CN108046250A - A kind of preparation method of two-dimensional material - Google Patents
A kind of preparation method of two-dimensional material Download PDFInfo
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- CN108046250A CN108046250A CN201711401284.5A CN201711401284A CN108046250A CN 108046250 A CN108046250 A CN 108046250A CN 201711401284 A CN201711401284 A CN 201711401284A CN 108046250 A CN108046250 A CN 108046250A
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- dimensional material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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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
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/003—Phosphorus
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- 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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- 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
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to a kind of universality methods that atom level two-dimensional material liquid phase microwave is removed, and belong to the preparation method technical field of two-dimensional material.Body phase material is freezed 30 60 minutes in liquid nitrogen, microwave flows back 10 20 minutes after adding in organic solvent, is centrifugally separating to obtain atom level two-dimensional material dispersion liquid, and atom level two-dimensional material powder is can obtain after freeze-drying.Body phase material is directly removed into large-sized atom level two-dimensional material by the present invention using microwave irradiation technology.This method is simple for process, with short production cycle, at low cost, and universality is strong, is suitable for industrial mass production, has very high application prospect and use value.
Description
Technical field
The present invention relates to a kind of universality methods that atom level two-dimensional material liquid phase microwave is removed, and belong to the system of two-dimensional material
Preparation Method technical field.
Background technology
Ultra-thin two-dimension (2D) nano material is a kind of emerging nano material, it has membrane structure, and lateral dimension is more than
100nm or up to several microns of even biggers, but thickness only has single or several atomic layers thicks (usually less than 5nm).First, super
Thin region, particularly in individual layer two-dimension nano materials, electronics can only carry out free fortune on the non-nanosize of two dimensions
It is dynamic, unique characteristic electron is made it have, this is ideal for condensed state physics and electronics/photoelectronic basic research
's；Secondly, mechanical strength, flexibility and the optical transparence that covalent bond and the thickness of atom level make its excellent in strong plane,
Possess huge potentiality in device generations；3rd, the thickness of atom level is kept while lateral dimension is bigger, is imparted
The specific surface area of their superelevation, this has very strong attraction for being catalyzed with building for surface and interfaces engineering strategy such as capacitors
Power.Finally, due to the high exposure rate of surface atom, makes surface modification or functionalization, element doping, defect, strain or phase work
Journey more easily adjusts material character and function.
At present, two-dimensional material mainly has preparation method from top to bottom and from bottom to top.Because block materials are readily synthesized,
The advantages that cost is very low and handling strong, top-down liquid phase stripping method have become the common preparation method of two-dimensional material.Liquid
It mutually removes in the method for preparing two-dimensional material, mainly there is the stripping of ion insertion auxiliary liquid, mechanical force auxiliary liquid to remove, ion
Auxiliary liquid is exchanged to remove, aoxidize auxiliary liquid stripping and selective etch liquid stripping method etc..But yield and quality, quantity with
And yield is all from industrializing and commercially produced very long a distance.
Microwave refers to the electromagnetic wave that frequency is 300MHz~300GHz, i.e. wavelength between 1mm~1m, energy 1.99 ×
l0-25-1.99×10-21Electromagnetic wave between J, due to its strong penetrating power, long wavelength and high-frequency, be otherwise known as hyperfrequency electromagnetism
Ripple.The polar solvent molecule vibrations per second that about 2,400,000,005 thousands of times occur that microwave can make dielectric dissipation factor big,
So that molecule is heated rapidly gasification.At present, using this characteristic, it is applied to liquid phase and removes field in the world not yet
It appears in the newspapers.
The content of the invention
The purpose of the present invention primarily directed to the deficiencies in the prior art, provide it is a kind of it is environmental-friendly, simple for process, be suitable for
Industrial production and environmental-friendly atom level two-dimensional material microwave liquid phase stripping means.Atom level two dimension material prepared by the present invention
Material has ultrathin and large-size no more than 5nm.
