Cl <-> doped epsilon-LiVOPO4 lithium fast ion conductor and liquid phase preparation method thereof

A lithium fast ion and lithium ion technology, applied in chemical instruments and methods, structural parts, inorganic chemistry, etc., can solve the problems of high temperature, high energy consumption, etc., and achieve the improvement of uniformity, uniform reaction raw materials, and favorable conduction Effect

Active Publication Date: 2021-01-29
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in occasions where the current requirement is high, the conductivity often reaches 5.0×10 -4 Only about S / cm can meet the needs of the normal operation of the battery. In addition, the synthesis temperature of the fast ion conductor is about 1350°C, which is high in temperature and consumes a lot of energy.

Method used

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  • Cl &lt;-&gt; doped epsilon-LiVOPO4 lithium fast ion conductor and liquid phase preparation method thereof
  • Cl &lt;-&gt; doped epsilon-LiVOPO4 lithium fast ion conductor and liquid phase preparation method thereof
  • Cl &lt;-&gt; doped epsilon-LiVOPO4 lithium fast ion conductor and liquid phase preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015]Example 1: According to LiVO(PO4)0.95Cl0.15Solid LiNO in stoichiometric molar ratio3, NH4H2PO4, LiCl, V2O5And 6 times V2O5The moles of oxalic acid are evenly mixed. While stirring vigorously, add deionized water until all the solid matter is dissolved. Note the mass of the added deionized water, and then continue to add 1.0 times the mass of the recorded deionized water. Ionized water and stir evenly and record this solution as I; mix 3 times the moles of chlorine in solution I of ethylenediaminetetraacetic acid and 2 times the moles of chlorine in solution I of ethylene glycol, mix and add The ammonia water containing the chlorine moles of ammonia in solution I was stirred vigorously while adding deionized water until all the solid matter was dissolved, and again noted the mass of the added deionized water, and then continued to add the deionized water recorded this time 3 times the mass of deionized water and stir it evenly and record this solution as II; add solution II to ...

Embodiment 2

[0016]Example 2: According to LiVO(PO4)0.9Cl0.3Solid LiNO in stoichiometric molar ratio3, NH4H2PO4, LiCl, V2O5And 6 times V2O5The moles of oxalic acid are mixed uniformly. While stirring vigorously, add deionized water until all the solid matter is dissolved. Note the mass of the added deionized water, and then continue to add 1.5 times the mass of the recorded deionized water. Ionized water and stir evenly and record this solution as I; mix 3 times the moles of chlorine in solution I of nitrilotriacetic acid and 2 times the moles of chlorine in solution I of glycerol, mix and add 10 times that of solution I Add the deionized water to the ammonia water with medium chlorine moles of ammonia while vigorously stirring until all the solid matter is dissolved, and again record the mass of the deionized water added, and then continue to add the deionized water recorded this time 5 Double the mass of deionized water and stir it evenly and record this solution as II; add solution II to solu...

Embodiment 3

[0017]Example 3: According to LiVO(PO4)0.93Cl0.21, Where: x = 0.05-0.10, the stoichiometric molar ratio of solid LiNO3, NH4H2PO4, LiCl, V2O5And 6 times V2O5The moles of oxalic acid are mixed uniformly. While vigorously stirring, add deionized water until all the solid matter is dissolved. Note the mass of the added deionized water, and then continue to add 1.2 times the mass of the recorded deionized water. Ionized water and stir evenly and record this solution as I; mix 3 times the moles of chlorine in solution I of nitrilotriacetic acid and 2 times the moles of chlorine in solution I of glycerol, mix and add 10 times that of solution I Add the deionized water to the ammonia water with medium chlorine moles of ammonia while vigorously stirring until all the solid matter is dissolved, and again record the mass of the deionized water added, and then continue to add the deionized water quality recorded this time 4 Double the mass of deionized water and stir it evenly and record this s...

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Abstract

The invention relates to a Cl-doped epsilon LiVOPO4 lithium fast ion conductor and a liquid phase preparation method, and the Cl-doped epsilon LiVOPO4 lithium fast ion conductor is characterized in that the stoichiometric formula is LiVO (PO4)1-xCl3x, and x is equal to 0.05-0.10; through Cl-doping, the acting force for conducting lithium ions and a crystal framework is reduced, the conduction activation energy of the lithium ions is greatly reduced, and the activity capability and the conductivity of the lithium ions are improved; in addition, through two calcining processes, the reaction rawmaterials are more uniform, and the purity of the obtained material is higher; the concentration of oxygen vacancies and defects in the material is increased through rapid room-temperature cooling, and conduction of the lithium ions is facilitated; through liquid-phase synthesis, a multi-component auxiliary agent is adopted, so that the uniformity degree of each component of reactants is improved,and a high-purity product can be obtained; and due to the measures, the normal-temperature lithium ion conductivity of the lithium fast ion conductor exceeds 5 * 10 < -4 > S/cm, and the application of the lithium fast ion conductor is facilitated.

Description

Technical field[0001]The invention relates to the manufacturing field of solid lithium fast ion conductors.Background technique[0002]Fast ionic conductor, also known as super ionic conductor, refers to a type of ionic conductivity comparable to that of liquid electrolyte in a certain temperature range (10-6S / cm) and low ion conductivity activation energy (generally less than 0.4eV). Fast ion conductors have important applications in the fields of energy storage battery electrode materials, gas detectors, solid electrolyte membranes, super-capacity capacitors, timers, coulomb counters and electrochromic displays.[0003]The migration rate of carriers in fast ion conductors is often much lower than the charge transfer on the electrode surface and the ion diffusion rate in the electrode material, which becomes the rate control step in the entire electrode reaction kinetics, so the development has a higher lithium ion conductivity The lithium fast ion conductor is the key to the developme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455H01M4/58H01M10/0525
CPCC01B25/455H01M4/5825H01M10/0525C01P2006/40Y02E60/10
Inventor 水淼舒杰任元龙
Owner NINGBO UNIV
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