• 专利标题:   Preparing graphene-molybdenum disulfide/titanium dioxide complex material having an accordion structure useful as catalyst comprises e.g. preparing graphite oxide, washing, dissolving, vacuum drying, dispersing and transferring.
  • 专利号:   CN110252345-A
  • 发明人:   YANG C, LI J, ZHANG Y, WEN Z, ZHAO M, JIANG Q
  • 专利权人:   UNIV JILIN
  • 国际专利分类:   B01J027/051, B01J027/224, B01J037/06, B01J037/10, B01J037/34, C25B001/02, C25B011/06
  • 专利详细信息:   CN110252345-A 20 Sep 2019 B01J-027/051 201985 Pages: 21 Chinese
  • 申请详细信息:   CN110252345-A CN10387501 10 May 2019
  • 优先权号:   CN10387501

▎ 摘  要

NOVELTY - Preparing graphene-molybdenum disulfide/titanium dioxide complex material having an accordion structure comprises e.g. preparing graphite oxide according to the modified Hummers method, preparing layered titanium carbide by acid etching, specifically by dissolving 2.8-3.2 g titanium aluminum carbide in 30-50 ml 5-20 wt.% hydrogen fluoride, mechanically stirring for 9-12 hours, washing with deionized water for 2-6 times and ethanol for 1-3 times, placing obtained black precipitate in vacuum drying oven at 40-80 degrees C for 10-14 hours to obtain titanium carbide, dissolving 20-30 mg titanium carbide, 30-50 mg ammonium molybdate tetrahydrate (AMT) and 0.5-0.8 g thiourea in 5-20 ml ultrapure water, stirring uniformly with magnetic stirrer, dispersing 0.2-1.2 ml graphite oxide in obtained solution, performing ultrasonication for 10-20 minutes, transferring to stainless steel reaction kettle, maintaining temperature at 150-200 degrees C for 20-30 hours, and washing obtained black powder. USE - The graphene-molybdenum disulfide/titanium dioxide complex material having an accordion structure is useful as catalyst (claimed). ADVANTAGE - The method is economical. DETAILED DESCRIPTION - Preparing graphene-molybdenum disulfide/titanium dioxide complex material having an accordion structure comprises (a) preparing graphite oxide according to the modified Hummers method, (b) preparing layered titanium carbide by acid etching, specifically by dissolving 2.8-3.2 g titanium aluminum carbide in 30-50 ml 5-20 wt.% hydrogen fluoride, mechanically stirring for 9-12 hours, washing with deionized water for 2-6 times and ethanol for 1-3 times, placing obtained black precipitate in vacuum drying oven at 40-80 degrees C for 10-14 hours to obtain titanium carbide, and (c) dissolving 20-30 mg titanium carbide, 30-50 mg ammonium molybdate tetrahydrate (AMT) and 0.5-0.8 g thiourea in 5-20 ml ultrapure water, stirring uniformly with magnetic stirrer, dispersing 0.2-1.2 ml graphite oxide in obtained solution, performing ultrasonication for 10-20 minutes, transferring to stainless steel reaction kettle, maintaining temperature at 150-200 degrees C for 20-30 hours, washing obtained black powder with water and ethanol, drying in vacuum oven to obtain graphene-molybdenum disulfide/titanium dioxide complex material. An INDEPENDENT CLAIM is also included for graphene-molybdenum disulfide/titanium dioxide complex material having an accordion structure which is electrochemically tested as a catalyst by (1) dispersing catalyst 2-3 mg graphene-molybdenum disulfide/titanium dioxide complex material in 0.4-0.6 ml water/isopropanol/naphthol solution, ultrasonically treating for 20-40 minutes to obtain catalyst ink solution, dropping 10-20 mu l solution on the glassy carbon electrode, and drying at room temperature to form uniform catalyst film, (2) carrying out electrochemical testing in standard three-electrode test system in which the electrode is a working electrode, carbon rod electrode is a counter electrode, saturated calomel electrode is a reference electrode, and 0.4-0.6 M sulfuric acid solution is an electrolyte, (3) adopting use of graphene-molybdenum disulfide/titanium dioxide as working electrode for testing on an Ivium-n-Stat electrochemical workstation, performing polarization curve test on rotating disk electrode with rotation speed of 2025 revolutions/minute relative to the reversible hydrogen electrode, where the potential scanning range is 0 to -0.767 V, and the scanning speed is 5 mV/second, performing electrochemical impedance mapping test at a constant voltage of -0.25 V with respect to the potential of the reversible hydrogen electrode at frequency of 100 KHz to 0.1 Hz, when the cyclic voltammetry test is performed, then potential scanning range with respect to the reversible hydrogen electrode is -0.2 to 0.1 V, and the scanning speed is 100 mV/second, and performing chronopotentiometry at current density of 10 mA/cm2 for 200000 seconds, and (d) adopting use of graphene-molybdenum disulfide/titanium dioxide complex material as a catalyst for hydrogen evolution reaction, where the initial potential is 90 mV, the Tafel slope is 49.5 mV/dec, where after the complex material has passed the cyclic voltammetry test of 150000 cycles, the current density is almost non-attenuating, and after 200000 s chronopotential test, the potential decay is only 5%.