CN104773720B - Method for preparing single-layer molybdenum disulfide flake doped graphene composite film - Google Patents
Method for preparing single-layer molybdenum disulfide flake doped graphene composite film Download PDFInfo
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- CN104773720B CN104773720B CN201510149438.0A CN201510149438A CN104773720B CN 104773720 B CN104773720 B CN 104773720B CN 201510149438 A CN201510149438 A CN 201510149438A CN 104773720 B CN104773720 B CN 104773720B
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Abstract
The invention relates to a method for preparing a single-layer molybdenum disulfide flake doped graphene composite film. The method comprises the following steps: preparing a uniformly dispersed single-layer molybdenum disulfide and oxidized graphene mixed dispersant, and performing suction filtering to obtain a single-layer molybdenum disulfide flake doped graphene composite film; then, reducing with hydroiodic acid to obtain the single-layer molybdenum disulfide flake doped graphene composite film; washing the reduced composite film with absolute ethyl alcohol and deionized water; and drying in vacuum to obtain the single-layer molybdenum disulfide flake doped graphene composite film. The method has the characteristics of simple process and easily industrial production, can be used for preparing single-layer molybdenum disulfide and graphene composite nano-materials in large scale, and can be applied to the fields of photocatalysis, electrocatalysis, hydrogen evolution catalysis, supercapacitors and the like.
Description
Technical field
The invention belongs to the preparation field of laminated film, particularly to the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates
Preparation method.
Background technology
Recently as the rise of the two-dimensional layer nano materials research upsurges such as Graphene, the two-dimensional layer compound that a class is novel
Class Graphene molybdenum bisuphide causes the extensive concern of the various fields research worker such as physics, chemistry, material, electronics.Class stone
The change with " sandwich " layer structure that ink alkene molybdenum bisuphide is made up of the single or multiple lift molybdenum bisuphide of hexagonal crystal system
Compound.Wherein monolayer molybdenum bisuphide is made up of three layers of atomic layer, and middle one layer is molybdenum atom layer, and upper and lower two-layer is sulphur atom layer,
Molybdenum atom layer is folded formation class " sandwich " structure by two-layer sulphur atom layer；There is strong covalent bond in Ceng, then there is weak model in interlayer
De Huali, interlamellar spacing is about 0.65nm.
Owing to monolayer molybdenum bisuphide has similar two-dimensional nano sheet pattern with Graphene, both are on microscopic appearance and crystal structure
There is good similarity.Monolayer molybdenum bisuphide and Graphene all can be applied as electrode material and catalyst.And by Graphene with
The compound electric conductivity that can improve composite of molybdenum disulfide nano sheet, strengthens in electrochemical electrode reaction and catalytic reaction process
The transmission of electronics, thus improve chemical property and the catalytic performance of composite.
But, so far, monolayer molybdenum bisuphide preparation be mainly based upon chemical gaseous phase deposition, micromechanics stripping method, this
The method of kind requires higher to experimental facilities or the response time is long, and the amount of preparation is the most little.Consider from large-scale application, research and develop one
Kind simple, be easily enlarged preparation doping monolayer molybdenum bisuphide and the method for graphene composite material be still that one challenging
Work.
Summary of the invention
The technical problem to be solved is to provide the preparation side of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates
Method, the method uses lithium ion graft process to prepare monolayer molybdenum bisuphide, and passes through the preparation difference doping that solwution method is controlled
Graphene composite film with the doping monolayer curing molybdenum sheet of different-thickness；The method preparation technology is simple, and to a great extent
Its macro morphology upper is regulatable, the nanometer different with preparing appearance structure according to different application for expanding commercial Application
Fiber mixed film tool is very helpful.
A kind of preparation method of the graphene composite film of the monolayer curing molybdenum sheet that adulterates of the present invention, including:
(1) preparation of monolayer molybdenum bisuphide dispersion liquid: with molybdenum bisuphide as raw material, by lithium ion graft process (P.Joensen, R.
