CN107651708A - A kind of method that microwave hydrothermal prepares 1T@2H MoS2 - Google Patents
A kind of method that microwave hydrothermal prepares 1T@2H MoS2 Download PDFInfo
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- CN107651708A CN107651708A CN201710856860.9A CN201710856860A CN107651708A CN 107651708 A CN107651708 A CN 107651708A CN 201710856860 A CN201710856860 A CN 201710856860A CN 107651708 A CN107651708 A CN 107651708A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C—CHEMISTRY; METALLURGY
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
Abstract
The present invention discloses a kind of microwave hydrothermal and prepares 1T@2H MoS2Method, the preparation method includes, first using deionized water as solvent, ammonium heptamolybdate, thiocarbamide are stirred into 30 min, 200 DEG C of 10 min of reaction of regulation temperature, secondly using alcohol as solvent, the product that the first step obtains is reacted into 4~10 min in 220 DEG C, that is, obtains 1T 2H MoS2Nanosphere.The inventive method uses microwave hydrothermal instrument, simple to operate, safely and fast, reproducible, low cost, and gained sample topography uniformly and has two kinds of phase structures of 1T and 2H.
Description
Technical field
The invention belongs to Nano semiconductor phase in version field, and in particular to microwave hydrothermal prepares 1T@2H-MoS2Method.
Background technology
At present, MoS2Because its unique photoelectric property is widely used to include catalysis, photoelectronics, spinning electron
The field such as, biological and chemical sensor, electric capacity, solar cell.MoS2Crystal structure mainly has two kinds of 1T and 2H.2H phases are
Rock-steady structure has semiconductor property, and its band gap is 1.2~1.9 eV.1T phases are that metastable structure has metalline, conductive
Property good and electron concentration it is high.In photocatalytic applications, the low energy gap width of 2H phases can be used as sensitising agent, and the metalline of 1T phases can
As co-catalyst.The combination of two-phase（1T@2H-MoS2）And then there are greater advantages applied to photocatalysis.First, made using 2H
For sensitising agent, visible ray more in sunshine is absorbed；Second, it is used as co-catalyst by the use of 1T phases, there is provided more polyelectron is joined
With redox reaction；The combination of 3rd, 2H phase and 1T phases can form cooperative effect, and it is compound simultaneously effectively to suppress electron hole pair
Accelerate electronics transfer, lift photocatalysis effect.Therefore, the MoS of two-phase coexistent is prepared2（1T@2H-MoS2）Will in photocatalysis
With huge applications potentiality.
In recent years, microwave as it is a kind of clean, efficiently, green new method by extensive concern.Compared to conventional hydrothermal method,
Microwave can the very fast time with it is relatively low under the conditions of prepare other method and be difficult to the material prepared and thing phase, have obvious excellent
Gesture：（1）With other molecular collisions of surrounding while polar molecule in microwave absorbs microwave energy, energy is transmitted to other points
Son, while excite molecule to rotate, chemical bond rupture can be contributed.（2）, can be to material using the ionic conduction characteristic of microwave
Inside and outside to heat simultaneously, reaction rate can improve several times, tens times even thousands of times.(3) instantaneity of microwave heating：As long as deposit
In microwave radiation, heated material is instantly available heating, and microwave procedure terminates, and stops heating immediately, avoids in building-up process
The misgrowth of material grains.In summary, microwave-hydrothermal method in a short period of time, can be synthesized more under stationary temperature
Purity height, good dispersion, the nano material of size uniformity, it is expected to turn into the extensive conventional method for preparing two-dimensional material.
Existing numerous preparation 1T, 2H and 1T@2H-MoS at present2Method, common preparation method has：1 chemical stripping method；
2 hydro-thermal methods；3 chemical vapour deposition techniques；4 ball-milling methods.
Now preparation method is summarized as follows：
1. chemical stripping method：Goki Eda et al. [1] are soaked with n-BuLi, ultrasound peels off MoS21T@2H- are made in crystal
MoS2.Mark A. Lukowski et al. [2] pass through lithium intercalation 2H-MoS2It is grown directly upon on graphene and forms 1T-MoS2;Qun
Xu et al. [3] is by MoS2The h of ultra sonic bath 6 in the solvent of ethanol/water mixture is scattered in, is transferred to supercritical CO afterwards2In device,
353.2 K reactions, 6 h, which are heated to, with autoclave obtains 1T@2H-MoS2;
2. hydro-thermal method：Qin Li [4] et al. synthesize 1T-MoS using ammonium heptamolybdate, thiocarbamide in 200 DEG C of 20 h2；Jie Li etc.
