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A kind of preparation method of lithium lanthanum zirconium oxide powder

A lithium lanthanum zirconium oxide and oxide powder technology, applied in electrochemical generators, electrolytes, structural parts, etc., can solve problems such as lowering temperature and energy consumption, and achieves lower calcination temperature, lower grain size, and lower energy consumption. energy consumption effect

Active Publication Date: 2020-08-28
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the above-mentioned technical status of LLZO, the present invention aims to improve the preparation method of LLZO powder, reduce the grain size of LLZO powder on the one hand, and reduce the temperature in the preparation process on the other hand, thereby not only reducing energy consumption, but also avoiding the It is necessary to add an excess lithium source to compensate for the loss of lithium due to high temperature during synthesis and sintering.

Method used

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  • A kind of preparation method of lithium lanthanum zirconium oxide powder
  • A kind of preparation method of lithium lanthanum zirconium oxide powder
  • A kind of preparation method of lithium lanthanum zirconium oxide powder

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Embodiment 1

[0031] In this example, the LLZO powder is made of Li 7 La 3 Zr 2 o 12 The matrix is ​​composed of doping element aluminum, Li:La:Zr:Al=7:3:2:0.24, and the synthesis steps are as follows:

[0032] (1) Put equivalent lithium acetate in a beaker, add water and magnetically stir for several minutes to dissolve completely, and obtain a clear and transparent solution;

[0033] (2) Add citric acid monohydrate with 15% product mass as an ion complexing agent and a powder leavening agent, stir magnetically for several minutes until completely dissolved, and obtain a clear and transparent solution;

[0034] (3) to the equivalent nano-Al in the above-mentioned clear transparent solution 2 o 3 Powder, magnetically stirred to obtain a uniform milky white suspension;

[0035] (4) Weigh the equivalent La 2 o 3 For the powder, pour it into the ball mill jar together with the above solution, and mechanically mill it for 2-3 hours;

[0036] (5) Weigh the equivalent of ZrO with high sp...

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Abstract

The invention provides a preparation method of LLZO powder. The LLZO powder is prepared by adopting soluble lithium acetate as a lithium source, water as a solvent medium and ZrO2 with high specific surface area as a coating template of a lithium salt through simple mechanical ball-milling and drying and calcining methods. According to the method, reduction of the grain size is facilitated, reduction of the calcination temperature is facilitated, the grain size of the prepared LLZO powder is in nanoscale, the phase is single and the energy consumption is low. The problem that the excessive lithium source needs to be added to compensate the loss of a lithium element due to high temperature in synthesis and sintering when the powder is synthesized is solved; and a compact sheet body with good lithium ion conductivity can be further obtained through granulation, compaction and sintering.

Description

technical field [0001] The invention belongs to the technical field of lithium lanthanum zirconium oxide oxide, and in particular relates to a preparation method of lithium lanthanum zirconium oxide powder. Background technique [0002] Traditional commercial lithium-ion batteries use organic electrolytes, which have potential safety hazards such as electrolyte leakage, combustion, and explosion. Lithium-sulfur, lithium-air batteries, and new battery anodes to increase energy density often use metallic lithium. The generation of lithium dendrites will cause short circuits in batteries and affect safe use. The all-solid-state battery using solid electrolyte fundamentally solves the short-circuit problem of the battery, improves safety, and is also beneficial to Invention and application of energy density battery. [0003] Inorganic oxide lithium-ion conductor Li with garnet structure 7 La 3 Zr 2 o 12 Since (LLZO) was discovered and prepared by Murugan et al. in 2007, it...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0525H01M10/0562H01M2300/0077Y02E60/10
Inventor 潘星星王建新官万兵
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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