F.Frindt, S.R.Morrison, Mater.Res.Bull.1986,21,457 461) prepare monolayer molybdenum bisuphide, by the list of preparation
Layer molybdenum bisuphide, is scattered in deionized water, is peeled off by water bath sonicator and cell pulverization and obtains dispersibility uniform monolayer two sulfur
Change molybdenum dispersion liquid；Wherein, monolayer molybdenum bisuphide dispersion concentration in deionized water is 0.1mg/mL～5mg/mL；
(2) preparation of graphene oxide dispersion: with graphite powder as raw material, employing Hummers method (Hummers WS,
Offeman RE.Preparation of graphite oxide.J Am Chem Soc 1958；80:1339) prepare graphite oxide, will system
The standby graphite oxide obtained, is scattered in deionized water, ultrasonic, obtains uniform graphene oxide dispersion；Wherein, oxidation
Graphene dispersion concentration in deionized water is 0.1mg/mL～10mg/mL；
(3) graphene oxide dispersion that monolayer molybdenum bisuphide dispersion liquid step (1) obtained and step (2) obtain according to
Volume ratio is 1:1～1:5 mixing, ultrasonic, it is thus achieved that the monolayer molybdenum bisuphide of mix homogeneously and graphene oxide mixed dispersion liquid, uses
Teflon membrane filter sucking filtration becomes thin film, vacuum drying, obtains the graphene composite thin film of doping monolayer curing molybdenum sheet；
(4) preparation of the graphene composite film of doping monolayer curing molybdenum sheet: doping monolayer two sulfur that step (3) is obtained
The graphene composite thin film changing molybdenum sheet is positioned in hydroiodic acid solution reduction, and the recovery time is 2～24h, takes out thin film, clearly
Wash, remove unnecessary hydroiodic acid solution, obtain the graphene composite film of doping monolayer curing molybdenum sheet.
In described step (1), lithium ion graft process is prepared the method for monolayer molybdenum bisuphide and is: by the stirring point of 300mg molybdenum bisuphide
It is scattered in the hexane solution of 3mL n-BuLi, at N2Stir 48h under the protection of atmosphere, add 5mL hexane solution dilute
Release reactant liquor, after stirring 0.5～3h, add ultrasonic stripping reaction 10～60min after deionized water, obtain monolayer molybdenum bisuphide.
In described step (1), the time of water bath sonicator is 10～60min.
The time that in described step (1), cell pulverization is peeled off is 5～30min.
In described step (2), Hummers method is prepared the process of graphite oxide and is: with potassium permanganate and concentrated sulphuric acid oxidation 200～500
Purpose graphite powder, the filter cake that sucking filtration obtains is placed at 50～80 DEG C vacuum drying 2～12h, grinds and obtains graphite oxide.
Time ultrasonic in described step (2) is 10～60min.
In described step (3), ultrasonic time is 5～30min.
In described step (3), the pore size of teflon membrane filter is 0.1 μm～5 μm.
In described step (3), vacuum drying temperature is 60～90 DEG C, and the time is 2～12h.
Cleaning in described step (4) is for repeatedly to clean with ethanol and deionized water.
By regulating monolayer molybdenum bisuphide solution concentration and graphene oxide solution concentration and controlling both solution in mixed liquor
Ratio, the pore size changing sucking filtration volume and filter membrane prepares the doping monolayer curing molybdenum sheet of different-shape and different-thickness
Graphene composite film.
The graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates prepared by the present invention, be according to graphene oxide with single point
Sub-molybdenum bisuphide the most all has preferable dispersibility, and due to two-dimensional nano sheet shape as special defects between them
Looks, both have good similarity on microscopic appearance and crystal structure.Solution mixing sucking filtration is obtained required laminated film,
The preparation of its technique is simple, and its macro morphology is regulatable, and elastic deformation can occur to a certain extent.
Beneficial effect
(1) present invention is simple to operate, and preparation process is convenient and swift；
(2) thickness of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates that the present invention prepares and volume size
Control, can occur elastic deformation to a certain extent.
Accompanying drawing explanation
Fig. 1 is the digital photograph figure of the graphene composite film of the doping monolayer curing molybdenum sheet of embodiment 1 preparation；
Fig. 2 is the digital photograph figure of the graphene composite film of the doping monolayer curing molybdenum sheet of embodiment 2 preparation；
Fig. 3 is the XRD figure spectrum of the graphene composite film of doping monolayer curing molybdenum sheet；Wherein, curve (a) is that embodiment 1 is made
The X-ray diffraction curve of the graphene composite film of standby doping monolayer curing molybdenum sheet；Curve (b) is prepared by embodiment 2
The X-ray diffraction curve of graphene composite film of doping monolayer curing molybdenum sheet；
Fig. 4 is the Raman spectrum diffraction pattern of the graphene composite film of doping monolayer curing molybdenum sheet；Wherein, curve (a) is embodiment
The graphene composite film Raman spectrum diffraction curve of the doping monolayer curing molybdenum sheet of 1 preparation；Curve (b) is that embodiment 2 is made
The Raman spectrum diffraction curve of the graphene composite film of standby doping monolayer curing molybdenum sheet；Curve (c) is prepared by embodiment 3
The Raman spectrum diffraction curve of graphene composite film of doping monolayer curing molybdenum sheet；
Fig. 5 is the scanning electron microscope (SEM) photograph of the graphene composite film of the doping monolayer curing molybdenum sheet of embodiment 2 preparation；
Fig. 6 is the HRTEM figure of the graphene composite film of the doping monolayer curing molybdenum sheet of embodiment 2 preparation.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not
For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can
To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
(1) lithium ion graft process prepares monolayer molybdenum bisuphide: under room temperature, is sufficiently stirred for being distributed to 3 by 300mg molybdenum bisuphide
In the hexane solution of mL n-BuLi, magneton stirring reaction 48h under the protection of N2 atmosphere, reaction is just adding 10mL after terminating
Hexane solution dilute reaction solution, adds ultrasonic stripping reaction after stirring 10min by 50mL deionized water after being sufficiently stirred for 2h
30min, obtains the monolayer molybdenum bisuphide peeled off by lithium ion intercalation.
