CN105399060A - Method for rapid synthesis of two-dimensional layered nanometer material - Google Patents
Method for rapid synthesis of two-dimensional layered nanometer material Download PDFInfo
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- CN105399060A CN105399060A CN201510626627.2A CN201510626627A CN105399060A CN 105399060 A CN105399060 A CN 105399060A CN 201510626627 A CN201510626627 A CN 201510626627A CN 105399060 A CN105399060 A CN 105399060A
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Abstract
The invention discloses a method for rapid synthesis of a two-dimensional layered nanometer material. The method comprises the following steps: a precursor A and a precursor B of the nanometer material with a laminated structure are provided, and vacuum packaging of the precursor A and the precursor B is carried out in a reaction tube according to a stoichiometric ratio; the packed reaction tube sample is placed in microwave plasma reaction equipment, and after reaction, a nanometer pure product with the laminated structure is obtained in a microwave environment. The embodiment of the invention provides the preparation method of the nanometer laminated structure, such as MoS2 and WS2, so that the reaction time is substantially reduced and pollutants are reduced, at the same time the obtained material has good morphology and reproducibility, and can be applied to the fields of energy storage and photocatalysis. In addition, the preparation method of electrodes is simple and has a low cost, and is easy to repeatedly realize; and thus the preparation method is good for industrialized production.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of method of Fast back-projection algorithm two-dimensional layer nano material.
Background technology
Microwave plasma technology is the novel method developed in the last few years, has great potential and industrial value.Simultaneously, the features such as it is active by force, cleanliness without any pollution, process control are good, chemical reaction is quick, favorable reproducibility cause the concern of people day by day, and be applied to the aspects such as nano material is prepared fast, sintered, vapour deposition fast, and as: the low temperature synthesis, long after glow luminous material, diamond thin, nanometre scale solid film etc. of CNT (carbon nano-tube).
Molybdenumdisulphide is combined into main lamellar compound with Van der Waals force, and its chemical bond S-Mo-S is main; There is very excellent electrocatalysis, mechanics, photochemical properties.Be widely used in the industries such as space flight, aviation, chemical industry, metallurgy, also can be used for the fields such as catalytic additive, coating and sealing material.At present, MoS is prepared
2method and technology of a great variety, mainly concentrate on (1) high temperature vulcanized method; (2) presoma decomposition method; (3) hydrothermal method; (4) solution method; (5) electrochemical deposition method; (6) template; (7) sonochemical method; (8) method such as molten-salt growth method.In all kinds of preparation method, the reaction of sonochemistry method is not easy to control, have side reaction to occur, and microwave reactor is expensive, can only be limited in laboratory and synthesize on a small scale, be difficult to large-scale industrial production.Electrochemical process faces that reactive component is poorly soluble equally, interphase mass transfer poor performance and the problem such as selectivity of product is low and energy consumption of reaction is large.Template removes the problems such as template energy consumption is large, template not easily removes completely, easily cause that structure collapse, template cannot be recycled.Hydrothermal method can not continuous seepage, and plot ratio is low, efficiency is low, and the high-temperature high-pressure apparatus cost of needs is high, and when temperature is low, crystalline form is usually imperfect, and industrialization is very difficult.
Summary of the invention
The deficiencies in the prior art in view of the above, the object of the present invention is to provide a kind of method of Fast back-projection algorithm two-dimensional layer nano material, realize quick, accurate, the low-cost production of two-dimension nano materials.
For achieving the above object and other relevant objects, technical scheme of the present invention is as follows: a kind of method of Fast back-projection algorithm two-dimensional layer nano material, comprise the following steps: nano-lamellar structure material precursor A and B is provided, and by A and B stoichiometrically Vacuum Package in reaction tubes; Packaged reaction tubes sample is put into microwave plasma conversion unit, under microwave environment, is obtained by reacting nano-lamellar structure sterling.
As preferably: precursor A and B are uniformly mixed to form mixed powder, are then placed in reaction tubes vacuum-sealing, reaction tubes internal pressure is kept to be 0.01-30Torr.
As preferably: preparing nano material lamellar spacing is 2-50 nanometer.
As preferably: after packaged sample being put into the tubular reactor chamber of microwave plasma conversion unit, pass into reactive gas, adjustment reaction chamber pressure 0.01-100Torr, open after microwave switch carries out reaction 5-30 minute and obtain nano-lamellar structure product.
As preferably: the diameter of described reaction tubes is 8mm-20mm.
As preferably: described precursor A and B are molybdenum source and sulphur source, finally prepare sheet MoS
2nano-powder; Or described presoma is molybdenum source and selenium source, finally prepares sheet MoSe
2nano-powder; Or presoma is tungsten source and selenium source, finally prepares sheet WSe
2nano-powder; Or presoma is tungsten source and sulphur source, finally prepares sheet WS
2nano-powder; Presoma is niobium source and selenium source, finally prepares sheet NbSe
2nano-powder.
