CN113333736A - Microwave stripping-based stibene and preparation method thereof - Google Patents
Microwave stripping-based stibene and preparation method thereof Download PDFInfo
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- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 27
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
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- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 9
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- 239000006228 supernatant Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 16
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- 239000010410 layer Substances 0.000 description 16
- 239000002135 nanosheet Substances 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000001878 scanning electron micrograph Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
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- 238000004299 exfoliation Methods 0.000 description 4
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- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ROUIDRHELGULJS-UHFFFAOYSA-N bis(selanylidene)tungsten Chemical compound [Se]=[W]=[Se] ROUIDRHELGULJS-UHFFFAOYSA-N 0.000 description 1
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- MHWZQNGIEIYAQJ-UHFFFAOYSA-N molybdenum diselenide Chemical compound [Se]=[Mo]=[Se] MHWZQNGIEIYAQJ-UHFFFAOYSA-N 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
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Abstract
The invention provides antimonene based on microwave stripping and a preparation method thereof, wherein the preparation method comprises the following steps: ball-milling the metal antimony crystals to obtain micron-sized antimony powder; mixing the micron-sized antimony powder with an isopropanol solution, stirring, and performing ultrasonic dispersion to obtain a mixed solution; and carrying out microwave treatment on the mixed solution, and then centrifuging, washing and drying the supernatant to obtain the antimonene based on microwave-assisted stripping. The invention adopts microwave-assisted liquid phase rapid stripping technology to prepare the high-quality two-dimensional few-layer stibene material with adjustable layers, modifiable surface and stable property, and has the advantages of simple process operation, short stripping time, low energy consumption and contribution to market popularization of the product.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to antimonene based on microwave-assisted stripping and a preparation method thereof.
Background
In recent years, two-dimensional semiconductor materials (such as molybdenum disulfide, molybdenum diselenide, tungsten disulfide, tungsten diselenide, and the like, which are typical two-dimensional semiconductor materials) have attracted considerable attention by researchers due to their unique properties in electrical, optical, chemical, and the like aspects. When reduced to a monoatomic layer, metallic antimony exhibits semiconductor material properties, becoming a graphene-like material, with its indirect bandgap converted to a direct bandgap under very little stress; meanwhile, the few-layer two-dimensional antimonene also has the energy band gap width of 2.28 eV; in addition, such two-dimensional materials have good stability.
In the existing research, the stibene material is prepared by methods such as mechanical stripping, liquid phase stripping, vapor phase growth and the like, but the mechanical stripping effect is not ideal, the liquid phase ultrasonic stripping method needs a large amount of time, and after the ultrasonic stripping is carried out for a long time, the obtained stibene can face the problems of transverse area reduction and abnormal structure defects.
How to rapidly and efficiently prepare the stibene nanometer material with excellent properties, establish surface interface property regulation science and effectively represent a novel two-dimensional material is a problem to be solved urgently at present.
Disclosure of Invention
In view of the above, the present invention is directed to provide an antimonene based on microwave-assisted stripping and a preparation method thereof, so as to solve the problems that the traditional mechanical stripping method is not ideal in effect, a large amount of time is consumed in a liquid-phase ultrasonic stripping method, and the obtained antimonene is exposed to a reduction in lateral area and abnormal structural defects after ultrasonic stripping is performed for a long time.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of antimonene based on microwave-assisted stripping comprises the following steps:
s1, carrying out ball milling on the metal antimony crystals to obtain micron-sized antimony powder;
s2, mixing the micron-sized antimony powder with an isopropanol solution, stirring, and performing ultrasonic dispersion to obtain a mixed solution;
and S3, performing microwave treatment on the mixed solution, and then centrifuging, washing and drying the supernatant to obtain the antimonene based on microwave-assisted stripping.
Optionally, in S1, the rotation speed of the ball milling is 2800-.
Optionally, in S2, the mass-to-volume ratio of the micron-sized antimony powder to the isopropanol solution is (1:4) mg/ml.
Optionally, in S2, the stirring time is 25-35 min.
Optionally, in S2, the time for ultrasonic dispersion is 0.5-1.5 h.
