CN112758950B - Boron alkene nanosheets and preparation method thereof - Google Patents
Boron alkene nanosheets and preparation method thereof Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 71
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 67
- -1 Boron alkene Chemical class 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title abstract description 33
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000009830 intercalation Methods 0.000 claims abstract description 32
- 230000002687 intercalation Effects 0.000 claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 29
- 239000007791 liquid phase Substances 0.000 claims abstract description 22
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 23
- 239000002904 solvent Substances 0.000 abstract description 16
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical class B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 69
- 229910000085 borane Inorganic materials 0.000 description 35
- 239000000047 product Substances 0.000 description 23
- 230000005540 biological transmission Effects 0.000 description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 10
- 238000010586 diagram Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 239000011229 interlayer Substances 0.000 description 8
- 239000002064 nanoplatelet Substances 0.000 description 8
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000000089 atomic force micrograph Methods 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000012046 mixed solvent Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000009775 high-speed stirring Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- BGECDVWSWDRFSP-UHFFFAOYSA-N borazine Chemical compound B1NBNBN1 BGECDVWSWDRFSP-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 description 2
- AHVYPIQETPWLSZ-UHFFFAOYSA-N N-methyl-pyrrolidine Natural products CN1CC=CC1 AHVYPIQETPWLSZ-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000004774 atomic orbital Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/023—Boron
-
- 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
Abstract
The invention discloses a boron alkene nano sheet and a preparation method thereof, which mainly solve the problem of preparing two-dimensional boron alkene nano sheets from boron powder at present. The boron alkene nano-sheet has a typical two-dimensional lamellar structure, the thickness of the boron alkene nano-sheet is 0.3nm to 10 mu m, the transverse dimension of the boron alkene nano-sheet is 100nm to 100 mu m, and the mass content of boron element is more than 90%. The preparation method comprises the following steps: providing boron powder, adding the boron powder into a solvent, performing ultrasonic treatment in a water bath, adding the obtained product into concentrated acid, performing ultrasonic treatment, and performing centrifugal drying to obtain an intercalation product. And then the intercalation product is subjected to high-temperature expansion to obtain the expanded boron powder. Finally, the boron-expansion powder is stripped by liquid phase to obtain the boron-alkene nano-sheet. The invention provides a simple, green, efficient and low-cost method for preparing the boron alkene nanosheets, and can also realize large-scale production.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a boron alkene nano sheet and a preparation method thereof.
Background
The two-dimensional material has great application prospect in the fields of catalysis, energy sources, electronic information and the like due to the excellent physical and chemical properties. The boracene is a new member of a two-dimensional material family, has ultrahigh conductivity (about 102 omega-1 cm-1), ultrahigh carrier migration rate (about 102cm 2V-1 s-1), good thermal stability and other physicochemical properties, and is attractive in the fields of information, biological medicine and energy environment. The current preparation of two-dimensional boranes is mainly based on chemical vapor deposition (Angew. Chem. Int. Ed.,2015,54,15473-15477,Nat chem,2016,8 (6): 563-568., science,2015,350 (6267): 1513-1516), which is expensive in equipment, energy-consuming and low in yield. In order to realize the large-scale application of the borazine, the low-cost batch preparation of the borazine is realized. Boron is essentially a 3D element, the number of valence electrons is 3, but the number of atomic orbitals is 4, so the number of valence electrons of boron is one less than the number of atomic orbitals, and the valence electron layer cannot be filled up during bonding, so the boron atoms belong to electron-deficient structures, and therefore the boron atoms usually form multicenter bonds. This particular electronic structure of boron atoms creates polyhedral character of boron, making it tend to form a substance having a complex polyhedral structure, not a layered structure. It is also because the special structure of boron is different from the existing two-dimensional material, so the process for preparing the borane nanosheets by adopting a low-cost and large-volume liquid phase stripping method is more difficult. There have been various groups of research to prepare the borane nanoplatelets by liquid phase exfoliation, for example, grand et al, using different organic solvents (chem. Commun.,2019,55,4246-4249;ACS Catal.2019,9,4609-4615) to ultrasonically exfoliate the boron powder to obtain the borane nanoplatelets, but the exfoliation efficiency is very low, the final product concentration is only a few milligrams per milliliter, and the yield of large-scale preparation is far from being reached. How to realize low-price large-scale preparation of the borane nanosheets is a key engineering problem which needs to be solved in engineering application of the borane.
