CN115259227B - Method for preparing room-temperature ferromagnetic molybdenum oxide nanosheets by using supercritical carbon dioxide - Google Patents
Method for preparing room-temperature ferromagnetic molybdenum oxide nanosheets by using supercritical carbon dioxide Download PDFInfo
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- CN115259227B CN115259227B CN202210909606.1A CN202210909606A CN115259227B CN 115259227 B CN115259227 B CN 115259227B CN 202210909606 A CN202210909606 A CN 202210909606A CN 115259227 B CN115259227 B CN 115259227B
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 42
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910000476 molybdenum oxide Inorganic materials 0.000 title claims abstract description 31
- 230000005294 ferromagnetic effect Effects 0.000 title claims abstract description 23
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 21
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 21
- 239000002135 nanosheet Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 15
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000002064 nanoplatelet Substances 0.000 claims description 6
- 230000007547 defect Effects 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000005291 magnetic effect Effects 0.000 abstract description 9
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000005307 ferromagnetism Effects 0.000 description 3
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical group [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C01G39/06—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention belongs to the technical field of preparation of ferromagnetic molybdenum oxide nano materials, and discloses a method for preparing room-temperature ferromagnetic molybdenum oxide nano sheets by using supercritical carbon dioxide. (1) Calcining molybdenum disulfide for 60-120 min at 200-500 ℃ in an air atmosphere; (2) Dispersing the powder obtained after calcination into 10-80 v% ethanol to obtain a dispersion liquid; transferring the dispersion liquid into a supercritical device, injecting carbon dioxide into the supercritical device, stirring and reacting for 3-6h under supercritical conditions, naturally cooling to room temperature, and then releasing pressure; and separating the system after supercritical treatment, collecting the separation liquid and drying to obtain the room-temperature ferromagnetic molybdenum oxide nano-sheet. According to the invention, firstly, molybdenum disulfide is calcined and oxidized at a high temperature in an air environment, and then, a local magnetic moment is introduced into a molybdenum oxide structure through a supercritical carbon dioxide means, so that the room-temperature ferromagnetic molybdenum oxide nanosheets are prepared, and compared with atomic doped magnetic molybdenum oxide obtained by a chemical vapor deposition method, the cost is lower, and the raw materials are easier to obtain.
Description
Technical Field
The invention belongs to the technical field of preparation of ferromagnetic molybdenum oxide nano materials, and particularly relates to a method for preparing room-temperature ferromagnetic molybdenum oxide nano sheets by using supercritical carbon dioxide.
Background
The ferromagnetic semiconductor can combine the advantages and performances of the semiconductor and the magnet, and is one of the candidate materials with the most application prospect in the spintronics. However, the low magnetic saturation strength and the low curie temperature limit the practical application, and the preparation of the ferromagnetic semiconductor with the curie temperature higher than room temperature and good air stability is always the direction of attention of researchers. The development of van der Waals two-dimensional ferromagnetic materials offers the hope of solving the problem, and such materials have layer-number dependent characteristics, are more sensitive to light and electrical stimulation, and have a large degree of controllable freedom. Thus, the design and construction of van der Waals two-dimensional materials with ferromagnetism will provide an important material basis for the promotion of the development of new spin electronics. The low-cost, polycrystalline-phase and high-activity molybdenum oxide is one of two-dimensional nano materials with ideal application prospects in the fields of energy conversion, optical devices, electrical devices and the like. Since bulk molybdenum oxide has paramagnetic properties, one can induce room temperature ferromagnetism by means of atomic doping, for example by doping with hydrogen, cobalt, nickel or tellurium atoms (nanoscales 2018, 10, 14100;Journal of Alloys and Compounds 2018, 741, 847;ACS Nano 2019, 13, 8717). In the preparation and application of room temperature ferromagnetic molybdenum oxide nano-materials, in order to reduce the production cost and achieve the purpose of green environmental protection, it is still a challenge to utilize simple and readily available raw materials and explore a simpler preparation technology of magnetic molybdenum oxide nano-materials.
Supercritical carbon dioxide is an environment-friendly reaction medium, and has wide application prospect in preparing two-dimensional layered materials due to special physical and chemical properties (such as non-polarity, low viscosity, high dispersibility and the like). To date, supercritical carbon dioxide has been reported to be useful in the exfoliation of non-layered materials to obtain two-dimensional ferromagnetic nanoplatelets (Nano Today 2021, 40, 101272;Angewandte Chemie International Edition 2022, 134, e 202117084). However, no document for preparing room-temperature ferromagnetic molybdenum oxide nano materials by using supercritical carbon dioxide is reported at present.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a method for preparing room-temperature ferromagnetic molybdenum oxide nano-sheets by using supercritical carbon dioxide.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for preparing room-temperature ferromagnetic molybdenum oxide nano-sheets by using supercritical carbon dioxide comprises the following steps:
(1) Calcining molybdenum disulfide for 60-120 min at 200-500 ℃ in an air atmosphere;
(2) Dispersing the powder obtained after calcination into 10-80 v% ethanol to obtain a dispersion liquid; transferring the dispersion liquid into a supercritical device, injecting carbon dioxide into the supercritical device, stirring and reacting for 3-6h under supercritical conditions, naturally cooling to room temperature, and then releasing pressure; and separating the system after supercritical treatment, collecting the separation liquid and drying to obtain the room-temperature ferromagnetic molybdenum oxide nano-sheet.
