CN104773720A - 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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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 a kind of preparation method of graphene composite film of the individual layer curing molybdenum sheet that adulterates.
Background technology
In recent years along with 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 molybdenumdisulphide causes the extensive concern of the various fields researchists such as physics, chemistry, material, electronics.The compound with " sandwich " laminate structure that class Graphene molybdenumdisulphide is made up of the single or multiple lift molybdenumdisulphide of hexagonal system.Wherein individual layer molybdenumdisulphide is made up of three layers of atomic shell, and middle one deck is molybdenum atom layer, is two-layerly up and down sulphur atom layer, and molybdenum atom layer is folded by two-layer sulphur atom layer and forms class " sandwich " structure; There is strong covalent bond in layer, then there is weak Van der Waals force in interlayer, interlamellar spacing is about 0.65nm.
Because individual layer molybdenumdisulphide and Graphene have similar two-dimensional nano sheet pattern, both have good similarity on microscopic appearance and crystalline structure.Individual layer molybdenumdisulphide and Graphene all can be used as electrode materials and catalyst application.And the compound of Graphene and molybdenum disulfide nano sheet can be improved the conductivity of matrix material, strengthen the transmission of electronics in electrochemical electrode reaction and catalytic reaction process, thus the chemical property of raising matrix material and catalytic performance.
But, so far, individual layer molybdenumdisulphide preparation mainly based on chemical vapour deposition, micromechanics stripping method, this method requires higher or the reaction times is long to experimental installation, and the amount of preparation is also little.Consider from large-scale application, research and develop a kind of simple, to be easy to expand method prepare adulterate individual layer molybdenumdisulphide and graphene composite material be still a challenging job.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of graphene composite film of the individual layer curing molybdenum sheet that adulterates, the method adopts lithium ion graft process to prepare unimolecular layer molybdenumdisulphide, and passes through the graphene composite film of the doping individual layer curing molybdenum sheet of the different doping of the controlled preparation of solution method and different thickness; The method preparation technology is simple, and its macro morphology is regulatable to a great extent, is very helpful for the nanofiber mixed film tool expanding industrial application different with preparing appearance structure according to different application.
The preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates of the present invention, comprising:
(1) preparation of individual layer molybdenumdisulphide dispersion liquid: take molybdenumdisulphide as raw material, by lithium ion graft process (P.Joensen, R.F.Frindt, S.R.Morrison, Mater.Res.Bull.1986,21,457 – 461) prepare individual layer molybdenumdisulphide, by the individual layer molybdenumdisulphide of preparation, be scattered in deionized water, peeled off by water bath sonicator and cell pulverization and obtain dispersed uniform individual layer molybdenumdisulphide dispersion liquid; Wherein, individual layer molybdenumdisulphide dispersion concentration is in deionized water 0.1mg/mL ~ 5mg/mL;
(2) preparation of graphene oxide dispersion: take Graphite Powder 99 as raw material, adopts Hummers method (Hummers WS, Offeman RE.Preparation of graphite oxide.J Am Chem Soc 1958; 80:1339) prepare graphite oxide, by the graphite oxide prepared, be scattered in deionized water, ultrasonic, obtain uniform graphene oxide dispersion; Wherein, graphene oxide dispersion concentration is in deionized water 0.1mg/mL ~ 10mg/mL;
(3) graphene oxide dispersion that individual layer molybdenumdisulphide dispersion liquid step (1) obtained and step (2) obtain is 1:1 ~ 1:5 mixing according to volume ratio, ultrasonic, obtain the individual layer molybdenumdisulphide and graphene oxide mixed dispersion liquid that mix, film is become with teflon membrane filter suction filtration, vacuum-drying, obtains the graphene composite thin film of doping individual layer curing molybdenum sheet;
(4) preparation of the graphene composite film of doping individual layer curing molybdenum sheet: the graphene composite thin film of doping individual layer curing molybdenum sheet step (3) obtained is positioned in hydroiodic acid HI solution and reduces, recovery time is 2 ~ 24h, take out film, cleaning, remove unnecessary hydroiodic acid HI solution, obtain the graphene composite film of doping individual layer curing molybdenum sheet.
The method that the middle lithium ion graft process of described step (1) prepares individual layer molybdenumdisulphide is: by 300mg molybdenumdisulphide dispersed with stirring in the hexane solution of 3mL n-Butyl Lithium, at N
2stir 48h under the protection of atmosphere, add 5mL hexane solution dilute reaction solution, after stirring 0.5 ~ 3h, after adding deionized water, ultrasonic stripping reaction 10 ~ 60min, obtains individual layer molybdenumdisulphide.