Disclosure of Invention
The invention mainly aims to provide a boron alkene nano-sheet and a preparation method thereof, which are used for overcoming the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
a boron alkene nano-sheet has a typical two-dimensional layered structure, the thickness of the boron alkene nano-sheet is 0.3nm-10 mu m, the transverse dimension of the boron alkene nano-sheet is 10nm-100 mu m, and the mass content of boron elements is more than 90%.
Further, the thickness of the boron alkene nano sheet is 0.8nm-20nm, the transverse dimension is 50nm-10 mu m, and the apparent density of the boron alkene nano sheet is 0.01g/cm 3 -100g/cm 3 。
The preparation method of the above-mentioned borane nanosheet comprises the following steps:
firstly, adding boron powder into a solvent to prepare a dispersion liquid, and then performing ultrasonic treatment in a water bath;
secondly, adding the obtained product into concentrated acid to form concentrated acid suspension, performing ultrasonic treatment, and performing centrifugal drying to obtain an intercalation product;
thirdly, the intercalation product is subjected to temperature programming expansion to obtain expanded boron powder;
and fourthly, stripping the expanded boron powder through a liquid phase to obtain the boron alkene nano sheet.
Further, in the preparation method of the boron alkene nanosheets, the particle size of the boron powder in the first step is 3000 meshes to 20 meshes, the boron element content is more than 90%, and the apparent density is 0.1g/cm 3 -100g/cm 3 . Further, the particle size of the boron powder is 500 to 200 meshes, and the apparent density is 0.5g/cm 3 -10g/cm 3 。
Further, in the preparation method of the borane nanosheet, the solvent in the first step comprises any one or a combination of more than two of water, ethanol, isopropanol, DMF, NMP or acetonitrile. Further, the solvent comprises a mixed solvent of ethanol and DMF and isopropanol and NMP in any proportion.
Further, in the preparation method of the boron alkene nanosheets, the concentration of the dispersion liquid prepared by adding the boron powder into the solvent in the first step is 20 mg/L-1.2 g/mL.
Further, in the preparation method of the borane nanosheet, in the second step, the concentrated acid comprises one or a combination of more than two of sulfuric acid, hydrochloric acid, phosphoric acid or perchloric acid, and the mass percentage concentration of the concentrated acid is 15% -65%.
Further, in the preparation method of the borane nanosheet, the concentration of the concentrated acid suspension formed in the second step is 50 mg/mL-800 mg/mL.
Further, in the preparation method of the borane nanosheet, the temperature-programmed heating range in the third step is 100-1000 ℃, wherein the temperature-programmed heating comprises a plurality of temperature zones, the temperature range of each temperature zone is less than 300 ℃, and the temperature-programmed heating rate is 0.1-50 ℃. Further, the temperature rise range is 250 ℃ to 600 ℃, the temperature of the sections is 3 to 5 sections, the temperature range of each section is 50 ℃ to 200 ℃, and the temperature rise rate is 2 ℃ to 20 ℃.
Further, in the preparation method of the borane nanosheet, the liquid phase stripping mode in the fourth step comprises one or a combination of any two or more of ultrasonic treatment, high-speed stirring, homogenization and sanding. Further, the ultrasonic power is 100 to 1500W, the ultrasonic temperature is 10 to 50 ℃, the high-speed stirring speed is 100 to 30000Rpm, and the homogenizing operation pressure is 50 to 500MPa.
