CN105836804A - Preparation method of hierarchical structured carbon intercalated MoS2@rGO - Google Patents

Preparation method of hierarchical structured carbon intercalated MoS2@rGO Download PDF

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CN105836804A
CN105836804A CN201610212081.0A CN201610212081A CN105836804A CN 105836804 A CN105836804 A CN 105836804A CN 201610212081 A CN201610212081 A CN 201610212081A CN 105836804 A CN105836804 A CN 105836804A
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preparation
rgo
mos
structure carbon
graded structure
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CN105836804B (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

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

The invention belongs to the field of preparation of nanomaterials, and concretely relates to a preparation method of hierarchical structured carbon intercalated MoS2@rGO. The method comprises the following steps: dispersing improved graphene oxide and Mo3O10(C2H10N2) in deionized water through a hummers technology, carrying out ultrasonic treatment for 0.5h, adding L-cysteine and glucose, carrying out a hydrothermal reaction, centrifuging the obtained reaction product, washing the centrifuged product, drying the washed product, and calcining dried product in inert atmosphere to obtain a compound which is the carbon intercalated MoS2 nanosheets vertically growing on the surface of graphene. The preparation method has the advantages of simplicity, good repeatability, large scale production facilitation and potential application values.

Description

A kind of graded structure carbon intercalation MoS2The preparation method of@rGO
Technical field
The invention belongs to the preparation field of nano material, be specifically related to a kind of graded structure carbon intercalation MoS2The preparation method of@rGO.
Background technology
The discovery of Graphene and the immense success obtaining its research institute, excite the great interest that other stratiform two-dimension nano materials are studied by people, MoS2Being the Layered dual compound of a kind of typical graphite-like structure, layer is combined by more weak Van der Waals force with interlayer, thus is easily stripped into relatively thin nanometer sheet, is with a wide range of applications in fields such as lubrication, catalysis and energy storage and conversions.Recently, the MoS of layer structure is constructed2/ Graphene binary composite, owing to it combines MoS2, the advantage of Graphene bi-material, become recent study hotspot.It has been reported that the different method of many kinds has synthesized the MoS of a lot of different-shape structure in document2/ graphene composite material, extends its application in fields such as catalysis, energy storage.But up to the present, also it is not related to the MoS of graded structure carbon intercalation2The report of@rGO composite.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of graded structure carbon intercalation MoS2The preparation method of@rGO.The present invention has prepared the MoS of carbon intercalation2Nanometer sheet vertical-growth is at the compound of graphenic surface so that MoS2The surface-active site of nanometer sheet maximizes.
For achieving the above object, the technical scheme is that
A kind of graded structure carbon intercalation MoS2The preparation method of@rGO, the graphene oxide that hummers method is improved and Mo3O10(C2H10N2) be scattered in deionized water, after ultrasonic 0.5 h, add Cys and glucose, after hydro-thermal reaction, more by centrifugation, wash, be dried, the product obtained is calcined under an inert atmosphere and get final product.
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 reactions 15h.
Described inert atmosphere is: H2With the gaseous mixture of Ar, H2Shared volume fraction is 5%；Described calcining is 800 DEG C of calcining 2h.
The preparation method of graphene oxide is: under ice-water bath, joins in the 60 ml concentrated sulfuric acids by 2 g crystalline flake graphites and 1 g sodium nitrate, after stirring 10 min, is slowly added to 6 g potassium permanganate, controls water temperature less than 5
DEG C, after potassium permanganate adds；Temperature is increased to 35 DEG C, water-bath two hours, it is then slowly added into 90 ml deionized waters, after stirring 10 min；Continue to add 280 ml deionized waters, be subsequently adding the H that 30 ml mass fractions are 30 %2O2, a week i.e. obtain graphene oxide water solution with dialysing after the HCl of mass fraction 5 % and deionized water cyclic washing successively.
The graded structure carbon intercalation MoS that a kind of preparation method as above prepares2@rGO。
The beneficial effects of the present invention is:
1) present invention has prepared the MoS of carbon intercalation2Nanometer sheet vertical-growth is at the compound of graphenic surface so that MoS2The surface-active site of nanometer sheet maximizes；
2) preparation method of the present invention is simple, reproducible, beneficially large-scale production, has potential using value.
Accompanying drawing explanation
Fig. 1 (a) is the MoS of graded structure carbon intercalation2The scanning electron microscope (SEM) photograph of@rGO compound；
Fig. 1 (b), Fig. 1 (c), Fig. 1 (d) are the MoS of graded structure carbon intercalation2The transmission electron microscope picture of@rGO compound；Wherein, the illustration in Fig. 1 (c) is electron diffraction diagram；
Fig. 2 is the MoS of graded structure carbon intercalation2The Raman spectrogram of@rGO compound.
Detailed description of the invention
Present invention the following example further illustrates the present invention, but protection scope of the present invention is not limited to the following example.
Embodiment 1
1) preparation method of graphene oxide is: under ice-water bath, joins in the 60 ml concentrated sulfuric acids by 2 g crystalline flake graphites and 1 g sodium nitrate, after stirring 10 min, is slowly added to 6 g potassium permanganate, controls water temperature and is less than 5 DEG C, after potassium permanganate adds；Temperature is increased to 35 DEG C, water-bath two hours, it is then slowly added into 90 ml deionized waters, after stirring 10 min；Continue to add 280 ml deionized waters, be subsequently adding the H that 30 ml mass fractions are 30 %2O2, a week i.e. obtain graphene oxide water solution with dialysing after the HCl of mass fraction 5 % and deionized water cyclic washing successively；
2) a kind of graded structure carbon intercalation MoS2The preparation method of@rGO, graphene oxide 10mg and Mo that hummers method is improved3O10(C2H10N2) 0.125g is scattered in deionized water, after ultrasonic 0.5 h, adds 0.375g Cys and 0.2g glucose, after hydro-thermal reaction, more by centrifugation, wash, be dried, the product obtained is calcined under an inert atmosphere and get final product.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent and modification, all should belong to the covering scope of the present invention.

