CN103818961A - Preparation method for molybdenum disulfide nanosheets at normal pressure - Google Patents
Preparation method for molybdenum disulfide nanosheets at normal pressure Download PDFInfo
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- CN103818961A CN103818961A CN201410087035.3A CN201410087035A CN103818961A CN 103818961 A CN103818961 A CN 103818961A CN 201410087035 A CN201410087035 A CN 201410087035A CN 103818961 A CN103818961 A CN 103818961A
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Abstract
The invention aims to provide a preparation method for a great amount of molybdenum disulfide nanosheets at a normal pressure. The specific steps are as follows: weighing a certain amount of commercially purchased molybdenum pentachloride (MoCl5); placing the molybdenum pentachloride (MoCl5) in a square ceramic boat and placing the ceramic boat at the middle part of a horizontal tube type furnace with a length of 90 cm; weighing a certain amount of powdered sulfur and placing the powdered sulfur into the other square ceramic boat; placing the square boat at the entrance of argon gas of the horizontal tube type furnace; sealing the horizontal tube type furnace and vacuumizing the horizontal tube type furnace; filling the furnace with the argon gas and maintaining certain flow velocity; increasing the temperature to the preset temperature and keeping the temperature for 30 min; finally, under the protection of the argon gas, naturally cooling off the temperature to a room temperature; collecting and obtaining the molybdenum disulfide nanosheets from the ceramic boat loaded with the raw materials of molybdenum pentachloride.
Description
Technical field
The invention belongs to the technical field of semiconductor nano material and preparation thereof, is a kind of preparation method of molybdenum disulfide nano sheet.
Background technology
Molybdenumdisulphide (MoS
2) be the chalcogenide materials with a kind of diamagnetism and semiconductor property, belong to hexagonal system.The MoS of nanostructure
2in many performances, further promoted, outstanding behaviours is in the following aspects: specific surface area is large, high adsorption capacity, reactive behavior are high, its catalytic performance especially performance of catalytic desulfurhydrogenation is stronger, can be used to prepare special catalytic material and air storage material, referring to: Inorganic nanotubes And fullerene-like materials, R.Tenne, Nature Nanotech., 2006,1,103-111; Nanometer MoS
2thin layer can be with the nearly 1.78eV of differential, match with the energy of light, on photocell material, have application prospect, referring to Photoluminescence from chemically exfoliated MoS
2, G. Eda, H. Yamaguchi, D. Voiry, et al, NanoLett., 2011,11,5111-5116; MoS
2the weak Van der Waals force of graphite-like structure and interlayer is conducive to the embedding of lithium and deviates from, the MoS of different-shape
2as nanotube, nanometer ball etc. were once used to Study on Li-ion batteries using, referring to: Exfoliated MoS
2nanocomposite as an anode material for lithium ion batteries, J. Xiao, D. Choi, L. Cosimbescu, et al, Chem. Mater. 2010,22,4522-4524; Along with MoS
2particle diameter diminish, it all obviously improves at tack and the level of coverage of friction material surface, and wear-resistant, antifriction performance is also significantly improved, referring to: Two-dimensional nanosheets produced by liquid exfoliation of layered materials, J. N. Coleman, M. Lotya, A. O'Neill, et al, Science, 2011,331,568-571.Under the environment that cannot use at liquid lubricants such as space technology, ultrahigh vacuum(HHV) or vehicle transmission, there is great science importance.
Molybdenum disulfide film is because of its unique microtexture and reason, voltinism matter, still there is the lot of advantages of Graphene in the shortcoming that overcomes zero band gap Graphene, thereby gather around and have broad application prospects in various fields such as secondary cell, field-effect transistor, sensor, electroluminescent, electricity storages simultaneously.But the research with two-dimensional layer nanostructure molybdenum disulfide film also has a lot of Fundamental Aspects theoretical and application to need to solve: first with regard to its preparation method, no matter conventional micromechanical forces stripping method, ion intercalation, liquid phase ultrasonic method etc. are the stripping method of master " from top to bottom ", or the synthesis method of " from bottom to top " take high temperature thermolysis etc. as representative is all left to be desired, how improves the preparation method of molybdenum disulfide film preparation technology is simple, preparation efficiency is high to realizing, favorable repeatability and mass production remain current research emphasis; With regard to structural characterization and photophysical property research aspect, find a kind of characterization method that fast, accurately and does not destroy sample structure significant.
