CN107747106B - Nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material and preparation - Google Patents

Nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material and preparation Download PDF

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CN107747106B
CN107747106B CN201710886672.0A CN201710886672A CN107747106B CN 107747106 B CN107747106 B CN 107747106B CN 201710886672 A CN201710886672 A CN 201710886672A CN 107747106 B CN107747106 B CN 107747106B
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nitrogen
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molybdenum disulfide
molybdenum
carbon
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CN107747106A (en
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何春年
刁乐晨
赵乃勤
师春生
刘恩佐
马丽颖
何芳
李家俊
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Tianjin University
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Abstract

The invention relates to a nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material, and provides a preparation method and application thereof. The material is prepared by loading molybdenum disulfide nanosheets on a nitrogen and sulfur doped three-dimensional carbon nano network, wherein the molybdenum disulfide nanosheets are 100-300nm thick, the nitrogen and sulfur doped three-dimensional carbon is 1-10nm thick, the radius of the three-dimensional graphene network is 10-50 mu m, and the mass percentage of molybdenum disulfide to the total carbon in the material is as follows: (0.3-0.8):(0.5-0.2).

Description

Nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material and preparation
Technical Field
The invention relates to nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide (MoS)2) A preparation method and application of a nano material, belonging to the field of electrocatalytic hydrogen evolution materials.
Background
With the increasing prominence of environmental and energy problems, people are in urgent need to seek renewable energy sources and energy carriers. H2Is a clean energy source with rich and renewable content, and can be used as an energy carrier to replaceTo replace fossil fuels. Generation of H2The method comprises methane gas reforming, photocatalytic water decomposition, electrocatalytic water decomposition and other methods. Electrocatalytic decomposition of water to produce H2Is the most efficient and cleaner large-scale production H2So that efficient electrocatalysts have been extensively studied. Currently, the most efficient electrocatalyst is Pt, but its large-scale application in industry is limited due to its high price and limited reserves. It is imperative to find an electrocatalyst that is cheap and has a sufficient earth reserve.
Wherein, MoS2Is widely studied as a highly efficient and stable HER electrocatalysis. But MoS2The conductivity of the catalyst is poor, which is not good for the performance of the catalytic performance. There are two main solutions at present: one is MoS of 2H phase2MoS changed to 1T phase by intercalation of n-butyllithium2(ii) a Secondly, MoS2The carbon material is compounded, so that the conductivity and the electrocatalytic hydrogen evolution performance of the carbon material are improved.
Disclosure of Invention
The invention aims to provide preparation and application of a nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material. The material is loaded on a nitrogen and sulfur doped three-dimensional carbon nano network by a molybdenum disulfide sheet layer, the preparation method is simple in process and can realize mass production, and the material has good performance and wide application prospect when being used as an electro-catalytic hydrogen evolution reaction catalyst. The technical scheme of the invention is realized by the following steps,
the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material is characterized in that molybdenum disulfide nanosheets are loaded on a nitrogen and sulfur doped three-dimensional carbon nano network, wherein the molybdenum disulfide nanosheets are 300nm in size at 100-: (0.3-0.8):(0.5-0.2).
The preparation method of the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material with the structure comprises the following steps:
(1) using cane sugar and grapeOne or more of sugar, citric acid and ammonium citrate as carbon source, ammonium paramolybdate tetrahydrate as molybdenum source, and sodium sulfate (Na)2SO4) Taking one or more of urea, melamine and dicyandiamide as a nitrogen source, taking the molar ratio of carbon in a carbon source to molybdenum in a molybdenum source as (20-100): 1, and taking molybdenum in the molybdenum source and Na as a template and a sulfur source2SO4The mass ratio of (1): (10-100) mixing a carbon source, a nitrogen source, a molybdenum source and Na in a molar ratio of carbon in the carbon source to nitrogen in the nitrogen source of (10-100): 12SO4Adding the mixture into deionized water for dissolving, stirring to prepare a solution, ultrasonically mixing the solution uniformly, freezing the solution, and performing vacuum drying to obtain a mixture;
