• 专利标题:   Preparing hetero atom-doped surface perforated hollow spherical graphene material used in lithium ion battery comprises e.g. providing oxide graphite and water, carrying out ultrasonic dispersing to obtain oxide graphite solution.
  • 专利号:   CN105152161-A, CN105152161-B
  • 发明人:   JIANG Z
  • 专利权人:   UNIV SOUTH CHINA TECHNOLOGY
  • 国际专利分类:   B82Y030/00, C01B031/04, C01B033/12, H01M010/0525, H01M004/36, H01M004/587, C01B032/184
  • 专利详细信息:   CN105152161-A 16 Dec 2015 C01B-031/04 201620 Pages: 20 English
  • 申请详细信息:   CN105152161-A CN10374574 30 Jun 2015
  • 优先权号:   CN10374574

▎ 摘  要

NOVELTY - Preparing hetero atom-doped surface perforated hollow spherical graphene material comprises e.g. providing oxide graphite and water, carrying out ultrasonic dispersing to obtain oxide graphite solution, stirring, adding oxide graphite solution and concentrated nitric acid into the sealed container, carrying out ultrasonic reaction, incubating, adding deionized water, centrifuging and removing acid, purifying, filtering and drying to obtain hetero atom-doped surface perforated hollow graphene. USE - The hetero atom-doped surface hollow spherical graphene material is used in lithium ion battery (claimed). ADVANTAGE - The prepared material has increased conductivity and heat stable character of electrode material. DETAILED DESCRIPTION - Preparing hetero atom-doped surface perforated hollow spherical graphene material comprises (i) providing oxide graphite and water, carrying out ultrasonic dispersing to obtain oxide graphite solution, stirring, adding oxide graphite solution and concentrated nitric acid into the sealed container, carrying out ultrasonic reaction at 4-60 degrees C for 0.5-10 hours, incubating for 1-3 hours, adding deionized water, centrifuging and removing acid, purifying, filtering, drying to obtain hetero atom-doped surface perforated hollow graphene, (ii) adding hexadecyl trimethyl ammonium bromide into deionized water, adding ammonia water and ethanediol into the reaction container, stirring to dissolve, heating at 40-70 degrees C and incubating for 20-60 minutes, stirring and adding tetra ethyl orthosilicate drop wise, adding 3-ammonia propyl triethoxy silane, stirring the reaction mixture at 40-70 degrees C for 2-4 hours, incubating under heat for 2-24 hours, placing the reaction material in an hydro-thermal reaction kettle and carrying out hydro-thermal reaction, washing the obtained product and filtering the liquor without foam and drying to obtain positively charged silicon dioxide sphere, (iii) preparing hetero atom-doped surface perforated hollow graphene: dispersing step (ii) positively charged silicon dioxide spheres into deionized water to obtain silicon dioxide sphere dispersion, adding acid solution dropwise and maintaining the pH to 2-2.5, adding perforated hollow oxide graphene dispersion liquid, stirring the reaction mixture for 24-48 hours, freezing and drying to obtain hetero atom-doped surface perforated hollow graphene silicon dioxide complex material and dispersing step (i) prepared hetero atom-doped surface perforated hollow graphene in water, (iv) adding 100-1000 mg hetero atom-doped surface perforated hollow graphene silicon dioxide sphere complex material into high temperature tubular reactor, vacuuming under low temperature of 1-10 Pa, maintaining the vacuum pump pressure to 102-103 Pa, passing the protection gas and gaseous state hetero atom-doped source pressure is at 0.1-20 Pa, heating the plasma high temperature tube reactor at 300-600 degrees C, operating the radio frequency power source to 100-600 W, carrying out plasma discharge for 10-60 minutes, closing radio frequency and heating power, adding hetero atom doped source is stopped, cooling, cleaning using hydrogen fluoride cleaning solution, using acetone-water mixture, washing the filter liquor using deionized water for less than 10 seconds and filtering solid material to obtain the hetero atom-doped surface hole hollow spherical graphene material. INDEPENDENT CLAIM is also included for plasma high temperature tube reactor comprises plasma high temperature quartz tube furnace, which is set with one protective gas air inlet tube and hetero atom-doped source gas air inlet pipe. The plasma high temperature quartz tube- furnace end is set with two air inlet pipe. The air inlet pipe connected with one liquid nitrogen cold trap and one air exhaust pipe. The liquid nitrogen cold trap is connected through pipeline and pump machine. The plasma high temperature quartz tube type furnace outside surface is wound with inductance coupled plasma coil, where the both ends of inductance coupled plasma coil is connected to the radio frequency power source. The protective gas air inlet pipe is connected with number display flow meter and regulating valve. The hetero atom doped source air inlet pipe is connected with number display flow meter and regulating valve. The liquid nitrogen cold trap is set on the air outlet pipe with the first control valve. The pipeline of the liquid nitrogen cold trap and machine pump is set with the third control valve. The pipeline of the third control valve and the liquid nitrogen cold trap is connected to the vacuum meter. The vacuum meter and the bypass pipeline is connected with the fourth control valve set. The molecule pump and pumping pipe set is connected to the second control valve. The liquid nitrogen cold trap is connected to the air outlet pipe and is set with air inlet pipe. The air inlet pipe is set with air control valve: and #the hetero atom-doped surface hollow spherical graphene material, prepared as mention above.