CN104609474A - Method for preparing few-layer MoS2 nanosheets - Google Patents

Method for preparing few-layer MoS2 nanosheets Download PDF

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Publication number
CN104609474A
CN104609474A CN201510045702.6A CN201510045702A CN104609474A CN 104609474 A CN104609474 A CN 104609474A CN 201510045702 A CN201510045702 A CN 201510045702A CN 104609474 A CN104609474 A CN 104609474A
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China
Prior art keywords
mos
mos2
nanometer sheet
hours
nanosheets
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CN201510045702.6A
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Chinese (zh)
Inventor
邢秋菊
包少魁
熊华萍
占玉霞
邹建平
罗胜联
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Nanchang Hangkong University
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Nanchang Hangkong University
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Priority to CN201510045702.6A priority Critical patent/CN104609474A/en
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C01P2004/36—Spheres fragmented
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a method for preparing few-layer MoS2 nanosheets. The method comprises the following steps: preparing 100ml of 3% ethanol solution and placing the ethanol solution in 250ml of a three-mouth flask, weighing 0.1g of MoS2 powder and pouring the MoS2 powder in the mixed solution; placing the three-mouth flask in a water bath and heating to flow back, and continuously and naturally cooling the three-mouth flask to a room temperature for 2-4 hours when a temperature achieves 75-85 DEG C; centrifuging the mixed solution for 20 minutes at a certain rotational speed, taking the supernatant, carrying out suction filtration by using an organic filtration membrane, and drying for 12 hours at 60 DEG C to obtain a target product. The method disclosed by the invention has the following advantages that the problem of difficult preparation for the MoS2 nanosheets is solved, and a foundation is laid for the application expansions of the MoS2 nanosheets in other fields; the few-layer MoS2 nanosheets disclosed by the invention are prepared by using a method of mixed solvent backflow stripping, and the method disclosed by the invention is simple to operate, low in production cost, high in product purity, good in repeatability, and suitable for the requirements of expanded production.

