CN115196681B - N-doped molybdenum trioxide and preparation method thereof - Google Patents
N-doped molybdenum trioxide and preparation method thereof Download PDFInfo
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- CN115196681B CN115196681B CN202210976817.7A CN202210976817A CN115196681B CN 115196681 B CN115196681 B CN 115196681B CN 202210976817 A CN202210976817 A CN 202210976817A CN 115196681 B CN115196681 B CN 115196681B
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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 108
- 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 5
- 239000011358 absorbing material Substances 0.000 claims abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 238000009832 plasma treatment Methods 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 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
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002939 conjugate gradient method Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000002596 correlated effect Effects 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000001105 regulatory effect Effects 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
Classifications
-
- 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, which belong to the technical field of electromagnetic wave absorbing materials. The method can obtain the N-doped molybdenum trioxide by simple nitrogen plasma treatment, is quick and simple, has mild reaction conditions, does not generate excessive pollutants, can adjust the N doping degree by controlling the reaction time of nitrogen plasma and molybdenum trioxide, and 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 absorbing materials.
Background
In recent years, the continuous progress of electronic information technology and the large-scale popularization of electronic products have brought more convenience to the lives of everyone. However, the consequent electromagnetic radiation inevitably causes complex problems of electromagnetic interference and pollution, information leakage, adverse effects on human health, etc. There is therefore a need to develop a high performance absorber material to absorb unwanted electromagnetic radiation.
MoO 3 Is a ternary oxide of a strongly correlated electron system, is a typical transition metal oxide, has the characteristics of wide storage range and good chemical stability, and has low electromagnetic wave absorption characteristic. It was found that by adjusting threeThe electronic structure of molybdenum oxide and its conductivity can improve the defect of lower electromagnetic wave absorption characteristic, in the prior art, moO is treated by a nonmetallic doping method 3 Further, the report of electromagnetic wave absorption performance is improved. However, such methods have severe laboratory conditions, such as preparation at high temperature or in strong acid and alkali environments, long reaction time, and pollutant generation, and are unfavorable for energy conservation and environmental protection, large-scale mass production and commercial application. Therefore, it is necessary to develop a safer method for preparing N-doped molybdenum trioxide in large quantities, which requires less laboratory requirements.
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 proposal
The preparation method of the N-doped molybdenum trioxide comprises the following steps: and placing the molybdenum trioxide in 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 obtained by the preparation method is prepared.
The N-doped molybdenum trioxide obtained by the preparation method is applied to electromagnetic wave absorbing materials.
The invention has the beneficial effects that:
the invention provides a preparation method of N-doped molybdenum trioxide, which is characterized in that the molybdenum trioxide can be processed by simple nitrogen plasma to obtain the N-doped molybdenum trioxide, the method is quick and simple, the reaction condition is mild, no excessive pollutant is generated, the N-doped degree can be regulated 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 prepared in example 1;
FIG. 2 is an SEM image and EDX image of N-doped molybdenum trioxide obtained in example 1;
FIG. 3 is a graph showing the results of N-doping content test of the N-doped molybdenum trioxide obtained in examples 1-3;
FIG. 4 is MoO 3 And the conductivity test results of the N-doped molybdenum trioxide prepared in example 1;
FIG. 5 is pure MoO 3 Is used for the wave absorbing performance of the (a);
FIG. 6 is a graph showing the wave-absorbing properties of N-doped molybdenum trioxide obtained in example 1;
FIG. 7 is a graph showing the wave-absorbing properties of N-doped molybdenum trioxide obtained in example 2;
fig. 8 shows the wave-absorbing properties of the N-doped molybdenum trioxide obtained in example 3.
Detailed Description
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
The preparation method of the N-doped molybdenum trioxide comprises the following steps: placing 30g molybdenum trioxide 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 flow rate of 50sccm, reacting for 0.5 min to obtain gray N-doped molybdenum trioxide material (N) 0.5 -MoO 3 ) A solid.
Example 2
The preparation method of the N-doped molybdenum trioxide comprises the following steps: placing 30g molybdenum trioxide 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 flow rate of 50sccm, and reacting for 1 min to obtain gray N-doped molybdenum trioxide material (N) 1.0 -MoO 3 ) A solid.
Example 3
The preparation method of the N-doped molybdenum trioxide comprises the following steps: putting 30g of molybdenum trioxide powder into a reaction container, and vacuumizingEmpty until the vacuum degree in the reaction vessel is lower than 10 -5 Pa, then introducing nitrogen plasma with the flow rate of 50sccm, and reacting for 3 min to obtain gray N-doped molybdenum trioxide material (N) 3.0 -MoO 3 ) A solid.