(2) grinding the mixture prepared in the step (1) into powder, paving the powder in a square boat, and calcining the powder in a constant-temperature area of a tube furnace: with N2Or one or two of Ar is used as an inert gas source, and inert gas is firstly introduced for 30-60 minutes at the flow rate of 200-400 ml/min to remove air; then, Ar is used as carrier gas, the flow rate of the carrier gas is fixed to be 50-200 ml/min, the tubular furnace is heated to 650-800 ℃ at the heating rate of 1-10 ℃/min, the temperature is kept for 1-8h for carbonization, and the product is cooled to room temperature after the reaction is finished to obtain a calcined product;
(3) collecting the calcined product obtained in the step (2), grinding, and washing with water until the calcined product is free from Na2SO4And drying at the temperature of 60-120 ℃ to obtain the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material.
The nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material is applied to electrocatalytic hydrogen evolution reaction.
The invention utilizes improved freeze drying-template pyrolysis method to prepare a three-dimensional carbon nano network with extremely thin lamella and self-assembled into nitrogen and sulfur doping, and simultaneously two-dimensional MoS is loaded on the surface of the three-dimensional carbon nano network2Nanosheets. The material realizes two-dimensional and three-dimensional composition in structure, thereby improving the conductivity of the catalyst. Has the following advantages: the invention utilizes cheap and easily available raw materials to prepare the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material, has low cost and simple reaction process, and can be used for preparing the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano materialStrong controllability and good molybdenum disulfide dispersibility. The material has the advantages of uniform structure, excellent appearance and excellent performance, and simultaneously, the doping of nitrogen and sulfur increases the active sites on the surface of the carbon material, so the material has good performance when being used for the electrocatalytic hydrogen evolution reaction.
Drawings
Fig. 1 is an SEM photograph of a nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material obtained in example 1 of the present invention. The morphology of the nitrogen and sulfur doped three-dimensional carbon network is obvious from the figure.
Fig. 2 is a TEM photograph of the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material obtained in example 1 of the present invention. It is evident from this figure that molybdenum disulfide nanoplates (black) are dispersed on a nitrogen, sulfur doped three-dimensional carbon network matrix.
Fig. 3 is an XRD spectrum of the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material obtained in example 1 of the present invention.
Fig. 4 is an LSV spectrum of the nitrogen-sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material as an electrocatalytic hydrogen evolution reaction catalyst obtained in example 1 of the present invention.
Detailed Description
The following specific contents of the present invention are specifically described with reference to the following specific examples:
example 1:
3.8g of citric acid, 0.24g of melamine, 0.25g of ammonium paramolybdate tetrahydrate and 2.8g of Na were weighed out2SO4Dissolving the mixture in 50ml of deionized water, stirring and dissolving the mixture by a magnetic stirrer with the stirring speed of 300r/min to prepare a solution, then carrying out ultrasonic treatment for 15min by an ultrasonic device with the power of 400W, uniformly mixing the solution, freezing the mixture in a freezer, and putting the frozen mixture in a freeze dryer for vacuum drying at the temperature of 50 ℃ below zero after the solution is completely frozen to obtain the mixture. Grinding the mixture, putting 10g of mixed powder into a square boat, putting the square boat into a tube furnace, introducing 200ml/min Ar inert gas for 30min to remove air, taking 200ml/min Ar as a carrier gas, raising the temperature to 750 ℃ at a temperature raising speed of 10 ℃/min, preserving the temperature for 2h to carry out carbonization reaction, and cooling under the protection of Ar atmosphere after the reaction is finishedAnd cooling to room temperature to obtain a calcined product. Collecting the calcined product, grinding, and washing with water until the product is free of Na2SO4And drying at 80 ℃ to obtain the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material.
