OBTAINING NANOSTRUCTURED MIXED LITHIUM AND ZIRCONIUM OXIDES BY SPRAY PYROLYSIS Russian patent published in 2024 - IPC C01B13/18 C01D1/02 C01G25/02 H01M4/131 B82Y40/00 

FIELD: chemistry.

SUBSTANCE: invention relates to chemical industry and can be used in making components of solid-state electrolytes, additives to liquid or gel electrolyte or electrodes of lithium-ion accumulator batteries. Mixed oxide containing lithium, zirconium and, optionally, at least one other metal is obtained by spray pyrolysis in flame. Spraying gas is used to spray at least one solution of precursors, such as lithium and zirconium carboxylates containing 5–20 carbon atoms, in a mixture of solvents, including alcohol and carboxylic acid, as well as less than 10 wt.% of water. Carboxylic acid contains 5–20 carbon atoms. Molar ratio of alcohol and carboxylic acid is from 1:20 to 20:1. Formed aerosol is reacted with a flame obtained by igniting a mixture of fuel and oxygen-containing gases in the reaction space of the reactor. Reaction stream is cooled, after which a solid mixed oxide is removed from it, which can be additionally heat treated at 600–1300 °C and milled in a ball mill. Obtained product is in form of aggregated primary particles and is a compound of general formula Li_aZr_bM_cO_0.5a+2b+d (I), where 1.5 ≤ a ≤ 15; 0.5 ≤ b ≤ 3.0; 0 ≤ c ≤ 5; d = 0.5c for M, which is Na, K; d = c for M, which is Be, Mg, Ca, Sr, Ba, Zn, Co, Ni, Cu, Mn; d = 1.5c for M, which is B, Al, Ga, In, Fe, Sc, Y, La; d = 2c for M, which is Ti, Zr, Hf, Ce, Si, Ge, Sn, Pb; d = 2.5c for M, representing V, Nb, Ta; d = 3c for M, which is Mo, W.

EFFECT: said mixed oxide is characterized by a BET surface area of less than 10 m²/g or 15–50 m²/g; number-average particle diameter d₅₀ = 0.1–2 mcm or d₅₀ = 1–50 mcm, determined by static light scattering (SLS), and tamping density of 30–150 g/l or 400–1000 g/l.

14 cl, 9 dwg, 2 tbl, 3 ex