CN114824247A - Inorganic solid electrolyte coated high-voltage positive electrode material and preparation method and application thereof - Google Patents

Inorganic solid electrolyte coated high-voltage positive electrode material and preparation method and application thereof Download PDF

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CN114824247A
CN114824247A CN202210494975.9A CN202210494975A CN114824247A CN 114824247 A CN114824247 A CN 114824247A CN 202210494975 A CN202210494975 A CN 202210494975A CN 114824247 A CN114824247 A CN 114824247A
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solid electrolyte
positive electrode
voltage positive
inorganic solid
electrode material
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张希
朱金辉
陈振营
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Shanghai Yili New Energy 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy

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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
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  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to the field of solid-state batteries, in particular to an inorganic solid-state electrolyte coated high-voltage positive electrode material, and a preparation method and application thereof a MX b . The invention has the beneficial effects that: by coating a layer of inorganic solid electrolyte on the surface of the high-voltage positive active material in situ, compared with the traditional coating materials such as zirconium dioxide, aluminum oxide and other transition metal oxides, sulfides and polymer solid electrolyte, the inorganic solid electrolyteThe electrolyte has good conductivity, does not generate side reaction with the high-voltage positive active material, and improves the performance of the full battery; the high-voltage positive electrode material obtained by the method has high matching degree with sulfide electrolyte, is used for all-solid-state batteries, and has better cycle performance.

Description

Inorganic solid electrolyte coated high-voltage positive electrode material and preparation method and application thereof
Technical Field
The invention relates to the field of solid-state batteries, in particular to an inorganic solid-state electrolyte coated high-voltage positive electrode material and a preparation method and application thereof.
Background
The all-solid-state battery uses non-flammable solid electrolyte to replace traditional organic flammable electrolyte, fundamentally avoids the safety problem, at present, the solid electrolyte mainly comprises oxide, sulfide and polymer solid electrolyte, wherein the oxide solid electrolyte is not afraid of water and oxygen, has more stable physical and chemical properties, but has lower conductivity. The polymer solid electrolyte is formed by complexing polar macromolecules and metal salts, has good film-forming property, flexibility and high safety performance, but has lower conductivity, smaller transference number of lithium ions and poorer mechanical performance. The sulfide solid electrolyte has ion conductivity comparable to that of a liquid electrolyte solution, has a wide electrochemical window, can be adapted to a high-voltage positive electrode material, and has serious side reactions with a high-voltage positive electrode active substance, so that the performance of the full battery is influenced.
Patent CN 109659507 a discloses a method for using a ternary material coated with a solid electrolyte of a sodium ion superconductor (NASICON structure) in an all-solid-state battery, the method selecting an inorganic solid electrolyte of this type with a conductivity of 10 - 6 S.cm -1 ～10 -2 S.cm -1 The lithium ion battery has low conductivity, is coated on the surface of a positive electrode material, is used in an all-solid-state battery with an electrolyte material being sulfide solid electrolyte, and has influence on the transmission rate of lithium ions, thereby influencing the performance of the all-solid-state battery. The synthesis method comprises the steps of grinding raw materials required for synthesizing the inorganic solid electrolyte by a grinding machine to obtain precursor slurry, mixing the precursor slurry with the anode, removing redundant volume by a spray drying mode, and finally sintering to obtain the coated anode material. The method is long in time consumption, and the cost is greatly increased from the point of commercialization.
Therefore, those skilled in the art have made an effort to develop a positive electrode material to solve the problems of low conductivity and poor mechanical properties in the prior art, to avoid side reactions between the solid electrolyte and the high-voltage positive electrode active material, to improve the performance of the full cell, and to provide an efficient synthesis method.
Disclosure of Invention
In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present invention is that the solid electrolyte in the prior art has low conductivity and poor mechanical properties, and is prone to side reaction with the high-voltage positive electrode active material.
In order to achieve the aim, the invention provides an inorganic solid electrolyte coated high-voltage positive electrode material, and a preparation method and application thereof.