Summary of the invention
The object of the present invention is to provide a kind of method that can prepare in a large number molybdenum disulfide nano sheet under normal pressure.Concrete steps are as follows: take certain molybdenum pentachloride (MoCl that directly business is bought
5) be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take certain sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas ingress, and after sealed horizontal tube furnace, vacuumizing, logical full argon gas also keeps certain flow rate; be warmed up to preset temp; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) figure of embodiment 1 gained sample, has illustrated that gained molybdenumdisulphide is nano-sheet structure.
Fig. 2 is transmission electron microscope (TEM) figure of embodiment 1 gained sample, has illustrated that gained molybdenum disulfide nano sheet shape structural thickness is very thin.
Fig. 3 is high-resolution-ration transmission electric-lens (HRTEM) figure of embodiment 1 gained sample, and the crystalline network that gained molybdenumdisulphide is nanometer sheet has been described.
Fig. 4 is the XRD figure of embodiment 1 gained sample, has illustrated that products therefrom is molybdenumdisulphide.
Embodiment
Embodiment 1:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 18cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 600 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 2:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 16cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 600 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 3:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 20cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 600 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 4:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 22cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 600 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 5:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 24cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 600 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 6:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 18cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 650 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 7:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 18cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 700 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 8:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 18cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 750 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 9:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 18cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 800 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Embodiment 10:
Take the MoCl that 200mg business is bought
5be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take 0.5g sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas entrance 18cm place, and after sealed horizontal tube furnace, vacuumize, leading to full argon gas and keeping flow velocity is 50sccm; be warmed up to 850 ℃; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
Claims (6)
1. the object of the present invention is to provide a kind of method that can prepare in a large number molybdenum disulfide nano sheet under normal pressure, concrete steps are as follows: take certain molybdenum pentachloride (MoCl that directly business is bought
5) be placed in square ceramic boat; and ceramic boat is placed on to the horizontal pipe furnace middle part that a length is 90cm; take certain sulphur powder and be placed in another square ceramic boat; and this Noah's ark is put in to horizontal pipe furnace argon gas ingress, and after sealed horizontal tube furnace, vacuumizing, logical full argon gas also keeps certain flow rate; be warmed up to preset temp; keep this temperature 30min, finally under argon shield, naturally cool to room temperature, in the ceramic boat that holds molybdenum pentachloride raw material, collect the product obtaining.
2. as claimed in claim 1, it is characterized in that, the Noah's ark that holds sulphur powder is put in horizontal pipe furnace argon gas entrance 16-24cm place.
3. as claimed in claim 1, it is characterized in that, reacting environment of living in is normal pressure.
4. as claimed in claim 1, it is characterized in that, the Ar of predetermined flow velocity is 50sccm.
5. as claimed in claim 1, it is characterized in that, horizontal pipe furnace range of reaction temperature is 600 ℃-850 ℃.
6. as claimed in claim 1, it is characterized in that, product molybdenum disulfide nano sheet is to hold raw material MoCl
5ceramic boat in obtain.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108557896A (en) * | 2018-05-02 | 2018-09-21 | 复旦大学 | A kind of preparation method of transition metal antimony sulfide |
| CN108585055A (en) * | 2018-05-25 | 2018-09-28 | 复旦大学 | A kind of Transition Metals V sulfide M V2S4Preparation method |
| CN114182290A (en) * | 2021-12-22 | 2022-03-15 | 北京科技大学 | Noble metal-two-dimensional transition metal chalcogenide heterostructure, preparation method and application thereof |
-
2014
- 2014-03-11 CN CN201410087035.3A patent/CN103818961A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108557896A (en) * | 2018-05-02 | 2018-09-21 | 复旦大学 | A kind of preparation method of transition metal antimony sulfide |
| CN108585055A (en) * | 2018-05-25 | 2018-09-28 | 复旦大学 | A kind of Transition Metals V sulfide M V2S4Preparation method |
| CN108585055B (en) * | 2018-05-25 | 2020-12-18 | 复旦大学 | Transition metal vanadium sulfide MV2S4Preparation method of (1) |
| CN114182290A (en) * | 2021-12-22 | 2022-03-15 | 北京科技大学 | Noble metal-two-dimensional transition metal chalcogenide heterostructure, preparation method and application thereof |
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Application publication date: 20140528 |
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