Description

One prepares few layer of MoS 2the method of nanometer sheet
Technical field
The present invention relates to a kind of Novel liquid-phase and peel off MoS 2powder, obtains few layer of MoS 2the preparation method of nanometer sheet.
Background technology
MoS 2the class grapheme material with " sandwich " laminate structure be made up of the single or multiple lift molybdenumdisulphide of hexagonal system.Individual layer MoS 2be made up of three layers of atomic shell, middle one deck is molybdenum atom layer, and two-layer is up and down sulphur atom layer.Some individual layer MoS 2superposition constituting body phase MoS 2, there is weak Van der Waals force in interlayer.Relative to body phase MoS 2, individual layer MoS 2the avtive spot having specific surface area large, exposed is many, and changes the characteristic of direct band-gap semicondictor into, and its photoelectric characteristic is also relatively outstanding, therefore individual layer MoS 2have a wide range of applications at the opto-electronic devices such as secondary cell, field-effect transistor, sensor, organic electroluminescent, electricity storage and photocatalysis field.But individual layer MoS 2prepare relative difficulty, directly synthesis individual layer MoS 2how unformed structure is, poor stability, by body phase MoS 2individual layer or few layer MoS are prepared in stripping 2obtaining increasing concern.
Peel off body phase MoS 2method mainly contain mechanically peel method, lithium ion graft process, liquid phase ultrasonic method etc.Although the wherein MoS that obtains of mechanically peel method 2the number of plies is minimum, and stripping rate is the highest, but its output is too low, cannot scale operation.Lithium ion graft process dissection scope is wide, charge stripping efficiency is high, but its cost is also the highest, and has bibliographical information to claim the MoS of lithium ion graft process process recently 2be provided with higher toxicity, be unfavorable for environment protection, therefore liquid phase is peeled off pollution-free because of it, simple to operate, the feature that Suitable commercial is produced, and becomes one of the most promising stripping means at present.With regard to the liquid phase stripping means reported, also still Shortcomings, such as energy consumption is high, high in cost of production.
Summary of the invention
One is the object of the present invention is to provide to prepare few layer of MoS 2the method of nanometer sheet, for solving MoS 2the problem of nanometer sheet preparation difficulty, and be MoS 2nanometer sheet lays the foundation in other field broadened application.The method adopting mixed solvent backflow to peel off prepared by material of the present invention, and it is simple to operate, low production cost, product purity are high and reproducible, is applicable to the requirement that extension is produced.
The present invention is achieved like this, and one prepares few layer of MoS 2the method of nanometer sheet, is characterized in that method steps is as follows:
(1) prepare 100 ml volumes and be placed in 250 milliliters of there-necked flasks than the ethanol-water solution being 30%, take 0.1 gram of MoS 2powder drops in above-mentioned mixing solutions;
(2) again there-necked flask is placed in water-bath temperature rising reflux, after temperature reaches 75 ~ 85 DEG C, continues 2 ~ 4 hours, then naturally cool to room temperature;
(3) mixing solutions under the rotating speed of 1500 ~ 2500 revs/min centrifugal 20 minutes, gets supernatant liquid, uses the organic filter membrane of 0.22 micron pore size to carry out suction filtration, then through 60 DEG C of dryings 12 hours, obtain target product.
The present invention peels off MoS by using the backflow of alcohol-water mixing solutions 2powder, obtains few layer of MoS 2nanometer sheet, uses different ratios alcohol-water mixing solutions reflow treatment body phase MoS by contrast 2several MoS obtained 2nanometer sheet, under simulated solar irradiation, using trolamine as sacrifice reagent, photochemical catalyzing hydrogen-producing speed, the prepared MoS of assessment 2the photocatalytic activity size of nanometer sheet, result shows that gained MoS is peeled off in 30% alcohol-water mixing solutions backflow 2nanometer sheet photocatalytic activity is the strongest.And X-ray powder diffraction, scanning electron microscope, transmissioning electric mirror test result display, MoS prepared by present method 2nanometer sheet purity is higher, and size is about 500 nanometers, and thickness is about 20 nanometers.
Advantage of the present invention is: solve MoS 2the problem of nanometer sheet preparation difficulty, and be MoS 2nanometer sheet lays the foundation in other field broadened application; The method adopting mixed solvent backflow to peel off prepared by material of the present invention, and it is simple to operate, low production cost, product purity are high and reproducible, is applicable to the requirement that extension is produced.
Accompanying drawing explanation
Fig. 1 is MoS in the present invention 2powder and different ratios alcohol-water mixing solutions reflow treatment MoS 2several MoS that powder obtains 2photochemical catalyzing hydrogen-producing speed comparison diagram (the wherein bulk MoS of nanometer sheet 2for MoS 2powder, 25%, 30%, 35%, 40% represents the MoS using the process of corresponding alcohol-water mixing solutions to obtain respectively 2nanometer sheet).
Fig. 2 uses 30% ethanol-water solution backflow to peel off the MoS obtained in the inventive method 2nanometer sheet and MoS 2(a spectral line is the MoS that the inventive method obtains to the X-ray powder diffraction comparison diagram of powder 2nanometer sheet, b spectral line are MoS 2powder, JCPDS:03-065-1951 are MoS 2the standard card of crystal).
Fig. 3 be use in the inventive method volume ratio be 30% ethanol-water solution backflow peel off the MoS that obtains 2the FESEM(field emission scanning electron microscope of nanometer sheet), TEM(transmission electron microscope), HRTEM(high resolution transmission electron microscope) (wherein a, b figure is respectively MoS to photo 2the MoS that powder and the inventive method obtain 2the stereoscan photograph of nanometer sheet, c figure are the MoS that the inventive method obtains 2the transmission electron microscope photo of nanometer sheet, d figure are the MoS that the inventive method obtains 2the high resolution TEM photo of nanometer sheet).
Embodiment
Preparation method of the present invention is as follows: prepare the ethanolic soln that four parts of 100 milliliters of ratios are respectively 25%, 30%, 40%, 45% respectively and be placed in 250ml there-necked flask, take four parts of 0.1 gram of MoS 2powder drops in above-mentioned mixing solutions respectively, then there-necked flask is placed in water-bath temperature rising reflux, continues 3 hours, then naturally cool to room temperature after temperature reaches 80 DEG C.Mixing solutions is at 2000rpm(rev/min) under rotating speed centrifugal 20 minutes, get supernatant liquid, use the organic filter membrane of 0.22 micron pore size to carry out suction filtration, then through 60 DEG C of dryings 12 hours, obtain target product.
Respectively to body phase MoS 2and the ethanolic soln of 25%, 30%, 40%, 45% refluxes the MoS peeled off 2nanometer sheet sample carries out the test of photochemical catalyzing hydrogen-producing speed, concrete grammar is as follows: take 30 milligrams of samples, be placed in 80ml 10% trolamine (sacrifice agent) solution, under simulated solar rayed, detect unit hour and produce hydrogen total amount, result as shown in Figure 1, gained four parts of treated MoS 2the hydrogen-producing speed of nanometer sheet is relative to MoS 2powder is all significantly increased, and wherein gained MoS is peeled off in 30% alcohol-water mixing solutions backflow 2nanometer sheet photocatalytic activity is the strongest, and its hydrogen-producing speed reaches MoS 2more than 8 times of powder.
As shown in Figure 2, gained MoS is peeled off in 30% alcohol-water mixing solutions backflow 2nanometer sheet is through X-ray powder diffraction test spectrogram and MoS 2powder and standard card contrast show, MoS 2powder peak position after method process of the present invention does not change, and illustrates that treating processes does not cause MoS 2chemical transformation, but wherein the peak of 002 crystal face significantly improves by force, this feature and MoS 2powder is after lift-off processing, and thickness reduces, and forms result that nanometer sheet causes and matches.Ultimate analysis also shows this few layer MoS 2nanometer sheet is only containing Mo and S two kinds of elements, and its ratio is also 2:1.
As shown in Figure 3, by contrast a, b two figure, can find out after backflow lift-off processing, MoS 2the size of nanoscale twins is in 500 nanometer to 2 micrometer ranges.As can be seen from c figure, MoS 2the size of nanometer sheet is 500 ran, and thickness is less.As can be seen from d figure, 3.01 nanometers and 2.94 nanometers are all 5 layers of lattice fringes, the spacing of individual layer lattice fringe and MoS 2crystal 002 crystal face thickness 0.61 nanometer is close, and 2.51 nanometers are 10 layers of lattice fringe, the spacing of its individual layer lattice fringe and MoS 2crystal 102 crystal face thickness 0.25 nanometer is close, and the thickness that picture shows this nanometer sheet is about 20 nanometers.

