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3D nitrogen-doped graphene/molybdenum disulfide compound and preparation method thereof

A nitrogen-doped graphene, molybdenum disulfide technology, applied in the manufacture of hybrid/electric double layer capacitors, hybrid capacitor electrodes, multiple hybrid/electric double layer capacitors, etc. Porous structure, large mass transfer resistance and other problems, to achieve the effects of improved electrochemical activity, superior rate performance, and easy operation

Active Publication Date: 2015-08-12
山东中合控股集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although both methods can obtain nitrogen-doped graphene / molybdenum disulfide composites, due to the lack of a good porous structure in the process of forming the composite, the surface area is relatively low and the mass transfer resistance is large, which is not conducive to material diffusion and charge transfer
[0007] Based on the above examples, although the graphene / MoS 2 The preparation method of the composite has been reported, but up to now, there is no use of bifunctional reagent thioacetamide as raw material, calcium oxalate homogeneous precipitation method to prepare graphene / MoS 2 Reports on domestic and foreign literature and patents related to the compound

Method used

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  • 3D nitrogen-doped graphene/molybdenum disulfide compound and preparation method thereof

Examples

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Effect test

Embodiment 1

[0048] Improved Hummer method to prepare graphene oxide (GO): First, add 2.5g of expanded graphite and 5g of sodium nitrate in a 500mL beaker, then, add 120mL of concentrated sulfuric acid with a mass concentration of 98% to it, and place the resulting mixture in an ice bath Stirring under the conditions for 120min; secondly, under the condition of strong stirring, slowly add 15g of potassium permanganate to the obtained mixture for reaction, the temperature of the reaction is controlled below 20°C, and the potassium permanganate is removed after adding Ice bath equipment, stir the obtained reaction product at room temperature overnight; then, under vigorous stirring, add 150mL of secondary water dropwise to the beaker, the reaction temperature rises rapidly to 98°C, foam can be observed, and the beaker The color of the reaction product turns yellow, and the reaction product is stirred at 98° C. for 2 h, and 50 mL of hydrogen peroxide with a mass concentration of 30% is added t...

Embodiment 2

[0051] After preparing graphene oxide (GO) with the same method as in Example 1, get 100 mg of pre-prepared GO and disperse it in 100 mL of aqueous solution (mass volume ratio is 1:1), after ultrasonic stirring for 30 min, add 1.0 g of calcium chloride and 0.82g of oxalic acid powder, 1.0g of thioacetamide and 0.32g of sodium molybdate were dissolved in 50ml of secondary water at the same time, ultrasonicated for 30min, and the two solutions were mixed, ultrasonicated for 2h. When transferred to a 1000W induction cooker and heated to 80°C, NaOH (0.5mol L -1 ) adjust the pH of the solution to 11, while continuing to heat, after reacting for 8 hours, take the precipitate, wash it several times with secondary water, and dry it in vacuum at 60°C for 24 hours to obtain nitrogen-doped graphene / molybdenum disulfide / calcium oxalate composite thing. Dissolve the prepared nitrogen-doped graphene / molybdenum disulfide / calcium oxalate in 5mol L -1 Hydrochloric acid aqueous solution, ultr...

Embodiment 3

[0053] After preparing graphene oxide (GO) with the same method as in Example 1, get 100 mg of pre-prepared GO and disperse it in 100 mL of aqueous solution (mass volume ratio is 1:1), after ultrasonic stirring for 30 min, add 0.5 g of calcium chloride and 0.41g of oxalic acid powder, 1.0g of thioacetamide and 0.96g of sodium molybdate were dissolved in 50ml of secondary water at the same time, sonicated for 30min, and the two solutions were mixed and sonicated for 2h. When transferred to a 1300W induction cooker and heated to 80°C, ammonia solution (0.1mol L -1 ) adjust the pH of the solution to 10, while continuing to heat, after reacting for 6 hours, take the precipitate, wash it several times with secondary water, and freeze-dry it at -30°C for 24 hours to obtain nitrogen-doped graphene / molybdenum disulfide / calcium oxalate Complex. Dissolve the prepared nitrogen-doped graphene / molybdenum disulfide / calcium oxalate in 5mol L -1 Hydrochloric acid aqueous solution, ultrasoni...

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Abstract

The invention discloses a 3D nitrogen-doped graphene / molybdenum disulfide compound and a preparation method thereof. A 3D nitrogen-doped graphene / molybdenum disulfide composite material (3D G-N / MoS2) is formed via synthesis under the alkaline condition in a homogeneous precipitation method by taking CaC2O4 as a pore forming agent and using a bifunctional reagent thioacetamide to provide a nitrogen source and a sulfur source. CaC2O4 in laminations is removed by ultrasonic dissolution under the acidic condition to form the 3D porous nitrogen-doped graphene / molybdenum disulfide composite material. The preparation method is simple and environment-friendly, MoS2 nano-sheets are uniformly distributed in the surface of graphene, the contact area with graphene is larger, the catalysis performance is high, and the method can be widely applied in the fields including electrocatalysis, photocatalysis and hydrogen evolution catalysis.

Description

technical field [0001] The invention relates to the technical field of nanometer material preparation. Specifically relates to a three-dimensional nitrogen-doped graphene / molybdenum disulfide composite and a preparation method thereof. Background technique [0002] Nanomaterials with two-dimensional layered structures (such as graphene and transition metal dichalcogenides) exhibit excellent properties in the fields of physics, chemistry, electricity, and mechanics due to their special structures, which have important research significance and extensive application prospects. In general, besides the composition and structure of materials, the dimensionality also plays a crucial role in determining the fundamental properties of materials. Molybdenum disulfide (MoS 2 ) is a typical transition metal dichalcogenide, which has a structure and properties very similar to graphene. Due to MoS 2 Layers are combined by van der Waals force, which allows foreign atoms or molecules t...

Claims

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Application Information

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IPC IPC(8): H01G11/86H01G11/24H01G11/26H01G11/36H01G11/12
CPCY02E60/13H01G11/86H01G11/24H01G11/26H01G11/36
Inventor 赵凯王宗花赵春芹桂日军杨敏金辉
Owner 山东中合控股集团有限公司
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