CN108588674A - A kind of synthetic method of single layered porous molybdenum disulfide - Google Patents

A kind of synthetic method of single layered porous molybdenum disulfide Download PDF

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Publication number
CN108588674A
CN108588674A CN201810415830.9A CN201810415830A CN108588674A CN 108588674 A CN108588674 A CN 108588674A CN 201810415830 A CN201810415830 A CN 201810415830A CN 108588674 A CN108588674 A CN 108588674A
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Prior art keywords
molybdenum disulfide
layered porous
single layered
temperature
step according
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CN201810415830.9A
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程文涛
蔡金明
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Priority to CN201810415830.9A priority Critical patent/CN108588674A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/305Sulfides, selenides, or tellurides
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of synthetic methods of single layered porous molybdenum disulfide.In an inert atmosphere, using common sulphur powder and MoO3For raw material, single layered porous shape MoS is grown using the chemical vapor deposition method of single temperature zone2, aperture is nanoscale;It it is at room temperature 650 DEG C by temperature control when depositing, heating rate should not be too large, most preferably 10 DEG C/min, and sedimentation time control is 5 to 15 minutes, can complete single layered porous MoS2Preparation;Wherein by the optimization of the preparation parameters such as ultrasonic cleaning processing, sulfur family elemental powders dosage, growth temperature and growth time to substrate, realize to single layered porous MoS2Stringent control.