Optionally, in S3, the microwave treatment power is 600W, the time is 3-15min, and the temperature is 80-130 ℃.
The invention also aims to provide the antimonene based on microwave-assisted stripping, which is prepared by adopting the preparation method of the antimonene based on microwave-assisted stripping.
Optionally, the microwave-assisted exfoliation based antimonene is a two-dimensional layered material consisting of fused, wrinkled and six-membered ring antimony.
Optionally, the number of layers of stibene is 5-100.
Optionally, the thickness of the stibene is 10nm to 100 nm.
Compared with the prior art, the antimonene based on microwave-assisted stripping and the preparation method thereof have the following advantages:
(1) the method adopts a microwave-assisted liquid phase rapid stripping technology, is based on a microwave dielectric selective absorption heating principle, prepares the antimony nanosheet stacking material with an MXene-like structure by regulating and controlling parameters such as a wave-absorbing solvent, microwave power, stripping time and the like, and performs interlayer regulation and control on MXene-like antimony by combining strategies such as ion embedding secondary stripping and the like again, thereby preparing the antimonene based on microwave-assisted stripping, which has adjustable interlayers, modifiable surface and stable property.
(2) The invention has simple preparation process operation, short stripping time and lower energy consumption, and the product is beneficial to market popularization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, a brief description will be given below to the drawings required for the description of the embodiments or the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is an SEM image of micron-sized antimony powder according to example 1 of the present invention;
FIG. 2 is an SEM image of antimonene based on microwave-assisted stripping as described in example 1 of the present invention;
FIG. 3 is an SEM image of antimonene based on microwave-assisted stripping as described in example 2 of the present invention;
FIG. 4 is an SEM image of antimonene based on microwave-assisted stripping as described in example 3 of the invention;
FIG. 5 is an SEM image of antimonene based on microwave-assisted stripping as described in example 4 of the invention;
FIG. 6 is an SEM image of antimonene based on microwave-assisted stripping as described in example 5 of the invention.
Detailed Description
The principles and features of this invention are described below in conjunction with specific embodiments, the examples given are intended to illustrate the invention and are not intended to limit the scope of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The terms "comprising," "including," "containing," and "having" are intended to be inclusive, i.e., that additional steps and other ingredients may be added without affecting the result.
The embodiment of the invention provides a preparation method of stibene based on microwave-assisted stripping, which comprises the following steps:
s1, carrying out ball milling on the metal antimony crystals to obtain micron-sized antimony powder;
s2, mixing the micron-sized antimony powder with an isopropanol solution, stirring, and performing ultrasonic dispersion to obtain a mixed solution;
and S3, performing microwave treatment on the mixed solution, and then centrifuging, washing and drying the supernatant to obtain the antimonene stripped under the assistance of microwave.
It can be understood that the microwave-assisted liquid phase stripping technology opens up a way for the preparation of the novel two-dimensional material stibene, and the advantages of using the microwave-assisted liquid phase stripping are as follows: microwave selective heating, reduced reaction time, increased product yield and improved product purity. Compared with the traditional liquid phase heating mode, the temperature outside the container is generally higher than that of the reaction system, so that the reaction system has an unbalanced temperature gradient to cause the heterogeneous nucleation problem. The microwave heating mode is realized by means of the directional arrangement of dipoles under an external electromagnetic field, the target temperature can be reached within several seconds basically, and great advantages are shown in efficiently stripping high-quality antimonene materials.
According to the embodiment of the invention, a microwave-assisted liquid phase rapid stripping technology is adopted, based on a microwave dielectric selective absorption heating principle, parameters such as a wave-absorbing solvent, microwave power and stripping time are regulated and controlled to prepare the MXene-like structure antimony nanosheet stacking material, and then strategies such as ion embedding secondary stripping are combined to carry out interlayer regulation and control on MXene-like antimony, so that the high-quality antimonene material which is controllable between layers, modifiable in surface and stable in property and based on microwave-assisted stripping is prepared.
Specifically, in step S1, the rotation speed of ball milling is 2800-.
