CN105836804B - A kind of graded structure carbon intercalation MoS2@rGO preparation method - Google Patents

A kind of graded structure carbon intercalation MoS2@rGO preparation method Download PDF

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CN105836804B
CN105836804B CN201610212081.0A CN201610212081A CN105836804B CN 105836804 B CN105836804 B CN 105836804B CN 201610212081 A CN201610212081 A CN 201610212081A CN 105836804 B CN105836804 B CN 105836804B
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preparation
mos
carbon intercalation
structure carbon
graded structure
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CN105836804A (en
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李亚峰
魏明灯
车宗洲
陈凯翔
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Fuzhou University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases

Abstract

The invention belongs to the preparation field of nano material, and in particular to a kind of graded structure carbon intercalation MoS2@rGO preparation method.By the improved graphene oxide of hummers methods and Mo3O10(C2H10N2) be scattered in deionized water, after ultrasonic 0.5 h, L cysteines and glucose are added, after hydro-thermal reaction, then through centrifuging, washing, dry, obtained product is calcined to the MoS for producing carbon intercalation under an inert atmosphere2Compound of the nanometer sheet vertical-growth in graphenic surface.The preparation method is simple, reproducible, be conducive to large-scale production, with potential application value.

Description

A kind of graded structure carbon intercalation MoS2@rGO preparation method
Technical field
The invention belongs to the preparation field of nano material, and in particular to a kind of graded structure carbon intercalation MoS2@rGO system Preparation Method.
Background technology
The discovery of graphene and acquired immense success is studied it, excite people to other stratiform two-dimensional nano materials Expect the great interest of research, MoS2It is a kind of Layered dual compound of typical graphite-like structure, layer passes through weaker with interlayer Van der Waals force combine, so as to easily be stripped into relatively thin nanometer sheet, in necks such as lubrication, catalysis and energy storage and conversions Domain is with a wide range of applications.Recently, the MoS of layer structure is constructed2/ graphene binary composite, because it is combined MoS2, two kinds of materials of graphene advantage, as recent study hotspot.It has been reported that the different method of many kinds in document The MoS of many different-shape structures is synthesized2/ graphene composite material, extends its application in fields such as catalysis, energy storage. But up to the present, it is not related to the MoS of graded structure carbon intercalation also2The report of@rGO composites.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of graded structure carbon intercalation MoS2@rGO's Preparation method.The MoS of carbon intercalation has been made in the present invention2Compound of the nanometer sheet vertical-growth in graphenic surface so that MoS2Receive The surface-active site of rice piece is maximized.
For achieving the above object, the technical scheme is that：
A kind of graded structure carbon intercalation MoS2@rGO preparation method, by the improved graphene oxide of hummers methods And Mo3O10(C2H10N2) be scattered in deionized water, after ultrasonic 0.5 h, Cys and glucose are added, through hydro-thermal reaction Afterwards, then through centrifuging, washing, dry, obtained product is calcined under an inert atmosphere and produced.
Graphene oxide, Mo3O10(C2H10N2), the mass ratio of Cys and glucose be：10mg:0.125g: 0.375g:0.2g。
Described hydro-thermal reaction is：200 DEG C of hydro-thermal reaction 15h.
Described inert atmosphere is：H2With Ar gaseous mixture, H2Shared volume fraction is 5%；Described calcining is 800 DEG C and forged Burn 2h.
The preparation method of graphene oxide is：Under ice-water bath, 2 g crystalline flake graphites and 1 g sodium nitrate are added to 60 ml In the concentrated sulfuric acid, after 10 min of stirring, 6 g potassium permanganate are slowly added to, control water temperature is no more than 5
DEG C, after potassium permanganate addition is finished；Temperature is increased to 35 DEG C, water-bath two hours is then slowly added into 90 ml After deionized water, 10 min of stirring；Continue to add 280 ml deionized waters, it is 30 %'s then to add 30 ml mass fractions H2O2, obtain graphene oxide in a week with being dialysed after the % of mass fraction 5 HCl and deionized water cyclic washing successively water-soluble Liquid.
Graded structure carbon intercalation MoS made from a kind of preparation method as described above2@rGO。
The beneficial effects of the present invention are：
1）The MoS of carbon intercalation has been made in the present invention2Compound of the nanometer sheet vertical-growth in graphenic surface so that MoS2 The surface-active site of nanometer sheet is maximized；
2）The preparation method of the present invention is simple, reproducible, be conducive to large-scale production, with potential application value.
Brief description of the drawings
Fig. 1（a）For the MoS of graded structure carbon intercalation2The scanning electron microscope (SEM) photograph of@rGO compounds；
Fig. 1（b）, Fig. 1（c）, Fig. 1（d）For the MoS of graded structure carbon intercalation2The transmission electron microscope picture of@rGO compounds；Its In, Fig. 1（c）In illustration be electron diffraction diagram；
Fig. 2 is the MoS of graded structure carbon intercalation2The Raman spectrogram of@rGO compounds.
Embodiment
The present invention further illustrates the present invention with the following example, but protection scope of the present invention is not limited to following reality Apply example.
Embodiment 1
1）The preparation method of graphene oxide is：Under ice-water bath, 2 g crystalline flake graphites and 1 g sodium nitrate are added to 60 In the ml concentrated sulfuric acids, after 10 min of stirring, 6 g potassium permanganate are slowly added to, control water temperature is no more than 5 DEG C, and potassium permanganate has been added Bi Hou；Temperature is increased to 35 DEG C, water-bath two hours is then slowly added into after 90 ml deionized waters, 10 min of stirring；Continue 280 ml deionized waters are added, the H that 30 ml mass fractions are 30 % is then added2O2, successively with the % of mass fraction 5 HCl and Dialysed after deionized water cyclic washing and obtain graphene oxide water solution in a week；
2）A kind of graded structure carbon intercalation MoS2@rGO preparation method, by the improved graphite oxide of hummers methods Alkene 10mg and Mo3O10(C2H10N2) 0.125g is scattered in deionized water, after ultrasonic 0.5 h, adds 0.375g Cys With 0.2g glucose, after hydro-thermal reaction, then through centrifuging, washing, dry, obtained product is calcined i.e. under an inert atmosphere .
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, should all belong to the covering scope of the present invention.