Description

A kind of synthetic method of single layered porous molybdenum disulfide
Technical field
The present invention relates to the fields of molybdenum disulfide material preparation, and in particular to a kind of synthesis side of single layered porous molybdenum disulfide Method.
Technical background
In the structure of every layer of molybdenum disulfide, molybdenum atom can be surrounded by six sulphur atoms, to form a triangle The structure of prism, many Mo-S faceted pebbles can be exposed outside by crossing, these faces Mo-S are analyzed in crystallography, the energy in this face Measure relatively high, surface-active is relatively high and unstable, can act as catalytic active center.Due to the hexagoinal lattice of molybdenum disulfide The structure of system is to be formed by octahedra and triangular prism structure, belongs to a kind of metastable crystal structure and molybdenum disulfide Stability at high temperature under high pressure, all so that molybdenum disulfide has a very wide range of applications in friction, lubrication, catalysis etc..
In being studied outside Current Domestic, molybdenum disulfide nano method for manufacturing thin film is gradually found, as presoma decomposes Method, lithium ion graft process, liquid phase ultrasonic method, hydro-thermal method etc..But all there is certain defects for these methods.Such as above-mentioned In method comparatively lithium ion graft process is a kind of method that efficiency is relatively high, but this preparation method is than relatively time-consuming, preparation Condition also comparatively it is harsher and it is extremely easy assemble, this is the major defect of lithium ion graft process.Hydro-thermal method can be with The preparation to the molybdenum disulfide nano film of various patterns is realized by changing experiment condition, however wants to prepare conforming layer Several molybdenum disulfide is difficult to accomplish, this is also the shared disadvantage of these methods.The molybdenum disulfide that is produced out is at present Reveal a variety of patterns, it is more a variety of than if any nano flower-like, pyramid shape and single layer monocrystal thin films etc., but single layered porous shape also not by It prepares.
Invention content
The technical problem to be solved in the present invention is to provide a kind of synthetic methods of single layered porous molybdenum disulfide, using the present invention The method of offer can obtain more uniform single layered porous shape MoS2Nano thin-film.
In order to solve the above technical problems, the present invention provides a kind of synthetic method of single layered porous molybdenum disulfide, including Following steps:
(1) dielectric base is cleaned by ultrasonic:The ultrasound 5min in acetone, absolute ethyl alcohol and deionized water successively;
(2) MoO of 20mg is weighed3Powder, as the sources S, pours into different crucibles respectively as the sulphur powder of the sources Mo and 450mg In;
(3) dielectric base after cleaning is dried up and MoO with nitrogen3Powder is placed in the same crucible, is then placed within The intermediate high-temperature region of single temperature zone CVD stoves, substrate are located at MoO3The crucible for being contained with sulphur powder is placed on the low temperature of upstream by downstream Area;
(4) under high vacuum condition, in atmosphere of inert gases, with the heating rate of the 10 DEG C/min of 50Pa by the height of CVD stoves Warm area is heated to 650 DEG C, and keeps the temperature 15min;After reaction, the lid fast cooling of CVD stoves to room temperature to get to single layer Cavernous MoS2
A kind of synthetic method of single layered porous molybdenum disulfide as the present invention:The mass ratio of molybdenum source and sulphur source most preferably 1: 25 (cannot be below 1:15).
A kind of improvement of the synthetic method of single layered porous molybdenum disulfide as the present invention:Heating rate should not super more 15 DEG C/min, most preferably 10 DEG C/min.
A kind of improvement of the synthetic method of single layered porous molybdenum disulfide as the present invention:Temperature is unsuitable excessively high, at room temperature 650 DEG C are risen to 10 DEG C/min most preferably.
Under the preferred version of the present invention, the molybdenum disulfide single layered porous shape of gained.
The present invention provides a kind of synthetic method of single layered porous molybdenum disulfide, and the method is simple and easy to do, required process conditions There is fabulous application prospect in terms of catalysis with molybdenum disulfide at low cost, prepared.
Description of the drawings
The specific implementation mode of the present invention is described in further details below in conjunction with the accompanying drawings.
Fig. 1 is atomic force microscope (AFM) figure of molybdenum disulfide prepared by embodiment 1;
Fig. 2 is Raman (Raman) the detection figure of molybdenum disulfide prepared by embodiment 1;
Fig. 3 is atomic force microscope (AFM) figure of molybdenum disulfide prepared by embodiment 2;
Fig. 4 is Raman (Raman) the detection figure of molybdenum disulfide prepared by embodiment 2;
Specific implementation mode
The present invention is further described with reference to specific embodiment, but protection scope of the present invention and is not only limited In this.
Embodiment 1, a kind of synthetic method of single layered porous molybdenum disulfide, follow the steps below successively:
(1) dielectric base is cleaned by ultrasonic:The ultrasound 5min in acetone, absolute ethyl alcohol and deionized water successively;
(2) MoO of 20mg is weighed3Powder, as the sources S, pours into different crucibles respectively as the sulphur powder of the sources Mo and 450mg In;
(3) dielectric base after cleaning is dried up and MoO with nitrogen3Powder is placed in the same crucible, is then placed within The intermediate high-temperature region of single temperature zone CVD stoves, substrate are located at MoO3The crucible for being contained with sulphur powder is placed on the low temperature of upstream by downstream Area;
(4) under high vacuum condition, in atmosphere of inert gases, with the heating rate of the 10 DEG C/min of 50Pa by the height of CVD stoves Warm area is heated to 650 DEG C, and keeps the temperature 15min;After reaction, the lid fast cooling of CVD stoves to room temperature to get to multilayer MoS2
Embodiment 2, by the substrate and MoO in the step (3) in embodiment 13It is respectively put into two two crucibles In, and crucible where substrate is located at downstream and is located next to MoO3Crucible is placed where powder, and the heating rate in step (4) makes into 15 DEG C/min, remaining is equal to example 1.
The AFM of molybdenum disulfide prepared by embodiment 1 is as shown in Figure 1:As can be seen from the figure MoS2Show porous membrane Shape, additionally as supplement, the structure under also using AFM scan porous shows smooth substrate;In conjunction with Raman detection figure (Fig. 2), it can be seen that MoS2The peak-to-peak wave-number difference △ of two features be 19.538cm-1(it is generally acknowledged that wave-number difference △≤ 20cm-1For single layer), so the MoS prepared2For the porous structure of single layer.
The AFM of comparative example 1, the molybdenum disulfide that embodiment 2 is prepared is characterized as shown in figure 3, as can be seen from the figure MoS2For porous membrane structure, in conjunction with Raman detection as shown in figure 4, being as a result shown as single layer, so prepared molybdenum disulfide is The porous structure of single layer.
Finally, it should also be noted that it is listed above be only the present invention two specific embodiments.Obviously, of the invention It is not limited to above example, acceptable there are many deformations.Those skilled in the art can be straight from present disclosure All deformations for connecing export or associating, are considered as protection scope of the present invention.

