CN107747106A - Nitrogen, the three-dimensional carbon nanometer network load molybdenum disulfide nano material of sulfur doping and preparation - Google Patents

Nitrogen, the three-dimensional carbon nanometer network load molybdenum disulfide nano material of sulfur doping and preparation Download PDF

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CN107747106A
CN107747106A CN201710886672.0A CN201710886672A CN107747106A CN 107747106 A CN107747106 A CN 107747106A CN 201710886672 A CN201710886672 A CN 201710886672A CN 107747106 A CN107747106 A CN 107747106A
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nitrogen
source
molybdenum disulfide
sulfur doping
molybdenum
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CN107747106B (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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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The present invention relates to the three-dimensional carbon nanometer network of a kind of nitrogen, sulfur doping to load molybdenum disulfide nano material, and provides its preparation method and application.The material is that molybdenum disulfide nano sheet is supported on the three-dimensional carbon nanometer network of nitrogen, sulfur doping, wherein molybdenum disulfide nano sheet is in 100 300nm, nitrogen, the three-dimensional carbon thickness of sulfur doping are 1 10nm, three-dimensional grapheme network radius mass percent of molybdenum disulfide and total carbon in 10 50 μm, the material is：(0.3‑0.8):(0.5‑0.2).

Description

Nitrogen, the three-dimensional carbon nanometer network load molybdenum disulfide nano material of sulfur doping and preparation
Technical field
The present invention relates to a kind of three-dimensional carbon nanometer network of nitrogen, sulfur doping load molybdenum disulfide (MoS2) nano material system Preparation Method and application, belong to electrocatalytic hydrogen evolution Material Field.
Background technology
With becoming increasingly conspicuous for environment and energy problem, people are badly in need of seeking reproducible energy source and energy carrier. H2It is a kind of rich content and reproducible clean energy resource, may be used as energy carrier to replace fossil fuel.Produce H2Side Method has the methods of methane gas reformation, photocatalysis Xie Shui, electro-catalysis solution water.Electro-catalysis water decomposition produces H2Be it is a kind of most efficiently, most The large-scale production H of cleaning2Method, therefore people widely study efficient elctro-catalyst.At present, efficiency highest electricity is urged Agent is Pt, but because Pt is expensive and reserves are limited, therefore limit its large-scale application in the industry.Find A kind of sufficient elctro-catalyst of cheap and earth reserves is imperative.
Wherein, MoS2Widely studied as a kind of efficient and stable HER electro-catalysis.But MoS2Itself Electric conductivity is poor, is unfavorable for the performance of its catalytic performance.Solution main at present has two：First, the MoS by 2H phases2Pass through The intercalation of n-BuLi becomes the MoS of 1T phases2；Second, by MoS2It is compound with carbon material, urged so as to improve its electric conductivity and electricity Change Hydrogen Evolution Performance.
The content of the invention
It is an object of the invention to provide the three-dimensional carbon nanometer network of a kind of nitrogen, sulfur doping to load molybdenum disulfide nano material Preparation and application.The material is loaded to by molybdenum disulfide lamella on the three-dimensional carbon nanometer network of nitrogen, sulfur doping, its preparation method mistake Journey is simple, can volume production, the material has good performance as electrocatalytic hydrogen evolution catalysts, has a extensive future.This hair Bright technical scheme realized by following steps,
The three-dimensional carbon nanometer network load molybdenum disulfide nano material of a kind of nitrogen, sulfur doping, it is characterised in that the material is Molybdenum disulfide nano sheet is supported on the three-dimensional carbon nanometer network of nitrogen, sulfur doping, and wherein molybdenum disulfide nano sheet is in 100- 300nm, nitrogen, the three-dimensional carbon thickness of sulfur doping are 1-10nm, and three-dimensional grapheme network radius is at 10-50 μm, two sulphur in the material The mass percent for changing molybdenum and total carbon is：(0.3-0.8):(0.5-0.2).
The preparation method of the nitrogen of the structure, the three-dimensional carbon nanometer network load molybdenum disulfide nano material of sulfur doping, bag Include following steps：