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.
The process that the middle Hummers method of described step (2) prepares graphite oxide is: with potassium permanganate and vitriol oil oxidation 200 ~ 500 object Graphite Powder 99s, vacuum-drying 2 ~ 12h at the filter cake that suction filtration obtains is placed in 50 ~ 80 DEG C, grinding 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 individual layer molybdenumdisulphide strength of solution and graphene oxide solution concentration and controlling the ratio of these two kinds of solution in mixed solution, the pore size changing suction filtration volume and filter membrane prepares the graphene composite film of the doping individual layer curing molybdenum sheet of different-shape and different thickness.
The graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates prepared by the present invention, in deionized water all there is good dispersiveness according to graphene oxide and unit molecule molybdenumdisulphide, and due to two-dimensional nano sheet pattern like special defects between them, both have good similarity on microscopic appearance and crystalline structure.Solution mixing suction filtration is obtained required laminated film, and the preparation of its technique is simple, and its macro morphology is regulatable, to a certain extent elastic deformation can occur.
beneficial effect
(1) the present invention is simple to operate, and preparation process is convenient and swift;
(2) a kind of thickness of graphene composite film of the individual layer curing molybdenum sheet that adulterates for preparing of the present invention and volume size all controlled, elastic deformation can be there is to a certain extent.
Accompanying drawing explanation
Fig. 1 is the digital photograph figure of the graphene composite film of doping individual layer curing molybdenum sheet prepared by embodiment 1;
Fig. 2 is the digital photograph figure of the graphene composite film of doping individual layer curing molybdenum sheet prepared by embodiment 2;
Fig. 3 is the XRD figure spectrum of the graphene composite film of doping individual layer curing molybdenum sheet; Wherein, the X-ray diffraction curve of the graphene composite film of doping individual layer curing molybdenum sheet prepared for embodiment 1 of curve (a); The X-ray diffraction curve of the graphene composite film of the doping individual layer curing molybdenum sheet that curve (b) is prepared for embodiment 2;
Fig. 4 is the Raman spectrum diffractogram of the graphene composite film of doping individual layer curing molybdenum sheet; Wherein, the graphene composite film Raman spectrum diffraction curve of doping individual layer curing molybdenum sheet prepared for embodiment 1 of curve (a); The Raman spectrum diffraction curve of the graphene composite film of the doping individual layer curing molybdenum sheet that curve (b) is prepared for embodiment 2; The Raman spectrum diffraction curve of the graphene composite film of the doping individual layer curing molybdenum sheet that curve (c) is prepared for embodiment 3;
Fig. 5 is the scanning electron microscope (SEM) photograph of the graphene composite film of doping individual layer curing molybdenum sheet prepared by embodiment 2;
Fig. 6 is the HRTEM figure of the graphene composite film of doping individual layer curing molybdenum sheet prepared by embodiment 2.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) lithium ion graft process prepares individual layer molybdenumdisulphide: under normal temperature; by abundant for 300mg molybdenumdisulphide dispersed with stirring in the hexane solution of 3mL n-Butyl Lithium; magneton stirring reaction 48h under the protection of N2 atmosphere; 10mL hexane solution dilute reaction solution is added after reaction terminates; after abundant stirring 2h, 50mL deionized water is added and stir ultrasonic stripping reaction 30min after 10min, obtain the unimolecular layer molybdenumdisulphide peeled off by lithium ion intercalation.
(2) utilize Hummers method to prepare graphite oxide: to be oxidized 500 object Graphite Powder 99s with potassium permanganate and the vitriol oil, vacuum-drying 24h at the filter cake that suction filtration obtains is placed in 60 DEG C, grinding obtains graphite oxide.
