	US 12,294,049 B2
	Method of preparation of a garnet-type inorganic material
Réka Toth, Paris (FR); Laure Bertry, Aubervilliers (FR); Valérie Buissette, Paris (FR); Thierry Le Mercier, Rosny-sous-Bois (FR); Marc-David Braida, Bry-sur-Marne (FR); and Robin Amisse, Issy-les-Moulineaux (FR)
Assigned to SPECIALTY OPERATIONS FRANCE, Lyons (FR)
Appl. No. 17/625,996
Filed by SPECIALTY OPERATIONS FRANCE, Lyons (FR)
PCT Filed Jul. 29, 2020, PCT No. PCT/EP2020/071436 § 371(c)(1), (2) Date Jan. 10, 2022, PCT Pub. No. WO2021/023599, PCT Pub. Date Feb. 11, 2021.
Claims priority of application No. 19315084 (EP), filed on Aug. 6, 2019.
Prior Publication US 2022/0278355 A1, Sep. 1, 2022
Int. Cl. H01M 10/05 (2010.01); C01G 25/00 (2006.01); C01G 33/00 (2006.01); C01G 49/00 (2006.01); H01M 10/0525 (2010.01); H01M 10/056 (2010.01)

CPC H01M 10/056 (2013.01) [C01G 25/006 (2013.01); C01G 33/006 (2013.01); C01G 49/0054 (2013.01); H01M 10/0525 (2013.01); C01P 2002/30 (2013.01); C01P 2002/52 (2013.01); C01P 2004/51 (2013.01); C01P 2004/61 (2013.01); C01P 2004/62 (2013.01); C01P 2006/40 (2013.01); H01M 2300/0091 (2013.01)]

20 Claims

1. An inorganic material M comprising a garnet oxide or garnet-type oxide containing, as constituent elements, the elements Li, La, Zr and at least one element A selected from the group consisting of Al, Ga, Nb, Fe, W, Ta, and a mixture thereof, the oxide being described by formula (I):

[Li_x1La₃Zr_zA_wO₁₂] (I)

wherein:

x1, z and w are positive real numbers;

1.20<z≤2.10;

0<w≤0.80; and

x1 is derived from the electroneutrality of the oxide; and

exhibiting:

a ratio R50 higher than 50%, R50 being defined by:

R50(%)=(D50−D_US50)/D50×100

wherein D50 and D_us50 are the median diameters of distributions in volume of the diameters of a dispersion of the particles of the inorganic material M in N-methyl-2-pyrrolidone (NMP), obtained with a laser diffractometer, D_us50 being measured after a treatment under ultrasound which consists of inserting an ultrasonic probe into a dispersion of 100 mg of the inorganic material M in 160 mL of NMP and in submitting the dispersion to sonication under a power of 140±10 W for 22 minutes and/or

a ratio R90 higher than 50%, R90 being defined by:

R90 (%)=(D90-D_us90)/D90×100

wherein D90 and D_us90 correspond to the diameters of the particles for which 90% of the particles have a diameter which is less than D90 and are determined from distributions in volume of the diameters of a dispersion of the particles of the inorganic material M in N-methyl-2-pyrrolidone (NMP), obtained with a laser diffractometer, D_us90 being measured after a treatment under ultrasound which consists of inserting an ultrasonic probe into a dispersion of 100 mg of the inorganic material M in 160 mL of NMP and in submitting the dispersion to sonication under a power of 140±10 W for 22 minutes.