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NASICON-type sodion solid electrolyte material and preparation method thereof

A solid electrolyte and sodium-ion battery technology, applied in the field of materials, can solve the problems of low ion conductivity and achieve the effects of simple preparation process, good safety performance, and low manufacturing cost

Active Publication Date: 2016-07-06
INST OF PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its ionic conductivity is far lower than that of liquid electrolytes, which has become a major factor limiting its application in all-solid-state batteries.

Method used

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  • NASICON-type sodion solid electrolyte material and preparation method thereof
  • NASICON-type sodion solid electrolyte material and preparation method thereof
  • NASICON-type sodion solid electrolyte material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1 of the present invention provides a solid electrolyte material, the general chemical formula is:

[0054] [Na 3+x-2y A y ][Zr 2-x M x ][Si 2-z M’ z ]PO 12 ;

[0055] Among them, A is a divalent alkaline earth metal element that dope and replace Na site, specifically one or more of Ca, Sr, and Ba; M is an element that dope and replace octahedral Zr site, specifically La One or more of, Y, Al, In, and Ga; M'is an element for doping and replacing the Si site, specifically one or two of Ge and Se;

[0056] The x, y, and z are respectively the mole percentages of the corresponding elements; where 0≤x≤0.3, 0≤y≤0.2, 0≤z≤0.3, and x, y, and z are not 0 at the same time.

[0057] in Figure 1-6 In the paper, the X-ray diffraction (X-ray diffraction, XRD) patterns of NASICON-type sodium ion solid electrolyte materials doped with different elements and different concentrations are given.

[0058] The NASICON type sodium ion solid electrolyte material provided in this embodimen...

Embodiment 2

[0060] This embodiment provides a method for preparing a NASICON-type sodium ion solid electrolyte material, specifically a solid phase method, such as Figure 7 Shown, including:

[0061] In step 701, the required stoichiometric amount of sodium is 110wt% to 115wt% of sodium carbonate and the required stoichiometric amount of A carbonate and / or nitrate, ZrO 2 , SiO 2 , GeO 2 And / or SeO 2 , NH 4 H 2 PO 4 And / or (NH 4 ) 2 HPO 4 And M oxides are mixed in proportion to form a precursor;

[0062] Specifically, the A is specifically one or more of Ca, Sr, and Ba, and the M is specifically one or more of La, Y, Al, Ga, and In.

[0063] Step 702, uniformly mixing the precursors by a ball milling method to obtain precursor powders;

[0064] Step 703: Place the precursor powder in a muffle furnace and heat-treat it in an air atmosphere at 750°C to 950°C for 10 to 24 hours;

[0065] In step 704, the heat-treated precursor powder is ground and compressed.

[0066] Step 705, sintering in an air atmo...

Embodiment 3

[0069] This embodiment provides a method for preparing a NASICON-type sodium ion solid electrolyte material, specifically a sol-gel method, such as Figure 8 Shown, including:

[0070] Step 801: Mix ethyl orthosilicate (TEOS), water, and ethanol at a molar ratio of 1:10:20, add the required stoichiometric amount of germanium isopropoxide and citric acid, and stir at room temperature to 70°C 1 hour, hydrolyze TEOS to form a mixed solution;

[0071] In step 802, the required stoichiometric amount of sodium is 110wt% to 115wt% of sodium nitrate or sodium acetate, the required stoichiometric amount of A nitrate and / or acetate, zirconyl nitrate, and M nitrate and / or The aqueous solution of acetate is sequentially added to the mixed solution, and then NH is added dropwise 4 H 2 PO 4 And / or (NH 4 ) 2 HPO 4 , To obtain a colorless and transparent sol;

[0072] Specifically, the A is specifically one or more of Ca, Sr, and Ba, and M is specifically one or more of La, Y, Al, Ga, and In;

[007...

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Abstract

The invention discloses an NASICON-type sodion solid electrolyte material and a preparation method thereof. A chemical general formula of the solid electrolyte material is [Na<3+x-2y>A<y>][Zr<2-x>M<x>][Si<2-z>M'<z>]PO<12>, wherein A is an Na-doped and substituted bivalent alkaline-earth metal element, particularly one or more of Ca, Sr and Ba; M is an octahedral Zr-doped and substituted element, in particularly one or more of La, Y, Al, In and Ga; M' is an Si-doped and substituted element, in particularly one or two of Ge and Se; x, y and z are mol percentages of the corresponding elements respectively; x is smaller than or equal to 0.3 and greater than or equal to 0; y is smaller than or equal to 0.2 and greater than or equal to 0; z is smaller than or equal to 0.3 and greater than or equal to 0; and x, y and z are not 0 at the same time.

Description

Technical field [0001] The invention relates to the technical field of materials, in particular to a NASICON type sodium ion solid electrolyte material and a preparation method thereof. Background technique [0002] Lithium ion secondary battery has the advantages of large specific energy density, wide operating temperature range, long charge and discharge life, small self-discharge, and small memory-free effect. Its mass energy density can reach 270Wh / kg, which is considered to be the most promising chemical power supply. Since Sony commercialized it in 1990, it has not only occupied a leading position in the field of small mobile consumer electronics such as notebook computers, mobile phones, camcorders, digital cameras, MP3, etc., but also in the field of power batteries and energy storage batteries in recent years. Eye-catching development prospects. [0003] However, the earth's lithium resources are not rich. The abundance of lithium in the earth's crust is only 0.0065%, an...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/05
CPCY02E60/10
Inventor 胡勇胜章志珍徐凯琪陈立泉黄学杰
Owner INST OF PHYSICS - CHINESE ACAD OF SCI
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