As preferably: described microwave plasma conversion unit comprises microwave source, the protective tube be placed in microwave source, admission passage and outlet pipe; described admission passage is connected with the inlet end of protective tube; described outlet pipe is connected with the outlet side of protective tube; described admission passage and outlet pipe are provided with control valve, described admission passage or outlet pipe are provided with weather gauge.
As preferably: described admission passage is connected by vacuum seal structure with protective tube two ends with outlet pipe; Described weather gauge is arranged on outlet pipe, between control valve and protective tube.
As preferably: described outlet pipe is connected with vacuum pump by flanged coupling, and described control valve is needle-valve.
As preferably: the stoichiometric ratio of precursor A and B by the mol ratio of A and B in generation material.
As mentioned above, the invention has the beneficial effects as follows: the preparation method of the nano-lamellar structure material that the invention process provides, can Reaction time shorten greatly, decreasing pollution object, the material simultaneously obtained has good pattern and reproducibility, can be applied to the field such as stored energy, photochemical catalysis.In addition, the preparation method of this electrode is simple, and cost is lower, is easy to repeat to realize, thus is beneficial to industrialization production.
Accompanying drawing explanation
Fig. 1 is the structural representation of microwave plasma conversion unit in the present invention;
Fig. 2 is the SEM image of sample of the present invention;
Fig. 3 is the TEM image of sample of the present invention
Fig. 4 is the diffraction image of sample of the present invention;
Fig. 5 is the Raman collection of illustrative plates of sample of the present invention.
Piece mark explanation
1 microwave source
2 protective tubes
3 reaction tubess
4 admission passages
5 outlet pipes
61,62 control valves
71,72 vacuum-sealing connecting joints
8 weather gauges
9 microwave switches
10 flanged couplings
Embodiment
By particular specific embodiment, embodiments of the present invention are described below, person skilled in the art scholar the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.
Embodiment 1
Below in conjunction with the accompanying drawings and the specific embodiments to sheet MoS provided by the invention
2fabrication method is described in further detail.
The invention provides one and be applied to Fast back-projection algorithm sheet MoS
2the preparation method of nano material: molybdenum source A and sulphur source B is pressed MoS
2mol ratio is uniformly mixed to form mixed powder.Wherein molybdenum source A is 0.1 mole, and sulphur source B is 0.2 mole, and wherein molybdenum source is the molybdenum powder of simple substance, and sulphur source is elemental sulfur powder.This mixture is placed in the reaction tubes 3 of a diameter 8-20mm, reaction tubes 3 is silica tube, and by its vacuum-sealing, keeps reaction tubes internal pressure to be 0.01-30Torr; Then put into the microwave plasma apparatus of structure as shown in Figure 1, and the tube chamber pressure adjusting plasma apparatus protective tube 2 is at 0.01-100Torr, opens microwave switch 9 (power 300W-1000W) and carry out reaction 5-30 minute and namely obtain sheet MoS
2powder, as shown in Figure 2-5, comparatively crystalline structure is better for result display product, lamellar spacing 2-30 nanometer, and the lamella distribution of sizes shown from SEM picture is homogeneous, represents that particle dispersion is better for powder style test result.TEM image represents that nanoscale twins cleanliness factor is better.In Fig. 5, Raman peaks only has two peaks of 396 and 405 nanometers, represents that composition is comparatively pure.
The method has fast, low cost, clean free of contamination feature; Meanwhile, MoS
2nano-powder, as a kind of high purity solid lubricant, has excellent high temperature resistant, the characteristic such as resistance to compression and stable chemical property, is widely used in the industries such as space flight, aviation, chemical industry, metallurgy, also can be used for the fields such as catalytic additive, coating and sealing material.
As shown in Figure 1; microwave plasma apparatus comprises microwave source 1, the protective tube 2 be placed in microwave source, admission passage 4 and outlet pipe 5; microwave source 1 provides microwave environment for protective tube 2 and reaction tubes 3; it has microwave switch 9; admission passage 4 is connected with the inlet end of protective tube 2 by vacuum sealing joint 71; outlet pipe 5 is connected with the outlet side of protective tube 2 by vacuum sealing joint 72; admission passage 4 and outlet pipe 5 are provided with control valve 61,62; for regulating the air pressure in protective tube 2, admission passage 4 or outlet pipe 5 are provided with weather gauge 8.
Weather gauge 8 described in this example is arranged on outlet pipe 5; between control valve 62 and the outlet side of protective tube 2; can also connect vacuum pump by 10 in the outlet side of outlet pipe 5 to be used for bleeding, make to form vacuum environment in protective tube 2, described control valve 61,62 is needle-valve.