(3) at room temperature, the unimolecular layer molybdenumdisulphide after being peeled off by 10mg is scattered in 50mL deionized water, and after fully stirring, water bath sonicator and cell disruptor ultrasonic time are respectively 30min and 10min.Taking 10mg graphite oxide powder ultrasonic is dispersed in 100mL deionized water, ultrasonic disperse 20min.Measure the above-mentioned scattered individual layer molybdenumdisulphide aqueous solution of 5mL and graphene oxide water solution respectively, mix rear ultrasonic 10min.The Teflon filtration being 0.5 μm by the 10mL mixed aqueous solution pore size mixed obtains suction filtration film.After suction filtration terminates, the film good by the suction filtration obtained and teflon membrane filter are put in dry 2h in 60 DEG C of vacuum drying ovens simultaneously, obtain the graphene composite thin film of doping individual layer curing molybdenum sheet.Laminated film hydroiodic acid HI soaking and reducing, reduces 5h under normal temperature, the graphene composite film of the individual layer curing molybdenum sheet that obtains after reduction adulterating.Respectively with the unnecessary hydroiodic acid HI solution that ethanol and deionized water repetitive scrubbing adulterate on the graphene composite film of individual layer curing molybdenum sheet, dry at normal temperatures, obtain the graphene composite film of doping individual layer curing molybdenum sheet.Wherein, Fig. 1 is the digital photograph figure of the graphene composite film of the doping individual layer curing molybdenum sheet of preparation; The X-ray diffraction curve of the graphene composite film of doping individual layer curing molybdenum sheet prepared by curve (a) in Fig. 3; In Fig. 4, curve (a) is the Raman spectrum diffraction curve of the graphene composite film of the doping individual layer curing molybdenum sheet of preparation.
Embodiment 2
Step (1) is identical with (2) with (1) in embodiment 1 with step (2).
(3) at room temperature, the unimolecular layer molybdenumdisulphide after being peeled off by 10mg is scattered in 100mL deionized water, and after fully stirring, water bath sonicator and cell disruptor ultrasonic time are respectively 10min and 30min.Taking 5mg graphite oxide powder ultrasonic is dispersed in 100mL deionized water, ultrasonic disperse 20min.Measure the above-mentioned scattered individual layer molybdenumdisulphide aqueous solution of 7.5mL and graphene oxide water solution respectively, mix rear ultrasonic 10min.The Teflon filtration being 0.6 μm by the 15mL mixed aqueous solution pore size mixed obtains suction filtration film.After suction filtration terminates, the film good by the suction filtration obtained and teflon membrane filter are put in dry 2h in 80 DEG C of vacuum drying ovens simultaneously, obtain the graphene composite thin film of doping individual layer curing molybdenum sheet.Laminated film hydroiodic acid HI soaking and reducing, reduces 12h under normal temperature, the graphene composite film of the individual layer curing molybdenum sheet that obtains after reduction adulterating.Respectively with the unnecessary hydroiodic acid HI solution that ethanol and deionized water repetitive scrubbing adulterate on the graphene composite film of individual layer curing molybdenum sheet, dry at normal temperatures, obtain the graphene composite film of doping individual layer curing molybdenum sheet.Wherein, Fig. 2 is the digital photograph figure of the graphene composite film of the doping individual layer curing molybdenum sheet of preparation; In Fig. 3, curve (b) is the X-ray diffraction curve of the graphene composite film of the doping individual layer curing molybdenum sheet of preparation; In Fig. 4, curve (b) is the Raman spectrum diffraction curve of the graphene composite film of the doping individual layer curing molybdenum sheet of preparation; Fig. 5 is the scanning electron microscope (SEM) photograph of the graphene composite film of the doping individual layer curing molybdenum sheet of preparation; Fig. 6 is the HRTEM figure of the graphene composite film of the doping individual layer curing molybdenum sheet of preparation.
Embodiment 3
Step (1) is identical with (2) with (1) in embodiment 1 with step (2).
(3) at room temperature, the unimolecular layer molybdenumdisulphide after being peeled off by 5mg is scattered in 100mL deionized water, and after fully stirring, water bath sonicator and cell disruptor ultrasonic time are respectively 30min and 60min.Taking 10mg graphite oxide powder ultrasonic is dispersed in 100mL deionized water, ultrasonic disperse 20min.Measure the above-mentioned scattered molybdenumdisulphide aqueous solution of 5mL and 10mL graphene oxide water solution, mix rear ultrasonic 10min.The Teflon filtration being 0.5 μm by the 15mL mixed aqueous solution pore size mixed obtains suction filtration film.After suction filtration terminates, the film good by the suction filtration obtained and teflon membrane filter are put in dry 2h in 60 DEG C of vacuum drying ovens simultaneously, obtain the graphene composite thin film of doping individual layer curing molybdenum sheet.Laminated film hydroiodic acid HI soaking and reducing, reduces 6h under normal temperature, the graphene composite film of the individual layer curing molybdenum sheet that obtains after reduction adulterating.Respectively with the unnecessary hydroiodic acid HI solution that ethanol and deionized water repetitive scrubbing adulterate on the graphene composite film of individual layer curing molybdenum sheet, dry at normal temperatures, obtain the graphene composite film of doping individual layer curing molybdenum sheet.Wherein, in Fig. 4, curve (c) is the Raman spectrum diffraction curve of the graphene composite film of the doping individual layer curing molybdenum sheet of preparation.