Claims (3)

1. a kind of graded structure carbon intercalation MoS2@rGO preparation method, it is characterised in that：By the improved oxygen of hummers methods Graphite alkene and Mo3O10( C2H10N2) be scattered in deionized water, after ultrasonic 0.5 h, Cys and glucose are added, After hydro-thermal reaction, then through centrifuging, washing, dry, obtained product is calcined under an inert atmosphere and produced；Graphene oxide, Mo3O10(C2H10N2), the mass ratio of Cys and glucose be：10mg:0.125g:0.375g:0.2g；200 DEG C of hydro-thermals React 15h.
2. graded structure carbon intercalation MoS according to claim 12@rGO preparation method, it is characterised in that：Described Inert atmosphere is：H2With Ar gaseous mixture, H2Shared volume fraction is 5%；Described calcining is 800 DEG C of calcining 2h.
3. graded structure carbon intercalation MoS according to claim 12@rGO preparation method, it is characterised in that：Aoxidize stone The preparation method of black alkene is：Under ice-water bath, 2 g crystalline flake graphites and 1 g sodium nitrate are added in the 60 ml concentrated sulfuric acids, stirred After 10 min, 6 g potassium permanganate are slowly added to, control water temperature is no more than 5 DEG C, after potassium permanganate addition is finished；Temperature is raised To 35 DEG C, water-bath two hours is then slowly added into after 90 ml deionized waters, 10 min of stirring；Continue to add 280 ml deionizations Water, then adds the H that 30 ml mass fractions are 30 %2O2, successively with the % of mass fraction 5 HCl and deionized water cyclic washing After dialyse and obtain graphene oxide in a week.
CN201610212081.0A 2016-04-07 2016-04-07 A kind of graded structure carbon intercalation MoS2@rGO preparation method Expired - Fee Related CN105836804B (en)

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CN106629851B (en) * 2016-11-04 2018-04-24 西安建筑科技大学 A kind of method that protein matter reduction prepares class graphene molybdenum disulfide
CN106564962B (en) * 2016-11-04 2018-05-18 西安建筑科技大学 A kind of method that protein matter reduction prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
CN106564953B (en) * 2016-11-04 2018-03-16 西安建筑科技大学 A kind of method that carbohydrate organic carbon reduction prepares class graphene molybdenum disulfide
CN106564963B (en) * 2016-11-04 2018-04-17 西安建筑科技大学 A kind of method that carbohydrate organic carbon reduction prepares class graphene molybdenum disulfide ferriferrous oxide composite material
CN106564952B (en) * 2016-11-04 2018-06-29 西安建筑科技大学 A kind of method that carbohydrate organic carbon reduction prepares class graphene molybdenum disulfide-graphene composite material
KR102483069B1 (en) * 2017-12-06 2022-12-29 한양대학교 산학협력단 Positive active material for lithium sulfur battery, and method of fabricating of the same

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CN102142548A (en) * 2011-02-25 2011-08-03 浙江大学 Compound nano material of graphene and MoS2 and preparation method thereof

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