CN115196681A - N-doped molybdenum trioxide and preparation method thereof - Google Patents
N-doped molybdenum trioxide and preparation method thereof Download PDFInfo
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- CN115196681A CN115196681A CN202210976817.7A CN202210976817A CN115196681A CN 115196681 A CN115196681 A CN 115196681A CN 202210976817 A CN202210976817 A CN 202210976817A CN 115196681 A CN115196681 A CN 115196681A
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- molybdenum trioxide
- doped molybdenum
- doped
- preparation
- nitrogen plasma
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000035484 reaction time Effects 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000011358 absorbing material Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 238000009832 plasma treatment Methods 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005670 electromagnetic radiation Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
Abstract
The invention discloses N-doped molybdenum trioxide and a preparation method thereof, belonging to the technical field of electromagnetic wave absorption materials. According to the invention, the N-doped molybdenum trioxide can be obtained by simple nitrogen plasma treatment of molybdenum trioxide, the method is rapid and simple, the reaction condition is mild, no redundant pollutant is generated, the N-doping degree can be adjusted by controlling the reaction time of the nitrogen plasma and the molybdenum trioxide, and the prepared N-doped molybdenum trioxide has excellent wave-absorbing performance.
Description
Technical Field
The invention relates to N-doped molybdenum trioxide and a preparation method thereof, belonging to the technical field of electromagnetic wave absorption materials.
Background
In recent years, the continuous progress of electronic information technology and the wide spread of electronic products have brought more convenience to the lives of everyone. However, the accompanying electromagnetic radiation inevitably causes complicated problems such as electromagnetic interference and contamination, information leakage, adverse effects on human health, and the like. It is therefore desirable to develop a high performance absorber material to absorb unwanted electromagnetic radiation.
MoO 3 The ternary oxide is a strongly-associated electron system ternary oxide, is a typical transition metal oxide, has the characteristics of wide storage range and good chemical stability, and has low electromagnetic wave absorption characteristic. Researches show that the defect of low electromagnetic wave absorption property can be improved by adjusting the electronic structure and the conductivity of molybdenum trioxide, and in the prior art, moO is treated by a non-metal doping method 3 Further improve the electromagnetic wave absorption performance. However, such methods have harsh laboratory conditions, such as preparation at high temperature or in strong acid and strong base environments, long reaction time, generation of pollutants, and are not favorable for energy conservation and environmental protection, and are also not favorable for large-scale mass production and commercial application. Therefore, it is necessary to develop a safer and less laboratory-demanding method for preparing N-doped molybdenum trioxide in large quantities.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides N-doped molybdenum trioxide and a preparation method thereof.
Technical scheme
A preparation method of N-doped molybdenum trioxide comprises the following steps: and putting the molybdenum trioxide into a reaction container, vacuumizing, introducing nitrogen plasma, and reacting to obtain the N-doped molybdenum trioxide.
Further, the reaction time is 0.5 to 5 minutes.
Further, the flow rate of the nitrogen plasma was 50sccm.
The N-doped molybdenum trioxide prepared by the preparation method is used.
The N-doped molybdenum trioxide prepared by the preparation method is applied as an electromagnetic wave absorption material.
The invention has the beneficial effects that:
the invention provides a preparation method of N-doped molybdenum trioxide, which is characterized in that the N-doped molybdenum trioxide can be obtained by simple nitrogen plasma treatment of molybdenum trioxide, the method is rapid and simple, the reaction condition is mild, no redundant pollutant is generated, the N doping degree can be adjusted by controlling the reaction time of the nitrogen plasma and the molybdenum trioxide, and the prepared N-doped molybdenum trioxide has excellent wave-absorbing performance.
Drawings
FIG. 1 is a photograph of molybdenum trioxide and N-doped molybdenum trioxide made in example 1;
FIG. 2 is an SEM and EDX of N-doped molybdenum trioxide made in example 1;
FIG. 3 is the results of N-doping content test of N-doped molybdenum trioxide obtained in examples 1 to 3;
FIG. 4 shows MoO 3 And conductivity test results of the N-doped molybdenum trioxide prepared in example 1;
FIG. 5 is pure MoO 3 The wave-absorbing property of (2);
FIG. 6 shows the wave-absorbing properties of the N-doped molybdenum trioxide prepared in example 1;
FIG. 7 shows the wave-absorbing properties of the N-doped molybdenum trioxide prepared in example 2;
fig. 8 shows the wave-absorbing properties of the N-doped molybdenum trioxide prepared in example 3.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
A preparation method of N-doped molybdenum trioxide comprises the following steps: putting 30g of molybdenum trioxide powder into a reaction vessel, vacuumizing until the vacuum degree in the reaction vessel is lower than 10 -5 Pa, then introducing nitrogen plasma with the introduction flow rate of 50sccm, and reacting for 0.5 min to obtain a gray N-doped molybdenum trioxide material (N) 0.5 -MoO 3 ) And (3) solid.
Example 2
A preparation method of N-doped molybdenum trioxide comprises the following steps: 30g of molybdenum trioxide powderPutting the powder into a reaction container, and vacuumizing until the vacuum degree in the reaction container is lower than 10 -5 Pa, then introducing nitrogen plasma with the introduction flow rate of 50sccm, and reacting for 1 minute to obtain a gray N-doped molybdenum trioxide material (N) 1.0 -MoO 3 ) And (3) a solid.
