CPC C01G 51/42 (2013.01) [C23C 14/085 (2013.01); C23C 14/3414 (2013.01); H01M 4/0421 (2013.01); H01M 4/131 (2013.01); H01M 4/1391 (2013.01); H01M 4/525 (2013.01); H01M 10/0525 (2013.01); H01M 10/0562 (2013.01); H01M 10/0565 (2013.01); C01P 2002/74 (2013.01); C01P 2002/82 (2013.01)] | 14 Claims |
1. A method of preparing a composition, the composition comprising:
(a) Co3O4, and
(b) crystalline lithium cobalt oxide or crystalline doped lithium cobalt oxide;
said crystalline lithium cobalt oxide or crystalline doped lithium cobalt oxide comprising the following component elements:
45 to 55 atomic % lithium;
20 to 55 atomic % cobalt; and
0 to 25 atomic % of at least one additional dopant element selected from the group consisting of: magnesium, calcium, strontium, titanium, zirconium, vanadium, chromium, manganese, iron, copper, ruthenium, nickel, zinc, molybdenum, boron, aluminium, gallium, tin, lead, bismuth, lanthanum, cerium, gadolinium and europium;
wherein said atomic % is expressed as a % of total atoms of said crystalline lithium cobalt oxide or crystalline doped lithium cobalt oxide, excluding oxygen;
wherein 0.01% to 10% total mass of said composition is Co3O4;
wherein 90% to 99.99% total mass of said composition is crystalline lithium cobalt oxide or crystalline doped lithium cobalt oxide;
wherein said composition has a bottom surface and a top surface;
where said crystalline lithium cobalt oxide or crystalline doped lithium cobalt oxide has a crystalline structure characterized by at least one of the following parameters (a) to (c):
(a) at least a portion of the crystalline structure has a crystal orientation, relative to a plane parallel to the bottom surface, selected from the group consisting of: (101), (104), (110) and (012);
(b) a Raman spectrum comprising bands at 484 cm−1, 593 cm−1, and at least one band selected from the group consisting of: 690 cm−1, 526 cm−1, and 625 cm−1 (each of said band ±25 cm−1);
(c) at least one X-ray powder diffraction peak measured using a Cu Kα X-ray source selected from the group consisting of: 2θ (±0.2°) 37.4°, 39.1°, 45.3° and 66.4°;
the method comprising the steps of:
providing a separate vapor source of each component element of the composition, wherein the vapour sources comprise at least a source of cobalt, a source of lithium, a source of oxygen, and, optionally, a source of at least one dopant element selected from the group consisting of: magnesium, calcium, strontium, titanium, zirconium, vanadium, chromium, manganese, iron, ruthenium, copper, molybdenum, nickel, zinc, boron, aluminium, gallium, tin, lead, bismuth, lanthanum, cerium, gadolinium and europium;
heating a substrate to between about 30° C. and about 900° C.;
co-depositing each said component element onto the substrate, wherein the component elements react on the substrate to form crystalline oxide comprising lithium, cobalt and optionally one or more of the dopant elements, and having a top surface and a bottom surface;
co-depositing the cobalt and the oxygen onto the substrate, wherein the cobalt and the oxygen react on the substrate to form Co3O4;
depositing the Co3O4 coincidentally with the crystalline oxide comprising lithium and cobalt and optionally one or more of the dopant elements and forming a mixed layer comprising the Co3O4 and the crystalline oxide comprising lithium, cobalt and optionally one or more of the dopant elements; and
depositing the mixed layer onto an existing layer of crystalline oxide comprising lithium and cobalt and optionally one or more of the dopant elements.
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