CN103613136B - A kind of preparation method of square MoO3 nanosheet - Google Patents
A kind of preparation method of square MoO3 nanosheet Download PDFInfo
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- CN103613136B CN103613136B CN201310589644.4A CN201310589644A CN103613136B CN 103613136 B CN103613136 B CN 103613136B CN 201310589644 A CN201310589644 A CN 201310589644A CN 103613136 B CN103613136 B CN 103613136B
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Abstract
The present invention relates to a kind of preparation method of square MoO3 nanosheet, it is characterized in that step is as follows: be dissolved in solvent by molybdenum source, sulphur source and reductive agent, make it be distributed to uniformly in solution by centrifugal mixer, move into stainless steel cauldron, sealing, after constant temperature 100 DEG C ~ 300 DEG C reaction 24h, be cooled to room temperature, obtain reaction product, be separated above-mentioned reaction product, washing, drying, obtain presoma MoS
2; By MoS
2nano material is placed in tube furnace, and in air or oxygen atmosphere, constant temperature insulation 24h at 300 DEG C ~ 600 DEG C, annealing 0.5 ~ 5h obtains MoO
3four directions nanometer sheet, thickness at 100-150nm, size 1 ~ 2 μm.The raw material of the inventive method is easy to get, cheap, preparation technology is simple, parameter is easily controlled, production process safety and environmental protection, and it can widespread use in air-sensitive, magnetic and lithium electric material etc.
Description
Technical field
The present invention relates to nano magnetic material field, particularly, is a kind of MoO
3the preparation method of four directions nanometer sheet.
Background technology
Molybdic oxide is the very potential semiconductor material of one, in solar cell, photochemical catalysis, air-sensitive and magnetic etc., have important application.Particularly nano level molybdic oxide tool more has excellent reversible photochromism and higher optical contrast, its performance has potential using value in information storage, image display and light regulating etc., can be used as the core material of the device such as electrochromism, photochromic, intelligent camouflage, in the field such as display equipment and military equipment, there is wide using value.
In recent years, along with the progress of science and technology, constantly there is many novel molybdic oxide powder preparing methods.The existing multiple method preparing powder at present, as the precipitator method, hydrothermal method, electrochemical deposition method, sputtering method, sol-gel method etc.But the regulation and control for molybdenum trioxide nano material morphology and structure are the focuses of nano material study on the synthesis always.
Summary of the invention
The object of the present invention is to provide a kind of using molybdenum disulfide nano material as presoma, synthesize MoO by low sintering mode
3the method of four directions nanometer sheet, with low cost, technique is simple and productive rate is high, synthesized MoO
3four directions nanometer sheet has better air-sensitive and chemical property.
Above-mentioned purpose is achieved by the following technical solution:
A preparation method for square MoO3 nanosheet, step is as follows:
(1) presoma MoS
2prepared by nano material:
Molybdenum source, sulphur source and reductive agent are dissolved in solvent, make it be distributed to uniformly in solution by centrifugal mixer, move into stainless steel cauldron, sealing, after constant temperature 100 DEG C ~ 300 DEG C reaction 24h, be cooled to room temperature, obtain reaction product, be separated above-mentioned reaction product, washing, drying, obtain presoma MoS
2;
Molybdenum source is 1:2-1:4 with the ratio of the amount of substance in sulphur source; Molybdenum source is 1:1-1:3 with the ratio of the amount of substance of reductive agent;
Described molybdenum source is soluble molybdenum salt, as Sodium orthomolybdate, ammonium molybdate, hexacarbonylmolybdenum;
Sulphur source is dissolvable sulfide, as sodium sulphite, potassium sulphide, thiocarbamide;
Reductive agent is organic reducing agent, as, citric acid, xitix etc.;
Solvent is deionized water or ethanol;
(2) aerobic annealing sintering synthesis MoO
3four directions nanometer sheet:
By the MoS of synthesis
2nano material is placed in tube furnace, and in air or oxygen atmosphere, the 0.5 ~ 5h that anneals at glucose 300 DEG C ~ 600 DEG C obtains MoO
3four directions nanometer sheet, thickness is greatly about 100nm, and size is the cubic nanometer sheet of 1 ~ 2 μm.
The cost of the inventive method is inexpensive, and production technique is simple and easy to control, and product rate is high, is applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the MoO that the embodiment of the present invention 1 obtains
3the XRD of four directions nanometer sheet, illustrate that XRD peak position is consistent with standard diffraction figure (PDF No.35-0609), product is MoO mainly
3four directions nanometer sheet;
Fig. 2 is the MoO that the embodiment of the present invention 1 obtains
3four directions nanometer sheet field emission scanning electron microscope (SEM) photo, Fig. 2 a and 2b is the SEM photo of product different multiples, clearly can see that product is that thickness is approximately 200nm, the MoO that diameter is 1 ~ 2 μm from figure
3four directions nanometer sheet.
Fig. 3 is the MoO that the embodiment of the present invention 1 obtains
3the transmission electron microscope (TEM figure) of four directions nanometer sheet, its result is consistent with SEM, proves that product is MoO further
3four directions nanometer sheet (unit scaling refers to 0.5nm).