The invention realizes the large-scale preparation of the boron alkene nanosheets through an intercalation-expansion-stripping three-step process. In the preparation method, the key point of the preparation of the boron alkene nano sheet is that the interlayer spacing of the boron alkene sheet is gradually opened, and firstly, the boron powder is wetted by a proper solvent, so that solvent molecules slowly permeate into the interlayer. The interlayer spacing is then further extended by oxidation with concentrated acid. The first step is to wet the boron powder with a proper solvent, and if the intercalation is directly carried out with concentrated acid, the intercalating agent cannot enter the interlayer due to the difference of surface energy, so that the surface of the boron powder is oxidized to obtain an unlanded intercalation product. The subsequent temperature programming expansion is carried out to further open the interlayer distance, wherein the temperature programming is adopted to match the decomposition temperature of different intercalators, and the temperature-increasing rate is controlled to effectively alleviate the problem of edge oxidation of the boron alkene nano sheet caused in the thermal expansion process.
Compared with the prior art, the invention has the advantages that:
(1) The method for preparing the boron alkene nanosheets has the advantages of simple process, environment friendliness, recycling of all reagents, simple equipment, easy industrialized mass production and wide market prospect, and is used for preparing the boron alkene nanosheets through three steps of intercalation, expansion and stripping;
(2) The boron alkene nanosheets provided by the invention are prepared by adopting a unique intercalation-expansion-stripping process method, high yield is realized while stripping efficiency is ensured, and the problem of low liquid phase stripping yield at present is solved;
(3) The boron alkene nanosheets provided by the invention are high in quality, high in purity, less in impurity and easy to prepare in batches.
Drawings
FIG. 1a is a transmission electron microscope image of a borane nanosheet obtained according to example 1 of the present invention;
FIG. 1b is an atomic force microscope image of a borane nanosheet obtained according to example 1 of the present invention;
FIG. 2a is a transmission electron microscope image of the boron alkene nanoplatelets obtained in example 2 of the present invention;
FIG. 2b is an atomic force microscope image of a borane nanosheet obtained according to example 2 of the present invention;
FIG. 3a is a transmission electron microscope image of the boron alkene nanoplatelets obtained in example 3 of the present invention;
FIG. 3b is an atomic force microscope image of a borane nanosheet obtained according to example 3 of the present invention;
FIG. 4a is a transmission electron microscope image of the boron alkene nanoplatelets obtained in example 4 of the present invention;
FIG. 4b is an atomic force microscope image of a borane nanosheet obtained according to example 4 of the present invention;
FIG. 5a is a transmission electron microscope image of the boron alkene nanoplatelets obtained in example 5 of the present invention;
FIG. 5b is an atomic force microscope image of a borane nanosheet obtained according to example 5 of the present invention.
The specific embodiment is as follows:
in view of the shortcomings in the prior art, the inventor of the present invention has long studied and practiced in a large number of ways to propose the technical scheme of the present invention. The technical scheme and implementation process, principle and the like will be further explained as follows.
Aiming at a series of problems of low yield, high energy consumption, high production cost and the like in the existing preparation process of the boron alkene, the invention organically combines two methods of liquid phase stripping and high-temperature expansion to form a special three-step preparation process of liquid phase intercalation, high-temperature expansion and liquid phase stripping, and the defects of low yield, long period, high equipment investment of chemical vapor deposition, high energy consumption and the like of the traditional liquid phase stripping method are avoided. The two-dimensional boracene prepared by the method has the characteristics of large lamellar, thin thickness, high purity and the like, and in order to further verify the properties of the boracene prepared by the method, the detection of an electron microscope is adopted to find out the nano-boraceneThe rice flake has a transverse dimension of 10nm-100 μm and a thickness of 0.3nm-10 μm; further, through element tests, the mass content of boron element in the prepared boron alkene is found to be more than 90%; the apparent density of the boron alkene nano sheet is 0.01g/cm 3 -100g/cm 3 。
The preparation method of the borane nanosheet comprises the following steps:
firstly, liquid phase intercalation is completed through two steps, firstly, the surface of boron powder is infiltrated into the interlayer through a solvent with the similar surface energy with the boron powder, and secondly, concentrated acid is selected for intercalation. Unlike the conventional liquid phase stripping, the present invention is to use two-step intercalation, the first step is to use solvent with better wettability with boron powder to open the layer edge, and the second step is to further expand the layer gap through acid intercalation. The two-step intercalation method solves the problems that the solvent intercalation layer with good wettability is smaller in interval and solvent molecules are easy to deviate from, and simultaneously avoids the defect that the surface of boron powder particles is seriously oxidized due to poor surface wettability when acid intercalation is adopted independently. Firstly adding boron powder into a solvent to prepare a dispersion liquid, and then performing ultrasonic treatment in a water bath; and adding the obtained product into concentrated acid to form concentrated acid suspension, performing ultrasonic treatment, and performing centrifugal drying to obtain an intercalation product.
