Abstract: Disclosed are methods and systems for the use of titration-gas chromatography (TGC) to differentiate and quantify metallic substances (M0) and ionic metal (Mn+) in an anode material, such as in rechargeable-battery anodes of metal type (e.g., Li, Na, K, Mg, Ca, Fe, Zn, Al, etc.) or compound type (e.g., LixC6, LixSi, LixSn, etc) by using the proper titrant.

Abstract: A lithium-excess cathode material according to Li1+xNiaMnbCocModO2?y (0<x<0.3, 0?a?1, 0?b?1, 0?c?1, 0?d?0.2, 0?y?0.25) in the form of secondary spherical microparticles formed from primary spherical nanoparticles. The primary nanoparticles can in the range of ˜130 nm to 170 nm and the secondary in the range of ˜2-3 ?m. A method of formation includes mixing a carbonates or hydroxides solution into a mixed solution of transition metal (M) ions with predetermined stoichiometry under stirring, and aging resulting transition metal carbonates or hydroxides at a predetermined temperature for period of time to produce primary nanoparticles of a predetermined size. A gas-solid interface reaction to uniformly creating oxygen vacancies without affecting structural integrity of Li-excess layered oxides is also provided.

Abstract: A lithium-excess cathode material according to Li1+xNiaMnbCocModO2?y (0<x<0.3, 0?a?1, 0?b?1, 0?c?1, 0?d?0.2, 0?y?0.25) in the form of secondary spherical microparticles formed from primary spherical nanoparticles. The primary nanoparticles can in the range of ˜130 nm to 170 nm and the secondary in the range of ˜2-3 ?m. A method of formation includes mixing a carbonates or hydroxides solution into a mixed solution of transition metal (M) ions with predetermined stoichiometry under stirring, and aging resulting transition metal carbonates or hydroxides at a predetermined temperature for period of time to produce primary nanoparticles of a predetermined size. A gas-solid interface reaction to uniformly creating oxygen vacancies without affecting structural integrity of Li-excess layered oxides is also provided.