For achieving the above object, mainly using following technical scheme：
A kind of atom level two-dimensional material microwave liquid phase stripping means, including step：
(1) body phase material that will be synthesized or buy freezing processing in liquid nitrogen；
(2) solid after freezing is disperseed in organic solvent；
(3) above-mentioned dispersion liquid condensing reflux in microwave reactor after being cooled to room temperature, is centrifugally separating to obtain atomic level
Two-dimensional material dispersion liquid；
(4) it is freeze-dried to obtain atomic level two-dimensional material powder.
Wherein, the body phase material described in step (1) is carbonitride (g-C3N4), boron nitride (BN), graphite (C) or black phosphorus
(BP)；The body phase material quality is 50-150mg, and the time of the freezing is 30-60min.
Wherein, the organic solvent is isopropanol (IPA), nitrogen dimethylformamide (DMF) or N-Methyl pyrrolidone
(NMP).In the industrial production, under cost and environmental protection consider, preferable organic solvent is isopropanol (IPA).
Further, in step (2), the organic solvent is the organic solvent after being diluted with water, organic solvent and water
Volume ratio is 0.5-1:1, the dosage of the organic solvent is 30-50mL.
Preferably, in step (3), the microwave reactor power is 500-700W, and the time of microwave reflux is
10-20min, the rotating speed of the centrifugation is 500-5000 revs/min, and the centrifugation time is 3-5min.
It is highly preferred that in step (4), the temperature of freeze-drying is subzero 60-80 DEG C.
Two-dimensional ultrathin carbonitride (2D g-C have been prepared in experimental method of the present invention3N4), two-dimensional ultrathin boron nitride
(2D BN), graphene (G) and black phosphorus alkene (2D BP) etc..
The beneficial effects of the present invention are：
(1) present invention has very strong universality, simple for process, low energy, environment friend using microwave liquid phase stripping method
Well, cost is relatively low, suitable for industrial mass production, has very high use value.
(2) two-dimensional material prepared by the present invention has ultrathin (being less than 5nm), possesses very in catalysis and capacitance field
High application prospect.
Description of the drawings
Fig. 1 is the 2D g-C that microwave liquid phase is removed in embodiment 13N4Atomic force microscope (AFM) figure.
Fig. 2 is atomic force microscope (AFM) figure of the 2D BN that microwave liquid phase is removed in embodiment 2.
Fig. 3 is atomic force microscope (AFM) figure of the graphene that microwave liquid phase is removed in embodiment 3.
Specific embodiment
The present invention is explained in detail rather than limited to the present invention below in conjunction with specific embodiment.
In embodiment, material used, reagent etc. unless otherwise instructed, are commercially available.
In embodiment, unless otherwise instructed, technological means used is this field conventional technology.
Embodiment 1
The g-C of body phase is obtained by calcining melamine 4h at 550 DEG C3N4.Weigh the g-C of 50mg body phases3N4In centrifugation
Guan Zhong adds in 40mL liquid nitrogen, and after keeping 1h, the volume ratio for being dispersed in 50mL and water is 1:In 1 IPA solution, (power is microwave
650W) flow back 20min.Above-mentioned solution centrifuges 3min, isolated 2D g-C under 3000 revs/min3N4Dispersion liquid.It is subzero
70 DEG C of freeze-dryings obtain 2D g-C3N4Powder.It is dropped in after above-mentioned dispersion liquid is diluted on mica sheet, carries out atomic force microscope
(AFM) characterize, lamellar spacing is about 1nm.
Embodiment 2
Weigh 60mg purchase body phase BN in centrifuge tube, add in 45mL liquid nitrogen, keep 0.5h after, be dispersed in 40mL with
The volume ratio of water is 0.5:In 1 IPA solution, microwave (power 700W) reflux 10min.Above-mentioned solution is at 5000 revs/min
Lower centrifugation 5min, the dispersion liquid of isolated 2D BN.Subzero 70 DEG C of freeze-dryings obtain 2D BN powders.Above-mentioned dispersion liquid is dilute
It is dropped in after releasing on mica sheet, carries out atomic force microscope (AFM) and characterize, lamellar spacing is about 3nm.