5mg of the prepared material is dispersed in a mixed solution consisting of 50 mu L of 5% Nafion solution and 950 mu L of isopropanol, and 5 mu L of the mixed solution is dropped on a glassy carbon electrode for natural drying. At 0.5M H2SO4As an electrolyte, a graphite rod was used as a counter electrode and an Ag/AgCl electrode as a reference electrode, which was swept from 0mV to-500 mV at a sweep rate of 5mV/s, as shown in FIG. 4, at 10mA/cm2The overpotential at the current density of (1) is 228 mV.
Example 2:
3.8g of citric acid, 0.24g of melamine, 0.25g of ammonium paramolybdate tetrahydrate and 2.8g of Na were weighed out2SO4Dissolving the mixture in 50ml of deionized water, stirring and dissolving the mixture by a magnetic stirrer with the stirring speed of 300r/min to prepare a solution, then carrying out ultrasonic treatment for 15min by an ultrasonic device with the power of 400W, uniformly mixing the solution, freezing the mixture in a freezer, and putting the frozen mixture in a freeze dryer for vacuum drying at the temperature of 50 ℃ below zero after the solution is completely frozen to obtain the mixture. Grinding the mixture, putting 10g of mixed powder into a square boat, putting the square boat into a tube furnace, introducing 200ml/min of Ar inert gas for 30min to remove air, taking 200ml/min of Ar as a carrier gas, heating to 700 ℃ at the heating rate of 10 ℃/min, preserving heat for 2h to carry out carbonization reaction, and cooling to room temperature under the protection of Ar atmosphere after the reaction is finished to obtain a calcined product. Collecting the calcined product, grinding, and washing with water until the product is free of Na2SO4And drying at 80 ℃ to obtain the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material.
Example 3:
3.8g of citric acid, 0.24g of melamine, 0.5g of ammonium paramolybdate tetrahydrate and 2.8g of Na were weighed out2SO4Dissolving the mixture in 50ml of deionized water, stirring and dissolving the mixture by a magnetic stirrer with the stirring speed of 300r/min to prepare a solution, then ultrasonically treating the solution for 15min by an ultrasonic device with the power of 400W, uniformly mixing the solution, putting the mixture in a refrigerator for freezing, and completely solidifying the solutionAfter freezing, the mixture was vacuum dried in a freeze dryer at-50 ℃ to obtain a mixture. Grinding the mixture, putting 10g of mixed powder into a square boat, putting the square boat into a tube furnace, introducing 200ml/min of Ar inert gas for 30min to remove air, taking 200ml/min of Ar as a carrier gas, heating to 750 ℃ at a heating rate of 10 ℃/min, preserving heat for 2h to carry out carbonization reaction, and cooling to room temperature under the protection of Ar atmosphere after the reaction is finished to obtain a calcined product. Collecting the calcined product, grinding, and washing with water until the product is free of Na2SO4And drying at 80 ℃ to obtain the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material.
Example 4:
3.8g of citric acid, 0.24g of melamine, 0.5g of ammonium paramolybdate tetrahydrate and 2.8g of Na were weighed out2SO4Dissolving the mixture in 50ml of deionized water, stirring and dissolving the mixture by a magnetic stirrer with the stirring speed of 300r/min to prepare a solution, then carrying out ultrasonic treatment for 15min by an ultrasonic device with the power of 400W, uniformly mixing the solution, freezing the mixture in a freezer, and putting the frozen mixture in a freeze dryer for vacuum drying at the temperature of 50 ℃ below zero after the solution is completely frozen to obtain the mixture. Grinding the mixture, putting 10g of mixed powder into a square boat, putting the square boat into a tube furnace, introducing 200ml/min of Ar inert gas for 30min to remove air, taking 200ml/min of Ar as a carrier gas, heating to 800 ℃ at the heating rate of 10 ℃/min, preserving heat for 1h to carry out carbonization reaction, and cooling to room temperature under the protection of Ar atmosphere after the reaction is finished to obtain a calcined product. Collecting the calcined product, grinding, and washing with water until the product is free of Na2SO4And drying at 80 ℃ to obtain the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material.

