• 专利标题:   Preparation of copper oxide-graphene nano composite modified electrode involves polishing glassy carbon electrode on alumina polishing powder, cleaning, drying, providing nano-composite modified electrode into sodium hydroxide.
  • 专利号:   CN102520035-A
  • 发明人:   DING Y, LI L, LI F, LUO L, WANG Z, ZHU L
  • 专利权人:   UNIV SHANGHAI
  • 国际专利分类:   G01N027/30, G01N027/327
  • 专利详细信息:   CN102520035-A 27 Jun 2012 G01N-027/30 201351 Pages: 9 Chinese
  • 申请详细信息:   CN102520035-A CN10345081 04 Nov 2011
  • 优先权号:   CN10345081

▎ 摘  要

NOVELTY - A glassy carbon electrode is polished on alumina polishing powder, polished to mirror surface and cleaned by super-pure water. Dilute nitric acid solution, absolute ethyl alcohol and ultra pure water ultrasonic are cleaned and dried. Certain amount of dispersing graphite oxide is dispersed in water, to obtain brown uniform suspension. The copper-graphite nano-composite modified electrode is provided into sodium hydroxide. Electrode is cleaned with super-pure water, to obtain copper oxide-graphene nano composite modified electrode. USE - Preparation of copper oxide-graphene nano composite modified electrode (claimed). ADVANTAGE - The copper oxide-graphene nano composite modified electrode is efficiently prepared. DETAILED DESCRIPTION - A glassy carbon electrode is polished on alumina polishing powder having diameter of 1 mu m, 0.3 mu m or 0.05 mu m, polished to mirror surface and cleaned by super-pure water. The dilute nitric acid solution, absolute ethyl alcohol and ultra pure water ultrasonic are cleaned and dried. The reaction bottle is assembled in ice water bath, proper amount of concentrated sulfuric acid is added and stirred. A certain amount of graphite powder and proper amount of sodium nitrate solid mixture are added, and then proper amount of potassium permanganate is added. The reaction temperature is controlled at 20 degrees C or less, stirred, reacted, and then heated at 35 degrees C, and continuously stirred for 30 minutes. The certain amount of deionized water is slowly added, stirred for 20 minutes, proper hydrogen peroxide reducing residual oxidizing agent is added until the solution becomes bright yellow, and filtered when it is hot. The product is washed using 5 %mass hydrochloric acid solution and ultra pure water until there is no sulfate in the filtrate is detected, filter cake is provided at 60 degrees C in the vacuum drying box, and fully dried, to obtain graphite oxide. A certain amount of dispersing graphite oxide is dispersed in 200 mL water at normal temperature under ultrasonic peeling off for 40 minutes, to obtain brown uniform suspension. The obtained suspension is centrifuged at speed of 5000 rpm for 5 minutes, and slag is removed to the dispersion liquid. The proper amount of hydrazine hydrate is added, obtained mixed solution is stirred for 5 minutes, and then heated in water bath at 100 degrees C, stirred under heat preservation for M hours, filtered and washed for three times and the filter cake is vacuum-oven at 60 degrees C in a vacuum drying box, to obtain black powder of hydrophobic graphite. The obtained graphite is stored at normal temperature, obtained graphene is dispersed in naphthol aqueous solution using 10 mL micropipette, and certain concentration of graphene dispersion liquid is dispensed with micro liquid transferring gun. The drip-painting step is processed with glassy carbon electrode surface, and dried at room temperature, to obtain graphene-modified electrode. The graphene modified glassy carbon electrode as working electrode, saturated calomel electrode and molybdenum electrode are provided, three-electrode system containing 0.01 M copper chloride and 0.1 M potassium chloride solution is provided under constant electric potential of -0.4 V, electro-deposited by super-pure water to wash, and nitrogen flow is finally dried, to obtain copper-graphene nano composite modified electrode. The copper-graphite nano-composite modified electrode is provided into 0.1 M sodium hydroxide using cyclic voltammetry of -0.5 V to + 0.3 V of potential window, scanning speed of 100 mV s-1 repeatedly to stable. The electrode is cleaned with super-pure water for 3 times, to obtain copper oxide-graphene nano composite modified electrode.