The particle size of the boron powder is 3000 to 20 meshes, the boron element content is more than 90 percent, and the apparent density is 0.1g/cm 3 -100g/cm 3 . Further, the particle size of the boron powder is 500 to 200 meshes, and the apparent density is 0.5g/cm 3 -10g/cm 3 。
The solvent comprises any one or a combination of any two or more of water, ethanol, isopropanol, DMF, NMP or acetonitrile. Further, the solvent comprises a mixed solvent of ethanol and DMF and isopropanol and NMP in any proportion.
Further, the concentration of the dispersion liquid prepared by adding the boron powder into the solvent is 20 mg/L-1.2 g/mL.
Further, the concentrated acid comprises one or a combination of more than two of sulfuric acid, hydrochloric acid, phosphoric acid or perchloric acid, and the mass percentage concentration of the concentrated acid is 15-65%.
Further, the concentration of the concentrated acid suspension is 50 mg/mL-800 mg/mL.
The intercalation product is obtained after intercalation by a two-step method, and then the interlayer spacing is further opened by high-temperature expansion, so that the interlayer interaction force is weakened. In order to avoid the problem that the expansion efficiency is poor due to the fact that raw materials are oxidized at high temperature or intercalation overflows in the thermal expansion process caused by one-step high-temperature expansion in the traditional thermal expansion method, a programmed heating expansion strategy is adopted in the invention, and the expansion effect is maximized by performing gradual thermal expansion through the temperature matched with the boiling point and the decomposition temperature of the intercalation. The temperature-programmed heating range adopted in the invention is 100-1000 ℃, wherein the temperature-programmed heating comprises a plurality of temperature zones, the temperature range of each temperature zone is less than 300 ℃, and the temperature-programmed heating rate is 0.1-50 ℃. Further, the temperature rise range is 250 ℃ to 600 ℃, the temperature of the sections is 3 to 5 sections, the temperature range of each section is 50 ℃ to 200 ℃, and the temperature rise rate is 2 ℃ to 20 ℃. And finally, obtaining the final boron alkene nanosheets through liquid phase stripping after obtaining an expansion product through programmed heating expansion. The liquid phase stripping mode adopted in the invention comprises one or a combination of any two or more of ultrasonic, high-speed stirring, homogenizing or sanding. Further, the ultrasonic power is 100 to 1500W, the ultrasonic temperature is 10 to 50 ℃, the high-speed stirring speed is 100 to 30000Rpm, and the homogenizing operation pressure is 50 to 500MPa. The borazine nano-sheet obtained by liquid phase stripping is detected by an electron microscope to determine the size and thickness of the sheet diameter and the purity of the element.
The technical scheme of the invention is further described in detail below through a plurality of embodiments and with reference to the accompanying drawings.
Example 1
A preparation method of a boron alkene nano-sheet comprises the following steps:
firstly, adding a certain amount of boron powder into an ethanol/DMP mixed solvent to prepare a dispersion liquid, and then carrying out water bath ultrasonic treatment by adopting an ultrasonic instrument with power of 500W, and keeping the temperature at not more than 30 ℃ to obtain an ultrasonic mixed liquid;
secondly, adding a product obtained by filtering the ultrasonic mixed solution into concentrated acid to form concentrated acid suspension, performing ultrasonic treatment in a 500W ultrasonic instrument, and performing centrifugal cleaning and drying to obtain an intercalation product;
thirdly, the intercalation product is subjected to temperature programming expansion to obtain expanded boron powder;
and fourthly, stripping the expanded boron powder through a liquid phase to obtain the boron alkene nano sheet. The specific process parameters are shown in Table 1.
