• 专利标题:   Preparing bismuth/reduced graphene oxide crystal comprises e.g. dissolving bismuth (III) nitrate pentahydrate in nitric acid, stirring, adding oleic acid, n-heptane and acetone, sodium hydroxide solution and forming precursor solution.
  • 专利号:   CN105734666-A, CN105734666-B
  • 发明人:   TAN G, XIA A, ZHAO C, REN H
  • 专利权人:   UNIV SHAANXI SCI TECHNOLOGY
  • 国际专利分类:   C30B029/00, C30B007/14
  • 专利详细信息:   CN105734666-A 06 Jul 2016 C30B-029/00 201663 Pages: 11 Chinese
  • 申请详细信息:   CN105734666-A CN10261098 25 Apr 2016
  • 优先权号:   CN10261098

▎ 摘  要

NOVELTY - Preparing bismuth/reduced graphene oxide crystal comprises e.g. dissolving bismuth (III) nitrate pentahydrate in nitric acid, stirring uniformly, orderly adding oleic acid, n-heptane and acetone, continuing stirring uniformly, adding sodium hydroxide solution, forming precursor solution, stirring to obtain bismuth (III) oxide, washing bismuth (III) oxide and drying, pouring sulfuric acid into cone bottle, cooling to 0 degrees C, maintaining constant temperature, under low stirring condition, orderly adding graphite, sodium nitrate, potassium permanganate. USE - The method is useful for preparing bismuth/reduced graphene oxide crystal (claimed). ADVANTAGE - The method is simple and economical, has good crystal growth and simple device. DETAILED DESCRIPTION - Preparing bismuth/reduced graphene oxide crystal comprises (i) dissolving A mmol bismuth (III) nitrate pentahydrate in B ml nitric acid, stirring uniformly, orderly adding C ml oleic acid, D ml n-heptane and E ml acetone, continuing stirring uniformly, adding F ml sodium hydroxide solution, forming precursor solution, stirring precursor solution under room temperature for 6-8 hours to obtain bismuth (III) oxide, washing bismuth (III) oxide and drying, where A:B:C:D:E:F = 1:8-10:2.5-3.5:2.5-3.5:9-11:4-6, dilute nitric acid concentration is 0.95-1.05 mol/l, concentration of sodium hydroxide solution is 9-11 mol/l, (ii) pouring M mL sulfuric acid into cone bottle, cooling to 0 degrees C, maintaining constant temperature, under low stirring condition, orderly adding X g graphite, Y g sodium nitrate, Z g potassium permanganate, where M:X:Y:Z = 100-130:5:4-6:12-18, stirring uniformly, obtaining mixed liquid, rising temperature of mixed liquid to 25 degrees C, stirring, maintaining temperature for 2.5-3.5 hours, continuing warming mixed liquid temperature to 35 degrees C, stirring, maintaining the temperature for 0.5-4 hours, cooling mixed liquid to 0 degrees C, maintaining constant temperature for 1.5-2.5 hours, orderly adding deionized water and hydrogen peroxide solution to obtain brown graphene oxide product, where mixed liquid, deionized water and hydrogen peroxide solution volume ratio is 100-130:300-500:50-100, washing brown GO product, centrifuging, drying to obtain graphene oxide sheet, (iii) ultrasonic dispersing graphene oxide sheet using aqueous solution of ethyl alcohol to obtain 1.8-2.2 g/l graphene oxide suspension, dissolving bismuth (III) oxide in anhydrous ethyl alcohol, adding acetic acid dropwise until turns to whitening solution to obtain 0.015-0.025 mol/l bismuth (III) oxide suspension, dissolving ammonium metavanadate in deionized water, heating with stirring to dissolve ammonium metavanadate to obtain 0.035-0.045 mol/l light brown ammonium metavanadate solution, (iv) according to bismuth:vanadium mol ratio of 1:1, mixing ammonium metavanadate solution and bismuth (III) oxide suspension, stirring uniformly, adding graphene oxide suspension, appearing bright yellow precipitate, continuing stirring uniformly to obtain brown mixed liquid, where in golden yellow liquid mixture the graphene oxide suspension mass is 15-40 wt.%, (v) adding reduction agent hydrazine hydrate into golden yellow mixture liquid, stirring for 30-60 minutes to obtain precursor solution, where the volume ratio of golden mixed liquid and hydrazine hydrate is 34-46:2-3, (vi) pouring precursor solution into hydro-thermal kettle, carrying out hydro-thermal reaction at 180 degrees C for 6-8 hours, cooling room temperature after reaction completes, washing the product and drying to obtain bismuth/reduced graphene oxide crystal.