# US 10,374,218 B2 · Methods for forming lithium manganese oxide layers > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,374,218 B2 - Document ID: US10374218B2 - Status: Granted - Kind: B2 - Application number: 15/339,577 - Filed: 2016-10-31 - Published: 2017-05-04 - Granted: 2019-08-06 - Earliest claimed: 2015-11-02 - Assignees: Imec Vzw; Katholieke Universiteit Leuven, KU LEUVEN R&D - Applicants: Imec Vzw; Katholieke Universiteit Leuven, KU LEUVEN R&D - Inventors: Nouha Labyedh; Marina Yurievna Timmermans; Philippe Vereecken - Web page: https://patentgrep.com/patent/US10374218B2 ## CPC - H01M 4/045: {Electrochemical coating; Electrochemical impregnation} - C25D 9/04: with inorganic materials - C25D 17/10: Electrodes {, e.g. composition, counter electrode} - H01M 4/0452: {from solutions} - H01M 4/0471: {involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis} - H01M 4/131: Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx - H01M 4/1391: of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx - H01M 4/505: of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy - H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries - H01M 4/661: {Metal or alloys, e.g. alloy coatings (H01M4/669 take precedence)} - H01M 4/664: {Ceramic materials} - H01M 10/0585: of accumulators having only flat construction elements, i.e. flat positive electrodes, flat negative electrodes and flat separators - H01M 2004/021: {Physical characteristics, e.g. porosity, surface area} - H01M 2220/30: Batteries in portable systems, e.g. mobile phone, laptop - Y02E 60/10: Energy storage using batteries - Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product - H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY - C25D: PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR - Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION - Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS ## Abstract A method is provided for forming a porous, electrochemically active lithium manganese oxide layer on a substrate, the method comprising: depositing a porous manganese oxide layer on the substrate; providing a Li containing layer on the porous manganese oxide layer; and afterwards performing an annealing step at a temperature in the range between 200° C. and 400° C., thereby inducing a solid-state reaction between the porous manganese oxide layer and the Li containing layer. The method may further comprise, before depositing the porous manganese oxide layer: depositing a seed layer on the substrate. A method of the present disclosure may be used for forming electrode layers of lithium-ion batteries. ## Claims ### Claim 1 A method for forming a porous, electrochemically active lithium manganese oxide (LixMnyOz) layer on a substrate, the method comprising: depositing a porous manganese oxide layer on the substrate; providing a Li containing layer on the porous manganese oxide layer; and afterwards performing an annealing step at a temperature in the range between 200° C. and 400° C., thereby inducing a solid-state reaction between the porous manganese oxide layer and the Li containing layer. ### Claim 2 (depends on 1) The method according to claim 1, wherein the lithium manganese oxide layer has a spinel structure. ### Claim 3 (depends on 1) The method according to claim 1, wherein the lithium manganese oxide layer is a LixMnyOz layer with x in the range between 0 and 2, y=2 and z in the range between 1.8y and 2.2y. ### Claim 4 (depends on 1) The method according to claim 1, wherein the porous manganese oxide layer is a porous MnOvOw layer with v=1 and win the range between 1.9 and 2.1. ### Claim 5 (depends on 1) The method according to claim 1, wherein the porous manganese oxide layer has a porosity in the range between 40% and 60%. ### Claim 6 (depends on 1) The method according to claim 1, wherein the porous manganese oxide layer comprises pores having a pore size in the range between 2 nm and 20 nm. ### Claim 7 (depends on 1) The method according to claim 1, wherein providing the Li containing layer comprises providing a Li2CO3 layer. ### Claim 8 (depends on 1) The method according to claim 1, wherein the substrate is a non-planar substrate. ### Claim 9 (depends on 8) The method according to claim 8 wherein the substrate comprises a plurality of high aspect-ratio micro-pillars and/or a plurality of high aspect-ratio micro-trenches, each having an aspect ratio in the range of 20 to 250. ### Claim 10 (depends on 1) The method according to claim 1, wherein the substrate comprises Al. ### Claim 11 (depends on 1) The method according to claim 1, wherein depositing the porous manganese oxide layer on the substrate comprises electrochemically depositing the porous manganese oxide layer. ### Claim 12 (depends on 11) The method according to claim 11, further comprising, before electrochemically depositing the porous manganese oxide layer depositing a seed layer on the substrate. ### Claim 13 (depends on 12) The method according to claim 12, wherein depositing the seed layer comprises depositing a dense manganese oxide layer by means of a method different from electrochemical deposition. ### Claim 14 (depends on 1) The method according to claim 1, wherein the lithium manganese oxide layer is a LixMnyOz layer with x in the range between 0 and 2, y=2 and z in the range between 1.8y and 2.2y; the porous manganese oxide layer is a porous MnOvOw layer with v=1 and w in the range between 1.9 and 2.1; the porous manganese oxide layer has a porosity in the range between 40% and 60%; and the porous manganese oxide layer comprises pores having a pore size in the range between 2 nm and 20 nm. ### Claim 15 (depends on 14) The method according to claim 14, wherein the lithium manganese oxide layer has a spinel structure. ### Claim 16 (depends on 1) A method for fabricating a lithium-ion battery, wherein the method comprises forming a porous, electrochemically active lithium manganese oxide electrode layer on a substrate, using a method according to claim 1. ### Claim 17 (depends on 1) The method according to claim 1, wherein the porous, electrochemically active lithium manganese oxide layer is conformally provided on said substrate, the substrate not withstanding temperatures higher than 700° C. ### Claim 18 (depends on 17) A method for fabricating lithium-ion battery, wherein the method comprises forming a porous, electrochemically active lithium manganese oxide electrode layer on a substrate, using a method according to claim 17. ### Claim 19 (depends on 1) The method according to claim 1, wherein the annealing is performed in air or in an inert atmosphere. ### Claim 20 (depends on 1) The method according to claim 1, wherein the annealing is performed in the absence of further deposition.