The high-voltage positive electrode material coated with the inorganic solid electrolyte comprises a high-voltage positive electrode active substance and the inorganic solid electrolyte coated on the surface of the high-voltage positive electrode active substance, wherein the inorganic solid electrolyte is a halide solid electrolyte Li a MX b 。
In a preferred embodiment of the present invention, the halide solid electrolyte is Li a MX b M is selected from one or more of Sc, Y, La-Lu, Al, Ga, In, Ti, V, Gr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Mg and Pb, and X is one or more of F, Cl, Br and I.
In a preferred embodiment of the present invention, the high voltage positive electrode active material is LiCoO 2 、LiNi x Co y Mn 1-x-y O 2 、LiNi x Co y Al 1-x-y O 2 、LiFe x Mn 1-x PO 4 、LiNi 0.5 Mn 1.5 O 4 Wherein 0 is one or a mixture of two or more of<x<1，0<y<1 and x + y<1。
In a preferred embodiment of the present invention, the high voltage positive electrode active material particles have a particle size of 6 to 10 μm.
In a preferred embodiment of the present invention, the inorganic solid electrolyte particles have a particle size of 1 to 20 μm.
In a preferred embodiment of the present invention, the inorganic solid electrolyte is coated to a thickness of 1 to 100 nm.
In a preferred embodiment of the present invention, the conductivity of the coated inorganic solid-state dot electrolyte is 0.5 to 25ms -1 。
The invention also provides a preparation method of the inorganic solid electrolyte coated high-voltage cathode material, which comprises the following steps:
step 1, dissolving a raw material for synthesizing the inorganic solid electrolyte in an ultra-dry solvent in an inert atmosphere to obtain a precursor solution;
step 2, putting the high-voltage positive active substance into the precursor solution and stirring;
and 3, drying the mixed solution in the step 2 in vacuum to obtain the inorganic solid electrolyte coated high-voltage positive electrode material.
In a preferred embodiment of the present invention, the ultra-dry solvent in step 1 is a non-polar or low-polar solvent.
The invention also provides an all-solid-state battery which comprises a positive electrode part, a negative electrode part and a sulfide solid-state electrolyte part, wherein the positive electrode part, the negative electrode part and the sulfide solid-state electrolyte part are constructed by the inorganic solid-state electrolyte coated high-voltage positive electrode material.
The invention has the beneficial effects that:
1. compared with the traditional coating materials such as zirconium dioxide, aluminum oxide and other transition metal oxides, sulfides and polymer solid electrolytes, the inorganic solid electrolyte has good conductivity, does not generate side reaction with the high-voltage positive active material, and improves the performance of the full battery.
2. The high-voltage positive electrode material obtained by the method has the advantages that the inorganic solid electrolyte layer coated by the high-voltage positive electrode material has relatively high ionic conductivity, high chemical stability and insensitivity to moisture in the air, the electrochemical stability is good when the high-voltage positive electrode material is mixed with the high-voltage positive electrode active material, the formation of space charge is inhibited, the problems of violent side reaction between the sulfide solid electrolyte and the high-voltage positive electrode active material and unmatched electrochemical windows when the sulfide solid electrolyte and the high-voltage positive electrode active material are mixed for use are successfully solved, and the cycle performance is better.
3. The invention has simple and efficient process and low cost, and is suitable for commercial mass production.
Drawings
Fig. 1 is an XRD pattern of a solid electrolyte coated ternary high voltage positive electrode material prepared in example 1 of the present invention;
fig. 2 is a graph comparing rate performance of an all-solid-state battery assembled with a solid electrolyte coated ternary high voltage positive electrode material prepared in example 1 of the present invention;
fig. 3 is a graph comparing rate performance of an all-solid-state battery assembled with a ternary high-voltage positive electrode material without a solid electrolyte according to comparative example 1 of the present invention.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
In one embodiment of the invention, the inorganic solid electrolyte coated high-voltage positive electrode material comprises a high-voltage positive electrode active substance and an inorganic solid electrolyte coated on the surface of the high-voltage positive electrode active substance, wherein the inorganic solid electrolyte is a halide solid electrolyte Li a MX b 。
In a preferred embodiment of the present invention, the halide solid electrolyte is Li a MX b M is selected from one or more of Sc, Y, La-Lu, Al, Ga, In, Ti, V, Gr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Mg and Pb, and X is one or more of F, Cl, Br and I.
