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Preparation method of NASICON type lithium fast ion conductor

A lithium fast ion and conductor technology, applied in chemical instruments and methods, inorganic chemistry, electrical components, etc., can solve problems such as poor density, low phase purity of ceramic materials, and low electrical conductivity

Inactive Publication Date: 2013-12-25
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for preparing NASICON-type structural compounds are mainly traditional high-temperature solid-phase method, melt-cooling method, etc. Although the preparation process of this method is simple, but the energy consumption is high, the obtained ceramic material has low phase purity, low electrical conductivity, and porosity. Many, poor density
These shortcomings limit the application of NASICON-type materials to a certain extent

Method used

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  • Preparation method of NASICON type lithium fast ion conductor
  • Preparation method of NASICON type lithium fast ion conductor
  • Preparation method of NASICON type lithium fast ion conductor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Adjust the oil bath temperature to 90°C, dissolve 17.6ml tetrabutyl titanate in 300ml, 0.2mol / L citric acid solution, and stir for 20 hours to form a sol. Lithium nitrate, aluminum nitrate, and ammonium dihydrogen phosphate were mixed according to the stoichiometric ratio of Li 1.1Al 0.1 Ti 1.9 (PO 4 ) 3 (x=0.1) ingredients, dissolved in 250ml, 0.2mol / L citric acid solution, slowly added to the sol, stirred for 0.5h, added 6.12ml of ethylene glycol, adjusted the oil bath temperature to 120°C, heated for 5h Take it out and form a gel. Put the gel in a corundum crucible in a muffle furnace, adjust the temperature to 150°C, and keep it warm for 8 hours to make it into a dry gel. Grinding the xerogel into powder particles in an agate mortar (in the present invention, the powder particles have no size requirement, as long as they are in granular form). The powder particles were placed in the crucible in the muffle furnace again, the heating rate was 2°C / min, the temper...

Embodiment 2

[0036] Adjust the oil bath temperature to 90°C, dissolve 17.6ml tetrabutyl titanate in 300ml, 0.2mol / L citric acid solution, and stir for 20 hours to form a sol. Lithium nitrate, aluminum nitrate, and ammonium dihydrogen phosphate were mixed according to the stoichiometric ratio of Li 1.2 Al 0.2 Ti 1.8 (PO 4 ) 3 (x=0.2) Ingredients, dissolved in 250ml, 0.2mol / L citric acid solution, slowly added to the sol, stirred for 0.5h, added 6.12ml of ethylene glycol, adjusted the oil bath temperature to 120°C, heated for 5h Take it out and form a gel. Put the gel in a corundum crucible in a muffle furnace, adjust the temperature to 150°C, and keep it warm for 8 hours to make it into a dry gel. Grind the xerogel into powder particles in an agate mortar. The powder particles were placed in the crucible in the muffle furnace again, the temperature was adjusted to 500°C, the heating rate was 2°C / min, and the temperature was kept for 4h, and then the temperature was raised to 800°C, an...

Embodiment 3

[0039] Adjust the oil bath temperature to 90°C, dissolve 17.6ml tetrabutyl titanate in 300ml, 0.2mol / L citric acid solution, and stir for 20 hours to form a sol. Lithium nitrate, aluminum nitrate, and ammonium dihydrogen phosphate were mixed according to the stoichiometric ratio of Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 (x=0.3) ingredients, after dissolving in 250ml, 0.2mol / L citric acid solution, slowly add to the sol, after stirring for 0.5h, add 6.12ml of ethylene glycol, adjust the oil bath temperature to 120°C, heat for 5h Take it out and form a gel. Put the gel in a corundum crucible in a muffle furnace, adjust the temperature to 150°C, and keep it warm for 8 hours to make it into a dry gel. Grind the xerogel into powder particles in an agate mortar. The powder particles were placed in the crucible in the muffle furnace again, the heating rate was 2°C / min, the temperature was adjusted to 500°C, and kept for 4h, then the temperature was raised to 800°C, and kept for 2h. Af...

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Abstract

The invention discloses a preparation method of an NASICON type lithium fast ion conductor. The preparation method comprises the following steps: adding butyl titanate into a citric acid solution, uniformly stirring the solution, adding a citric acid solution of lithium nitrate, aluminum nitrate and diammonium phosphate, uniformly stirring the solution and adding ethylene glycol, heating the solution to a certain temperature, and stirring the solution to completely gelatinize the same; drying the gel to obtain dry gel, and grinding and calcining the dry gel to obtain precursor powder; and grinding the precursor powder fine powder, carrying out isostatic press molding on the fine powder on a tablet press to obtain an electrolyte sheet of the NASICON type lithium fast ion conductor. The preparation method is used for reducing the sintering temperature of the material, perfecting the sintering performance of the material and improving the density of the material to improve the ionic conductivity of the material. The ionic conductivity of the NASICON type lithium fast ion conductor prepared by the preparation method reaches 6.34*10<-4> S / cm (25 DEG C), so that compared with a traditional preparation method, the ionic conductivity is significantly improved.

Description

technical field [0001] The invention belongs to the field of preparation of lithium fast ion conductors, in particular to a preparation method of a NASICON type lithium fast ion conductor. Background technique [0002] Energy issues and environmental issues have become two bottlenecks restricting the development of human society. It is speculated that by 2050, human demand for electrical energy will be twice what it is now. In order to reduce dependence on petroleum, renewable energy such as solar energy, wind energy, and tidal energy have been widely valued, researched, and utilized. In the process of effectively utilizing these energy sources, energy storage and transmission problems need to be solved urgently. Research and development of efficient, safe and green chemical power sources is an effective way to solve this problem. [0003] Solid electrolytes are key materials for next-generation high-performance energy storage devices and are effective alternatives to liqu...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M10/0562
CPCY02E60/10
Inventor 朱文贾迎宾李镜人赵旭东
Owner HUAZHONG UNIV OF SCI & TECH
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