Claims (10)
1. adulterate the preparation method of graphene composite film of individual layer curing molybdenum sheet, comprising:
(1) take molybdenumdisulphide as raw material, prepare individual layer molybdenumdisulphide by lithium ion graft process, by the individual layer molybdenumdisulphide of preparation, be scattered in deionized water, peeled off by water bath sonicator and cell pulverization and obtain dispersed uniform individual layer molybdenumdisulphide dispersion liquid; Wherein, individual layer molybdenumdisulphide dispersion concentration is in deionized water 0.01mg/mL ~ 1mg/mL;
(2) take Graphite Powder 99 as raw material, adopt Hummers method to prepare graphite oxide, by the graphite oxide prepared, be scattered in deionized water, ultrasonic, obtain uniform graphene oxide dispersion; Wherein, graphene oxide dispersion concentration is in deionized water 0.01mg/mL ~ 10mg/mL;
(3) graphene oxide dispersion that individual layer molybdenumdisulphide dispersion liquid step (1) obtained and step (2) obtain is 1:1 ~ 1:5 mixing according to volume ratio, ultrasonic, obtain the individual layer molybdenumdisulphide and graphene oxide mixed dispersion liquid that mix, film is become with teflon membrane filter suction filtration, vacuum-drying, obtains the graphene composite thin film of doping individual layer curing molybdenum sheet;
(4) graphene composite thin film of doping curing molybdenum sheet step (3) obtained is positioned in hydroiodic acid HI solution and reduces, and the recovery time is 2 ~ 24h, takes out, cleaning, obtains the graphene composite film of doping individual layer curing molybdenum sheet.
2. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, it is characterized in that, the method that the middle lithium ion graft process of described step (1) prepares individual layer molybdenumdisulphide is: by 300mg molybdenumdisulphide dispersed with stirring in the hexane solution of 3mL n-Butyl Lithium, at N
2stir 48h under the protection of atmosphere, add 5mL hexane solution dilute reaction solution, after stirring 0.5 ~ 3h, after adding deionized water, ultrasonic stripping reaction 10 ~ 60min, obtains individual layer molybdenumdisulphide.
3. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, is characterized in that, in described step (1), the time of water bath sonicator is 10 ~ 60min.
4. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, is characterized in that, the time that in described step (1), cell pulverization is peeled off is 5 ~ 30min.
5. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, it is characterized in that, the process that the middle Hummers method of described step (2) prepares graphite oxide is: with potassium permanganate and vitriol oil oxidation 200 ~ 500 object Graphite Powder 99s, vacuum-drying 2 ~ 12h at the filter cake that suction filtration obtains is placed in 50 ~ 80 DEG C, grinding obtains graphite oxide.
6. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, it is characterized in that, the time ultrasonic in described step (2) is 10 ~ 60min.
7. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, is characterized in that, in described step (3), ultrasonic time is 5 ~ 30min.
8. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, is characterized in that, in described step (3), the pore size of teflon membrane filter is 0.1 μm ~ 5 μm.
9. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, it is characterized in that, in described step (3), vacuum drying temperature is 60 ~ 90 DEG C, and the time is 2 ~ 12h.
10. the preparation method of the graphene composite film of a kind of individual layer curing molybdenum sheet that adulterates according to claim 1, it is characterized in that, the cleaning in described step (4) is for repeatedly to clean with ethanol and deionized water.
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| CN112875754A (en) * | 2021-01-19 | 2021-06-01 | 北京科技大学 | Preparation and application method of graphene intercalation molybdenum disulfide composite material |
| CN112960671A (en) * | 2021-02-03 | 2021-06-15 | 西北工业大学 | Graphene oxide/molybdenum disulfide composite thin film device, preparation method and application |
| CN113351230A (en) * | 2021-06-21 | 2021-09-07 | 华侨大学 | Isolated cobalt atom doped single-layer or few-layer MoS2Process for preparing catalyst |
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