In step S2, the mass-to-volume ratio of the micron-sized antimony powder to the isopropanol solution is 1 (3-5) mg/ml, preferably 1:4mg/ml, that is, 40mg of antimony powder after ball milling is mixed with 160ml of isopropanol solution.
Further, in step S2, the stirring time is 25-35min, and the ultrasonic dispersion time is 0.5-1.5 h. Preferably, the stirring time in the embodiment of the invention is 30min, and the ultrasonic dispersion time is 1 h.
In step S3, the microwave treatment power is 600W, the time is 3-15min, the temperature is 80-130 ℃, and the preferred temperature is 100 ℃.
The preparation method provided by the embodiment of the invention has the advantages that the antimonene with few layers is obtained by a microwave-assisted liquid phase rapid stripping method, the preparation process is simple to operate, the energy consumption is low, the stripping time is short, and the obtained two-dimensional antimonene material with few layers is pure and free of impurities; meanwhile, the prepared microwave-assisted stripping-based antimonene material has controllable layer number and stable property, and further can obtain a key preparation technology of a two-dimensional antimonene material with an adjustable structure and a modified surface interface.
The invention further provides antimonene based on microwave-assisted stripping, and the antimonene is prepared by adopting the preparation method of the antimonene based on microwave-assisted stripping.
The antimonene based on microwave-assisted stripping is a two-dimensional layered material consisting of fusion, folding and six-membered ring antimony. The number of layers of the stibene is 5-100, and the thickness of the stibene is 10nm-100 nm.
According to the antimonene based on microwave-assisted stripping, the antimonene sheets are stacked to form a few-layer two-dimensional plane structure, the antimonene sheet is pure, free of impurities and stable in property, and a typical two-dimensional structure is presented.
Due to the advantages, the antimonene based on microwave-assisted stripping provided by the invention can be used for aspects such as a crystal triode with ultrahigh switching ratio, a novel two-dimensional crystal-carried micro-nano mechanical sensor, an electrochemical energy storage device and the like.
On the basis of the above examples, the invention is further illustrated below in connection with a preparation method of antimonene based on microwave-assisted stripping. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer. Unless otherwise indicated, percentages and parts are by mass.
Example 1
The embodiment provides a preparation method of antimonene based on microwave-assisted stripping, which comprises the following steps:
1) 2g of metal antimony crystals are placed in a stainless steel ball milling tank, the rotating speed in the ball milling process is 3000r/min, and the ball milling time is 2 hours, so that micron-sized antimony powder is obtained;
2) mixing the ball-milled 40mg micron-sized antimony powder with 160ml isopropanol solution, stirring for 30 minutes at normal temperature, and performing ultrasonic treatment for 1 hour to obtain a mixed solution;
3) putting the mixed solution into a microwave reaction kettle, setting the microwave power at 600W, heating to 100 ℃ at the heating rate of 10 ℃/min, and carrying out microwave for 7 minutes; standing the liquid after the microwave treatment, taking supernatant, centrifuging, washing with ethanol, and drying to finally obtain the antimonene stripped based on microwave assistance.
The microwave assisted exfoliation based antimonenes prepared in example 1 were used as an example for testing by Scanning Electron Microscope (SEM) imaging.
Fig. 1 is an SEM image of the micron-sized antimony powder prepared in example 1, and it can be seen from fig. 1 that the ball-milled antimony powder shows relatively uniform particle size distribution, the particle size is in the micron level, no significant agglomeration phenomenon occurs after ball milling, and it can be seen that the layered stacking structure of the antimony nanosheets is well preserved, which indicates that the layered structure of the antimony powder is not damaged during ball milling, and provides a basis for obtaining antimonene through later microwave liquid phase stripping.
Fig. 2 is an SEM image of the antimonene prepared in example 1 and based on microwave-assisted stripping, and it can be seen from fig. 2 that after microwave liquid phase stripping, the framework of the "accordion-like" antimony has a uniform thickness (about 10 nm), and exhibits a typical two-dimensional structure, that is, an antimony nanosheet stacking material with an MXene-like structure is prepared. The prepared antimonene based on microwave-assisted stripping has a large transverse area, obvious abnormal structure defects can be observed, and meanwhile, the distance between antimonene layers is about 50nm, which shows the effectiveness of microwave stripping. This also illustrates the advantage of using microwaves to assist liquid phase stripping.