(2) Hummers method is utilized to prepare graphite oxide: to aoxidize the graphite powder of 500 mesh with potassium permanganate and concentrated sulphuric acid, take out
The filter cake that filter obtains is placed at 60 DEG C vacuum drying 24h, grinds and obtains graphite oxide.
(3) the monolayer molybdenum bisuphide after at room temperature, being peeled off by 10mg is scattered in 50mL deionized water, fully
After stirring, water bath sonicator and cell disruptor ultrasonic time are respectively 30min and 10min.Weigh 10mg graphite oxide powder
Ultrasonic disperse in 100mL deionized water, ultrasonic disperse 20min.Measure the above-mentioned scattered monolayer curing of 5mL respectively
Molybdenum aqueous solution and graphene oxide water solution, ultrasonic 10min after mix homogeneously.The 10mL mixed aqueous solution of mix homogeneously is used
Pore size is that the Teflon filtration of 0.5 μm obtains sucking filtration thin film.After sucking filtration terminates, by thin film good for the sucking filtration that obtains with
Teflon membrane filter is put in 60 DEG C of vacuum drying ovens simultaneously and is dried 2h, obtains the graphene oxide of doping monolayer curing molybdenum sheet
Laminated film.Laminated film hydroiodic acid soaking and reducing, reduction 5h under room temperature, obtain the monolayer curing molybdenum sheet that adulterates after reduction
Graphene composite film.Respectively with ethanol and the graphene composite film of deionized water cyclic washing doping monolayer curing molybdenum sheet
On unnecessary hydroiodic acid solution, dry at normal temperatures, obtain adulterate monolayer curing molybdenum sheet graphene composite film.Wherein,
Fig. 1 is the digital photograph figure of the graphene composite film of the doping monolayer curing molybdenum sheet prepared；In Fig. 3 prepared by curve (a)
The X-ray diffraction curve of the graphene composite film of doping monolayer curing molybdenum sheet；In Fig. 4, curve (a) is the doping of preparation
The Raman spectrum diffraction curve of the graphene composite film of monolayer curing molybdenum sheet.
Embodiment 2
Step (1) is identical with (1) and (2) in embodiment 1 with step (2).
(3) the monolayer molybdenum bisuphide after at room temperature, being peeled off by 10mg is scattered in 100mL deionized water, fully
After stirring, water bath sonicator and cell disruptor ultrasonic time are respectively 10min and 30min.Weigh 5mg graphite oxide powder
Ultrasonic disperse in 100mL deionized water, ultrasonic disperse 20min.Measure above-mentioned scattered monolayer two sulfur of 7.5mL respectively
Change molybdenum aqueous solution and graphene oxide water solution, ultrasonic 10min after mix homogeneously.By the 15mL mixed aqueous solution of mix homogeneously
Sucking filtration thin film is obtained with the Teflon filtration that pore size is 0.6 μm.After sucking filtration terminates, by thin film good for the sucking filtration that obtains
It is put in 80 DEG C of vacuum drying ovens with teflon membrane filter simultaneously and is dried 2h, obtain the graphite oxide of doping monolayer curing molybdenum sheet
Alkene laminated film.Laminated film hydroiodic acid soaking and reducing, reduction 12h under room temperature, obtain monolayer curing of adulterating after reduction
The graphene composite film of molybdenum sheet.It is combined with the Graphene of ethanol and deionized water cyclic washing doping monolayer curing molybdenum sheet respectively
Unnecessary hydroiodic acid solution on thin film, dries at normal temperatures, obtains the graphene composite film of doping monolayer curing molybdenum sheet.Its
In, Fig. 2 is the digital photograph figure of the graphene composite film of the doping monolayer curing molybdenum sheet prepared；In Fig. 3, curve (b) is
The X-ray diffraction curve of the graphene composite film of the doping monolayer curing molybdenum sheet of preparation；In Fig. 4, curve (b) is preparation
The Raman spectrum diffraction curve of graphene composite film of doping monolayer curing molybdenum sheet；Fig. 5 is doping monolayer two sulfur prepared
Change the scanning electron microscope (SEM) photograph of the graphene composite film of molybdenum sheet；Fig. 6 is the Graphene THIN COMPOSITE of the doping monolayer curing molybdenum sheet prepared
The HRTEM figure of film.