Fig. 1 is a photograph of molybdenum trioxide and N-doped molybdenum trioxide prepared in example 1, wherein fig. 1A is a photograph of molybdenum trioxide, which is light gray, and fig. 1B is a photograph of N-doped molybdenum trioxide prepared in example 1, which is changed to dark gray powder, and the success of N-doping can be primarily judged by a simple color change (deepening).
FIG. 2 is a SEM image and EDX image of N-doped molybdenum trioxide obtained in example 1, wherein FIG. 2 (a) is a SEM image of N-doped molybdenum trioxide obtained in example 1, and FIG. 2 (b) is an EDX image 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, illustrating that N element is successfully doped into MoO 3 A surface.
Fig. 3 shows the results of testing the N-doped content of the N-doped molybdenum trioxide prepared in examples 1-3, which shows that the higher the N content, the more the N plasma treatment time, indicating that the N element content is in a positive relationship with the treatment time.
FIG. 4 is MoO 3 And the conductivity test result of the N-doped molybdenum trioxide prepared in the embodiment 1 shows that the conductivity of the N-doped molybdenum trioxide is remarkably improved.
Pure MoO was tested in the 2-18GHz band using a network analyzer (VNA, N5245A, agilent, usa) 3 And the electromagnetic parameters of the N-doped molybdenum trioxide prepared in examples 1-3. The mass ratio of the test sample to the polyurethane is 6:4, and all the samples are pressed into a standard annular space (phi) by the same grinding tool in :3.04mm，Φ out 7.00 mm) to maintain geometric certainty. The thickness of all annulus is kept at 2.5mm. The Vienna ab initio software automatically outputs relevant electromagnetic parameters according to the conjugate gradient method algorithm. The test results are shown in FIGS. 5-8.
FIG. 5 is pure MoO 3 FIG. 6 is a graph showing the wave-absorbing properties of N-doped molybdenum trioxide obtained in example 17 is the wave-absorbing property of the N-doped molybdenum trioxide obtained in example 2, and fig. 8 is the wave-absorbing property of the N-doped molybdenum trioxide obtained in example 3. It can be seen that the higher the N content, the better the wave-absorbing performance as the N plasma treatment time is longer.
It will be appreciated by those skilled in the art that the present invention can be carried out in other embodiments without departing from the spirit or essential characteristics thereof. Accordingly, the above disclosed embodiments are illustrative in all respects, and not exclusive. All changes that come within the scope of the invention or equivalents thereto are intended to be embraced therein.
Claims (3)
1. The preparation method of the N-doped molybdenum trioxide is characterized in that molybdenum trioxide is placed in a reaction vessel, nitrogen plasma is introduced after vacuumizing, and the N-doped molybdenum trioxide is obtained after reaction; the reaction time is 0.5-5 minutes; the flow rate of the nitrogen plasma is 50sccm.
2. An N-doped molybdenum trioxide prepared by the method of claim 1.
3. Use of the N-doped molybdenum trioxide prepared by the method of claim 1 as an electromagnetic wave absorbing material.
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| CN202210976817.7A CN115196681B (en) | 2022-08-15 | 2022-08-15 | N-doped molybdenum trioxide and preparation method thereof |
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| CN202210976817.7A CN115196681B (en) | 2022-08-15 | 2022-08-15 | N-doped molybdenum trioxide and preparation method thereof |
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| Publication Number | Publication Date |
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| CN115196681A CN115196681A (en) | 2022-10-18 |
| CN115196681B true CN115196681B (en) | 2024-03-08 |
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Citations (2)
| 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 |
| CN114481188A (en) * | 2022-01-30 | 2022-05-13 | 吉林大学 | Preparation method of surface nitrogen-doped electrode |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010182637A (en) * | 2009-02-09 | 2010-08-19 | Fujifilm Corp | Organic electroluminescent element manufacturing method and organic electroluminescent element |
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- 2022-08-15 CN CN202210976817.7A patent/CN115196681B/en active Active
Patent Citations (2)
| 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 |
| CN114481188A (en) * | 2022-01-30 | 2022-05-13 | 吉林大学 | Preparation method of surface nitrogen-doped electrode |
Non-Patent Citations (3)
| Title |
|---|
| 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;Chao Lv et al.;《Applied Surface Science》;第1-11页 * |
| Nitrogen-Plasma-Treated Continuous Monolayer MoS2 for Improving Hydrogen Evolution Reaction;Anh Duc Nguyen et al.;《ACS Omega》;第21509−21515页 * |
| Superior lithium-ion storage of V-doped MoO 3 nanosheets via plasma evaporation;Ramon A et al.;《Electrochimica Acta》;第1-11页 * |
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