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CN-122000439-A - Method for preparing halide electrolyte and solid-state battery

CN122000439ACN 122000439 ACN122000439 ACN 122000439ACN-122000439-A

Abstract

The embodiment of the application provides a preparation method of a halide electrolyte and a solid-state battery, wherein the method comprises the following steps: firstly weighing raw materials according to components and molar ratio shown in chemical formula of the halide electrolyte, and then mixing the raw materials to obtain first precursor powder. And then presintering the first precursor powder in an inert atmosphere to obtain a first reactant. Finally, the first reactant is subjected to heat treatment in an inert atmosphere to obtain the halide electrolyte. The method is used for achieving the technical effect of improving the ion conductivity of the prepared halide electrolyte.

Inventors

  • ZHOU YUNAN
  • WU ZHEN
  • WU YANG
  • LIU JINGCHAO
  • FU XIAOLAN

Assignees

  • 浙江绿色智行科创有限公司
  • 浙江吉利控股集团有限公司

Dates

Publication Date
20260508
Application Date
20250908

Claims (9)

  1. 1. A method for preparing a halide electrolyte, comprising: weighing raw materials according to components shown in a chemical general formula of the halide electrolyte and molar ratios; mixing the raw materials to obtain first precursor powder; presintering the first precursor powder in inert atmosphere to obtain a first reactant; carrying out heat treatment on the first reactant in an inert atmosphere to obtain a halide electrolyte; Wherein the chemical general formula of the halide electrolyte is Li a MO b X c , M is Hf, zr, nb, ta or Ti, X is Cl, br or I, a is more than or equal to 0.1 and less than or equal to 5, b is more than or equal to 0<b and less than or equal to 2, and c is more than or equal to 2 and less than or equal to 6; The pre-sintering treatment is carried out on the first precursor powder in inert atmosphere to obtain a first reactant, which comprises the following steps: Determining a corresponding pre-sintering temperature according to at least one volatile element in the first precursor powder; And presintering the first precursor powder according to at least one presintering temperature in the inert atmosphere from low to high to obtain the first reactant.
  2. 2. The method for producing a halide electrolyte according to claim 1, wherein a has a value of 1≤a≤3.5, b has a value of 0≤b≤1.5, and c has a value of 4.5≤c≤5.5.
  3. 3. The method for producing a halide electrolyte according to claim 1, wherein the heat-treating the first reactant in an inert atmosphere to obtain a halide electrolyte comprises: Grinding the first reactant to obtain a ground first reactant; And carrying out heat treatment on the ground first reactant in an inert atmosphere to obtain the halide electrolyte.
  4. 4. A method for producing a halide electrolyte as claimed in any one of claims 1 to 3, wherein the pre-firing temperature of the pre-firing treatment is 150 to 350 ℃.
  5. 5. A method of preparing a halide electrolyte as claimed in any one of claims 1 to 3, wherein the sintering temperature of the heat treatment is 150 to 350 ℃ and the pre-firing temperature is lower than the sintering temperature.
  6. 6. A method for producing a halide electrolyte as claimed in any one of claims 1 to 3, wherein the pre-firing treatment is for a pre-firing period of 1 to 40 hours.
  7. 7. A method for producing a halide electrolyte as claimed in any one of claims 1 to 3, wherein the heat treatment is carried out for a sintering period of 1 to 40 hours.
  8. 8. A method of preparing a halide electrolyte as claimed in any one of claims 1 to 3, wherein the gas in the inert atmosphere is at least one of argon, nitrogen and helium.
  9. 9. A solid-state battery is characterized by comprising a positive electrode, a negative electrode and a halide electrolyte; The halide electrolyte is a halide electrolyte produced by the production method of a halide electrolyte according to any one of claims 1 to 8.