(1) is mixed into carbon source with the one or more in sucrose, glucose, citric acid, ammonium citrate, secondary with four hydrations Ammonium molybdate is molybdenum source, with sodium sulphate (Na2SO4) it is template and sulphur source, with the one or more in urea, melamine, dicyandiamide Nitrogen source is mixed into, using the molybdenum mol ratio in the carbon and molybdenum source in carbon source as (20~100):1, with the molybdenum and Na in molybdenum source2SO4's Mass ratio is 1：(10~100), using the nitrogen mol ratio in the carbon and nitrogen source in carbon source as (10~100):1 meter, by carbon source, nitrogen Source, molybdenum source and Na2SO4Add in deionized water and dissolve, stir wiring solution-forming, then ultrasonic mixing uniformly freezes afterwards, then carry out vacuum Dry, obtain mixture；
(2) mixture grind into powder made from step (1) is laid in Noah's ark, is placed in tube furnace flat-temperature zone and is forged by Burn：With N2Or Ar one or two are first passed through inert gas 30- as inert gas source by 200~400ml/min of flow 60 minutes to exclude air；Again using Ar as carrier gas, carrier gas flux is fixed as 50~200ml/min, with 1~10 DEG C/min's Programming rate heats up tube furnace to 650~800 DEG C, and insulation 1-8h is carbonized, and reaction is cooled to room temperature after terminating, and is calcined Product；
(3) calcined product made from collection steps (2), finely ground, being washed in calcined product does not have Na2SO4Untill, in temperature Spend the three-dimensional carbon nanometer network load molybdenum disulfide nano material for dry at 60~120 DEG C, obtaining nitrogen, sulfur doping.
The nitrogen, the three-dimensional carbon nanometer network load molybdenum disulfide nano materials application of sulfur doping react in electrocatalytic hydrogen evolution.
The present invention utilizes improved freeze-drying --- template pyrolysismethod, and it is very thin to prepare lamella, and is self-assembled into nitrogen, sulphur The three-dimensional carbon nanometer network of doping, while have two-dimentional MoS in its area load2Nanometer sheet.This material realizes in structure Two and three dimensions it is compound, so as to improve the electric conductivity of catalyst.With advantages below：The present invention utilizes original cheap and easy to get Material prepares the three-dimensional carbon nanometer network load molybdenum disulfide nano material of nitrogen, sulfur doping, and cost is cheap, and course of reaction is simple, can Control property is strong, and molybdenum disulfide dispersiveness is preferably.The material structure is homogeneous, and pattern is excellent, excellent performance, while nitrogen, sulfur doping also increase The avtive spot of carbon material surface is added, there is good performance for electrocatalytic hydrogen evolution reaction.
Brief description of the drawings
Fig. 1 is that nitrogen, the three-dimensional carbon nanometer network of sulfur doping that the embodiment of the present invention 1 obtains load molybdenum disulfide nano material SEM photograph.From this view it is apparent that nitrogen, the three-dimensional carbon network morphology of sulfur doping.
Fig. 2 is that nitrogen, the three-dimensional carbon nanometer network of sulfur doping that the embodiment of the present invention 1 obtains load molybdenum disulfide nano material TEM photos.From this view it is apparent that from this view it is apparent that molybdenum disulfide nano sheet (black) be dispersed in nitrogen, sulfur doping three Tie up on carbon network matrix.
Fig. 3 is that nitrogen, the three-dimensional carbon nanometer network of sulfur doping that the embodiment of the present invention 1 obtains load molybdenum disulfide nano material XRD spectrum.
Fig. 4 is that nitrogen, the three-dimensional carbon nanometer network of sulfur doping that the embodiment of the present invention 1 obtains load molybdenum disulfide nano material LSV collection of illustrative plates as electrocatalytic hydrogen evolution catalysts.
Embodiment
The particular content of the present invention is described as follows with reference to specific embodiment：
Embodiment 1：