Embodiment 3
Step (1) is identical with (1) and (2) in embodiment 1 with step (2).
(3) the monolayer molybdenum bisuphide after at room temperature, being peeled off by 5mg is scattered in 100mL deionized water, fully
After stirring, water bath sonicator and cell disruptor ultrasonic time are respectively 30min and 60min.Weigh 10mg graphite oxide powder
Ultrasonic disperse in 100mL deionized water, ultrasonic disperse 20min.Measure the above-mentioned scattered molybdenum bisuphide aqueous solution of 5mL
With 10mL graphene oxide water solution, ultrasonic 10min after mix homogeneously.By the 15mL mixed aqueous solution hole of mix homogeneously
Footpath size is that the Teflon filtration of 0.5 μm obtains sucking filtration thin film.After sucking filtration terminates, by thin film good for the sucking filtration that obtains with poly-
Tetrafluoroethene filter membrane is put in 60 DEG C of vacuum drying ovens simultaneously and is dried 2h, and the graphene oxide obtaining doping monolayer curing molybdenum sheet is multiple
Close thin film.Laminated film hydroiodic acid soaking and reducing, reduction 6h under room temperature, obtain the monolayer curing molybdenum sheet that adulterates after reduction
Graphene composite film.Respectively on the graphene composite film with ethanol and deionized water cyclic washing doping monolayer curing molybdenum sheet
Unnecessary hydroiodic acid solution, dry at normal temperatures, obtain adulterate monolayer curing molybdenum sheet graphene composite film.Wherein, figure
The Raman spectrum diffraction curve of the graphene composite film of the doping monolayer curing molybdenum sheet that in 4, curve (c) is preparation.
Claims (10)
1. adulterate the preparation method of graphene composite film of monolayer curing molybdenum sheet, including:
(1) with molybdenum bisuphide as raw material, monolayer molybdenum bisuphide is prepared by lithium ion graft process, by the monolayer molybdenum bisuphide of preparation,
It is scattered in deionized water, is peeled off by water bath sonicator and cell pulverization and obtain dispersibility uniform monolayer molybdenum bisuphide dispersion liquid；
Wherein, monolayer molybdenum bisuphide dispersion concentration in deionized water is 0.01mg/mL～1mg/mL；
(2) with graphite powder as raw material, Hummers method is used to prepare graphite oxide, the graphite oxide that will prepare, point
Dissipate in deionized water, ultrasonic, obtain uniform graphene oxide dispersion；Wherein, graphene oxide is dispersed in deionized water
In concentration be 0.01mg/mL～10mg/mL；
(3) graphene oxide dispersion that monolayer molybdenum bisuphide dispersion liquid step (1) obtained and step (2) obtain according to
Volume ratio is 1:1～1:5 mixing, ultrasonic, it is thus achieved that the monolayer molybdenum bisuphide of mix homogeneously and graphene oxide mixed dispersion liquid, uses
Teflon membrane filter sucking filtration becomes thin film, vacuum drying, obtains the graphene composite thin film of doping monolayer curing molybdenum sheet；
(4) graphene composite thin film of doping curing molybdenum sheet step (3) obtained is positioned in hydroiodic acid solution also
Former, the recovery time is 2～24h, takes out, and cleans, and obtains the graphene composite film of doping monolayer curing molybdenum sheet.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature exists
In, in described step (1), lithium ion graft process is prepared the method for monolayer molybdenum bisuphide and is: by the stirring point of 300mg molybdenum bisuphide
It is scattered in the hexane solution of 3mL n-BuLi, at N2Stir 48h under the protection of atmosphere, add 5mL hexane solution dilute
Release reactant liquor, after stirring 0.5～3h, add ultrasonic stripping reaction 10～60min after deionized water, obtain monolayer molybdenum bisuphide.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature exists
In, in described step (1), the time of water bath sonicator is 10～60min.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature exists
In, the time that in described step (1), cell pulverization is peeled off is 5～30min.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature exists
In, in described step (2), Hummers method is prepared the process of graphite oxide and is: with potassium permanganate and concentrated sulphuric acid oxidation 200～500
Purpose graphite powder, the filter cake that sucking filtration obtains is placed at 50～80 DEG C vacuum drying 2～12h, grinds and obtains graphite oxide.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature exists
In, the time ultrasonic in described step (2) is 10～60min.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature exists
In, in described step (3), ultrasonic time is 5～30min.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature exists
In, in described step (3), the pore size of teflon membrane filter is 0.1 μm～5 μm.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature exists
In, in described step (3), vacuum drying temperature is 60～90 DEG C, and the time is 2～12h.
The preparation method of the graphene composite film of a kind of monolayer curing molybdenum sheet that adulterates the most according to claim 1, its feature
Being, the cleaning in described step (4) is for repeatedly to clean with ethanol and deionized water.
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