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Nasicon structure sodium ion solid electrolyte, its preparation method and solid state sodium ion battery

A solid electrolyte, sodium-ion battery technology, used in secondary batteries, circuits, electrical components, etc., can solve the problem of low ionic conductivity and achieve the effect of high conductivity

Active Publication Date: 2021-04-20
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the preparation of NASICON structure sodium ion solid electrolyte is mainly the traditional solid-phase synthesis method, which is low in cost and suitable for large-scale production. However, the ionic conductivity of the NASICON structure sodium ion solid electrolyte prepared by this method is not high.

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  • Nasicon structure sodium ion solid electrolyte, its preparation method and solid state sodium ion battery
  • Nasicon structure sodium ion solid electrolyte, its preparation method and solid state sodium ion battery
  • Nasicon structure sodium ion solid electrolyte, its preparation method and solid state sodium ion battery

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preparation example Construction

[0046] The invention provides a preparation method of a NASICON structure sodium ion solid electrolyte, comprising:

[0047] A) Na source, P source, ZrO 2 , SiO 2 mixing with metal oxides, and heat-treating the obtained mixture in a sintering atmosphere at 700-1000° C. for 6-24 hours to obtain a precursor; the sintering atmosphere is a nitrogen atmosphere, an argon atmosphere or an oxygen atmosphere;

[0048] B) heat-treating the precursor at 1000-1400°C for 2-24 hours in a sintering atmosphere to obtain a NASICON structure sodium ion solid electrolyte; the sintering atmosphere is a nitrogen atmosphere, an argon atmosphere or an oxygen atmosphere;

[0049] The NASICON structure sodium ion solid electrolyte has a general chemical formula shown in formula (I):

[0050] Na 1+2a+b-d+e+f [Zr 2-a-b-c-d A II a A Ⅲ b A Ⅳ c A V d ]Si e [P 3-e-f B Ⅳ f ]O 12 (I);

[0051] Among them, A II A divalent metal element that is doped and substituted for the Zr site; A Ⅲ A t...

Embodiment 1

[0090] Preparation of Na by solid phase method 3.1 [Zr 1.95 Mg 0.05 ]Si 2 PO 12 solid electrolyte material.

[0091] According to Na source, P source, ZrO 2 , SiO 2 The molar ratio to metal oxide is 1.55:1:1.95:2:0.05, and 0.0155mol Na 2 CO 3 , 0.01mol NH 4 h 2 PO 4 , 0.0195mol ZrO 2 , 0.02mol SiO 2 Mix with 0.0005mol MgO, ball mill evenly and dry. The obtained mixture was placed in a tube furnace and fed with oxygen. In an oxygen atmosphere, it was heated to 900° C. and kept for 6 hours. After cooling, it was ball-milled and dried to obtain a precursor powder. The precursor powder was pressed into tablets, then placed in a tube furnace and fed with oxygen, and heat-treated at 1225°C for 12 hours in an oxygen atmosphere to obtain a sheet-shaped NASICON structure sodium ion solid electrolyte sample.

[0092] The obtained flake NASICON structure sodium ion solid electrolyte sample is subjected to scanning electron microscope scanning analysis, and the results are a...

Embodiment 2

[0099] Preparation of Na by solid phase method 3.1 [Zr 1.9 sc 0.1 ]Si 2 PO 12 solid electrolyte material.

[0100] According to Na source, P source, ZrO 2 , SiO 2 The molar ratio to metal oxide is 3.1:1:1.9:2:0.05, and 0.031mol NaHCO 3 , 0.01mol (NH 4 ) 2 HPO 4 , 0.019mol ZrO 2 , 0.02mol SiO 2 and 0.0005mol Sc 2 o 3 Mix, ball mill evenly and dry. The obtained mixture was placed in a tube furnace and fed with oxygen. In an oxygen atmosphere, it was heated to 950° C. and kept for 6 hours. After cooling, it was ball-milled and dried to obtain a precursor powder. The precursor powder was pressed into tablets, then placed in a tube furnace and fed with oxygen, and heat-treated at 1275 °C for 10 h in an oxygen atmosphere to obtain a sheet-shaped NASICON structure sodium ion solid electrolyte sample.

[0101] The obtained flake NASICON structure sodium ion solid electrolyte sample is subjected to scanning electron microscope scanning analysis, and the results are as fo...

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Abstract

The present invention provides a kind of preparation method of NASICON structure sodium ion solid electrolyte, Na source, P source, ZrO 2 , SiO 2 and metal oxides are heat treated in a specific sintering atmosphere to prepare a NASICON structure sodium ion solid electrolyte with the general chemical formula shown in formula (I). The method is simple, feasible and easy to operate, can be applied to large-scale production, and has low cost. At the same time, the sodium ion solid electrolyte with NASICON structure prepared by the invention has higher room temperature ion conductivity, better chemical stability, long service life and wide applicable temperature range. The NASICON structure sodium ion solid electrolyte in the present invention is made into a solid sodium ion battery, and the obtained solid sodium ion battery has better cycle stability and rate performance.

Description

technical field [0001] The invention relates to the technical field of solid electrolyte materials, in particular to a NASICON structure sodium ion solid electrolyte, a preparation method thereof and a solid sodium ion battery. Background technique [0002] Energy is the basic condition for human survival and an important pillar for the development of the world economy. At present, the energy crisis and environmental pollution have become prominent problems restricting the sustainable development of the world and urgently need to be resolved. In order to alleviate the current situation of environmental degradation and change the existing irrational energy structure, the development and storage of new green and clean energy has become an urgent task. Due to the volatility and intermittency of green and clean energy such as solar energy, wind energy, and tidal energy, direct input to the grid will have an impact on the entire grid system, so they cannot be directly integrated...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562H01M10/054
CPCH01M10/054H01M10/0562Y02E60/10
Inventor 姚霞银杨菁刘高瞻万红利
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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