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Preparation method of Na3+2xZr2-xMxSi2PO12 solid electrolyte powder material

A solid electrolyte and powder material technology, applied in electrolytes, circuits, electrical components, etc., can solve the problems of powder agglomeration, low conductivity, high reaction temperature, etc., and achieve lower sintering temperature, high reactivity, and lower reaction temperature. Effect

Active Publication Date: 2016-11-02
黑龙江省工研院资产经营管理有限公司
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AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to solve the problems of high reaction temperature, low electrical conductivity and serious agglomeration of powder obtained by the existing sol-gel process in the existing high-temperature solid-phase method, and provide a Na 3+2x Zr 2–x m x Si 2 PO 12 Preparation method of solid electrolyte powder material

Method used

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  • Preparation method of Na3+2xZr2-xMxSi2PO12 solid electrolyte powder material
  • Preparation method of Na3+2xZr2-xMxSi2PO12 solid electrolyte powder material
  • Preparation method of Na3+2xZr2-xMxSi2PO12 solid electrolyte powder material

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specific Embodiment approach 1

[0025] Specific embodiment one: a kind of Na of this embodiment 3+2x Zr 2–x m x Si 2 PO 12 The preparation method of solid electrolyte powder material is carried out according to the following steps:

[0026] 1. NaNO 3 , ZrO(NO 3 ) 2 2H 2 O, M (NO 3 ) 2 ·nH 2 O and (NH 4 ) 2 HPO 4 Dissolve in deionized water respectively to obtain NaNO with a concentration of 1.5mol / L~6mol / L 3 Solution, ZrO(NO 3 ) 2 Solution, M(NO 3 ) 2 Solution and concentration of 0.25mol / L~1mol / L (NH 4 ) 2 HPO 4 solution; the M(NO 3 ) 2 ·nH 2 M=Co in O 2+ 、Ni 2+ , Zn 2+ or Mg 2+ ;

[0027] 2. Add deionized water and dispersant to absolute ethanol, stir until the dispersant is completely dissolved to obtain a dispersant solution, then add TEOS to the dispersant solution, use a magnetic stirrer at a speed of 15r / min to 25r / min Stir under the condition of mixing until uniform, then drop the catalyst to adjust the pH to 0.5-3.5, and then hydrolyze for 1h-5h at a temperature of 40-60...

specific Embodiment approach 2

[0039] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the dispersant in step 2 is citric acid, PEG1000 or CTAB. Other steps and parameters are the same as those in the first embodiment.

specific Embodiment approach 3

[0040] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the catalyst described in step 2 is concentrated nitric acid, oxalic acid or acetic acid. Other steps and parameters are the same as those in Embodiment 1 or 2.

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Abstract

A preparation method of a Na3+2xZr2-xMxSi2PO12 solid electrolyte powder material is disclosed. The invention belongs to the technical field of solid electrolyte materials and especially relates to a preparation method of a natrium super ionic conductor powder material. The invention aims to solve the problems of high reaction temperature and low conductivity by existing high-temperature solid state methods and the problem that powders obtained by existing sol-gel technologies are severely agglomerated. The method provided by the invention comprises the following steps: Step 1, dissolving NaNO3, ZrO(NO3)2.2H2O, M(NO3)2.nH2O and (NH4)2HPO4 by the use of deionized water; Step 2, adding deionized water and a dispersant into anhydrous ethanol, adding TEOS, and adjusting pH; Step 3, successively dropwise adding four solutions obtained in the Step 1 into sol obtained in the Step 2; Step 4, standing and ageing under sealed and light-proof conditions, and drying to obtain a precursor; and Step 5, calcining and grinding to obtain the Na3+2xZr2-xMxSi2PO12 powder.

Description

technical field [0001] The invention belongs to the technical field of solid electrolyte materials, in particular to a preparation method of a sodium fast ion conductor powder material. Background technique [0002] At present, traditional secondary batteries mostly use liquid electrolytes, which are prone to problems such as liquid leakage and electrode corrosion, and may explode at high temperatures. In contrast, solid-state electrolytes have high thermal stability, reliability, long cycle life, and diverse geometric configurations. Na + with Li + It has a similar intercalation and conduction mechanism, and the Na element is widely distributed in the earth's crust, with an abundance of 2.64%. It is easy to obtain and low in price, and can be used in the field of stationary energy storage. This means that the sodium ion electrolyte has a good application prospect. Therefore, sodium ion solid electrolytes have received extensive attention. [0003] Sodium fast ion condu...

Claims

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Application Information

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IPC IPC(8): C01B33/32H01M10/0562
CPCC01B33/32C01P2002/72C01P2004/03C01P2004/62H01M10/0562H01M2300/0071Y02E60/10
Inventor 刘占国贺思博任哲欧阳家虎
Owner 黑龙江省工研院资产经营管理有限公司
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