Description

Method for preparing halide electrolyte and solid-state battery Technical Field The application relates to the technical field of solid-state batteries, in particular to a preparation method of a halide electrolyte and a solid-state battery. Background The halide solid-state electrolyte is becoming a new research hot spot at present due to the key characteristics of high ionic conductivity, good deformability, excellent electrochemical oxidation stability and the like. At present, precursor powder is prepared mainly through mechanical ball milling, and then the prepared halide solid electrolyte can be obtained through annealing treatment. However, the halide electrolyte prepared by the above method has low ionic conductivity. Disclosure of Invention The embodiment of the application provides a preparation method of a halide electrolyte and a solid-state battery, which are used for achieving the technical effect of improving the ion conductivity of the prepared halide electrolyte. In a first aspect, embodiments of the present application provide a halide electrolyte having a chemical formula of Li aMObXc; Wherein M is at least one of Hf, zr, nb, ta and Ti, X is at least one of Cl, br and I, a is more than or equal to 0.1 and less than or equal to 5, b is more than or equal to 0<b and less than or equal to 2, and c is more than or equal to 2 and less than or equal to 6. In one possible embodiment, a has a value of 1≤a≤3.5, b has a value of 0≤b≤1.5, and c has a value of 4.5≤c≤5.5. In a second aspect, the present embodiment provides a method for preparing a halide electrolyte as shown in the above first aspect and/or various possible embodiments of the first aspect, the method comprising: weighing raw materials according to components shown in a chemical general formula of the halide electrolyte and molar ratios; mixing the raw materials to obtain first precursor powder; presintering the first precursor powder in inert atmosphere to obtain a first reactant; and carrying out heat treatment on the first reactant in an inert atmosphere to obtain the halide electrolyte. In one possible embodiment, the heat treating the first reactant in an inert atmosphere to obtain the halide electrolyte comprises: Grinding the first reactant to obtain a ground first reactant; And carrying out heat treatment on the ground first reactant in an inert atmosphere to obtain the halide electrolyte. In one possible embodiment, the burn-in temperature of the burn-in process is 150-350 ℃. In one possible embodiment, the sintering temperature of the heat treatment is 150-350 ℃ and the burn-in temperature is lower than the sintering temperature. In one possible embodiment, the burn-in duration of the burn-in treatment is 1 to 40 hours. In one possible embodiment, the heat treatment is performed for a sintering period of 1 to 40 hours. In one possible embodiment, the gas in the inert atmosphere is at least one of argon, nitrogen and helium. In a third aspect, embodiments of the present application provide a solid state battery comprising a positive electrode, a negative electrode, and a halide electrolyte; The halide electrolyte is a halide electrolyte as shown in the above first aspect and/or various possible embodiments of the first aspect, or a halide electrolyte prepared by the method for preparing a halide electrolyte as shown in the above second aspect and/or various possible embodiments of the second aspect. The preparation method of the halide electrolyte and the solid-state battery provided by the embodiment of the application comprise the steps of weighing raw materials according to components and molar ratios shown in a chemical general formula of the halide electrolyte, and then mixing the raw materials to obtain first precursor powder. And then presintering the first precursor powder in an inert atmosphere to obtain a first reactant. Finally, the first reactant is subjected to heat treatment in an inert atmosphere to obtain the halide electrolyte. In the technical scheme, a presintering treatment is added before the heat treatment to drive the metal element (Ta/Nb) to be fully combined with the halogen/oxygen source to form a metal oxyhalide intermediate phase. The metal oxyhalide mesophase has one dimension with disordered orientationAnionic chains. The disorder of the anion sub-lattice induces disorder distribution of a plurality of equivalent sites in the lithium ion sub-lattice, thereby reducing the energy barrier for lithium ion migration and effectively improving the ion conductivity of the halide electrolyte. Meanwhile, the technical scheme does not need to use a high-energy ball milling mode to simplify the process flow, improves the operability, reduces the preparation cost, is easy to prepare in large quantities, and is suitable for industrial production. Drawings The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and t