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Alkali metal doped garnet type lithium lanthanum zirconium oxide powder and preparation method thereof

A technology of lithium lanthanum zirconium oxide and garnet type, which is applied in the field of alkali metal doped garnet type lithium lanthanum zirconium oxide powder and its preparation, can solve the unfavorable application of flexible composite solid electrolyte, unsatisfactory particle size of powder materials, particle size Uneven distribution and other problems, to achieve the effect of easy industrial production, small grain size and narrow particle size distribution

Inactive Publication Date: 2020-07-10
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is conducive to reducing the grain size and the calcination temperature. The grain size of the prepared LLZ0 powder is nano-scale and the phase is single, but its particle size distribution is not uniform.
Patent CN109678205A announced the use of LiNO 3 and La(N0 3 ) 3 , zirconium ketone, etc. as raw materials, high-purity LLZO powder materials are obtained by preparing sol-gel and roasting below 1000 ° C. The particle size of the powder materials obtained by this method is not ideal, and ball milling is required before use.
[0004] At present, the particle size of lithium lanthanum zirconium oxide powder materials widely used in composite solid electrolytes is about 1 μm, the particle size distribution range is wide, and the grain size is not small enough, which is not conducive to its application in flexible composite solid electrolytes.

Method used

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  • Alkali metal doped garnet type lithium lanthanum zirconium oxide powder and preparation method thereof
  • Alkali metal doped garnet type lithium lanthanum zirconium oxide powder and preparation method thereof
  • Alkali metal doped garnet type lithium lanthanum zirconium oxide powder and preparation method thereof

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Embodiment 1

[0039] A kind of alkali metal doped garnet type lithium lanthanum zirconium oxide powder (Li 7.2 La 2.9 Rb 0.1 Zr 2 o 12 ), the specific preparation method is as follows:

[0040] Dissolve 0.36mol of lithium carbonate, 0.29mol of lanthanum nitrate, and 0.2mol of zirconium hydroxide in 100mL of deionized water, and stir until completely dissolved to obtain solution A; dissolve 0.01mol of rubidium chloride in 100mL of deionized water to obtain solution B; Add cyclohexane, 20mL cetyltrimethylammonium bromide, and 80mL n-butanol into a beaker and stir evenly to obtain solution C. Divide solution C into two equal parts of 150mL each, and record them as C 1 、C 2; Add solution A dropwise to solution C under ultrasonic vibration 1 , the dropping time is 10 minutes to obtain emulsion D, and solution B is added dropwise to solution C under the condition of ultrasonic vibration 2 Emulsion E was obtained in , and the dropping time was 10 minutes. Mix solution D and solution E evenl...

Embodiment 2

[0044] A kind of alkali metal doped garnet type lithium lanthanum zirconium oxide powder (chemical formula Li 7.2 La 2.9 K 0.1 Zr 2 o 12 ), the specific preparation method is as follows:

[0045] Dissolve 0.72mol lithium hydroxide, 0.29mol lanthanum hydroxide, and 0.2mol zirconium hydroxide in 100mL deionized water, stir until completely dissolved to obtain solution A; dissolve 0.005mol potassium carbonate in 100mL deionized water to obtain solution B; Add 200mL of cyclohexane, 20mL of cetyltrimethylammonium chloride, and 80mL of n-butanol into a beaker and stir evenly to obtain solution C. Divide solution C into two equal parts of 150mL each, and record them as C 1 、C 2 ; Add solution A dropwise to solution C under ultrasonic vibration 1 , the dropping time is 15 minutes to obtain emulsion D, and solution B is added dropwise to solution C under the condition of ultrasonic vibration 2 Emulsion E was obtained in , the dropping time was 15 minutes, and the solution D and ...

Embodiment 3

[0047] A kind of alkali metal doped garnet type lithium lanthanum zirconium oxide powder (chemical formula Li 7.2 La 2.9 Cs 0.1 Zr 2 o 12 ), the specific preparation method is as follows:

[0048] Dissolve 0.72mol of lithium nitrate, 0.29mol of lanthanum nitrate, and 0.2mol of zirconium oxynitrate in 100mL of deionized water, and stir until completely dissolved to obtain solution A; dissolve 0.01mol of cesium nitrate in 100mL of deionized water to obtain solution B; Add hexane, 20mL cetyldimethylammonium oxide, and 80mL n-butanol into a beaker and stir evenly to obtain solution C. Divide solution C into two equal parts of 150mL each, and record them as C 1 、C 2 ; Add solution A dropwise to solution C under ultrasonic vibration 1 , the dropping time is 20 minutes to obtain emulsion D, and solution B is added dropwise to solution C under the condition of ultrasonic vibration 2 Emulsion E was obtained in , the dropping time was 20 minutes, and solution D and solution E wer...

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Abstract

The invention relates to alkali metal doped garnet type lithium lanthanum zirconium oxide powder and a preparation method thereof. The chemical formula of the powder is Li<7+2a>La<3-a>MZr2O12, a islarger than 0 and smaller than or equal to 0.2, the crystal structure is a cubic phase, and the alkali metal M is one of potassium, rubidium and cesium. The alkali metal doped garnet type lithium lanthanum zirconium oxide powder provided by the invention is high in purity, small in grain size, narrow in grain size distribution and good in dispersity, and can be better applied to composite solid electrolyte. Besides, the preparation method provided by the invention is simple in process, good in repeatability, low in sintering temperature (the solid-phase sintering temperature of a standard cubic-phase garnet crystal is generally 1100-1300 DEG C), more energy-saving and environment-friendly, and easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to an alkali metal doped garnet type lithium lanthanum zirconium oxide powder and a preparation method thereof. Background technique [0002] Li 7 La 3 Zr 2 o 12 (LLZO) is a garnet-type oxide solid electrolyte with high Li-ion conductivity (~10 -3 S / cm), high chemical stability to lithium metal, and high electrochemical window above 5V, therefore, it is one of the most promising solid electrolytes for all-solid-state lithium-ion batteries. However, the main reason limiting the application of garnet-structured solid electrolytes in lithium-ion batteries is that their electrical conductivity is still lower than that of liquid polymer electrolytes. Therefore, it is very important to improve the performance of lithium lanthanum zirconium oxide. [0003] Patent CN108417889A discloses a preparation method of lithium lanthanum zirconium oxide powder, using s...

Claims

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Application Information

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IPC IPC(8): C01G25/00H01M10/0562H01M10/0525
CPCC01G25/006C01P2002/72C01P2004/03C01P2004/62H01M10/0525H01M10/0562H01M2300/0071Y02E60/10
Inventor 唐浩林朱泰洋李丹鹏林文
Owner WUHAN UNIV OF TECH
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