Example 3
A preparation method of N-doped molybdenum trioxide comprises the following steps: putting 30g of molybdenum trioxide powder into a reaction vessel, and vacuumizing until the vacuum degree in the reaction vessel is lower than 10 -5 Pa, then introducing nitrogen plasma with the introduction flow rate of 50sccm, and reacting for 3 minutes to obtain a gray N-doped molybdenum trioxide material (N) 3.0 -MoO 3 ) And (3) a solid.
Fig. 1 is a photograph of molybdenum trioxide and N-doped molybdenum trioxide obtained in example 1, in which fig. 1A is a photograph of molybdenum trioxide in light gray, and fig. 1B is a photograph of N-doped molybdenum trioxide obtained in example 1, which is changed into dark gray powder, and success of N-doping can be preliminarily judged through a simple color change (deepening).
FIG. 2 is a SEM photograph and an EDX photograph of N-doped molybdenum trioxide obtained in example 1, wherein FIG. 2 (a) is a SEM photograph of N-doped molybdenum trioxide obtained in example 1, and FIG. 2 (b) is an EDX photograph of N-doped molybdenum trioxide obtained in example 1, and it can be seen that N element is uniformly distributed on the surface of Mo element, indicating that N element is successfully doped into MoO 3 A surface.
Fig. 3 is a result of testing the N-doping content of the N-doped molybdenum trioxide obtained in examples 1-3, and it can be seen that the N content is higher as the N plasma treatment time is longer, indicating that the N element content is in a positive relationship with the treatment time.
FIG. 4 shows MoO 3 And the conductivity test result of the N-doped molybdenum trioxide prepared in example 1, it can be seen that the conductivity of the N-doped molybdenum trioxide is significantly improved.
Pure MoO is tested in a 2-18GHz frequency band by adopting a network analyzer (VNA, N5245A, agilent, usa) 3 And the electromagnetic parameters of the N-doped molybdenum trioxide produced in examples 1-3. Test specimen and polyurethaneThe mass ratio of ester is 6 in :3.04mm，Φ out 7.00 mm) to maintain the certainty of the geometry. The thickness of all annuli was maintained at 2.5mm. Vienna ab initio software automatically outputs relevant electromagnetic parameters according to a joint gradient method algorithm. The test results are shown in FIGS. 5-8.
FIG. 5 is pure MoO 3 Fig. 6 is the wave-absorbing property of the N-doped molybdenum trioxide prepared in example 1, fig. 7 is the wave-absorbing property of the N-doped molybdenum trioxide prepared in example 2, and fig. 8 is the wave-absorbing property of the N-doped molybdenum trioxide prepared in example 3. It can be seen that the longer the N plasma treatment time is, the higher the N content is, the better the wave absorbing performance is.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (5)
1. A preparation method of N-doped molybdenum trioxide is characterized by placing molybdenum trioxide in a reaction vessel, vacuumizing, introducing nitrogen plasma, and reacting to obtain the N-doped molybdenum trioxide.
2. The method of preparing N-doped molybdenum trioxide of claim 1 wherein the reaction time is from 0.5 to 5 minutes.
3. The method for producing N-doped molybdenum trioxide according to claim 1 or 2, wherein the nitrogen plasma is introduced at a flow rate of 50 seem.
4. An N-doped molybdenum trioxide prepared by the method of claim 1, 2 or 3.
5. Use of the N-doped molybdenum trioxide produced by the method of claim 1, 2 or 3 as an electromagnetic wave absorbing material.
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| CN115196681B CN115196681B (en) | 2024-03-08 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101548582A (en) * | 2006-11-17 | 2009-09-30 | 法国圣-戈班玻璃公司 | Electrode for an organic light-emitting device, acid etching thereof, and also organic light-emitting device incorporating it |
| US20100200883A1 (en) * | 2009-02-09 | 2010-08-12 | Fujifilm Corporation | Method for producing organic electroluminescence element and organic electroluminescence element |
| CN114481188A (en) * | 2022-01-30 | 2022-05-13 | 吉林大学 | Preparation method of surface nitrogen-doped electrode |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101548582A (en) * | 2006-11-17 | 2009-09-30 | 法国圣-戈班玻璃公司 | Electrode for an organic light-emitting device, acid etching thereof, and also organic light-emitting device incorporating it |
| US20100200883A1 (en) * | 2009-02-09 | 2010-08-12 | Fujifilm Corporation | Method for producing organic electroluminescence element and organic electroluminescence element |
| CN114481188A (en) * | 2022-01-30 | 2022-05-13 | 吉林大学 | Preparation method of surface nitrogen-doped electrode |
Non-Patent Citations (3)
| Title |
|---|
| ANH DUC NGUYEN ET AL.: "Nitrogen-Plasma-Treated Continuous Monolayer MoS2 for Improving Hydrogen Evolution Reaction", 《ACS OMEGA》, pages 21509 * |
| CHAO LV ET AL.: "An efficient inverse opal (IO)-TiO2-MoO3-x for photocatalytic H2 evolution and RhB degradation – The synergy effect of IO structure and plasmonic MoO3-x", 《APPLIED SURFACE SCIENCE》, pages 1 - 11 * |
| RAMON A ET AL.: "Superior lithium-ion storage of V-doped MoO 3 nanosheets via plasma evaporation", 《ELECTROCHIMICA ACTA》, pages 1 - 11 * |
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