[5] with ammonium heptamolybdate, thiocarbamide in 200 DEG C of 24 h synthesis stratiforms 1T-MoS2Nanometer sheet；Yong Liu et al. [6] are by three block
Copolymer is added in graphite ammonia water and obtains uniform solution, secondly adds ammonium molybdate and thiocarbamide, continues after stirring 1 h, turns
Enter in stainless steel autoclave, 230 DEG C of 24 h of heating obtains the 2H/1TMoS of graphene parcel2Structure.
3. chemical vapour deposition technique：Manish Chhowalla et al. [7] obtain individual layer by chemical vapour deposition technique
MoS2, the 2H-MoS for having 1T associated is obtained using beamwriter lithography and electron beam evaporation afterwards2Electrochemistry electrochemistry micro electric
Pond.
4. ball-milling method：Peifu Cheng et al. [8] pass through ball milling MoS21T@2H-MoS are made in powder2；
5. other method：0.5 m mol Li of Hong Du et al. [9]2CO3With 0.5 m mol MoS2Nanometer sheet is ground in agate
After alms bowl is ground 15 minutes, 700 °C of 4 h of heating has obtained 1T-Li in nitrogen atmospherexMoS2Nanometer sheet.
From above-mentioned report, existing preparation 1T@2H-MoS2Method：Complex operation, sample preparation duration, Part Methods need
Carrier gas is wanted, condition is whard to control and potential safety hazard be present.For the above method, microwave-hydrothermal method is simple to operate, sample preparation is fast
Speed, without carrier gas, low cost, pollution-free, be a kind of novel method beneficial to industrialized production.
The content of the invention
It is an object of the invention to provide be that a kind of microwave hydrothermal prepares 1T@2H-MoS2Method.
Microwave-hydrothermal method advantage：
1. microwave directly heats internal and rapid temperature rise and drop process, the sample preparation time shortens 10 times；
2. reaction temperature is low, mild condition, without carrier gas；
3. kinds of experiments factor can be adjusted by program, it is simple to operate；
4. safety pre-warning system, program terminates automatically；
5. sample preparation is installed, scientific and precise；
6. the dispersiveness of product is preferably, crystallinity is high.
The present invention is realized by following technical process：
In microwave hydrothermal reaction, first using deionized water as solvent, ammonium heptamolybdate, thiocarbamide are stirred into 30 min, regulation temperature
200 DEG C of 10 min of reaction of degree, secondly using alcohol as solvent, the product that the first step obtains is reacted into 4~10 min in 220 DEG C,
Deposit is collected after EP (end of program), CS is used after centrifugation2Sample is filtrated to get, it is repeatedly clear with absolute ethyl alcohol and deionized water afterwards
Wash, obtained product 60 DEG C of h of freeze-day with constant temperature 6 in vacuum drying chamber, finally obtain sample.
It is safely and fast, easy to spread meanwhile the inventive method is simple to operate, it is suitable for large-scale industrial production.
Brief description of the drawings
Fig. 1 is the XRD of embodiment 1；
Fig. 2 is that the SEM of embodiment 1 schemes；
Fig. 3 is that the TEM of embodiment 2 schemes；
Fig. 4 is that the HRTEM of embodiment 2 schemes；
Fig. 5 is the XRD spectra of sample.
Embodiment
The present invention is described in further details below in conjunction with drawings and examples.
Embodiment 1
1m mol ammonium heptamolybdates and 15 m mol thiocarbamides are dissolved in 35 ml distilled water, at room temperature continuing magnetic force stirring 30
Min, uniform solution is formed, is transferred the solution into polytetrafluoroethyllining lining microwave apparatus, and microwave procedure is arranged to 200
DEG C 10 min, room temperature is cooled to after EP (end of program).By being collected by centrifugation to obtain the step sample of microwave one（It is designated as M1）.Second will
M1 samples are dissolved in 25 ml alcohol and are transferred in teflon lined microwave apparatus, and now program setting is 220 DEG C
4 min, room temperature is cooled to after EP (end of program).By the way that the product of collection is dissolved into 20 min of ultrasound in ethanol and 60 after centrifugation
It is dried in vacuo at DEG C, obtains 1T@2H-MoS2.（It is designated as M-1T@2H-MoS2）.As shown in figure 1, the XRD for products therefrom.Phase
Than in 2H-MoS2, 1T@2H-MoS2In (002)（004）There is new diffraction maximum in position, shows that interlamellar spacing expands, two-phase coexistent shape
Into；As shown in Fig. 2 scheme for the SEM of products therefrom.