Preferably, in the step (2), the parameters of the supercritical condition are: the temperature is 40-100deg.C, and the pressure is 10-20Mpa.
Preferably, in the step (2), the concentration of the powder obtained after calcination in the dispersion is 50-20 mg/ml.
Preferably, in step (2), the separation is centrifugation.
In the present invention, molybdenum disulfide is commercially available molybdenum disulfide which has not undergone any modification treatment.
Compared with the prior art, the invention has the following advantages:
the invention provides a method for preparing room-temperature ferromagnetic molybdenum oxide nanosheets by using supercritical carbon dioxide, which comprises the steps of calcining and oxidizing molybdenum disulfide at high temperature in an air environment, and then introducing local magnetic moment into a molybdenum oxide structure by means of supercritical carbon dioxide (stress is generated due to the difference of adsorption strength of high-diffusivity carbon dioxide on different structures, so that defects are introduced); the method utilizes the original commercial molybdenum disulfide which is not modified to prepare the room-temperature ferromagnetic molybdenum oxide nanosheets, and compared with the atomic doped magnetic molybdenum oxide obtained by a chemical vapor deposition method, the method has the advantages that the cost is lower, and the raw materials are easier to obtain; from the whole preparation process, the method is simple and feasible, is environment-friendly and pollution-free, and has great application prospects in the fields of spin electronic devices, information storage and the like.
Drawings
Fig. 1 is a high resolution transmission chart (HRTEM) and a fast fourier transform chart (FFT, bottom right inset) of the molybdenum oxide nanoplatelets prepared in example 1 of the present invention.
FIG. 2 shows the hysteresis loop (M-H curve) of the molybdenum oxide nanoplatelets prepared in example 1 of the present invention at 300K.
FIG. 3 is a graph showing the field-cooled (FC) and zero-field-cooled (ZFC) M-T curves of the molybdenum oxide nanoplatelets prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail below for the purpose of making the present invention clearer and more specific. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A method for preparing room-temperature ferromagnetic molybdenum oxide nano-sheets by using supercritical carbon dioxide comprises the following steps:
(1) Calcining 100mg of commercially available molybdenum disulfide in a carbonization furnace for 90min in an air environment at 350 ℃;
(2) Dispersing all the powder obtained after calcining in the step (1) in 10ml of 45v% ethanol for 30min, transferring to a reaction kettle, injecting carbon dioxide into the reaction kettle to reach a supercritical state (14 mpa,80 ℃), reacting for 3h under magnetic stirring, and releasing carbon dioxide for pressure relief; and centrifuging for 15min at 6000rpm by using a centrifuge, taking supernatant and drying in a vacuum oven at 60 ℃ to obtain the molybdenum oxide nano-sheets.
The obtained molybdenum oxide nano-sheet is characterized by a transmission electron microscope on a carbon support film, wherein the HRTEM and a fast Fourier transform (FFT, lower right corner inset) chart are shown in figure 1, the FFT shows that the atomic arrangement lattice accords with the orthorhombic phase of molybdenum trioxide, the HRTEM shows that the lattice spacing is 0.38nm, and the intermittent atomic arrangement in the chart shows that the structure contains a large number of defects.
The resulting molybdenum oxide nanoplatelets were characterized for magnetic properties using a magnetic measurement system-MPMS 3, which has hysteresis loops (M-H curves) and Field Cooling (FC) and Zero Field Cooling (ZFC) M-T curves at 300K temperature, see fig. 2 and 3. It can be seen that: the M-H curve has ferromagnetic response signals under the condition of 300K, the magnetic saturation intensity is 0.01emu/g, and meanwhile, the Field Cooling (FC) and Zero Field Cooling (ZFC) curves in the M-T curve are not overlapped at 300K, which shows that the Curie temperature of the molybdenum oxide nano-sheet is higher than the room temperature, and the product has room temperature ferromagnetism.
Claims (2)
1. A method for preparing room-temperature ferromagnetic molybdenum oxide nano-sheets by using supercritical carbon dioxide is characterized by comprising the following steps:
(1) Calcining molybdenum disulfide for 60-120 min at 200-500 ℃ in an air atmosphere; the molybdenum disulfide is commercially available molybdenum disulfide which is not subjected to any modification treatment;
(2) Dispersing the powder obtained after calcining every 100mg of molybdenum disulfide in the step (1) into 10ml of 10-80 v% ethanol to obtain a dispersion liquid; transferring the dispersion liquid into a supercritical device, injecting carbon dioxide into the supercritical device, stirring and reacting for 3-6h under the supercritical condition of the temperature of 80 ℃ and the pressure of 14Mpa, naturally cooling to room temperature, and then releasing pressure; separating the system after supercritical treatment, collecting the separating liquid and drying to obtain the room-temperature ferromagnetic molybdenum oxide nano-sheet which is of an orthorhombic lattice structure containing defects.
2. The method for preparing room temperature ferromagnetic molybdenum oxide nanoplatelets by supercritical carbon dioxide according to claim 1, wherein: in step (2), the separation is a centrifugal separation.
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| CN107601566A (en) * | 2017-11-07 | 2018-01-19 | 郑州大学 | A kind of method that the amorphous oxide molybdenum quantum dot with LSPR effects is prepared using body molybdenum disulfide |
| CN110015692A (en) * | 2019-01-22 | 2019-07-16 | 复旦大学 | A kind of preparation method of molybdenum trioxide quantum dot |
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- 2022-09-15 CN CN202210909606.1A patent/CN115259227B/en active Active
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