The structure and performance of the borane nanosheets obtained in this example are characterized: the lateral dimension of the borane nanometer is 5 mu m and the thickness is 7nm through the test of a transmission electron microscope and an atomic force microscope, the transmission mirror diagram of the borane nanometer is shown in figure 1a, and the atomic force microscope diagram is shown in figure 1b. The specific performance parameters of the boron alkene nanosheets are shown in table 2.
Example 2
A preparation method of a boron alkene nano-sheet comprises the following steps:
firstly, adding a certain amount of boron powder into an isopropanol/DMF mixed solvent to prepare a dispersion liquid, and then carrying out water bath ultrasonic treatment by adopting an ultrasonic instrument with power of 500W, and keeping the temperature at not more than 30 ℃ to obtain an ultrasonic mixed liquid;
secondly, adding a product obtained by filtering the ultrasonic mixed solution into concentrated acid to form concentrated acid suspension, performing ultrasonic treatment in a 500W ultrasonic instrument, and performing centrifugal cleaning and drying to obtain an intercalation product;
thirdly, the intercalation product is subjected to temperature programming expansion to obtain expanded boron powder;
and fourthly, stripping the expanded boron powder through a liquid phase to obtain the boron alkene nano sheet. The specific process parameters are shown in Table 1.
The structure and performance of the borane nanosheets obtained in this example are characterized: the lateral dimension of the borane nanometer is 3 mu m and the thickness is 4.5nm through the test of a transmission electron microscope and an atomic force microscope, the transmission mirror diagram of the borane nanometer is shown in figure 2a, and the atomic force microscope diagram is shown in figure 2b. The specific performance parameters of the boron alkene nanosheets are shown in table 2.
Example 3
A preparation method of a boron alkene nano-sheet comprises the following steps:
firstly, adding a certain amount of boron powder into isopropanol to prepare dispersion liquid, and then carrying out water bath ultrasonic treatment by adopting an ultrasonic instrument with power of 500W, and keeping the temperature at not more than 30 ℃ to obtain ultrasonic mixed liquid;
secondly, adding a product obtained by filtering the ultrasonic mixed solution into concentrated acid to form concentrated acid suspension, performing ultrasonic treatment in a 500W ultrasonic instrument, and performing centrifugal cleaning and drying to obtain an intercalation product;
thirdly, the intercalation product is subjected to temperature programming expansion to obtain expanded boron powder;
and fourthly, stripping the expanded boron powder through a liquid phase to obtain the boron alkene nano sheet. The specific process parameters are shown in Table 1.
The structure and performance of the borane nanosheets obtained in this example are characterized: the lateral dimension of the borane nanometer is proved to be 2 mu m and the thickness is proved to be 13nm by the test of a transmission electron microscope and an atomic force microscope, the transmission mirror diagram of the borane nanometer is shown in figure 3a, and the atomic force microscope diagram is shown in figure 3b. The specific performance parameters of the boron alkene nanosheets are shown in table 2.
Example 4
A preparation method of a boron alkene nano-sheet comprises the following steps:
firstly, adding a certain amount of boron powder into NMP to prepare a dispersion liquid, and then carrying out water bath ultrasonic treatment by adopting an ultrasonic instrument with power of 500W, and keeping the temperature at not more than 30 ℃ to obtain an ultrasonic mixed liquid;
secondly, adding a product obtained by filtering the ultrasonic mixed solution into concentrated acid to form concentrated acid suspension, performing ultrasonic treatment in a 500W ultrasonic instrument, and performing centrifugal cleaning and drying to obtain an intercalation product;
thirdly, the intercalation product is subjected to temperature programming expansion to obtain expanded boron powder;
and fourthly, stripping the expanded boron powder through a liquid phase to obtain the boron alkene nano sheet. The specific process parameters are shown in Table 1.
The structure and performance of the borane nanosheets obtained in this example are characterized: the lateral dimension of the borane nanometer is 1 mu m and the thickness is 4nm through the test of a transmission electron microscope and an atomic force microscope, the transmission mirror diagram of the borane nanometer is shown in fig. 4a, and the atomic force microscope diagram is shown in fig. 4b. The specific performance parameters of the boron alkene nanosheets are shown in table 2.