Embodiment 3
Weigh 50mg purchase body phase graphite in centrifuge tube, add in 40mL liquid nitrogen, keep 1h after, be dispersed in 50mL with
The volume ratio of water is 1:In 1 IPA solution, microwave (power 700W) reflux 15min.Above-mentioned solution is under 1500 revs/min
Centrifuge 3min, the dispersion liquid of isolated graphene.Subzero 80 DEG C of freeze-dryings obtain graphene powder.Above-mentioned dispersion liquid is dilute
It is dropped in after releasing on mica sheet, carries out atomic force microscope (AFM) and characterize, lamellar spacing is about 4.5nm.
Embodiment 4
Weigh 50mg purchase body phase black phosphorus in centrifuge tube, add in 30mL liquid nitrogen, keep 1h after, be dispersed in 45mL with
The volume ratio of water is 0.8:In 1 IPA solution, microwave (power 700W) reflux 20min.Above-mentioned solution is at 3000 revs/min
Lower centrifugation 5min, the dispersion liquid of isolated black phosphorus alkene.Subzero 80 DEG C of freeze-dryings obtain black phosphorus alkene powder.By above-mentioned dispersion liquid
It is dropped in after dilution on mica sheet, carries out atomic force microscope (AFM) and characterize, lamellar spacing is about 2.5nm.
Above disclosed is only the preferred embodiments of the present invention, is not departing from the situation of above method thought of the present invention
Under, the various replacements or improvement made according to ordinary skill knowledge and customary means should be included in the guarantor of the present invention
Within the scope of shield.
Claims (7)
1. a kind of preparation method of two-dimensional material, which is characterized in that be as follows：
(1) body phase material that will be synthesized or buy freezing processing in liquid nitrogen；
(2) solid after freezing is disperseed in organic solvent, to obtain dispersion liquid；
(3) above-mentioned dispersion liquid condensing reflux in microwave reactor after being cooled to room temperature, is centrifugally separating to obtain atomic level two dimension
Material dispersion liquid；
(4) it is freeze-dried to obtain atomic level two-dimensional material powder.
2. a kind of preparation method of two-dimensional material as described in claim 1, which is characterized in that in step (1), the body phase
Material is carbonitride (g-C3N4), boron nitride (BN), graphite (C) or black phosphorus (BP)；The body phase material quality is 50-150mg,
The time of the freezing is 30-60min.
3. a kind of preparation method of two-dimensional material as described in claim 1, which is characterized in that in step (2), described is organic
Solvent is isopropanol (IPA), nitrogen dimethylformamide (DMF) or N-Methyl pyrrolidone (NMP).
4. a kind of preparation method of two-dimensional material as claimed in claim 3, which is characterized in that organic solvent is isopropanol
(IPA)。
5. a kind of preparation method of two-dimensional material as described in claim 1, which is characterized in that in step (2), in step (2),
The organic solvent, which is adopted, to be diluted with water, and the volume ratio of organic solvent and water is 0.5-1:1, the dosage of the organic solvent after dilution is equal
For 30-50mL.
6. a kind of preparation method of two-dimensional material as described in claim 1, which is characterized in that in step (3), the microwave
Reactor power is 500-700W, and the time of the microwave reflux is 10-20min；The rotating speed of the centrifugation is 500-
5000 revs/min, the centrifugation time is 3-5min.