Example 2:
the embodiment provides a preparation method of antimonene based on microwave-assisted stripping, which comprises the following steps:
1) 2g of metal antimony crystals are placed in a stainless steel ball milling tank, the rotating speed in the ball milling process is 3000r/min, and the ball milling time is 2 hours, so that micron-sized antimony powder is obtained;
2) mixing the ball-milled 40mg micron-sized antimony powder with 160ml isopropanol solution, stirring for 30 minutes at normal temperature, and performing ultrasonic treatment for 1 hour to obtain a mixed solution;
3) putting the mixed solution into a microwave reaction kettle, setting the microwave power at 600W, heating to 100 ℃ at the heating rate of 10 ℃/min, and carrying out microwave for 3 minutes; standing the liquid after the microwave treatment, taking supernatant, centrifuging, washing with ethanol, and drying to finally obtain the antimonene stripped based on microwave assistance.
FIG. 3 is an SEM image of the antimonene prepared in example 2 and based on microwave-assisted stripping, and it can be seen from FIG. 3 that after 3min of microwave liquid phase stripping, the stacking of the antimonene nanosheets is obvious, the stacking thickness is 5-10um, the interlayer distance of the antimonene is small, and a poor stripping effect is shown. Analysis shows that the reduction of the microwave treatment time leads to the failure of obtaining enough energy to overcome the interlayer acting force and influences the stripping of the antimony nanosheets.
Example 3:
the embodiment provides a preparation method of antimonene based on microwave-assisted stripping, which comprises the following steps:
1) 2g of metal antimony crystals are placed in a stainless steel ball milling tank, the rotating speed in the ball milling process is 3000r/min, and the ball milling time is 2 hours, so that micron-sized antimony powder is obtained;
2) mixing the ball-milled 40mg micron-sized antimony powder with 160ml isopropanol solution, stirring for 30 minutes at normal temperature, and performing ultrasonic treatment for 1 hour to obtain a mixed solution;
3) putting the mixed solution into a microwave reaction kettle, setting the microwave power at 600W, heating to 100 ℃ at the heating rate of 10 ℃/min, and carrying out microwave for 30 minutes; standing the liquid after the microwave treatment, taking supernatant, centrifuging, washing with ethanol, and drying to finally obtain the antimonene stripped based on microwave assistance.
FIG. 4 is an SEM image of the antimonene prepared in example 3 and based on microwave-assisted stripping, and it can be seen from FIG. 4 that after 30min of microwave liquid-phase stripping, the number of layers of the layered stacking structure of the antimoney nanosheets is reduced, but the transverse area is reduced, the transverse length of the antimoney particles is 2-50um, and the transverse integrity of the few-layer antimoney is damaged. Through analysis, the increase of the microwave treatment time can be presumed, the antimony nanosheets are stripped by enough energy, and in the microwave treatment process, the complete antimony nanosheets are cracked, so that the transverse apparent area of the few-layer antimonene is influenced.
Example 4:
the embodiment provides a preparation method of antimonene based on microwave-assisted stripping, which comprises the following steps:
1) mixing 40mg of antimony powder which is not subjected to ball milling with 160ml of isopropanol solution, stirring for 30 minutes at normal temperature, and performing ultrasonic treatment for 1 hour to obtain a mixed solution;
2) putting the mixed solution into a microwave reaction kettle, setting the microwave power at 600W, heating to 100 ℃ at the heating rate of 10 ℃/min, and carrying out microwave for 7 minutes; standing the liquid after the microwave treatment, taking supernatant, centrifuging, washing with ethanol, and drying to finally obtain the antimonene stripped based on microwave assistance.