Example 5
A preparation method of a boron alkene nano-sheet comprises the following steps:
firstly, adding a certain amount of boron powder into a water/isopropanol mixed solvent to prepare a dispersion liquid, and then carrying out water bath ultrasonic treatment by adopting an ultrasonic instrument with power of 500W, and keeping the temperature at not more than 30 ℃ to obtain an ultrasonic mixed liquid;
secondly, adding a product obtained by filtering the ultrasonic mixed solution into concentrated acid to form concentrated acid suspension, performing ultrasonic treatment in a 500W ultrasonic instrument, and performing centrifugal cleaning and drying to obtain an intercalation product;
thirdly, the intercalation product is subjected to temperature programming expansion to obtain expanded boron powder;
and fourthly, stripping the expanded boron powder through a liquid phase to obtain the boron alkene nano sheet. The specific process parameters are shown in Table 1.
The structure and performance of the borane nanosheets obtained in this example are characterized: the lateral dimension of the borane nanometer is 3.5 mu m and the thickness is 12nm through the test of a transmission electron microscope and an atomic force microscope, the transmission mirror diagram of the borane nanometer is shown in fig. 5a, and the atomic force microscope diagram is shown in fig. 5b. The specific performance parameters of the boron alkene nanosheets are shown in table 2.
Table 1 examples 1-5 borane nanoplatelets preparation process parameters.
TABLE 2 physical parameters of examples 1-5 boron alkene nanoplatelets
As can be seen from the above, the boron alkene nanosheets prepared in examples 1 to 5 have a typical two-dimensional lamellar structure, the thickness of the nanosheets is 4 to 13nm, the transverse dimension is 1 to 5 μm, the boron element content is over 95%, the oxygen element content is over 0.7%, and the apparent density is 0.06 to 0.3g/cm 3 While the present invention has been studied in other embodimentsIn the process, the preparation method of the invention can be used for obtaining the boron alkene nanosheets with the thickness of 0.3nm-10 mu m and the transverse dimension of 10nm-100 mu m. The boron alkene nanosheets obtained by the technical scheme of the invention have excellent performance, the preparation process is environment-friendly, continuous industrial production can be realized, and the preparation method has wide application prospect.
It should be understood that the foregoing is only a few embodiments of the present invention, and it should be noted that other modifications and improvements can be made by those skilled in the art without departing from the inventive concept of the present invention, which fall within the scope of the present invention.
Claims (2)
1. The boron alkene nanosheets are characterized by being prepared by the following steps:
firstly, adding a certain amount of boron powder into NMP to prepare dispersion liquid, wherein the concentration of the dispersion liquid is 80mg/ml, and then carrying out water bath ultrasonic treatment by adopting an ultrasonic instrument with power of 500W, and keeping the temperature at not more than 30 ℃ to obtain ultrasonic mixed liquid;
secondly, adding a product obtained by filtering the ultrasonic mixed solution into concentrated acid, wherein the concentrated acid is perchloric acid with the mass percent concentration of 15% to form concentrated acid suspension, the concentration of the suspension is 65mg/ml, performing ultrasonic treatment in a 500W ultrasonic instrument, and performing centrifugal cleaning and drying to obtain an intercalation product;
thirdly, the intercalation product is subjected to temperature programming expansion to obtain expanded boron powder, wherein the temperature programming conditions are as follows: 20-150 ℃ and 20 ℃/min; 150-400 ℃ and 10 ℃/min; 400-450 ℃,5 ℃/min; 450-650 ℃ and 1 ℃/min;
fourthly, the expanded boron powder is subjected to liquid phase stripping to obtain the boron alkene nano sheet, and the stripping mode of the liquid phase stripping is sanding.
2. The boron-containing nanosheets of claim 1, wherein the boron powder in the first step has a particle size of 3000 mesh to 20 mesh, a boron element content of greater than 90%, and an apparent density of 0.1g/cm 3 -100g/cm 3 。
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