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment 1:
0.44g Na
2mO
4, 0.6g Na
2s and 0.4g glucose sugar is dissolved completely in the deionized water of 60mL, after continuing to stir 30min, is transferred to by mixed solution in the stainless steel cauldron of 100ml, is placed in vacuum drying oven in 180 DEG C of insulation 24h, is cooled to room temperature.Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and finally 80 DEG C of dry 10h obtain the powder of grey black under vacuum, i.e. presoma MoS
2nano material.By under above-mentioned product 400 DEG C of conditions, the 2h that anneals in tube furnace obtains powder product and the MoO of black
3four directions nanometer sheet.
Embodiment 2:
0.44g Na
2mO
4, 0.6g Na
2what S and 0.6g citric acid was dissolved completely in 60mL goes in ethanol, after continuing to stir 30min, is transferred to by mixed solution in the stainless steel cauldron of 100ml, is placed in vacuum drying oven in 160 DEG C of insulation 24h, is cooled to room temperature.Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and finally 80 DEG C of dry 10h obtain the powder of grey black under vacuum, i.e. presoma MoS
2nano material.By under above-mentioned product 450 DEG C of conditions, the 1h that anneals in tube furnace obtains powder product and the MoO of black
3four directions nanometer sheet, thickness is approximately 200nm, diameter 1 ~ 2 μm.
The reagent different from embodiment 1 that embodiment 3-5 adopts and parameter are in table 1.
Table 1
Claims (1)
1. a preparation method for square MoO3 nanosheet, is characterized in that step is as follows:
(1) presoma MoS
2prepared by nano material:
Molybdenum source, sulphur source and reductive agent are dissolved in solvent, make it be distributed to uniformly in solution by centrifugal mixer, move into stainless steel cauldron, sealing, after constant temperature 100 DEG C ~ 300 DEG C reaction 24h, be cooled to room temperature, obtain reaction product, reaction product isolated, washing, drying, obtain presoma MoS
2nano material;
Described molybdenum source is Sodium orthomolybdate, ammonium molybdate or hexacarbonylmolybdenum; Sulphur source is sodium sulphite, potassium sulphide or thiocarbamide; Reductive agent is citric acid or xitix; Described solvent is deionized water, ethanol or ethylene glycol;
Molybdenum source is 1:2-1:4 with the ratio of the amount of substance in sulphur source; Molybdenum source is 1:1-1:3 with the ratio of the amount of substance of reductive agent;
(2) aerobic annealing sintering synthesis MoO
3four directions nanometer sheet:
By the MoS of synthesis
2nano material is placed in tube furnace, and in air or oxygen atmosphere, 0.5 ~ 5 h that anneals at 300 DEG C ~ 600 DEG C obtains MoO
3rhombic system nanometer sheet, thickness at 100-150nm, size 1 ~ 2 micron.
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| CN103613136B true CN103613136B (en) | 2015-09-16 |
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| CN104649323B (en) * | 2015-01-21 | 2016-06-22 | 济南大学 | A kind of preparation method of strip molybdenum trioxide |
| CN104709943A (en) * | 2015-03-13 | 2015-06-17 | 济南大学 | Preparation method of molybdenum trioxide microsphere in three-dimensional hierarchical structure |
| CN105789030A (en) * | 2016-03-14 | 2016-07-20 | 暨南大学 | Preparation method of molybdenum trioxide two-dimensional atomic crystals with reduced layers |
| CN105944712B (en) * | 2016-05-23 | 2018-06-26 | 南京信息工程大学 | A kind of preparation method of cerous molybdate sodium/molybdenum trioxide composite photo-catalyst |
| CN106745262B (en) * | 2016-12-12 | 2017-12-29 | 郑州大学 | A kind of method for preparing amorphous oxide molybdenum nanometer sheet using the few layer molybdenum sulfide of oxidation |
| CN108279540B (en) * | 2018-02-01 | 2022-07-15 | 深圳市光羿科技有限公司 | Inorganic metal oxide ion storage layer, low-temperature solution processing method and application thereof |
| CN109205676B (en) * | 2018-08-30 | 2021-02-02 | 济南大学 | MoO (MoO)3Electrostatic spinning synthetic method of sheet structure |
| CN108996549B (en) * | 2018-10-10 | 2021-06-15 | 金堆城钼业光明（山东）股份有限公司 | MoO (MoO)3Sheet-assembled network structure nano material and preparation method thereof |
| CN110441380B (en) * | 2019-08-07 | 2021-07-23 | 暨南大学 | Electrochemical sensor based on molecular imprinting electrode technology and preparation method and application thereof |
| CN110879238B (en) * | 2019-10-25 | 2021-08-24 | 东北大学 | Molybdenum trioxide nano-structure sensitive material, corresponding ammonia gas sensor and preparation method |
| CN112520789B (en) * | 2020-12-29 | 2022-05-31 | 杭州电子科技大学 | Preparation method of molybdenum trioxide nano film |
| CN113697857B (en) * | 2021-09-14 | 2023-01-24 | 河北地质大学 | Preparation method and application of two-dimensional flaky molybdenum oxide nano material |
| CN114609197B (en) * | 2022-03-25 | 2023-11-21 | 电子科技大学 | Gas-sensitive material, preparation method and NH (NH) thereof 3 Application in gas sensor |
| CN115347083A (en) * | 2022-09-19 | 2022-11-15 | 陕西科技大学 | Morphology-controllable molybdenum disulfide nano material and preparation method and application thereof |
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