• 专利标题:   Preparation method of high-pressure single crystal lithium vanadium fluorophosphate positive electrode material used in field of lithium ion battery, involves mixing vanadium phosphate with lithium fluoride, supplementary fluorine source, flux, carbon source, and ball-milling dispersant.
  • 专利号:   CN114351252-A, CN114351252-B
  • 发明人:   SONG M, WEI J, DU N
  • 专利权人:   DALIAN BORONG NEW MATERIALS CO LTD, DALIAN RONGKE POWER GROUP CO LTD
  • 国际专利分类:   C30B001/10, C30B029/22, H01M010/0525, H01M004/58
  • 专利详细信息:   CN114351252-A 15 Apr 2022 C30B-029/22 202244 Chinese
  • 申请详细信息:   CN114351252-A CN11588955 23 Dec 2021
  • 优先权号:   CN11588955

▎ 摘  要

NOVELTY - Preparation method of high-pressure single crystal lithium vanadium fluorophosphate positive electrode material involves i. adding vanadium source, ammonium source and phosphorus source into water in sequence under stirring condition, control the vanadium solution concentration in the medium is 0.5-10 mol per liter, and the stirring is continued until a stable viscous solution or solid is formed; ii. placing viscous solution or solid described in step (1) in an oven to dry, then calcining in a non-oxidizing atmosphere, pulverizing and grinding to obtain powdery vanadium phosphate; and iii. mixing vanadium phosphate obtained in the step (2) with lithium fluoride, supplementary fluorine source, flux, carbon source, and ball-milling dispersant, high-energy grinding is carried out, and after vacuum drying, amorphous roasting precursor powder is obtained; and iv. pressing amorphous calcined precursor powder into tablets and then sintered in a non-oxidizing atmosphere. USE - High-pressure single crystal lithium vanadium fluorophosphate positive electrode material used in field of lithium ion batteries (Claimed). ADVANTAGE - Microstructure of the high-compaction single crystal lithium vanadium fluorophosphate prepared by the preparation method is micron-sized large crystal grains, and the material has high compaction density and good cycle performance. DETAILED DESCRIPTION - Preparation method of high-pressure single crystal lithium vanadium fluorophosphate positive electrode material involves: i. weighing vanadium source, ammonium source and phosphorus source with the molar ratio of vanadium, nitrogen and phosphorus elements of 0.95-1.05:0.95-1.5:1, adding vanadium source, ammonium source and phosphorus source into water in sequence under stirring condition, control the vanadium solution concentration in the medium is 0.5-10 mol per liter, and the stirring is continued until a stable viscous solution or solid is formed; ii. placing viscous solution or solid described in step (1) in an oven to dry, then calcining at 700-1000 degreesC for 1-15 hours in a non-oxidizing atmosphere, pulverizing and grinding to obtain powdery vanadium phosphate; and iii. mixing vanadium phosphate obtained in the step (2) with lithium fluoride, supplementary fluorine source, flux, carbon source, and ball-milling dispersant, high-energy grinding is carried out, and after vacuum drying, amorphous roasting precursor powder is obtained, molar ratio of vanadium and lithium elements of the vanadium phosphate to lithium fluoride is 1:0.9-1.1, 0-5.0 wt.% supplementary fluorine source of the total solid, and 1-10 wt.% flux of the total solid, 1-40 wt.% carbon source of the total mass, and the 25-80 wt.% ball milling dispersant of the total mass; and iv. pressing amorphous calcined precursor powder into tablets and then sintered in a non-oxidizing atmosphere, sintering temperature is 700-1200 degreesC and the holding time is 4-6 hours. An INDEPENDENT CLAIM is included for high-pressure single crystal lithium vanadium fluorophosphate positive electrode material.