• 专利标题:   Lithium-sulfur battery cathode material comprises transition metal oxide nanorod, carbon skeleton, internal pore canal and sulfur attached to surface and conductive polyaniline wrapped on outer surface, where catalytic transition metal oxide nanorod is obtained by screening and controlling reaction.
  • 专利号:   CN114497487-A
  • 发明人:   FENG T, ZHAO T, ZHANG N, CHEN R
  • 专利权人:   BEIJING INST TECHNOLOGY
  • 国际专利分类:   H01M010/052, H01M010/42, H01M004/36, H01M004/38, H01M004/62
  • 专利详细信息:   CN114497487-A 13 May 2022 H01M-004/36 202266 Chinese
  • 申请详细信息:   CN114497487-A CN10019031 10 Jan 2022
  • 优先权号:   CN10019031

▎ 摘  要

NOVELTY - Lithium-sulfur battery cathode material comprises transition metal oxide nanorod, carbon skeleton, internal pore canal and sulfur attached to surface and conductive polyaniline wrapped on the outer surface. The catalytic transition metal oxide is obtained by screening and precisely controlling the reaction conditions. The carbon skeleton structure is obtained by reasonably selecting and proportioning carbon particles, carbon tubes and graphene. The sulfur attached to the carbon skeleton and its internal pores is obtained by controlling the ratio of reactants and by chemical reaction. The conductive polyaniline coating layer is obtained by precisely controlling the reaction conditions. The mass fraction of sulfur in the material is 80-92%, the mass fraction of carbon is 5-18%, and the mass fraction of transition oxide is 1-5%. USE - Used as lithium-sulfur battery cathode material containing transition metal oxide nanorod. ADVANTAGE - The cathode material: can serve as the carrier of active materials; catalyzes the mutual conversion between polysulfides; accelerates the reaction rate of the battery; slows down the shuttle effect; improves the rate performance of the battery; at the same time, can ensure high utilization of sulfur; can suppress the volume change of the cathode material and the shuttle effect of polysulfides; and realizes the high specific energy and long cycle characteristics of lithium-sulfur batteries. The method is simple in process, economical and easy for large-scale production. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is also included for preparing the cathode material, comprising (1) adding total of 10-20 g 0-dimensional carbon particles and one-dimensional carbon tubes and two-dimensional graphene placing in beaker, adding 500-1500 ml ethanol and 300-600 ml water, stirring and uniformly mixing under ultrasonic condition, (2) adding 10-30 ml phosphoric acid to the dispersion liquid in the step (1), keeping the water bath in which the whole reaction device is placed and keeping warm, continuously adding the aniline solution of 20-50 ml in the beaker, and stirring and uniformly mixing, (3) placing 8-25 g ammonium persulfate in beaker, adding 200-500 ml water, stirring and dissolving, pumping the ammonium persulfate solution into the beaker with carbon powder in the step (2) using peristaltic pump, adding 2-5 l ethanol solution whose volume fraction is 50-90% to this dispersion system, and keeping stirring, (4) taking 250-1000 ml manganese chloride solution with appropriate concentration in sealable container, adding 2-20 ml hydrogen peroxide suitable concentration to the container, stirring and uniformly mixing, adding 2-15 ml ammonia solution with certain concentration to the mixed system, stirring and uniformly mixing as well, placing the mixed solution in 30-180degrees Celsius oven for 1-7 days, filtering the solution, and keeping the filter cake to obtain the oxide of the transition metal manganese, catalytic material of cathode material of the lithium-sulfur battery, (5) taking 300-500 g sodium sulfide nonahydrate and placing it in suitable container, adding 5-15 l water and stirring to dissolve, taking 100-300 g of sulfur powder and adding it to the above sodium sulfide solution, and stirring to dissolve fully, (6) taking 300-500 ml concentrated hydrochloric acid and adding 600-1000 ml water to fully stir and dissolve, (7) adding the transition metal oxide obtained in the step (4) into the dispersion obtained in the step (3) after ball milling, uniformly mixing, and pumping the two solutions in step (5) and step (6) into the system in which the carbon powder is in the step (3) to react, while using water bath to control the temperature of the reaction system, (8) filtering the reaction system dispersion after the reaction is completed, removing the filtrate, keeping the filter cake, and fully washing the filter cake until the filtrate is neutral, (9) placing the filter cake washed to neutrality in beaker, adding ethanol solution to the beaker, fully stirring and dispersing, at the same time taking 100-150 g polyvinylpyrrolidone (PVP) (K-30 or K50) into beaker, adding 300-600 ml water, stirring and dissolving in 40-60degrees Celsius water bath, (10) directly adding the PVP solution that dissolves completely in the step (8) in the beaker that is dispersed with neutral filter cake, stirring and dispersing again, at the same time, adding 100-150 ml of concentrated phosphoric acid and aniline to the system under stirring, and controlling the temperature of the system with water bath, (11) taking 15-25 g ammonium persulfate and placing it in beaker, adding 200-300 ml water and stirring to dissolve it thoroughly, pouring the ammonium persulfate solution into the dispersion in the step (9) under stirring, making it fully react, using water bath to carry out accurate temperature control to the reaction system in the whole reaction process, and (12) filtering the dispersion system after the reaction is completed, removing the filtrate, keeping the filter cake, fully washing the filter cake, washing the filter cake to neutrality until the pH of the filtrate is about 6, and transferring to 50-80degrees Celsius oven for vacuum drying for about week to obtain the target material (lithium-sulfur battery cathode material on catalytic transition metal oxide nano-rod).