Garnet powder, manufacturing method thereof, solid electrolyte sheet using hot press and manufacturing method thereof

Patent metadata

Field	Value
Publication number	US-10008740-B2
Application number	US-201514716491-A
Country	US
Kind code	B2
Filing date	May 19, 2015
Priority date	Aug 18, 2014
Publication date	Jun 26, 2018
Grant date	Jun 26, 2018

Abstract

The present disclosure relates to garnet powder, a manufacturing method thereof, a solid electrolyte sheet using a hot press, and a manufacturing method thereof. In particular, the present disclosure provides a method for manufacturing Li 7 La 3 Zr 2 O 12 (LLZ) garnet powder including preparing a mixture by first dry mixing Li 2 CO 3 , La 2 O 3 , ZrO 2 , and Al 2 O 3 . The mixture is first calcinated for 5 to 7 hours in a temperature range of 800 to 1000° C. The calcinated mixture is ground to a powder with an average particle size of 1 to 4 μm through dry grinding. A cubic-phased LLZ garnet powder is prepared by second calcinating the ground mixture for 10 to 30 hours in a temperature range of 1100 to 1300° C.

First claim

What is claimed is:

1. A method for manufacturing Li 7 La 3 Zr 2 O 12 (LLZ) garnet powder comprising:
preparing a mixture by first dry mixing Li 2 CO 3 , La 2 O 3 , ZrO 2 , and Al 2 O 3 ;
first calcining the mixture for 5 to 7 hours in a temperature range of 800 to 1000° C.;
grinding the calcinated mixture to a powder with an average particle size of 1 to 4 μm by dry grinding to form a ground mixture; and
preparing a cubic-phased LLZ garnet powder by second calcining the ground mixture for 10 to 30 hours in a temperature range of 1100 to 1300° C.,
wherein Al substitutes some of the Li of LLZ garnet powder, and is doped in the form of Al 2 O 3 to the LLZ garnet powder.

2. The method for manufacturing LLZ garnet powder of claim 1 , wherein, in the LLZ garnet powder, a molar ratio of the Li 2 CO 3 , the La 2 O 3 , the ZrO 2 , and the Al 2 O 3 is 7:3:4:0.02 to 1.075.

3. The method for manufacturing LLZ garnet powder of claim 1 , wherein the substituted Al is included in 0.02 to 1.075 mol, and Al is doped in the form of Al 2 O 3 at 0.1 to 5% by weight with respect to the LLZ garnet powder.

4. The method for manufacturing LLZ garnet powder of claim 1 further comprising analyzing the LLZ garnet powder, wherein the analysis is carried out using X-Ray Diffraction (XRD), Raman Spectroscopy, or Inductively Coupled Plasma Mass Spectrometry (ICP-MS).

Assignees

• Hyundai Motor Co Ltd

Inventors

• Sung Ju Young
• Lee Ho Taek
• Kwon Eun Ji
• Jang Yong Jun
• Kim Ji Na

Classifications

• C01B33/26

  Aluminium-containing silicates {, i.e. silico-aluminates} · CPC title

• H01M2300/0071

  Oxides · CPC title

• H01M10/0562 Primary

  Solid materials · CPC title

• H01M10/0525

  Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries · CPC title

• C01G25/006

  Compounds containing zirconium, with or without oxygen or hydrogen, and containing two or more other elements · CPC title