This microwave plasma apparatus; after reaction tubes 3 puts into protective tube 2; be sealingly connected in pipeline by protective tube 2 two ends, bled by protective tube 2 outlet side, inlet end passes into gas; and by control valve 61,62 adjustments of gas size; thus the pressure in Control protection pipe 2 is in claimed range, it can be rare gas element or other reactive gass that admission passage 4 passes into gas, can not participate in reaction; mainly regulate the low vacuum effect in pressure maintenance protective tube 2, plasma is generated.
It should be noted that: method of the present invention does not also rely on the microwave plasma apparatus provided in the present invention, can also adopt other microwave plasma apparatus of the prior art.
Embodiment 2
The present embodiment is substantially identical with described embodiment 1, and difference is, described active material precursor A, B are respectively molybdenum source and selenium source, finally prepare sheet MoSe
2nano-powder.
A kind of Fast back-projection algorithm sheet MoSe
2the preparation method of nano material: molybdenum source A and selenium source B is uniformly mixed to form mixed powder.Wherein molybdenum source A is the molybdenum elemental powders of 0.1 mole, and selenium source B is the selenium elemental powders of 0.2 mole.This mixture is placed in the reaction tubes 3 of a diameter 8-20mm, reaction tubes 3 is silica tube, and by its vacuum-sealing, keeps reaction tubes internal pressure to be 2-10Torr; Then put into the microwave plasma apparatus of structure as shown in Figure 1, and the tube chamber pressure adjusting plasma apparatus protective tube 2 is at 20-30Torr, opens microwave switch 9 (power 770W) and carry out reaction and namely obtain sheet MoSe in 20 minutes
2powder, comparatively structure is comparatively complete for powder style test result display product, lamellar spacing 20-30 nanometer, and has good dispersiveness.
Embodiment 3
The present embodiment is substantially identical with described embodiment 1, and difference is, described electrode active material precursor A, B are respectively tungsten source and selenium source, finally prepare sheet WSe
2nano-powder.
A kind of Fast back-projection algorithm sheet WSe
2the preparation method of nano material: molybdenum source A and selenium source B is uniformly mixed to form mixed powder.Wherein molybdenum source A is the elemental powders of 0.1 mole of tungsten, and selenium source B is the elemental powders of 0.2 mole of selenium.This mixture is placed in the reaction tubes 3 of a diameter 8-20mm, reaction tubes 3 is silica tube, and by its vacuum-sealing, keeps reaction tubes internal pressure to be 2-10Torr; Then put into the microwave plasma apparatus of structure as shown in Figure 1, and the tube chamber pressure adjusting plasma apparatus protective tube 2 is at 15-30Torr, opens microwave switch 9 (power 600W) and carry out reaction 15-20 minute and namely obtain sheet WSe
2powder, comparatively structure is comparatively complete for powder style test result display product, lamellar spacing 15-30 nanometer, and has good dispersiveness.
Embodiment 4
The present embodiment is substantially identical with described embodiment 1, and difference is, described electrode active material precursor A, B are respectively tungsten source and sulphur source, finally prepare sheet WS
2nano-powder.
A kind of Fast back-projection algorithm sheet WS
2the preparation method of nano material: tungsten source and sulphur source are uniformly mixed to form mixed powder.Wherein tungsten source is 0.1 mole, and sulphur source is 0.2 mole, and tungsten source is tungsten elemental powders, and sulphur source is sulphur elemental powders.This mixture is placed in the reaction tubes 3 of a diameter 8-20mm, reaction tubes 3 is silica tube, and by its vacuum-sealing, keeps reaction tubes internal pressure to be 8-15Torr; Then the microwave plasma apparatus of structure is as shown in Figure 1 put into; by pass into gas or the tube chamber pressure of adjustment plasma apparatus protective tube 2 of bleeding at 10-20Torr, open microwave switch 9 (power 800W) and carry out reaction 5-10 minute and namely obtain sheet WS
2powder, powder style test result display product is comparatively complete, lamellar spacing 30-50 nanometer, and has good dispersiveness.
Embodiment 5
The present embodiment is substantially identical with described embodiment 1, and difference is, described electrode active material precursor A, B are respectively niobium source and selenium source, finally prepare sheet NbSe
2nano-powder.