Claims (6)

1. a graded structure carbon intercalation MoS2The preparation method of@rGO, it is characterised in that: the graphene oxide that hummers method is improved and Mo3O10(C2H10N2) be scattered in deionized water, after ultrasonic 0.5 h, add Cys and glucose, after hydro-thermal reaction, more by centrifugation, wash, be dried, the product obtained is calcined under an inert atmosphere and get final product.
Graded structure carbon intercalation MoS the most according to claim 12The preparation method of@rGO, graphene oxide, Mo3O10(C2H10N2), the mass ratio of Cys and glucose be: 10mg:0.125g:0.375g:0.2g.
Graded structure carbon intercalation MoS the most according to claim 12The preparation method of@rGO, it is characterised in that: described hydro-thermal reaction is: 200 DEG C of hydro-thermal reactions 15h.
Graded structure carbon intercalation MoS the most according to claim 12The preparation method of@rGO, it is characterised in that: described inert atmosphere is: H2With the gaseous mixture of Ar, H2Shared volume fraction is 5%；Described calcining is 800 DEG C of calcining 2h.
Graded structure carbon intercalation MoS the most according to claim 12The preparation method of@rGO, it is characterised in that: the preparation method of graphene oxide is: under ice-water bath, joins in the 60 ml concentrated sulfuric acids by 2 g crystalline flake graphites and 1 g sodium nitrate, after stirring 10 min, is slowly added to 6 g potassium permanganate, controls water temperature less than 5
DEG C, after potassium permanganate adds；Temperature is increased to 35 DEG C, water-bath two hours, it is then slowly added into 90 ml deionized waters, after stirring 10 min；Continue to add 280 ml deionized waters, be subsequently adding the H that 30 ml mass fractions are 30 %2O2, a week i.e. obtain graphene oxide with dialysing after the HCl of mass fraction 5 % and deionized water cyclic washing successively.
6. the graded structure carbon intercalation MoS prepared according to the preparation method described in any one of claim 1-52@rGO。
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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CN106564963A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-ferroferric oxide composite material through reduction for organic carbon of saccharides
CN106564962A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-ferroferric oxide composite material through reduction for proteic substances
CN106564952A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-graphene composite material by reducing carbohydrate organic carbon
CN106564953A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for reducing preparation of graphene-like molybdenum disulfide through carbohydrate organic carbon
CN106629851A (en) * 2016-11-04 2017-05-10 西安建筑科技大学 Method for reducing preparation of graphene-like molybdenum disulfide from protein substance
CN111902975A (en) * 2017-12-06 2020-11-06 汉阳大学校产学协力团 Anode active material for lithium-sulfur secondary battery and method for preparing same

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WO2015021056A2 (en) * 2013-08-05 2015-02-12 Kansas State University Research Foundation ROBUST MoS2/GRAPHENE COMPOSITE ELECTRODES FOR NA+ BATTERY APPLICATIONS

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CN102142558A (en) * 2011-02-25 2011-08-03 浙江大学 Graphene/MoS2 graphene and amorphous carbon composite material and preparation method thereof
WO2015021056A2 (en) * 2013-08-05 2015-02-12 Kansas State University Research Foundation ROBUST MoS2/GRAPHENE COMPOSITE ELECTRODES FOR NA+ BATTERY APPLICATIONS

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106564963A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-ferroferric oxide composite material through reduction for organic carbon of saccharides
CN106564962A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-ferroferric oxide composite material through reduction for proteic substances
CN106564952A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for preparing graphene-like molybdenum disulfide-graphene composite material by reducing carbohydrate organic carbon
CN106564953A (en) * 2016-11-04 2017-04-19 西安建筑科技大学 Method for reducing preparation of graphene-like molybdenum disulfide through carbohydrate organic carbon
CN106629851A (en) * 2016-11-04 2017-05-10 西安建筑科技大学 Method for reducing preparation of graphene-like molybdenum disulfide from protein substance
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
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
CN111902975A (en) * 2017-12-06 2020-11-06 汉阳大学校产学协力团 Anode active material for lithium-sulfur secondary battery and method for preparing same

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