Ultrafine-grained garnet type solid electrolyte powder and preparation method thereof

A solid electrolyte and garnet-type technology, which is applied in the manufacture of electrolyte batteries, electrolytes, non-aqueous electrolyte batteries, etc., can solve the problems of unsuitable industrial production, complicated operation, and long cycle, so as to avoid waste, reduce sintering temperature, and reduce The effect of production costs

Pending Publication Date: 2020-10-16
CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, although the co-precipitation method, sol-gel method, etc. can theoretically obtain ultra-fine LLZO powders with uniform particle size, in fact, during the high-temperature calcination synthesis process, the precursors are agglomerated, resulting in the final product. Still need ball milling Crushing is carried out by advanced technology, and this type of method is complex in operation, long in cycle and low in output, and is not suitable for large-scale industrial production

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  • Ultrafine-grained garnet type solid electrolyte powder and preparation method thereof
  • Ultrafine-grained garnet type solid electrolyte powder and preparation method thereof
  • Ultrafine-grained garnet type solid electrolyte powder and preparation method thereof

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preparation example Construction

[0055] A garnet-type lanthanum lithium zirconate (LLZO) solid electrolyte powder with ultrafine particle size and a preparation method thereof, the method specifically comprising the following steps:

[0056] (1) Preparation of mixed slurry: weigh the compounds of lithium, lanthanum, zirconium, and doping elements according to a predetermined ratio (for example, taking Nb doping as an example, wherein lithium hydroxide is 6.6 parts, lanthanum oxide is 1.5 parts, oxide 1.6 parts of zirconium, 0.2 parts of niobium oxide, the preparation of L i6.6 La 3 Zr 1.6 Nb 0.4 o 12 powder), and mixed with ball milling solvent and ball milling medium in respective proportions to prepare mixed slurry;

[0057] In (1) of this step, the compound forms of lithium, lanthanum, zirconium and dopant elements include but not limited to oxides, nitrates, carbonates, hydroxides and the like. Preferably, lithium hydroxide, lanthanum oxide, zirconium oxide and niobium oxide are used in this embodime...

Embodiment 1

[0073] Lithium hydroxide, lanthanum oxide, zirconia, and niobium oxide were weighed according to the stoichiometric ratio, wherein 6.6 parts of lithium hydroxide, 1.5 parts of lanthanum oxide, 1.6 parts of zirconia, and 0.2 parts of niobium oxide were used to prepare Li 6.6 La 3 Zr 1.6 Nb 0.4 o 12 Powder. Add the above raw materials into a nylon ball mill jar, add isopropanol with a mass ratio of 1.5:1, and yttrium-stabilized zirconia ball milling media with a mass ratio of 5:1, wherein the diameters of yttrium-stabilized zirconia are 3mm and 6mm, and its mass The ratio is 1:1.4. The mixed raw materials were placed in a planetary ball mill for ball milling, the ball milling speed was 800r / min, and the ball milling time was 6h. The obtained mixed raw material slurry was placed in a blast drying oven, and dried at 70° C. for 20 h to obtain mixed raw material powder. Put the mixed raw material powder in a corundum crucible, vibrate the powder and place it in a muffle furnac...

Embodiment 2

[0076] Lithium hydroxide, lanthanum oxide, zirconia, and niobium oxide were weighed according to the stoichiometric ratio, wherein lithium hydroxide was 6.8 parts, lanthanum oxide was 1.5 parts, zirconia was 1.8 parts, and niobium oxide was 0.1 part, to prepare Li 6.8 La 3 Zr 1.8 Nb 0.2 o 12 Powder. Add the above raw materials into a nylon ball mill jar, add isopropanol with a mass ratio of 1.5:1, and yttrium-stabilized zirconia ball milling media with a mass ratio of 5:1, wherein the diameters of yttrium-stabilized zirconia are 3mm and 6mm, and its mass The ratio is 1:1.4. The mixed raw materials were placed in a planetary ball mill for ball milling, the ball milling speed was 800r / min, and the ball milling time was 6h. The obtained mixed raw material slurry was placed in a blast drying oven, and dried at 70° C. for 20 h to obtain mixed raw material powder. Put the mixed raw material powder in a corundum crucible, place the powder in a muffle furnace after vibration, ra...

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Abstract

The invention discloses ultrafine-grained garnet type solid electrolyte powder and a preparation method thereof, and belongs to the field of preparation of all-solid-state lithium battery solid electrolyte materials. The ultrafine-grained garnet type solid electrolyte powder is of a cubic phase structure, the particle size of the powder is smaller than 1 micron, particle size distribution is unimodal distribution, and the specific surface area is high (larger than 1500 m <2>.Kg <-1>). The ultrafine-grained garnet type solid electrolyte powder is crushed by adopting a wet ball milling process.According to the ball milling process, when ultrafine-grained powder is prepared through crushing, the slurry viscosity is controlled to be 20-100 mPa.s. The ultrafine-grained garnet type solid electrolyte powder prepared by adopting the method has high sintering activity, and can be sintered at a relatively low temperature or in a relatively short time to obtain a high-density and high-ionic conductivity electrolyte ceramic chip.

Description

technical field [0001] The invention relates to the field of preparation of solid electrolyte materials for all-solid lithium batteries, in particular to an ultrafine-grained garnet-type lithium lanthanum zirconate (LLZO) solid electrolyte powder and a preparation method thereof. Background technique [0002] Today, with the rapid development and progress of society, various types of electronic products, new energy vehicles, and smart grids using lithium-ion batteries have widely existed in social life. At the same time, with the development of society, people have put forward a demand for lithium-ion batteries that are safer, lighter and have higher capacity. However, the current lithium-ion batteries that use organic electrolytes as the lithium-ion transport medium have brought many safety issues while continuously increasing their specific capacity and operating voltage. Therefore, all-solid-state batteries using lithium-ion solid electrolytes have become the focus of at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/058H01M10/0525H01M10/42
CPCH01M10/0562H01M10/058H01M10/0525H01M10/4235H01M2300/0077H01M2300/0091H01M2220/10H01M2220/20H01M2220/30Y02E60/10Y02P70/50
Inventor 陈召勇吉闫朱华丽
Owner CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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