In another preferred embodiment of the present invention, the high voltage positive active material is LiCoO 2 、LiNi x Co y Mn 1-x-y O 2 、LiNi x Co y Al 1-x-y O 2 、LiFe x Mn 1-x PO 4 、LiNi 0.5 Mn 1.5 O 4 Wherein 0 is one or a mixture of two or more of<x<1，0<y<1 and x + y<1。
The preparation method of the inorganic solid electrolyte material coated high-voltage anode material comprises the following steps:
(1) under the argon atmosphere, raw materials required for synthesizing the inorganic solid electrolyte are weighed according to the molar ratio and dissolved in an ultra-dry solvent, and the precursor solution is obtained by stirring.
(2) And (2) adding the high-voltage positive electrode active substance into the precursor solution in the step (1), and stirring.
(3) And (3) drying the mixed solution in the step (2) in vacuum to obtain the high-voltage anode material coated by the inorganic solid electrolyte material.
Preferably, the ultra-dry solvent in step (1) is a non-polar or low-polar solvent including one of anhydrous THF, Ethylenediamine (EDA), Ethyl Propionate (EP), N-methylformamide (NMF) Ethyl Acetate (EA)1, 2-Dimethylaminomethane (DME) or a mixed solvent such as THF-ethanol.
Preferably, the stirring time in step (1) is 6-10 h. The rotation speed is 800 and 1000 rpm.
Preferably, the stirring time in step (2) is 2-5 h. The rotation speed is 200-500rpm
Preferably, the vacuum drying time in the step (3) is 8-12h, and the temperature is 80-200 ℃.
The working atmosphere in step (1) is preferably an argon atmosphere, and other inert gases capable of realizing corresponding conditions are also in an alternative range.
In a preferred embodiment of the present invention, the positive electrode part is formed by mixing a high-voltage positive electrode active material coated with an inorganic solid electrolyte, a sulfide solid electrolyte, and conductive carbon, and the positive electrode active material is one or more of spinel-type transition metal oxide, lithium transition metal oxide having a layered structure, and olivine.
The invention also relates to an all-solid-state battery which comprises a positive electrode part, a negative electrode part and a sulfide solid electrolyte part, wherein the preparation method of the all-solid-state battery comprises the steps of firstly preparing the positive electrode part, mixing the positive electrode active substance coated by the inorganic solid electrolyte, the conductive carbon and the sulfide solid electrolyte according to a certain proportion, grinding and uniformly mixing the positive electrode active substance, the conductive carbon and the sulfide solid electrolyte, and pressing the mixture into a positive electrode sheet to prepare the positive electrode part.
The all-solid-state battery assembling step is that solid electrolyte powder is placed in a tabletting mold and is pressed into a solid electrolyte sheet to form a solid electrolyte part, then the positive plate is placed on one side of the solid electrolyte sheet and is pressed under pressure, and finally lithium foil is attached to the other side of the solid electrolyte sheet to form the all-solid-state battery with a sandwich structure.
Example 1
LiCl and InCl are weighed in a glove box according to the molar ratio of 3:1 3 Then adding the reactant raw materials into a round-bottom flask, adding an ultra-dry solvent DME, and fully contacting and reacting the reactant raw materials in the solvent to obtain the solid electrolyte Li 3 InCl 6 Precursor paste, said LiCl, InCl 3 The molar ratio of 3:1 can reduce the generation of intermediate products and ensure the purity of precursor slurry; adding LiNi 0.8 Co 0.1 Mn 0.1 O 2 Stirring for 2 hours; and then vacuum drying is carried out to obtain the ternary high-voltage anode material coated with the inorganic solid electrolyte in situ, namely the high-voltage anode material coated with the solid electrolyte, which is represented as Li3InCl6@ NCM 811.