Fig. 5 is an SEM image of the microwave-assisted exfoliation-based antimonene prepared in example 4, and it can be seen from fig. 5 that, in the antimony powder without ball milling treatment, after the microwave liquid phase exfoliation treatment, the antimony nanosheets have no obvious change, showing that the antimony nanosheets are relatively tightly stacked, no obvious few layers of antimonene exist, and the antimony particles have a transverse length of 50-100 um. Through analysis, the particle size of the antimony powder can be presumed to have obvious influence on a product stripped by a microwave liquid phase, the particle size is larger, and the energy provided by the microwave is not enough to enable larger antimony nanosheets to overcome interlayer acting force to separate, so that the stripping effect is not obvious.
Example 5:
the embodiment provides a preparation method of antimonene based on microwave-assisted stripping, which comprises the following steps:
1) 2g of metal antimony crystals are placed in a stainless steel ball milling tank, the rotating speed in the ball milling process is 3000r/min, and the ball milling time is 2 hours, so that micron-sized antimony powder is obtained;
2) mixing the ball-milled 40mg micron-sized antimony powder with 160ml of ethanol solution, stirring for 30 minutes at normal temperature, and performing ultrasonic treatment for 1 hour to obtain a mixed solution;
3) putting the mixed solution into a microwave reaction kettle, setting the microwave power at 600W, heating to 100 ℃ at the heating rate of 10 ℃/min, and carrying out microwave for 30 minutes; standing the liquid after the microwave treatment, taking supernatant, centrifuging, washing with ethanol, and drying to finally obtain the antimonene stripped based on microwave assistance.
Fig. 6 is an SEM image of the microwave-assisted stripping-based antimonene prepared in example 5, and it can be seen from fig. 6 that, after the microwave liquid-phase stripping treatment, with ethanol as the wave-absorbing solvent and the stripping liquid, the antimonene nanosheets do not change significantly, showing that the antimonene nanosheets are relatively densely stacked, and there is no significant few layer of antimonene, and the transverse length of the antimonene particles is 50-100 um. Through analysis, the number of dipoles of different solvents is different, the heating speed and energy transfer caused by the directional arrangement under an external electromagnetic field are different, and meanwhile, the size of solvent molecules influences the embedding of the solvent molecules between the antimony nanosheets, so that the stripping effect is influenced.
In conclusion, the invention utilizes a microwave-assisted liquid phase rapid stripping method, and can obtain the antimonene based on microwave-assisted stripping, which has adjustable layers, modifiable surface and stable property, by adjusting and controlling parameters such as wave-absorbing solvent, microwave power, stripping time and the like.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. The preparation method of the antimonene based on microwave-assisted stripping is characterized by comprising the following steps:
s1, carrying out ball milling on the metal antimony crystals to obtain micron-sized antimony powder;
s2, mixing the micron-sized antimony powder with an isopropanol solution, stirring, and performing ultrasonic dispersion to obtain a mixed solution;
and S3, performing microwave treatment on the mixed solution, and then centrifuging, washing and drying the supernatant to obtain the antimonene based on microwave-assisted stripping.
2. The method as claimed in claim 1, wherein in S1, the rotation speed of the ball mill is 2500-.
3. The preparation method according to claim 1, wherein in S2, the mass-to-volume ratio of the micron-sized antimony powder to the isopropanol solution is 1 (3-5) mg/ml.
4. The method according to claim 1, wherein the stirring time in S2 is 25 to 35 min.
5. The method according to any one of claims 1 to 4, wherein the time for the ultrasonic dispersion in S2 is 0.5 to 1.5 hours.
6. The method according to claim 5, wherein in S3, the microwave treatment has a power of 600W, a time of 3-15min, and a temperature of 80-130 ℃.
7. An antimonene based on microwave-assisted stripping, which is characterized by being prepared by the preparation method of the antimonene based on microwave-assisted stripping as claimed in any one of claims 1-6.
8. The antimonene based on microwave-assisted stripping according to claim 7, wherein the antimonene based on microwave-assisted stripping is a two-dimensional layered material consisting of fused antimony, wrinkled antimony and six-membered ring antimony.
9. The antimonene based on microwave-assisted stripping according to claim 7 or 8, wherein the number of antimonene layers is 5-100.
10. The antimonene based on microwave-assisted stripping according to claim 9, wherein the thickness of the antimonene is 10nm to 100 nm.
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