Weigh 3.8g citric acids, 0.24g melamines, 0.25g tetra- and be hydrated ammonium paramolybdate and 2.8g Na2SO4, by mixture Be dissolved in 50ml deionized water, with mixing speed 300r/min magnetic stirring apparatus, stirring and dissolving wiring solution-forming, then again with Power is 400W ultrasonic device ultrasound 15min, well mixed to be placed in refrigerator freezing, and freeze-drying is placed in after solution freeze over Machine is dried in vacuo in -50 DEG C, obtains mixture.Milled mixtures, 10g mixed-powder is taken to be placed in Noah's ark, by Noah's ark Be put into tube furnace, be passed through 200ml/min Ar inert gases 30min exclude air, then using 200ml/min Ar as carrier gas, And 750 DEG C of temperature is warming up to 10 DEG C/min programming rate, insulation 2h carries out carburizing reagent, and reaction is protected after terminating in Ar atmosphere Room temperature is cooled under shield, obtains calcined product.Calcined product is collected, finely ground, being washed in product does not have Na2SO4Untill, 80 Dried at DEG C, obtain the three-dimensional carbon nanometer network load molybdenum disulfide nano material of nitrogen, sulfur doping.
Obtained material 5mg is taken to be scattered in the mixed solution of 5% μ L of Nafion solution 50, the μ L of isopropanol 950 composition In, 5 μ L drops are taken in being spontaneously dried on glass-carbon electrode.With 0.5M H2SO4As electrolyte, using graphite rod as to electrode, Ag/ AgCl electrodes are as reference electrode, and it sweeps to -500mV under speed in sweeping for 5mV/s by 0mV, as shown in figure 4, in 10mA/cm2's Overpotential is 228mV under current density.
Embodiment 2：
Weigh 3.8g citric acids, 0.24g melamines, 0.25g tetra- and be hydrated ammonium paramolybdate and 2.8g Na2SO4, by mixture Be dissolved in 50ml deionized water, with mixing speed 300r/min magnetic stirring apparatus, stirring and dissolving wiring solution-forming, then again with Power is 400W ultrasonic device ultrasound 15min, well mixed to be placed in refrigerator freezing, and freeze-drying is placed in after solution freeze over Machine is dried in vacuo in -50 DEG C, obtains mixture.Milled mixtures, 10g mixed-powder is taken to be placed in Noah's ark, by Noah's ark Be put into tube furnace, be passed through 200ml/min Ar inert gases 30min exclude air, then using 200ml/min Ar as carrier gas, And 700 DEG C of temperature is warming up to 10 DEG C/min programming rate, insulation 2h carries out carburizing reagent, and reaction is protected after terminating in Ar atmosphere Room temperature is cooled under shield, obtains calcined product.Calcined product is collected, finely ground, being washed in product does not have Na2SO4Untill, 80 Dried at DEG C, obtain the three-dimensional carbon nanometer network load molybdenum disulfide nano material of nitrogen, sulfur doping.
Embodiment 3：
Weigh 3.8g citric acids, 0.24g melamines, 0.5g tetra- and be hydrated ammonium paramolybdate and 2.8g Na2SO4, by mixture Be dissolved in 50ml deionized water, with mixing speed 300r/min magnetic stirring apparatus, stirring and dissolving wiring solution-forming, then again with Power is 400W ultrasonic device ultrasound 15min, well mixed to be placed in refrigerator freezing, and freeze-drying is placed in after solution freeze over Machine is dried in vacuo in -50 DEG C, obtains mixture.Milled mixtures, 10g mixed-powder is taken to be placed in Noah's ark, by Noah's ark Be put into tube furnace, be passed through 200ml/min Ar inert gases 30min exclude air, then using 200ml/min Ar as carrier gas, And 750 DEG C of temperature is warming up to 10 DEG C/min programming rate, insulation 2h carries out carburizing reagent, and reaction is protected after terminating in Ar atmosphere Room temperature is cooled under shield, obtains calcined product.Calcined product is collected, finely ground, being washed in product does not have Na2SO4Untill, 80 Dried at DEG C, obtain the three-dimensional carbon nanometer network load molybdenum disulfide nano material of nitrogen, sulfur doping.
Embodiment 4：
Weigh 3.8g citric acids, 0.24g melamines, 0.5g tetra- and be hydrated ammonium paramolybdate and 2.8g Na2SO4, by mixture Be dissolved in 50ml deionized water, with mixing speed 300r/min magnetic stirring apparatus, stirring and dissolving wiring solution-forming, then again with Power is 400W ultrasonic device ultrasound 15min, well mixed to be placed in refrigerator freezing, and freeze-drying is placed in after solution freeze over Machine is dried in vacuo in -50 DEG C, obtains mixture.Milled mixtures, 10g mixed-powder is taken to be placed in Noah's ark, by Noah's ark Be put into tube furnace, be passed through 200ml/min Ar inert gases 30min exclude air, then using 200ml/min Ar as carrier gas, And 800 DEG C of temperature is warming up to 10 DEG C/min programming rate, insulation 1h carries out carburizing reagent, and reaction is protected after terminating in Ar atmosphere Room temperature is cooled under shield, obtains calcined product.Calcined product is collected, finely ground, being washed in product does not have Na2SO4Untill, 80 Dried at DEG C, obtain the three-dimensional carbon nanometer network load molybdenum disulfide nano material of nitrogen, sulfur doping.

