▎ 摘　　要

NOVELTY - Preparing graphene composite material loaded with hollow carbon ball involves pre-oxidizing graphite oxide in 100-120 mL concentrated sulfuric acid into 250 mL flask on ice bath condition. 2-2.5 g potassium peroxymonosulfate and 2-2.5 g phosphorus pentoxide are added in concentrated sulfuric acide and stirred followed by the addition of 2-3 g crystalline flake graphite. The potassium peroxymonosulfate and phosphorus pentoxide are dissolved and transferred into flask at 60-100 degrees C on oil bath for 4-8 hours to obtain mixed solution. The mixed solution is mixed with 1000 mL distilled water. USE - Method for preparing graphene composite material loaded with hollow carbon ball (claimed). ADVANTAGE - The method enables to prepare graphene composite material loaded with hollow carbon ball which has has large area, good repeatability and assembling super capacitor with high performance. DETAILED DESCRIPTION - Preparing graphene composite material loaded with hollow carbon ball involves pre-oxidizing graphite oxide in 100-120 mL concentrated sulfuric acid into 250 mL flask on ice bath condition. 2-2.5 g potassium peroxymonosulfate and 2-2.5 g phosphorus pentoxide are added in concentrated sulfuric acid and stirred followed by the addition of 2-3 g crystalline flake graphite. The potassium peroxymonosulfate and phosphorus pentoxide are dissolved and transferred into flask at 60-100 degrees C on oil bath for 4-8 hours to obtain mixed solution. The mixed solution is mixed with 1000 mL distilled water and diluted, where diluted mixture is filtered and washed with distilled water to neutral. The neutral mixture is dried at 50-100 degrees C for 6-24 hours to obtain oxidized graphite powder. The 1-3 g oxidized graphite powder is mixed with graphite oxide followed by the addition of 50-100 mL concentrated sulfuric acid. 5-10 g potassium permanganate is added and reacted for 2-4 hours at 30-50 degrees C for 2-24 hours. The mixture is mixed and diluted with 100 mL distilled water under ice bath condition. The reaction mixture is transferred into flask at 80-98 degrees C and reacted for 15-60 minutes. 6-12 mL 30 wt.% hydrogen peroxide is added to obtain golden yellow solution which is allowed to stand and supernatant is poured and washed with 5-10 wt.% hydrochloric acid for three times. The washed precipitate is washed with distilled water to neutral and drying at 50-80 degrees C in vacuum drying box for 12-24 hours to obtain graphite oxide powder. 8-12 mL ammonia hydrate, 100-150 mL ethanol and 80-100 mL super-pure water are mixed to obtain first solution, and 10-15 mL tetraethoxysilane and 30-60 mL ethanol are mixed to obtain second solution. The first and second solution are mixed and stirred for 30-10 minutes folowed by the addition of 1-2 g resorcinol and 1.5-3 mL formaldehyde solution at room temperature and reacted for 12-48 hour in reaction kettle, which is further reacted for 12-48 hours at to 80-120 to obtain resorcinol/formaldehyde silicon dioxide precursor. The resorcinol/formaldehyde silicon dioxide precursor is washed for three times by ethanol and dried. 0.3-1 g resorcinol/formaldehyde silicon dioxide precursor is dissolved in 20-50 mL ultrapure water ultrasonic and reacted for 2-4 hours to obtain thirs liquid. 10-30 milligrams graphite powder is added into 5-20 mL ultra-pure water and ultrasonically treated for 2-4 hours to obtain graphene oxide solution. The graphene oxide solution is mixed with third liquid followed by the addition of 0.2-0.5 g ascorbate and raected for 1-4 hours to obtain mixed solution. The mixed solution is added into high pressure reaction kettle at 160-240 degrees c and reacted for 6-24 hours to obtain grapheneresorcinol/ formaldehyde silicon dioxide composite material. The graphene-hollow carbon ball composite material is passed high temperature carbonizing to obtain graphene-carbon spherical silicon dioxide composite material. The graphene-carbon spherical silicon dioxide composite material is treated in the presence of carbide with protection of nitrogen gas and reacted with a heating speed of 1-3 degrees C/minute at 300-500 degrees C for 1-2 hours followed by the addition of 5-10 wt.% hydrofluoric acid to remove silicon dioxide balls. The mixture is washed by using distilled water and ethanol for 6-3 times at 60-120 degrees C for 10-24 hours to obtain hollow carbon ball-graphene composite material. The electrode active material, conductive carbon black and polytetrafluoroethylene are mixed in mass ratio of (7:1:1)-(9:1:1) and ground to obtain slurry which is loaded on the foam nickel and dried at 80-120 degrees C for 0.5-2 hours and electrode is pressed at 5-12 megaPascal and 80-120 degrees C for 10-24 hours. The area of electrode material is 1.0-2.0 centimeter square. The amount of active substance is loaded on each current collector is 5.0-6.0 mg. The electrode active material is taken as working electrode, platinum as counter electrode, mercury/mercury oxide electrode as reference electrode, where concentration of potassium hydroxide aqueous solution is 3.0-6.0 moles/liter.