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Highly conductive solid electrolyte prepared by coprecipitation method

A technology of solid electrolyte and co-precipitation method, which is applied in the field of high-conductivity solid electrolyte, can solve problems such as environmental pollution, many chemical reagents, and large safety hazards, and achieve easy control and simple operation, excellent electrochemical stability, and small environmental pollution Effect

Inactive Publication Date: 2020-03-06
GUIZHOU MEILING POWER SUPPLY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, Ge 4+ and Ti 4+ will be reduced by lithium, leading to a significant increase in interfacial resistance, which in turn makes the electrochemical stability of these two materials unsatisfactory for lithium.
[0004] The general co-precipitation method is to prepare the ions to be precipitated into a uniformly mixed solution in advance, and then use a certain precipitant to make the ions in the system reach the precipitation conditions to be precipitated, which is usually used to prepare ultrafine nanopowders; this method It has the characteristics of easy operation, but there are too many chemical reagents in this method, which is easy to cause environmental pollution and has great safety hazards. Secondly, the solid electrolyte prepared by coprecipitation method has low ion conductivity.
[0005] At present, only the preparation of Ce 0.8 m 0.2 o 1.9 Research on the Properties of Solid Electrolytes", how to use co-precipitation to prepare solid electrolytes with NASICON structure is still under study

Method used

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  • Highly conductive solid electrolyte prepared by coprecipitation method
  • Highly conductive solid electrolyte prepared by coprecipitation method
  • Highly conductive solid electrolyte prepared by coprecipitation method

Examples

Experimental program
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Embodiment 1

[0032] A method for preparing a high-conductivity solid electrolyte by coprecipitation, comprising the steps of:

[0033] Step 1: Weigh the dopant, aluminum nitrate, tetrabutyl titanate, and ammonium dihydrogen phosphate, put the raw materials into the reaction container in turn, and stir continuously at room temperature until a light yellow slurry is formed;

[0034] Step 2: Slowly add ammonia water to the light yellow slurry to dissolve, and adjust the pH to 12;

[0035] Step 3: Heat the reaction vessel to 88°C, and magnetically stir in a constant temperature water bath for 0.8h to form a uniform and stable layered white precipitate;

[0036] Step 4: transfer the white precipitate to a blast drying oven, and heat at 145°C for 9.7 hours to obtain a white precursor;

[0037] Step 5: Heat the white precursor to the pre-calcination temperature (650°C) at a heating rate of 3°C / min in the air, and keep it warm for 8 hours to obtain a white powder;

[0038] Step 6: Use a planetar...

Embodiment 2

[0045] A method for preparing a high-conductivity solid electrolyte by coprecipitation, comprising the steps of:

[0046] Step 1: Weigh the dopant, aluminum nitrate, tetrabutyl titanate, and ammonium dihydrogen phosphate, put the raw materials into the reaction container in turn, and stir continuously at room temperature until a light yellow slurry is formed;

[0047] Step 2: Slowly add ammonia water to the light yellow slurry to dissolve, and adjust the pH to 12;

[0048] Step 3: Heat the reaction vessel to 90°C, and magnetically stir in a constant temperature water bath for 1.1 hours to form a uniform and stable layered white precipitate;

[0049] Step 4: transfer the white precipitate into a blast drying oven, and heat at 155°C for 10.3 hours to obtain a white precursor;

[0050] Step 5: Heat the white precursor to the pre-calcination temperature (750°C) at a heating rate of 5°C / min in the air, and keep it warm for 12 hours to obtain a white powder;

[0051] Step 6: Use a p...

Embodiment 3

[0058] A method for preparing a high-conductivity solid electrolyte by coprecipitation, comprising the steps of:

[0059] Step 1: Weigh the dopant, aluminum nitrate, tetrabutyl titanate, and ammonium dihydrogen phosphate, put the raw materials into the reaction container in turn, and stir continuously at room temperature until a light yellow slurry is formed;

[0060] Step 2: Slowly add ammonia water to the light yellow slurry to dissolve, and adjust the pH to 7;

[0061] Step 3: Heat the reaction vessel to 88-90°C, and magnetically stir in a constant temperature water bath for 1 hour to form a uniform and stable layered white precipitate;

[0062] Step 4: transfer the white precipitate to a blast drying oven, and heat at 150°C for 10 hours to obtain a white precursor;

[0063] Step 5: Heat the white precursor to the pre-calcination temperature (700°C) at a heating rate of 5°C / min in the air, and keep it warm for 10 hours to obtain a white powder;

[0064] Step 6: Use a plan...

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Abstract

The invention relates to the technical field of solid electrolytes, and in particular, relates to a highly conductive solid electrolyte prepared by a coprecipitation method, wherein a preparation method comprises the steps: step 1, weighing a dopant, aluminum nitrate, tetrabutyl titanate and ammonium dihydrogen phosphate, sequentially putting the raw materials into a reaction container, and continuously stirring at room temperature until faint yellow slurry is formed; step 2, slowly adding ammonia water into the faint yellow slurry and dissolving; step 3, heating the reaction container to 88-90 DEG C, and carrying out constant-temperature water bath magnetic stirring for 0.8-1.1 h, to form a white precipitate; step 4, transferring the white precipitate into a blast drying oven, and heatingto obtain a white precursor; step 5, presintering the white precursor to obtain white powder; and step 6, carrying out ball milling on the white powder, tabletting, molding and calcining to obtain asolid electrolyte sintered body. The solid electrolyte provided by the invention has an NASICON structure, small interface resistance and excellent electrochemical stability, and the particle size reaches nanoscale.

Description

technical field [0001] The invention relates to the technical field of solid electrolytes, in particular to a high-conductivity solid electrolyte prepared by a co-precipitation method. Background technique [0002] Among many emerging energy storage technologies, lithium batteries are still the most promising energy storage devices. The application fields range from portable electronic devices to electric vehicles, hybrid vehicles and smart grids. All-solid-state lithium batteries can provide higher energy density and Safety has become the development direction of next-generation energy storage technology. Solid electrolyte is the core material of all-solid-state lithium batteries, which must meet a series of high ion conductivity, a large number of vacancies and charge carriers, wide electrochemical window and low electronic conductivity. Requirements, electrolytes with NASICON structure have been widely used in the field of electrochemical energy storage due to their good ...

Claims

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Application Information

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IPC IPC(8): C04B35/447C04B35/622H01M10/0562
CPCC04B35/447C04B35/622C04B2235/443C04B2235/447C04B2235/48C04B2235/483H01M10/052H01M10/0562H01M2300/0068Y02E60/10
Inventor 石斌杨程响王庆杰陈晓涛陈铤王振吴宁宁张红梅张亮康树森
Owner GUIZHOU MEILING POWER SUPPLY CO LTD
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