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 PDFInfo
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- 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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- molybdenum disulfide
- layered porous
- single layered
- temperature
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 46
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000010189 synthetic method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 9
- 239000005864 Sulphur Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 239000007789 gas Substances 0.000 claims 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 2
- 239000000126 substance Substances 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical group [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 abstract 1
- 238000000151 deposition Methods 0.000 abstract 1
- 238000005457 optimization Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000004062 sedimentation Methods 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 238000004506 ultrasonic cleaning Methods 0.000 abstract 1
- 238000001069 Raman spectroscopy Methods 0.000 description 6
- 239000002356 single layer Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical 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
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.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
-
2018
- 2018-05-03 CN CN201810415830.9A patent/CN108588674A/en active Pending
Cited By (6)
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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