7. a kind of preparation method of two-dimensional material as described in claim 1, which is characterized in that in step (4), freeze-drying
Temperature is subzero 60-80 DEG C.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467021A (en) * | 2018-04-26 | 2018-08-31 | 昆明理工大学 | A kind of method that liquid nitrogen stripping black phosphorus prepares nanometer black phosphorus |
| CN108706641A (en) * | 2018-07-23 | 2018-10-26 | 江苏大学 | A kind of preparation method of ultra-thin sulfide nanometer sheet |
| CN109046329A (en) * | 2018-07-04 | 2018-12-21 | 江苏大学 | A kind of preparation method of atomic level two dimensional oxidation platinum quantum dot |
| CN109052347A (en) * | 2018-08-22 | 2018-12-21 | 昆明理工大学 | A kind of method that electric field cooperates with up-stripping black phosphorus preparation nanometer black phosphorus with microwave field |
| CN110627028A (en) * | 2019-09-17 | 2019-12-31 | 江苏大学 | High-stability two-dimensional black phosphorus alkene, and preparation method and application thereof |
| CN111394153A (en) * | 2020-04-08 | 2020-07-10 | 扬州大学 | Hexagonal boron nitride nanosheet base lubricating grease and preparation method thereof |
| CN111807335A (en) * | 2020-07-08 | 2020-10-23 | 陕西科技大学 | Microwave-assisted method for preparing boron nitride nanosheets |
| CN112717973A (en) * | 2020-11-16 | 2021-04-30 | 中北大学 | Preparation of rod-like g-C by microwave hydrothermal method3N4Method and application of nanosheet |
| CN113527998A (en) * | 2021-08-12 | 2021-10-22 | 青岛金芳华新型建材科技有限公司 | Flame-retardant polyurethane waterproof coating and preparation method thereof |
| WO2024047822A1 (en) * | 2022-08-31 | 2024-03-07 | 国立大学法人東北大学 | LAYERED MATERIAL NANOSHEET PRODUCTION METHOD, LAYERED MoS2 NANOSHEET, AND LAYERED GRAPHITE NANOSHEET |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467021A (en) * | 2018-04-26 | 2018-08-31 | 昆明理工大学 | A kind of method that liquid nitrogen stripping black phosphorus prepares nanometer black phosphorus |
| CN109046329A (en) * | 2018-07-04 | 2018-12-21 | 江苏大学 | A kind of preparation method of atomic level two dimensional oxidation platinum quantum dot |
| CN108706641A (en) * | 2018-07-23 | 2018-10-26 | 江苏大学 | A kind of preparation method of ultra-thin sulfide nanometer sheet |
| CN109052347A (en) * | 2018-08-22 | 2018-12-21 | 昆明理工大学 | A kind of method that electric field cooperates with up-stripping black phosphorus preparation nanometer black phosphorus with microwave field |
| CN110627028A (en) * | 2019-09-17 | 2019-12-31 | 江苏大学 | High-stability two-dimensional black phosphorus alkene, and preparation method and application thereof |
| CN111394153A (en) * | 2020-04-08 | 2020-07-10 | 扬州大学 | Hexagonal boron nitride nanosheet base lubricating grease and preparation method thereof |
| CN111394153B (en) * | 2020-04-08 | 2021-11-09 | 扬州大学 | Hexagonal boron nitride nanosheet base lubricating grease and preparation method thereof |
| CN111807335A (en) * | 2020-07-08 | 2020-10-23 | 陕西科技大学 | Microwave-assisted method for preparing boron nitride nanosheets |
| CN111807335B (en) * | 2020-07-08 | 2023-01-31 | 陕西科技大学 | Microwave-assisted method for preparing boron nitride nanosheets |
| CN112717973A (en) * | 2020-11-16 | 2021-04-30 | 中北大学 | Preparation of rod-like g-C by microwave hydrothermal method3N4Method and application of nanosheet |
| CN113527998A (en) * | 2021-08-12 | 2021-10-22 | 青岛金芳华新型建材科技有限公司 | Flame-retardant polyurethane waterproof coating and preparation method thereof |
| WO2024047822A1 (en) * | 2022-08-31 | 2024-03-07 | 国立大学法人東北大学 | LAYERED MATERIAL NANOSHEET PRODUCTION METHOD, LAYERED MoS2 NANOSHEET, AND LAYERED GRAPHITE NANOSHEET |
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