Claims (8)

1. a kind of synthetic method of single layered porous molybdenum disulfide, which is characterized in that include the following steps:
(1) dielectric base is cleaned by ultrasonic:The ultrasound 5min in acetone, absolute ethyl alcohol and deionized water successively;
(2) dielectric base after cleaning is dried up with nitrogen, is placed on the intermediate high-temperature region of single temperature zone CVD stoves, is placed in MoO3Under Sulphur simple substance, is placed on the low-temperature space of upstream by trip;
(3) under high vacuum condition, in atmosphere of inert gases, with the heating rate of the 10 DEG C/minn of 50Pa by the high-temperature region of CVD stoves 650 DEG C are heated to, and keeps the temperature 15min;After reaction, the lid fast cooling of CVD stoves to room temperature to get to single layered porous MoS2
2. a kind of synthetic method of single layered porous molybdenum disulfide according to claim 1, it is characterised in that:
The dielectric base is titanium dioxide silicon chip.
3. the method that an a kind of step according to claim 1 prepares multilayer molybdenum disulfide, it is characterised in that:
The cleaning step of the dielectric base can not omit.
4. the method that an a kind of step according to claim 1 prepares multilayer molybdenum disulfide, it is characterised in that:
The sulphur powder simple substance purity requirement is not high, purity >=99%.
5. the method that an a kind of step according to claim 1 prepares multilayer molybdenum disulfide, it is characterised in that:
The inert gas is the gas of the prices material benefits such as nitrogen, argon gas, purity >=99.9%.
6. the method that an a kind of step according to claim 1 prepares multilayer molybdenum disulfide, it is characterised in that:
The CVD stoves must can open bell, realize fast cooling.
7. the method that an a kind of step according to claim 1 prepares multilayer molybdenum disulfide, it is characterised in that:
The heating rate of high-temperature region can reach 15 DEG C/min or more.
8. the method that an a kind of step according to claim 1 prepares multilayer molybdenum disulfide, it is characterised in that:
The CVD stoves can be realized for single temperature zone.
CN201810415830.9A 2018-05-03 2018-05-03 A kind of synthetic method of single layered porous molybdenum disulfide Pending CN108588674A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357162A (en) * 2019-07-22 2019-10-22 金堆城钼业股份有限公司 A method of efficiently synthesizing high pure alcohol
CN110436525A (en) * 2019-07-22 2019-11-12 金堆城钼业股份有限公司 A kind of preparation method of micro-/ nano molybdenum disulfide
CN112978798A (en) * 2021-02-02 2021-06-18 昆明理工大学 Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size
CN113772731A (en) * 2021-08-18 2021-12-10 昆明理工大学 Method for synthesizing molybdenum disulfide in vacuum

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357162A (en) * 2019-07-22 2019-10-22 金堆城钼业股份有限公司 A method of efficiently synthesizing high pure alcohol
CN110436525A (en) * 2019-07-22 2019-11-12 金堆城钼业股份有限公司 A kind of preparation method of micro-/ nano molybdenum disulfide
CN110436525B (en) * 2019-07-22 2021-09-28 金堆城钼业股份有限公司 Preparation method of micro/nano molybdenum disulfide
CN110357162B (en) * 2019-07-22 2021-11-09 金堆城钼业股份有限公司 Method for efficiently synthesizing high-purity molybdenum disulfide
CN112978798A (en) * 2021-02-02 2021-06-18 昆明理工大学 Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size
CN113772731A (en) * 2021-08-18 2021-12-10 昆明理工大学 Method for synthesizing molybdenum disulfide in vacuum

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