Claims (1)

1. prepare few layer of MoS for one kind 2the method of nanometer sheet, is characterized in that method steps is as follows:
(1) prepare 100 ml volumes and be placed in 250 milliliters of there-necked flasks than the ethanol-water solution being 30%, take 0.1 gram of MoS 2powder drops in above-mentioned mixing solutions;
(2) again there-necked flask is placed in water-bath temperature rising reflux, after temperature reaches 75 ~ 85 DEG C, continues 2 ~ 4 hours, then naturally cool to room temperature;
(3) mixing solutions under the rotating speed of 1500 ~ 2500 revs/min centrifugal 20 minutes, gets supernatant liquid, uses the organic filter membrane of 0.22 micron pore size to carry out suction filtration, then through 60 DEG C of dryings 12 hours, obtain target product.
CN201510045702.6A 2015-01-29 2015-01-29 Method for preparing few-layer MoS2 nanosheets Pending CN104609474A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105551909A (en) * 2015-12-23 2016-05-04 深圳先进技术研究院 Field emission cathode and preparation method and application thereof
CN106064833A (en) * 2016-05-26 2016-11-02 金堆城钼业股份有限公司 One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet
CN106925301A (en) * 2017-02-28 2017-07-07 杭州电子科技大学 A kind of base metal base two dimension MoS2/ Graphene water reducing catalyst with and its preparation method and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周凯歌: "新型有机分子器件与二维纳米材料的设计、合成和表征", 《中国博士学位论文全文数据库 工程科技I辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105551909A (en) * 2015-12-23 2016-05-04 深圳先进技术研究院 Field emission cathode and preparation method and application thereof
CN106064833A (en) * 2016-05-26 2016-11-02 金堆城钼业股份有限公司 One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet
CN106925301A (en) * 2017-02-28 2017-07-07 杭州电子科技大学 A kind of base metal base two dimension MoS2/ Graphene water reducing catalyst with and its preparation method and application

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Application publication date: 20150513