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Nasicon type sodium ion solid electrolyte material and preparation method thereof

A solid electrolyte, sodium ion battery technology, applied in the field of materials, can solve problems such as low ionic conductivity, and achieve the effects of simple preparation process, good safety performance, and excellent cycle performance

Active Publication Date: 2018-02-13
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 sodium ion solid electrolyte material and preparation method thereof
  • Nasicon type sodium ion solid electrolyte material and preparation method thereof
  • Nasicon type sodium ion 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 with a general chemical formula:

[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 is doped and substituted for the Na site, specifically one or more of Ca, Sr, and Ba; M is an element that is doped and substituted for the octahedral Zr site, specifically La , one or more of Y, Al, In, Ga; M' is an element for doping and replacing the Si site, specifically one or two of Ge and Se;

[0056] Said x, y, and z are the molar percentages of the corresponding elements; wherein 0≤x≤0.3, 0≤y≤0.2, 0≤z≤0.3, and x, y, z are not 0 at the same time.

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

[0058] The NASICON type sodium ion solid electrolyte material prov...

Embodiment 2

[0060] This embodiment provides a preparation method of a NASICON type sodium ion solid electrolyte material, specifically a solid phase method, such as Figure 7 shown, including:

[0061] Step 701, the sodium carbonate of required stoichiometric 110wt%~115wt% and the carbonate and / or nitrate of required stoichiometric A, 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, Ba, and the M is specifically one or more of La, Y, Al, Ga, In.

[0063] Step 702, using a ball milling method to uniformly mix the precursor to obtain a precursor powder;

[0064] Step 703, placing the precursor powder in a muffle furnace, and heat-treating 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 pressed into tablets.

[0066] Step 705, sintering in an ai...

Embodiment 3

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

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

[0071] Step 802, the stoichiometric 110wt%~115wt% sodium nitrate or sodium acetate of required sodium, the nitrate and / or acetate of required stoichiometric A, zirconium oxynitrate, and the nitrate of M and / or Aqueous solution of acetate was added in the mixed solution successively, and then NH 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, Ba, and M is specifically one or more of La, Y, Al, Ga, In;

[0073] Step 803, heating up ...

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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 field of material technology, in particular to a NASICON type sodium ion solid electrolyte material and a preparation method thereof. Background technique [0002] Lithium-ion secondary batteries have the advantages of large specific energy density, wide operating temperature range, long charge and discharge life, small self-discharge, and no memory effect. Its mass energy density can reach 270Wh / kg, and it is considered to be the most promising chemical power supply. Since Sony commercialized it in 1990, it has not only occupied a dominant position in the field of small mobile consumer electronics such as notebook computers, mobile phones, video cameras, digital cameras, and MP3, but also has shown impressive performance in the fields of power batteries and energy storage batteries in recent years. Eye-catching development prospects. [0003] However, the lithium resources on the earth are not abundant. The abundance of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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