder, S powder, LiCl, LiBr and LiI, putting the powder into a zirconia ball-milling tank with an automatic pressure release valve, adding zirconia balls with the diameter of 5mm, wherein the material-ball ratio is 1: 70. and packaging the ball milling tank, and filling inert gas argon to ensure that the relative pressure in the ball milling tank is more than 0.01 MPa. And (4) placing the ball milling tank after the packaging in a planetary ball mill for ball milling for 20 hours at the rotating speed of 1000 r/min. Cooling the ball milling tank, and then carrying out ball milling on sulfide solid electrolyte Li5.5PS4.5Cl0.75Br0.5I0.25Grinding and sieving with 300 mesh sieve to obtain Li with particle size less than 50 μm5.5PS4.5Cl0.75Br0.5I0.25And (5) obtaining a solid electrolyte finished product. Fig. 6 is an XRD spectrum of the solid electrolyte powder. Pressing solid electrolyte powder under 200MPa, maintaining the pressure for 5min to obtain solid electrolyte sheet with lithium ion conductivity of 2.1 × 10 at room temperature-3S cm-1. The whole process is carried out under the protection of argon.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations are possible to those skilled in the art in light of the above teachings, and that all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.

Claims (9)

1. A method of preparing a sulfide solid state electrolyte, comprising the steps of:
mixing Li3N, P or P3N5S to obtain a mixture; or, adding Li3N, P or P3N5Mixing S and LiX to obtain a mixture, wherein X is one or more of Cl, Br and I;
carrying out high-energy ball milling on the mixture, and grinding and screening the mixture after ball milling to obtain the sulfide solid electrolyte;
the sulfide solid electrolyte is Li3PS4Or Li7-xPS6-xXxWherein x is more than or equal to 0 and less than or equal to 2.
2. The method according to claim 1, wherein the step of subjecting the mixture to high energy ball milling comprises:
placing the mixture in a ball milling tank, and sealing the ball milling tank in a positive pressure state;
and placing the sealed ball milling tank in a ball mill for high-energy ball milling.
3. The method for producing a sulfide solid electrolyte according to claim 1 or 2, wherein the ratio of (1-3): (1-2): (4-7) adding Li3N, P, S mixing;
or, according to the stoichiometric ratio of (1-3) to (0.3-0.7) to (4-7), adding Li3N、P3N5And S are mixed.
4. The method for producing a sulfide solid electrolyte according to claim 1 or 2, wherein the high energy ball milling is performed with the aid of zirconia balls having a diameter of 5 to 15mm and a ball-to-material mass ratio of 15 to 70: 1.
5. The method for preparing a sulfide solid electrolyte according to claim 2, wherein the material of the ball mill pot is any one of corundum, agate, zirconia and polytetrafluoroethylene.
6. The method of producing a sulfide solid state electrolyte according to claim 2, wherein the relative atmospheric pressure of the positive pressure state is >0.01 MPa.
7. The method for preparing the sulfide solid electrolyte as claimed in claim 1 or 2, wherein the high energy ball milling is performed by a planetary mechanical ball milling, the rotation speed of the high energy ball milling is 400-.
8. The method of claim 2, wherein the ball milling pot is a ball milling pot with a pressure relief valve, and the pressure relief valve automatically relieves pressure when the pressure in the ball milling pot is greater than 2atm during the high energy ball milling process.
9. The method for producing a sulfide solid electrolyte according to claim 1 or 2, wherein the particle size of the sulfide solid electrolyte obtained after the grinding and sieving is 10 to 75 μm.
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