And (3) mixing the inorganic solid electrolyte coated positive electrode material obtained in the step (3), the sulfide solid electrolyte material, the conductive carbon and the binder in a ratio of 75:20:1:4, and grinding the mixture uniformly to obtain positive electrode powder. The positive electrode powder is dissolved in DME, the mixture is magnetically stirred uniformly and then coated on an aluminum foil, the positive electrode part is formed by mixing according to the proportion, and the coated inorganic solid electrolyte layer has relatively high ionic conductivity, high chemical stability, insensitivity to moisture in air, good electrochemical stability when being mixed with a high-pressure positive electrode active substance and inhibition of formation of space charge, so that the problems of violent side reactions between the sulfide solid electrolyte and the high-pressure positive electrode active substance and mismatching of electrochemical windows when being mixed and used are successfully solved. And placing the powder of the sulfide solid electrolyte material in a tabletting mold, pressing into a solid electrolyte sheet, then placing the positive plate on one side of the solid electrolyte sheet, pressing under pressure, finally attaching a lithium sheet on the other side of the solid electrolyte sheet, and pressing into the all-solid-state battery. Referring to fig. 1 to 2, fig. 1 is an XRD pattern of a solid electrolyte coated ternary high voltage positive electrode material prepared in example 1, and fig. 2 is a graph comparing rate performance of an all-solid battery assembled with the solid electrolyte coated ternary high voltage positive electrode material prepared in example 1.
Example 2
LiCl and YCl are weighed in a glove box according to the molar ratio of 3:1 3 Then adding the reactant raw materials into a round-bottom flask, adding an ultra-dry solvent DME, and allowing the reactant raw materials to fully contact and react in the solvent to obtain the solid electrolyte Li 3 InCl 6 Precursor slurry; adding LiNi 0.8 Co 0.1 Mn 0.1 O 2 Stirring for 2 hours; vacuum drying is carried out to obtain the ternary high-voltage anode material coated with the inorganic solid electrolyte in situ, namely the solid electrolyte coated high-voltage anode material is represented as Li 3 YCl 6 @NCM811。
And (3) mixing the inorganic solid electrolyte coated high-voltage positive electrode material obtained in the step (3), the sulfide solid electrolyte, the conductive carbon and the binder in a ratio of 75:20:1:4, and grinding the mixture uniformly to obtain positive electrode powder. Dissolving the anode powder in DME, and coating the mixture on an aluminum foil after uniformly stirring by magnetic force. And placing the powder of the sulfide solid electrolyte material in a tabletting mold, pressing into a solid electrolyte sheet, then placing the positive plate on one side of the solid electrolyte sheet, pressing under pressure, finally attaching a lithium sheet on the other side of the solid electrolyte sheet, and pressing into the all-solid-state battery.
Example 3
LiCl and ScCl are weighed in a glove box according to the molar ratio of 3:1 3 Adding reactant raw materials into a round-bottom flask, adding an ultra-dry solvent DME, and allowing the reactant raw materials to fully contact and react in the solvent to obtain the solid electrolyte Li 3 InCl 6 Precursor slurry; adding LiNi 0.8 Co 0.1 Mn 0.1 O 2 Stirring for 6 hours; vacuum drying is carried out to obtain the ternary high-voltage anode material coated with the inorganic solid electrolyte in situ, namely the solid electrolyte coated high-voltage anode material is represented as Li 3 ScCl 6 @NCM811。
And (4) mixing the solid electrolyte coating high-voltage positive electrode material obtained in the step (3), the sulfide solid electrolyte, the conductive carbon and the binder in a ratio of 75:20:1:4, and grinding the mixture uniformly to obtain positive electrode powder. Dissolving the anode powder in DME, and coating the mixture on an aluminum foil after uniformly stirring by magnetic force. And placing the powder of the sulfide solid electrolyte material in a tabletting mold, pressing into a solid electrolyte sheet, then placing the positive plate on one side of the solid electrolyte sheet, pressing under pressure, finally attaching a lithium sheet on the other side of the solid electrolyte sheet, and pressing into the all-solid-state battery.