Claims (1)

1. A nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material applied to electrocatalytic hydrogen evolution reaction is characterized in that a molybdenum disulfide nanosheet is loaded on a nitrogen and sulfur doped three-dimensional carbon nano network, wherein the molybdenum disulfide nanosheet is 100-300nm in thickness, the nitrogen and sulfur doped three-dimensional carbon is 1-10nm in thickness, the radius of a three-dimensional graphene network is 10-50 mu m, and the mass percentages of molybdenum disulfide and total carbon in the material are as follows: (0.3-0.8): (0.5-0.2), the preparation method of the material comprises the following steps:
(1) one or more of sucrose, glucose, citric acid and ammonium citrate are mixed as a carbon source, ammonium paramolybdate tetrahydrate is used as a molybdenum source, and sodium sulfate Na is used2SO4Taking one or more of urea, melamine and dicyandiamide as a nitrogen source, taking the molar ratio of carbon in a carbon source to molybdenum in a molybdenum source as (20-100): 1, and taking molybdenum in the molybdenum source and Na as a template and a sulfur source2SO4The mass ratio of (1): (10-100) mixing a carbon source, a nitrogen source, a molybdenum source and Na in a molar ratio of carbon in the carbon source to nitrogen in the nitrogen source of (10-100): 12SO4Adding the mixture into deionized water for dissolving, stirring to prepare a solution, ultrasonically mixing the solution uniformly, freezing the solution, and performing vacuum drying to obtain a mixture;
(2) grinding the mixture prepared in the step (1) into powder, paving the powder in a square boat, and calcining the powder in a constant-temperature area of a tube furnace: with N2Or one or two of Ar is used as an inert gas source, and inert gas is firstly introduced for 30-60 minutes at the flow rate of 200-400 ml/min to remove air; then, Ar is used as carrier gas, the flow rate of the carrier gas is fixed to be 50-200 ml/min, the tubular furnace is heated to 650-800 ℃ at the heating rate of 1-10 ℃/min, the temperature is kept for 1-8h for carbonization, and the product is cooled to room temperature after the reaction is finished to obtain a calcined product;
(3) collecting the calcined product obtained in the step (2), grinding, and washing with water until the calcined product is free from Na2SO4And drying at the temperature of 60-120 ℃ to obtain the nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material.
CN201710886672.0A 2017-09-22 2017-09-22 Nitrogen and sulfur doped three-dimensional carbon nano network loaded molybdenum disulfide nano material and preparation Expired - Fee Related CN107747106B (en)

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CN108636426B (en) * 2018-03-22 2020-12-08 西北工业大学 Three-dimensional ordered oriented molybdenum disulfide/graphene high-efficiency photocatalytic hydrogen production composite nano material and preparation method thereof
CN108636427B (en) * 2018-04-27 2021-02-02 重庆文理学院 Molybdenum disulfide-nitrogen sulfur doped graphite foil composite nanomaterial and preparation method thereof
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CN109351363A (en) * 2018-10-16 2019-02-19 安徽理工大学 A kind of evolving hydrogen reaction catalyst of layered mesoporous structure and preparation method thereof
CN111106325B (en) * 2018-10-27 2021-03-05 中国石油化工股份有限公司 Nitrogen-doped molybdenum disulfide/C/graphene composite material
CN111106326B (en) * 2018-10-27 2021-11-09 中国石油化工股份有限公司 Nitrogen-doped molybdenum disulfide/graphene composite material
CN111235602B (en) * 2018-11-28 2021-08-31 中国科学院大连化学物理研究所 High-performance hydrogen evolution electrode and preparation and application thereof
CN112522726A (en) * 2020-10-30 2021-03-19 徐州瑞鑫新材料研究院有限公司 Preparation method and application of nitrogen-doped porous carbon/molybdenum disulfide composite material derived from natural agar
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