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US 2016/0111751 A1Published application
Lithium-ion conductive garnet and method of making membranes thereof
AssigneeCorning Incorporated
InventorsMichael Edward Badding, Curtis Robert Fekety, Tricia Anne Harnas, Yanxia Ann Lu, Ying Shi, Zhen Song
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Abstract
A gallium doped garnet composition of the formula: Li7-3yLa3Zr2GayO12 where y is from 0.4 to 2.0, and as defined herein. Also disclosed is a method for making a dense Li-ion conductive cubic garnet membrane, comprising one of two alternative lower temperature routes, as defined herein.
Claims15
A method of making a Li-ion conductive cubic garnet, comprising:
- forming a nitrate source aqueous solution comprised of a first nitrate source and a nitrate dopant source;
- contacting the nitrate source aqueous solution and a carbohydrate source in mole ratio of from 1:1 to 1:4, and a first heating from 200 to 550° C., to form a nano-particle ash;
- a second heating of the nano-particle ash at from 650 to 700° C. to produce a garnet nanoprecursor having nano-sized particles of from 10 to 100 nm;
- pelletizing the garnet nanoprecursor to form a Li-ion conductive cubic garnet pellet;
- and
- a third heating of the pelletized garnet pellet at a top temperature of from 950 to 1200° C., at from 0.5 to 30 hrs, to form a dense membrane of the Li-ion conductive cubic garnet.
3 more elements
A method of making a Li-ion conductive cubic garnet, comprising:
- forming a nitrate source aqueous solution comprised of a first nitrate source and a nitrate dopant source;
- contacting the nitrate source aqueous solution and a carbohydrate source in mole ratio of from 1:1 to 1:4, and a first heating of the mixture from 200 to 550° C., to form a nano-particle ash;
- a second heating of the nano-particle ash at from 775 to 1000° C. to produce a Li-ion conductive pure cubic garnet powder having micron-sized particles having irregular shape;
- milling the cubic garnet powder to produce a sub-micron powder;
- pelletizing the sub-micron powder to form a garnet pellet;
- and
- a third heating of the garnet pellet at from about 950 to about 1200° C. to form a dense Li-ion conductive cubic garnet membrane.
4 more elements
A gallium doped garnet composition of the formula:
- Li7-3yLa3Zr2GayO12
- where
- y is from 0.4 to 2.0,
- the formula is determined by ion coupled plasma (ICP), and
- the cubic phase of the composition is determined by x-ray diffraction (XRD) to have a lattice constant of 13.045 Angstroms.
2 more elements
Dependencies are inferred from the claim text.