Method of preparing Li1+x MN2-x O4 for use as secondary battery electrode

Claim 1

A continuous method of preparing a single phase lithiated manganese oxide intercalation compound of the formula Li 1+x Mn 2-x O 4 having a spinel-type structure comprising the steps of (a) mixing intimately in amounts, based on said lithiated manganese oxide compound, a lithium hydroxide or a lithium salt and a manganese oxide or a manganese salt; (b) feeding the intimately mixed compounds to a reactor; (c) continuously agitating the mixed compounds in the reactor; (d) heating the agitated mixed compounds in the reactor in the presence of air or an oxygen-enriched atmosphere at a temperature of from about 650° C. to about 800° C. for a time not in excess of about 4 hours to form an oxygen deficient spinel structure intercalation compound; and (e) cooling the oxygen deficient compound to less than about 100° C. in about 2 hours or less; to form Li 1+x Mn 2-x O 4 wherein x is from about 0.022 to about 0.125 and the a-axis lattice parameter is about 8.235 Å or less.

Claim 50

A method of synthesizing a lithium manganese oxide of the formula Li 1+x Mn 2-x O 4 having a spinel-type crystal structure with an a-axis lattice parameter of about 8.235 Å or less, and wherein x is from about 0.022 to about 0.2 comprising forming an intimate mixture in finely divided solid form of at least one lithium hydroxide or lithium salt reactant selected from the group consisting of LiOH, Li 2 CO 3 , LiNO 3 and mixtures thereof and at least one manganese oxide or manganese salt reactant selected from the group consisting of MnO 2 , Mn 2 O 3 , MnCO 3 , Mn 3 O 4 , MnO, manganese acetate and mixtures thereof continuously agitating and heating the mixture in a reactor under a continuous purge of countercurrent air at a temperature in the range of from about 650° C. to about 800° C. for a period not in excess of about 4 hours to cause said reactants to react with each other to form an oxygen deficient spinel structure intercalation compound and cooling the oxygen deficient product to less than about 100° C. in about two hours or less to form Li 1+x Mn 2-x O 4 wherein x is from about 0.022 to about 0.2 and the a-axis lattice parameter is about 8.235 Å or less.

Claim 51

A method of synthesizing a lithium manganese oxide of the formula Li 1+x Mn 2-x O 4 having a spinel-type crystal structure with an a-axis lattice parameter of about 8.235 Å or less, and wherein x is from about 0.022 to about 0.2 comprising forming an intimate mixture in finely divided solid form of at least one lithium hydroxide or lithium salt reactant selected from the group consisting of LiOH, Li 2 CO 3 , LiNO 3 and mixtures thereof and at least one manganese oxide or manganese salt reactant selected from the group consisting of MnO 2 , Mn 2 O 3 , MnCO 3 , Mn 3 O 4 , MnO, manganese acetate and mixtures thereof continuously agitating and heating the mixture in a reactor under a continuous purge of countercurrent air at a temperature in the range of from about 650° C. to about 800° C. for a period not in excess of about 4 hours to cause said reactants to react with each other to form an oxygen deficient spinel structure intercalation compound and cooling the oxygen deficient product to less than about 100° C. in about two hours or less to form Li 1+x Mn 2-x O 4 wherein x is from about 0.022 to about 0.2 and the a-axis lattice parameter is about 8.235 Å or less.

Claim 55

A method of preparing a single phase lithiated manganese oxide intercalation compound of the formula Li 1+x Mn 2-x O 4 having a spinel-type structure by a batch process comprising the steps of (a) mixing intimately in stoichiometric amounts, based on said lithiated manganese oxide compound, a lithium hydroxide or a lithium salt and a manganese oxide or a manganese salt; (b) feeding the intimately mixed compounds to a reactor; (c) agitating the mixed compounds in the reactor; (d) heating the agitated mixed compounds in the reactor in the presence of air or an oxygen-enriched atmosphere at a temperature of from about 650° C. to about 800° C. for a time not in excess of about 4 hours to form an oxygen deficient spinel structure intercalation compound; and (e) cooling the oxygen deficient compound to less than about 100° C. in about 2 hours or less; to form Li 1+x Mn 2-x O 4 wherein x is from about 0.022 to about 0.125 and the a-axis lattice parameter is about 8.235 Å or less.

Claim 56

A method of preparing a single phase lithiated manganese oxide intercalation compound of the formula Li 1+x Mn 2-x O 4 having a spinel-type structure by a batch process comprising the steps of (a) mixing intimately in stoichiometric amounts, based on said lithiated manganese oxide compound, a lithium hydroxide or a lithium salt and a manganese oxide or a manganese salt; (b) feeding the intimately mixed compounds to a reactor; (c) agitating the mixed compounds in the reactor; (d) heating the agitated mixed compounds in the reactor in the presence of air or an oxygen-enriched atmosphere at a temperature of from about 650° C. to about 800° C. for a time not in excess of about 4 hours to form an oxygen deficient spinel structure intercalation compound; and (e) cooling the oxygen deficient compound to less than about 100° C. in about 2 hours or less; to form Li 1+x Mn 2-x O 4 wherein x is from about 0.022 to about 0.125 and the a-axis lattice parameter is about 8.235 Å or less.