Embodiment 2
1m mol ammonium heptamolybdates and 15 m mol thiocarbamides are dissolved in 35 ml distilled water, at room temperature continuing magnetic force stirring 30
Min, uniform solution is formed, is transferred the solution into polytetrafluoroethyllining lining microwave apparatus, and microwave procedure is arranged to 200
DEG C 10 min, room temperature is cooled to after EP (end of program).By being collected by centrifugation to obtain the step sample of microwave one（It is designated as M1）.Second will
M1 samples are dissolved in 25 ml alcohol and are transferred in teflon lined microwave apparatus, and now program setting is 220 DEG C
6 min, room temperature is cooled to after EP (end of program).By the way that the product of collection is dissolved into 20 min of ultrasound in ethanol and 60 after centrifugation
It is dried in vacuo at DEG C, obtains 1T@2H-MoS2.（It is designated as M-1T@2H-MoS2）.As shown in Figure 3；Scheme for the TEM of products therefrom, card
Bright prepared MoS2For solid nanospheres；As shown in Figure 4；Scheme for the HRTEM of products therefrom, it can be clearly seen that two kinds of not isomorphous
Lattice.
Embodiment 3
1m mol ammonium heptamolybdates and 15 m mol thiocarbamides are dissolved in 35 ml distilled water, at room temperature continuing magnetic force stirring 30
Min, uniform solution is formed, is transferred the solution into polytetrafluoroethyllining lining microwave apparatus, and microwave procedure is arranged to 200
DEG C 10 min, room temperature is cooled to after EP (end of program).By being collected by centrifugation to obtain the step sample of microwave one（It is designated as M1）.Second will
M1 samples are dissolved in 25 ml alcohol and are transferred in teflon lined microwave apparatus, and now program setting is 220 DEG C
8 min, room temperature is cooled to after EP (end of program).By the way that the product of collection is dissolved into 20 min of ultrasound in ethanol and 60 after centrifugation
It is dried in vacuo at DEG C, obtains 1T@2H-MoS2.（It is designated as M-1T@2H-MoS2）.
Embodiment 4
1m mol ammonium heptamolybdates and 15 m mol thiocarbamides are dissolved in 35 ml distilled water, at room temperature continuing magnetic force stirring 30
Min, uniform solution is formed, is transferred the solution into polytetrafluoroethyllining lining microwave apparatus, and microwave procedure is arranged to 200
DEG C 10 min, room temperature is cooled to after EP (end of program).By being collected by centrifugation to obtain the step sample of microwave one（It is designated as M1）.Second will
M1 samples are dissolved in 25 ml alcohol and are transferred in teflon lined microwave apparatus, and now program setting is 220 DEG C
10 min, room temperature is cooled to after EP (end of program).By after centrifugation by the dissolving of the product of collection in ethanol 20 min of ultrasound and
It is dried in vacuo at 60 DEG C, obtains 1T@2H-MoS2.（It is designated as M-1T@2H-MoS2）.As shown in figure 5, it is the sample of embodiment 2-4
The XRD of product, its diffraction maximum is in (002)（004）There is new peak in position, shows that interlamellar spacing expands, two-phase coexistent is formed.
Bibliography
[1]Eda G, Yamaguchi H, Voiry D, Fujita T, Chen MChhowalla M,
Photoluminescence from chemically exfoliated MoS2. J.Nano Letters 2011;11
(12):5111.
[2]Lukowski M A, Daniel A S, Meng F, Forticaux A, Li LJin S, Enhanced
Hydrogen Evolution Catalysis from Chemically Exfoliated Metallic MoS2
Nanosheets. J.Journal of the American Chemical Society 2013;135(28):10274-7.
[3]Qi Y, Xu Q, Wang Y, Yan B, Ren YChen Z, CO2-Induced Phase Engineering:
Protocol for Enhanced Photoelectrocatalytic Performance of 2D MoS2
Nanosheets. J.ACS nano 2016;10(2):2903.
[4]Liu Q, Shang Q, Khalil A, Fang Q, Chen S, He Q, Xiang T, Liu D, Zhang
QLuo Y, In situ Integration of a Metallic 1T‐MoS2/CdS Heterostructure as a
means To Promote Visible‐Light‐Driven Photocatalytic Hydrogen Evolution.
J.Chemcatchem2016;8(16):2614-2619.
[5]Li J, Zhan G, Yu YZhang L, Superior visible light hydrogen evolution
of Janus bilayer junctions via atomic-level charge flow steering. J.Nature Communications 2016;7(11480).
[6]Zhou Y, Liu Y, Zhao W, Xu R, Wang D, Li B, Zhou XShen H, Rational
design and synthesis of 3D MoS2 hierarchitecture with tunable nanosheets and
2H/1T phase within graphene for superior lithium storage. J.Electrochimica Acta 2016;211(1048-1055.
[7]Voiry D, Fullon R, Yang J, Kappera R, Bozkurt I, Kaplan D, Lagos M J,
Batson P EGupta G, The role of electronic coupling between substrate and 2D
MoS2 nanosheets in electrocatalytic production of hydrogen. J.Nature Materials 2016;15(9):1003.
[8]Cheng P, Sun KHu Y H, Mechanically-induced reverse phase
transformation of MoS2 from stable 2H to metastable 1T and its memristive
behavior. J.Rsc Advances 2016;6(70).
