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Mg < 2 + > doped and modified NASCION type sodium ion solid electrolyte and preparation method thereof

A technology of solid electrolytes and sodium ions, applied in solid electrolytes, non-aqueous electrolytes, circuits, etc., can solve the problems of low room temperature sodium ion conductivity and complex synthesis process, so as to improve room temperature sodium ion conductivity, stable and mature process, Effects with universality and industrial applicability

Pending Publication Date: 2022-03-11
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the technical problems such as low room temperature sodium ion conductivity and complex synthesis process in the NASCION type sodium ion solid electrolyte and its improved type in the prior art, the purpose of the present invention is to provide a Mg 2+ Doping-modified NASCION-type sodium-ion solid-state electrolyte and its preparation method, by optimizing the synthesis process and using Mg 2+ For Zr in the NASCION structure 2+ position doping to further improve the room temperature lithium ion conductivity of the NASCION type sodium ion solid electrolyte and improve the structural stability of the solid electrolyte, so that it can meet the application requirements of all solid sodium ion batteries

Method used

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  • Mg &lt; 2 + &gt; doped and modified NASCION type sodium ion solid electrolyte and preparation method thereof
  • Mg &lt; 2 + &gt; doped and modified NASCION type sodium ion solid electrolyte and preparation method thereof
  • Mg &lt; 2 + &gt; doped and modified NASCION type sodium ion solid electrolyte and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The present embodiment is prepared by the general formula Na 3.3 Zr 2-x Mg x Si 2.3 P 0.7 o 12-x Expressed Mg 2+ The doped modified NASCION type sodium ion solid electrolyte, where x=0.05, specifically includes the following steps:

[0030] (1) Ingredients: with Na 3 PO 4 ﹒ 12H 2 O, Na 2 CO 3 ﹒ h 2 O, SiO 2 , ZrO 2 , MgO as raw material, according to the general formula Na 3.3 Zr 2- x Mg x Si 2.3 P 0.7 o 12-x Determine the molar ratio to weigh the ingredients;

[0031] (2) Primary ball milling: use absolute ethanol as the wet grinding medium for each raw material prepared in step (1), mix and wet grind the planetary ball mill for 12 hours until fully mixed, and obtain primary powder after drying, and use the primary powder in a mold Dry press under 10MPa into a columnar disc, that is, a primary billet, for later use;

[0032] (3) Calcination: calcining the primary billet at 1200°C for 12 hours to obtain a calcined block;

[0033] (4) Secondary b...

Embodiment 2

[0037] The present embodiment is prepared by the general formula Na 3.3 Zr 2-x Mg x Si 2.3 P 0.7 o 12-x Expressed Mg 2+ The doped modified NASCION type sodium ion solid electrolyte, where x=0.10, specifically includes the following steps:

[0038] (1) Ingredients: with Na 3 PO 4 ﹒ 12H 2 O, Na 2 CO 3 ﹒ h 2 O, SiO 2 , ZrO 2 , MgO as raw material, according to the general formula Na 3.3 Zr 2- x Mg x Si 2.3 P 0.7 o 12-x Determine the molar ratio to weigh the ingredients;

[0039] (2) Primary ball milling: use absolute ethanol as the wet grinding medium for each raw material prepared in step (1), mix and wet grind the planetary ball mill for 12 hours until fully mixed, and obtain primary powder after drying, and use the primary powder in a mold Dry press under 10MPa into a columnar disc, that is, a primary billet, for later use;

[0040] (3) Calcination: calcining the primary billet at 1200°C for 12 hours to obtain a calcined block;

[0041] (4) Secondary b...

Embodiment 3

[0045] The present embodiment is prepared by the general formula Na 3.3 Zr 2-x Mg x Si 2.3 P 0.7 o 12-x Expressed Mg 2+ The doped modified NASCION type sodium ion solid electrolyte, where x=0.05, specifically includes the following steps:

[0046] (1) Ingredients: with Na 3 PO 4 ﹒ 12H 2 O, Na 2 CO 3 ﹒ h 2 O, SiO 2 , ZrO 2 , MgO as raw material, according to the general formula Na 3.3 Zr 2- x Mg x Si 2.3 P 0.7 o 12-x Determine the molar ratio to weigh the ingredients;

[0047] (2) Primary ball milling: use absolute ethanol as the wet grinding medium for each raw material prepared in step (1), and wet-mill the planetary ball mill for 8 hours until fully mixed, and obtain primary powder after drying, and use the primary powder in a mold Dry press under 10MPa into a columnar disc, that is, a primary billet, for later use;

[0048] (3) Calcination: calcining the primary billet at 1100°C for 8 hours to obtain a calcined block;

[0049] (4) Secondary ball mil...

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Abstract

The invention discloses a Mg < 2 + > doped and modified NASCION type sodium ion solid electrolyte and a preparation method thereof, the general formula of the solid electrolyte is Na < 3.3 > Zr < 2-x > Mg < x > Si < 2.3 > P < 0.7 > O < 12-x >, and x is more than or equal to 0.05 and less than or equal to 0.10 in the general formula. The solid electrolyte is prepared by adopting a traditional solid phase method, and the preparation method comprises the working procedures of batching, primary ball milling, compression molding, pre-sintering, secondary ball milling, compression molding, sintering, gold plating and the like. According to the Mg < 2 + > doped and modified NASCION type sodium ion solid-state electrolyte provided by the invention, the NASCION type sodium ion solid-state electrolyte with excellent room-temperature lithium ion conductivity performance is obtained by optimizing a synthesis process and doping Mg < 2 + > at a Zr < 2 + > site in a NASCION structure, and the total room-temperature sodium ion conductivity of the NASCION type sodium ion solid-state electrolyte can reach 4.8 mS / cm. The preparation method of the sodion solid electrolyte is stable and mature in process, the adopted raw materials are easy to obtain, and the sodion solid electrolyte has universality and industrial practicability and is easy to industrialize.

Description

technical field [0001] The invention belongs to the field of sodium-ion solid-state batteries, and relates to a NASCION-type sodium-ion solid-state electrolyte, in particular to a Mg 2+ Doping modified NASCION type sodium ion solid state electrolyte and preparation method thereof. Background technique [0002] With the rapid consumption of fossil fuels, the greenhouse effect and environmental problems caused by the massive emission of carbon dioxide are becoming more and more serious. The development of large-scale efficient and clean energy storage technology has attracted the attention of researchers from all over the world. In recent years, sodium batteries have become a research hotspot due to their abundant resources, low cost, and similar chemical properties to lithium batteries. However, most of the current reported studies on sodium batteries are based on liquid electrolytes in organic solvents, such as ethers and carbonates. Organic solvents are flammable and easy...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/054
CPCH01M10/054H01M10/0562H01M2300/0068Y02E60/10
Inventor 朱小红江跃李雪燕刘鑫程星晏乔宏
Owner SICHUAN UNIV
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