Claims (3)

1. the three-dimensional carbon nanometer network load molybdenum disulfide nano material of a kind of nitrogen, sulfur doping, it is characterised in that the material is two Molybdenum sulfide nanometer sheet is supported on the three-dimensional carbon nanometer network of nitrogen, sulfur doping, wherein molybdenum disulfide nano sheet in 100-300nm, Nitrogen, the three-dimensional carbon thickness of sulfur doping are 1-10nm, three-dimensional grapheme network radius at 10-50 μm, in the material molybdenum disulfide with The mass percent of total carbon is：(0.3-0.8):(0.5-0.2).
2. the nitrogen of structure, the three-dimensional carbon nanometer network of sulfur doping load molybdenum disulfide nano material described in a kind of claim 1 Preparation method, comprise the following steps：
(1) is mixed into carbon source with the one or more in sucrose, glucose, citric acid, ammonium citrate, with four hydration para-molybdic acids Ammonium is molybdenum source, with sodium sulphate (Na2SO4) it is template and sulphur source, mixed with the one or more in urea, melamine, dicyandiamide For nitrogen source, using the molybdenum mol ratio in the carbon and molybdenum source in carbon source as (20~100):1, with the molybdenum and Na in molybdenum source2SO4Quality Than for 1：(10~100), using the nitrogen mol ratio in the carbon and nitrogen source in carbon source as (10~100):1 meter, by carbon source, nitrogen source, molybdenum Source and Na2SO4Add in deionized water and dissolve, stir wiring solution-forming, then ultrasonic mixing uniformly freezes afterwards, then be dried in vacuo, Obtain mixture；
(2) mixture grind into powder made from step (1) is laid in Noah's ark, is placed in tube furnace flat-temperature zone and is calcined by： With N2Or Ar one or two are first passed through inert gas 30-60 as inert gas source by 200~400ml/min of flow Minute to exclude air；Again using Ar as carrier gas, carrier gas flux is fixed as 50~200ml/min, with 1~10 DEG C/min liter Warm speed heats up tube furnace to 650~800 DEG C, and insulation 1-8h is carbonized, and reaction is cooled to room temperature after terminating, and obtains calcining production Thing；
(3) calcined product made from collection steps (2), finely ground, being washed in calcined product does not have Na2SO4Untill, it is in temperature Dried at 60~120 DEG C, obtain the three-dimensional carbon nanometer network load molybdenum disulfide nano material of nitrogen, sulfur doping.
3. the three-dimensional carbon nanometer network load molybdenum disulfide nano materials application of nitrogen, sulfur doping described in claim 1 is urged in electricity Change evolving hydrogen reaction.
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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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
CN114130413A (en) * 2021-10-26 2022-03-04 浙江大学衢州研究院 Preparation method and application of N, S-double-heterocarbon-supported tungsten-based catalyst

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CN108636426A (en) * 2018-03-22 2018-10-12 西北工业大学 Three-dimensional order is orientated molybdenum disulfide/graphene high-efficiency photocatalysis hydrogen production composite nano materials and preparation method
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CN108636427A (en) * 2018-04-27 2018-10-12 重庆文理学院 A kind of molybdenum disulfide-nitrogen sulfur doping graphite foil composite nano materials and preparation method
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
CN109346686A (en) * 2018-09-12 2019-02-15 天津大学 Three-dimensional grapheme network structure loads the preparation method of Prussian blue similar object
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
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
CN111106326A (en) * 2018-10-27 2020-05-05 中国石油化工股份有限公司 Nitrogen-doped molybdenum disulfide/graphene composite material
CN111106325A (en) * 2018-10-27 2020-05-05 中国石油化工股份有限公司 Nitrogen-doped molybdenum disulfide/C/graphene composite material
CN111235602A (en) * 2018-11-28 2020-06-05 中国科学院大连化学物理研究所 High-performance hydrogen evolution electrode and preparation and application thereof
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
CN114130413A (en) * 2021-10-26 2022-03-04 浙江大学衢州研究院 Preparation method and application of N, S-double-heterocarbon-supported tungsten-based catalyst

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