A kind of Fast back-projection algorithm sheet NbSe
2the preparation method of nano material: the elemental powders of niobium and selenium is uniformly mixed to form mixed powder.Wherein niobium source is 0.1 mole, and selenium source is 0.2 mole, and niobium source is niobium elemental powders, and selenium source is selenium elemental powders.This mixture is placed in the reaction tubes 3 of a diameter 8-20mm, reaction tubes 3 is silica tube, and by its vacuum-sealing, keeps reaction tubes internal pressure to be 2-5Torr; Then put into the microwave plasma apparatus of structure as shown in Figure 1, and the tube chamber pressure adjusting plasma apparatus protective tube 2 is at 20-40Torr, opens microwave switch 9 (power 650W) and carry out reaction 20-30 minute and namely obtain sheet NbSe
2powder, powder style test result display product is comparatively pure, lamellar spacing 2-30 nanometer, and has good dispersiveness.
It should be noted that and the object of the present invention is to provide above-mentioned preparation method, reaction tubes internal pressure wherein, official jargon pressure, microwave power and reaction times etc. can be arranged according to concrete reactant.
Above preferred embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, and any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or change.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. a method for Fast back-projection algorithm two-dimensional layer nano material, is characterized in that, comprises the following steps: provide nano-lamellar structure material precursor A and B, and is encapsulated in reaction tubes by A and B mixing final vacuum; Packaged reaction tubes sample is put into microwave plasma conversion unit, under microwave environment, is obtained by reacting nano-lamellar structure sterling.
2. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, is characterized in that: precursor A and B are uniformly mixed to form mixed powder, is then placed in reaction tubes vacuum-sealing, keeps reaction tubes internal pressure to be 0.01-30Torr.
3. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, is characterized in that: preparing nano material lamellar spacing is 2-50 nanometer.
4. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, it is characterized in that: after packaged sample being put into the tubular reactor chamber of microwave plasma conversion unit, pass into gas, adjustment reaction chamber pressure 0.01-100Torr, open after microwave switch carries out reaction 5-30 minute and obtain nano-lamellar structure product.
5. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, is characterized in that: the diameter of described reaction tubes is 8mm-20mm.
6. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, is characterized in that: described precursor A and B are molybdenum source and sulphur source, finally prepare sheet MoS
2nano-powder; Or described presoma is molybdenum source and selenium source, finally prepares sheet MoSe
2nano-powder; Or presoma is tungsten source and selenium source, finally prepares sheet WSe
2nano-powder; Or presoma is tungsten source and sulphur source, finally prepares sheet WS
2nano-powder; Presoma is niobium source and selenium source, finally prepares sheet NbSe
2nano-powder.
7. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 1; it is characterized in that: described microwave plasma conversion unit comprises microwave source, the protective tube be placed in microwave source, admission passage and outlet pipe; described admission passage is connected with the inlet end of protective tube; described outlet pipe is connected with the outlet side of protective tube; described admission passage and outlet pipe are provided with control valve, described admission passage or outlet pipe are provided with weather gauge.
8. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 7, is characterized in that: described admission passage is connected by vacuum seal structure with protective tube two ends with outlet pipe; Described weather gauge is arranged on outlet pipe, between control valve and protective tube.
9. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 8, it is characterized in that: described outlet pipe is connected with vacuum pump by flanged coupling, described control valve is needle-valve.
10. the method for a kind of Fast back-projection algorithm two-dimensional layer nano material according to claim 1, is characterized in that: the stoichiometric ratio of precursor A and B is mol ratio.
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| CN107601443A (en) * | 2017-11-09 | 2018-01-19 | 安徽大学 | A kind of preparation method of ultra-thin tungsten selenide nanometer sheet |
| CN108793096A (en) * | 2018-06-04 | 2018-11-13 | 武汉理工大学 | A kind of NbSe of making Nano surface2Electrode material and its preparation method and application |
| CN109879315A (en) * | 2019-04-09 | 2019-06-14 | 陕西科技大学 | A kind of porous hexagon nano-titanium dioxide of two-dimensional layer and its preparation method and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601443A (en) * | 2017-11-09 | 2018-01-19 | 安徽大学 | A kind of preparation method of ultra-thin tungsten selenide nanometer sheet |
| CN107601443B (en) * | 2017-11-09 | 2020-01-14 | 安徽大学 | Preparation method of ultrathin tungsten selenide nanosheets |
| CN108793096A (en) * | 2018-06-04 | 2018-11-13 | 武汉理工大学 | A kind of NbSe of making Nano surface2Electrode material and its preparation method and application |
| CN108793096B (en) * | 2018-06-04 | 2022-03-01 | 武汉理工大学 | NbSe with nano-sized surface2Electrode material and preparation method and application thereof |
| CN109879315A (en) * | 2019-04-09 | 2019-06-14 | 陕西科技大学 | A kind of porous hexagon nano-titanium dioxide of two-dimensional layer and its preparation method and application |
| CN109879315B (en) * | 2019-04-09 | 2021-06-01 | 陕西科技大学 | Two-dimensional layered porous hexagonal nano titanium dioxide and preparation method and application thereof |
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