Comparative example 1
Positive electrode material LiNi 0.8 Co 0.1 Mn 0.1 O 2 Without coating treatment, fig. 3 is a graph comparing rate performance of an all-solid-state battery assembled by a ternary cathode material without coating a solid electrolyte in comparative example 1, which is otherwise the same as example 1.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims (10)

1. The inorganic solid electrolyte coated high-voltage positive electrode material is characterized by comprising a high-voltage positive electrode active substance and an inorganic solid electrolyte coated on the surface of the high-voltage positive electrode active substance, wherein the inorganic solid electrolyte is a halide solid electrolyte Li a MX b 。
2. The inorganic solid electrolyte coated high voltage positive electrode material of claim 1, wherein the halide solid electrolyte Li a MX b M is one or more selected from Sc, Y, La-Lu, Al, Ga, In, Ti, V, Gr, Mn, Fe, Co, Ni, Cu, Zn, Cd, Mg and Pb, and X is F, Cl, Br or IOne or more of (a).
3. The inorganic solid electrolyte coated high voltage positive electrode material according to claim 1, wherein the high voltage positive electrode active material is LiCoO 2 、LiNi x Co y Mn 1-x-y O 2 、LiNi x Co y Al 1-x-y O 2 、LiFe x Mn 1-x PO 4 、LiNi 0.5 Mn 1.5 O 4 Wherein 0 is one or a mixture of two or more of<x<1，0<y<1 and x + y<1。
4. The inorganic solid electrolyte coated high voltage positive electrode material according to claim 1, wherein the high voltage positive electrode active material particles have a particle size of 6 to 10 μm.
5. The inorganic solid electrolyte coated high voltage positive electrode material according to claim 1, wherein the inorganic solid electrolyte particles have a particle size of 1 to 20 μm.
6. The inorganic solid electrolyte coated high voltage positive electrode material according to claim 1 to 5, wherein the thickness of the coated inorganic solid electrolyte is 1 to 100 nm.
7. The inorganic solid electrolyte coated high voltage positive electrode material according to claim 1 to 5, wherein the conductivity of the coated inorganic solid electrolyte is 0.5 to 25ms -1 。
8. A method of preparing the inorganic solid electrolyte coated high voltage positive electrode material of claim 1, comprising the steps of:
step 1, dissolving a raw material for synthesizing the inorganic solid electrolyte in an ultra-dry solvent in an inert atmosphere to obtain a precursor solution;
step 2, putting the high-voltage positive active substance into the precursor solution and stirring;
and 3, drying the mixed solution in the step 2 in vacuum to obtain the inorganic solid electrolyte coated high-voltage positive electrode material.
9. The method according to claim 8, wherein the ultra-dry solvent in step 1 is a non-polar or low-polar solvent.
10. An all-solid battery comprising a positive electrode part, a negative electrode part and a sulfide solid electrolyte part, which are constructed of the inorganic solid electrolyte-coated high-voltage positive electrode material according to claim 1.
CN202210494975.9A 2022-05-07 2022-05-07 Inorganic solid electrolyte coated high-voltage positive electrode material and preparation method and application thereof Withdrawn CN114824247A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115275331A (en) * 2022-08-16 2022-11-01 中国科学技术大学 Halide all-solid-state battery material and preparation method and application thereof
CN115395087A (en) * 2022-09-06 2022-11-25 上海屹锂新能源科技有限公司 Coated solid electrolyte material and preparation method and application thereof
CN117154080A (en) * 2023-10-31 2023-12-01 有研(广东)新材料技术研究院 Coated halide positive electrode composite material and preparation method and application thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115275331A (en) * 2022-08-16 2022-11-01 中国科学技术大学 Halide all-solid-state battery material and preparation method and application thereof
CN115275331B (en) * 2022-08-16 2024-07-05 中国科学技术大学 Halide all-solid-state battery material, and preparation method and application thereof
CN115395087A (en) * 2022-09-06 2022-11-25 上海屹锂新能源科技有限公司 Coated solid electrolyte material and preparation method and application thereof
CN117154080A (en) * 2023-10-31 2023-12-01 有研(广东)新材料技术研究院 Coated halide positive electrode composite material and preparation method and application thereof
CN117154080B (en) * 2023-10-31 2024-02-23 有研(广东)新材料技术研究院 All-solid-state battery coated halide positive electrode composite material and preparation method and application thereof

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