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A method for preparing solid electrolyte by coating powder with lithium lanthanum zirconium oxygen precursor

A technology of solid electrolyte, lithium lanthanum zirconium oxide, which is applied in circuits, electrical components, secondary batteries, etc., can solve the problems of sintering temperature, long sintering time, and insufficient fineness of powder easily mixed with impurities, and achieve easy control of preparation conditions, Lower calcination temperature and lower cost

Active Publication Date: 2016-06-01
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is: aiming at the disadvantages of the current preparation technology of lithium lanthanum zirconium oxide precursor composite powder, such as uneven mixing, powder not fine enough, easy to mix impurities, high sintering temperature and long sintering time, etc., to provide a A method for preparing lithium lanthanum zirconium oxide solid electrolyte by chemical precipitation surface coating powder, the powder prepared by this method has uniform composition, fine particle size, high purity, and its specific coating structure makes the calcination temperature of the powder low, short sintering time

Method used

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  • A method for preparing solid electrolyte by coating powder with lithium lanthanum zirconium oxygen precursor
  • A method for preparing solid electrolyte by coating powder with lithium lanthanum zirconium oxygen precursor
  • A method for preparing solid electrolyte by coating powder with lithium lanthanum zirconium oxygen precursor

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Embodiment 1

[0034] Weigh lanthanum nitrate (LaN 3 o9 ·6H 2 O) 2.6055g, zirconium nitrate (N 4 o 12 Zr·5H 2 O,) 1.722g is dissolved in 500ml water, and in the above solution, add precipitating agent ammonium carbonate ((NH 4 ) 2 CO 3 ) 0.9636g, adjust the pH of the solution with ammonia water, control the pH of the solution to be 7, make La 3+ 、Zr 4+ The ions were simultaneously precipitated, and the precipitate was subsequently filtered and washed three more times with deionized water. Weigh lithium oxalate (Li 2 C 2 o 4 ) 0.6725g was dissolved in 200ml of water, and the washed precipitate was added to the lithium oxalate solution, stirred and evaporated to crystallize in a water bath at 60°C until all the water was evaporated to obtain a precursor composite powder. Then it was calcined at 600°C for 8 hours, and the calcined powder was pressed into a tablet at 20 MPa, and then sintered at 600°C under normal pressure for 10 hours, and the obtained product was the solid electroly...

Embodiment 2

[0036] Weigh lanthanum nitrate (LaN 3 o 9 ·6H 2 O) 2.5835g, zirconium nitrate (N 4 o 12 Zr·5H 2 (O) 1.7075g is dissolved in 500ml water, adds precipitation agent ammonium carbonate ((NH 4 ) 2 CO 3 ) 1.4332g, adjust the pH of the solution with ammonia water, and control the pH of the solution to be 8, so that La 3+ 、Zr 4+ The ions were simultaneously precipitated, and the precipitate was subsequently filtered and washed three more times with deionized water. Weigh lithium oxalate (Li 2 C 2 o 4 ) 0.7090g was dissolved in 250ml of water, and the washed precipitate was added to the lithium oxalate solution, stirred and evaporated to crystallize in a water bath at 80°C until all the water was evaporated to obtain a precursor composite powder. Then it was calcined at 700°C for 6 hours, and the calcined powder was pressed into a tablet at 40 MPa, and then sintered at 700°C under normal pressure for 8 hours, and the obtained product was the solid electrolyte material of th...

Embodiment 3

[0038] Weigh lanthanum nitrate (LaN 3 o 9 ·6H 2 O) 2.5650g, zirconium nitrate (N 4 o 12 Zr·5H 2 (O) 1.6955g is dissolved in 600ml water, adds precipitation agent ammonium carbonate ((NH 4 ) 2 CO 3 ) 1.8974g, adjust the pH of the solution with ammonia water, and control the pH of the solution to be 9, so that La 3+ 、Zr 4+ The ions were simultaneously precipitated, and the precipitate was subsequently filtered and washed three more times with deionized water. Weigh lithium oxalate (Li 2 C 2 o 4 ) 0.7395g was dissolved in 250ml of water, and the washed precipitate was added to the lithium oxalate solution, stirred and evaporated to crystallize in a 90°C water bath until all the water was evaporated to obtain a precursor composite powder. Then calcined at 800°C for 4 hours, the calcined powder was sintered with electric field assistance, the sintering pressure was 20MPa, the heating rate was 300°C / min, the sintering temperature was 800°C, and the holding time was 5 min...

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Abstract

The invention discloses a method for preparing a solid electrolyte by using lithium lanthanum zirconium oxide precursor coated powder. The method specifically comprises the steps of dissolving a certain amount of lanthanum nitrate and zirconium nitrate into water, adding a precipitator, namely ammonium carbonate, controlling the pH value to ensure that La<3+> and Zr<4+> ions are simultaneously precipitated, and filtering and washing the precipitate; weighing a certain amount of lithium oxalate, dissolving lithium oxalate into water, adding the precipitate into the lithium oxalate solution, stirring, evaporating, crystallizing, and separating out lithium oxalate crystal on the surface of the precipitate to form precursor powder with a coated structure. The prepared powder has the advantages of uniform mixing, fine grains, high purity and the like; through the formed specific coated structure, the calcination temperature of the powder is low, the sintering time of the powder is short, and the room-temperature lithium ion electric conductivity of the sintered lithium lanthanum zirconium oxide is more than 2.2*10<-4>S / cm. According to the method, the process is simple, the cost is low, the preparation conditions are easy to control, and the prepared solid electrolyte is good in electrochemical stability and high in electric conductivity and can be used for preparing all-solid-state lithium ion batteries.

Description

Technical field: [0001] The invention specifically relates to a method for preparing a solid electrolyte by coating a powder with a lithium lanthanum zirconium oxide precursor, and belongs to the technical field of preparation of solid electrolyte materials. Background technique: [0002] With the rapid development of mobile phones, computers, etc., lithium-ion batteries have attracted great attention in the past few decades. Scientists are currently trying to use these batteries to power cars to avoid the carbon dioxide and other pollutants produced by traditional gasoline-powered vehicles. These new applications require lithium-ion batteries to have high safety, high energy density, long life and high temperature resistance. Current lithium-ion batteries based on liquid electrolytes cannot meet these requirements because the organic liquid electrolytes they use are flammable, volatile, leaky and decompose at high temperatures (C.A. Geiger, E. Alekseev, W. Weppner, Inorg. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562
CPCH01M10/0525H01M10/0562Y02E60/10
Inventor 张联盟张艳华陈斐涂溶沈强黄志锋
Owner WUHAN UNIV OF TECH
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