[9]Du H, Guo H L, Liu Y N, Xie X, Liang K, Zhou X, Wang XXu A W, Metallic
1T-LixMoS2 Cocatalyst Significantly Enhanced the Photocatalytic H2 Evolution
over Cd0.5Zn0.5S Nanocrystals under Visible Light Irradiation. J.Acs Applied Materials & Interfaces 2016;8(6):4023.
Claims (3)
1. a kind of microwave hydrothermal prepares 1T@2H-MoS2Method, the preparation method includes, first using deionized water as solvent, will
Ammonium heptamolybdate, thiocarbamide stir 30 min, 200 DEG C of 10 min of reaction of regulation temperature, secondly using alcohol as solvent, the first step are obtained
The product arrived reacts 4~10 min in 220 DEG C, that is, obtains 1T 2H-MoS2。
2. according to claim 1, it is characterised in that methods described is carried out in microwave hydrothermal instrument.
3. according to claim 1, it is characterised in that the ammonium heptamolybdate, the mol ratio 1 of thiocarbamide:15.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108314084A (en) * | 2018-02-09 | 2018-07-24 | 西北工业大学 | A kind of preparation method of metal phase molybdenum disulfide nano ball |
| CN109148842A (en) * | 2018-07-29 | 2019-01-04 | 大连理工大学 | A kind of no gradient-heated quickly prepares the method and its application of carbon load disulphide |
| CN109183065A (en) * | 2018-09-19 | 2019-01-11 | 台州学院 | A kind of method that hydro-thermal prepares 1T/2H phase MoSSe |
| CN109553181A (en) * | 2018-12-11 | 2019-04-02 | 中国科学院生态环境研究中心 | A kind of method generated free radicals using trivalent molybdenum and its method for handling organic wastewater |
| CN110615907A (en) * | 2019-10-22 | 2019-12-27 | 湖北大学 | 1T/2H mixed phase molybdenum disulfide material and preparation method and application thereof |
| CN113461060A (en) * | 2021-05-07 | 2021-10-01 | 电子科技大学 | Preparation method and application of interlayer spacing expanded nano spherical 1T phase molybdenum disulfide |
| US20220041463A1 (en) * | 2020-07-17 | 2022-02-10 | Mcmaster University | Systems and methods for the production of tunable conductive molybdenum disulfide thin films |
| CN114887631A (en) * | 2022-05-05 | 2022-08-12 | 中国石油大学(华东) | Solvothermal method for preparing mixed morphology 1T-2H MoS 2 Preparation method and application of |
| US11964880B2 (en) * | 2021-07-19 | 2024-04-23 | Mcmaster University | Systems and methods for the production of tunable conductive molybdenum disulfide thin films |
-
2017
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|---|---|---|---|---|
| CN108314084A (en) * | 2018-02-09 | 2018-07-24 | 西北工业大学 | A kind of preparation method of metal phase molybdenum disulfide nano ball |
| CN108314084B (en) * | 2018-02-09 | 2019-12-20 | 西北工业大学 | Preparation method of metal phase molybdenum disulfide nanospheres |
| CN109148842A (en) * | 2018-07-29 | 2019-01-04 | 大连理工大学 | A kind of no gradient-heated quickly prepares the method and its application of carbon load disulphide |
| CN109183065A (en) * | 2018-09-19 | 2019-01-11 | 台州学院 | A kind of method that hydro-thermal prepares 1T/2H phase MoSSe |
| CN109553181A (en) * | 2018-12-11 | 2019-04-02 | 中国科学院生态环境研究中心 | A kind of method generated free radicals using trivalent molybdenum and its method for handling organic wastewater |
| CN110615907A (en) * | 2019-10-22 | 2019-12-27 | 湖北大学 | 1T/2H mixed phase molybdenum disulfide material and preparation method and application thereof |
| US20220041463A1 (en) * | 2020-07-17 | 2022-02-10 | Mcmaster University | Systems and methods for the production of tunable conductive molybdenum disulfide thin films |
| CN113461060A (en) * | 2021-05-07 | 2021-10-01 | 电子科技大学 | Preparation method and application of interlayer spacing expanded nano spherical 1T phase molybdenum disulfide |
| US11964880B2 (en) * | 2021-07-19 | 2024-04-23 | Mcmaster University | Systems and methods for the production of tunable conductive molybdenum disulfide thin films |
| CN114887631A (en) * | 2022-05-05 | 2022-08-12 | 中国石油大学(华东) | Solvothermal method for preparing mixed morphology 1T-2H MoS 2 Preparation method and application of |
| CN114887631B (en) * | 2022-05-05 | 2023-08-18 | 中国石油大学(华东) | Solvothermal method for preparing mixed morphology 1T-2H MoS 2 Preparation method and application of (C) |
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