CN108284220B - Bismuth-alkene nanosheet and preparation method thereof - Google Patents
Bismuth-alkene nanosheet and preparation method thereof Download PDFInfo
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Abstract
本发明提供了一种铋烯纳米片的制备方法，包括：(1)将铋粉分散在有机溶剂中，得到分散液；(2)先对所述分散液进行第一次水浴超声，再进行探头式超声，得到第一超声液；然后对所述第一超声液进行第二次水浴超声，得到第二超声液；(3)对所述第二超声液在2000‑4000rpm下进行超低速离心，收集上清液，然后对所述上清液在5000‑7000rpm下进行低速离心，收集沉淀，所得沉淀即为铋烯纳米片。该方法工艺简单易操作、重现性好，易制得尺寸可控的单分散性好的铋烯纳米片。本发明还提供了制得的铋烯纳米片。
The present invention provides a method for preparing bismuthene nanosheets, comprising: (1) dispersing bismuth powder in an organic solvent to obtain a dispersion; (2) first performing water bath ultrasound on the dispersion, and then performing Probe type ultrasonic, obtain the first ultrasonic liquid; Then carry out the second water bath ultrasonic to the described first ultrasonic liquid, obtain the second ultrasonic liquid; (3) carry out ultra-low speed centrifugation to the described second ultrasonic liquid at 2000-4000rpm , collect the supernatant, then carry out low-speed centrifugation to the supernatant at 5000-7000 rpm, collect the precipitation, and the obtained precipitation is the bismuthene nanosheet. The method is simple and easy to operate, has good reproducibility, and can easily prepare bismuthene nanosheets with controllable size and good monodispersity. The invention also provides the prepared bismuthene nanosheet.
Description
Technical Field
The invention relates to the field of two-dimensional materials, in particular to a bismuth-alkene nanosheet and a preparation method thereof.
Background
Two-dimensional materials, refers to materials in which electrons can move freely (planar motion) only in two dimensions, on a non-nanoscale (1-100nm), such as a nano-film. Graphene was first produced in 2004 by the tape method by two scientists of the university of manchester, england, andem, and knowavlov. Thereafter, a series of quasi-two-dimensional materials, such as black phosphorus (phospholene), silylene, germanene, stibene, boron nitride, molybdenum disulfide, etc., having a thickness of only a single atomic layer were successively found.
Bismuth ene (Bismuthene) is a two-dimensional material exfoliated from bulk metallic bismuth, having a graphene-like structure. However, the bismuth-alkene is a direct band-gap semiconductor with an energy gap of 0.306eV (the bottom of a conduction band and the top of a valence band are at the same position), can be directly coupled with light, and has a wide absorption spectrum range. In addition, bismuth has strong biocompatibility and low biological toxicity, so that bismuth has wide application potential in the aspects of optics, electrics, biological medicine and pharmacology and the like. The two-dimensional bismuth-alkene lamellar structure is a potential biomedical substrate material in the fields of biological medicine carrying, photo-thermal, photodynamic therapy and the like.
At present, the lamellar bismuth-alkene material is prepared by a mechanical stripping method (such as a transparent adhesive tape tearing method), a chemical vapor deposition method and other technologies. However, the flaky bismuth-alkene material prepared by the mechanical stripping method has low yield, is not suitable for commercial production, and has the disadvantages of complex operation and long time consumption; the chemical vapor deposition method is less in the amount of the prepared bismuth alkene and is not easy to repeat.
Disclosure of Invention
In view of the above, the invention provides a bismuth alkene nano-sheet and a preparation method thereof, and the preparation method combines probe ultrasound and water bath ultrasound, and realizes the stripping of bismuth powder through synergistic effect, so as to obtain the bismuth alkene nano-sheet with good monodispersity and uniform size. The method has the advantages of simple and easy operation process, good reproducibility, high yield of the bismuth-alkene nanosheets, and easy realization of low-cost industrial production.
In a first aspect, the invention provides a preparation method of a bismuth-alkene nanosheet, which comprises the following steps:
(1) dispersing bismuth powder in an organic solvent to obtain a dispersion liquid; wherein the concentration of the bismuth powder in the dispersion liquid is 0.5-10 mg/mL;
(2) firstly, carrying out first water bath ultrasound on the dispersion liquid, wherein the power of the first water bath ultrasound is 400-; performing probe type ultrasonic treatment at the power of 1080-;
then carrying out second water bath ultrasound on the first ultrasonic liquid to obtain a second ultrasonic liquid; wherein the power of the second water bath ultrasound is 400-600W;
(3) and carrying out ultra-low speed centrifugation on the second ultrasonic liquid at 2000-4000rpm, collecting supernatant, carrying out low speed centrifugation on the supernatant at 5000-7000rpm, collecting precipitate, and obtaining the precipitate, namely the bismuth alkene nanosheet.
Alternatively, the organic solvent includes one or more of N-methylpyrrolidone (NMP), Dimethylformamide (DMF), dimethyl sulfoxide (DMSO), acetone, tetrahydrofuran, absolute ethanol, methanol, isopropanol, chloroform, and dichloromethane, but is not limited thereto. The surface energy of the used organic solvent is matched with the surface energy of the two-dimensional layered bismuth-alkene material, and a certain interaction exists between the organic solvent and the two-dimensional layered bismuth-alkene material, so that the energy required by stripping the bismuth powder is balanced.
Optionally, the bismuth powder has a particle size of no more than 75 μm. For example 55-70 μm, 1-50 μm, 2-45 μm or 1-4 μm. Further optionally, the particle size of the bismuth powder is not more than 50 μm.
In the embodiment of the invention, the power of the first water bath ultrasound can be 400W, 450W, 500W, 550W, 580W or 600W. Optionally, the power of the first water bath ultrasound is 420-.
Optionally, the time of the second water bath ultrasound is 1-6 hours. Further optionally 1-3 hours.
Wherein the power of the second water bath ultrasound can be 400W, 450W, 500W, 550W, 580W or 600W. Optionally, the power of the second water bath ultrasound is 420-. The power or time of the second water bath ultrasound can be the same as or different from the power or time of the first water bath ultrasound.
In the embodiment of the invention, the power of the probe-type ultrasound can be 1100W, 1200W, 1300W, 1400W, 1500W, 1600W or 1700W. Optionally, the power of the probe-type ultrasound is 1200-.
In the embodiment of the invention, the time of the probe type ultrasonic treatment can be 10h, 12h, 15h, 20h or 24 h. Optionally, the probe-type ultrasound is performed for 12-24 hours.
Optionally, the probe sonication is performed in an ice bath at a temperature not exceeding 10 ℃. Preferably, the temperature during probe-type ultrasound is 0 to 10 ℃, more preferably 4 to 10 ℃. The ice-bath condition refers to that in the probe type ultrasonic process, a container filled with the solution to be subjected to ultrasonic treatment is placed in another container (such as a beaker and a test tube) filled with ice blocks.
Optionally, the first water bath ultrasound is performed at a temperature of 5-10 ℃.
Optionally, the second water bath ultrasound is performed at a temperature of 5-10 ℃.
Optionally, the ultra-low speed centrifugation is performed for 15-30 min. For example 12, 15, 20, 25 or 30 min.
Optionally, the rotation speed of the ultra-low speed centrifugation is 2000-3000 rpm.
Optionally, the ultra-low speed centrifugation is performed for 15-30 min. For example 12, 15, 20, 25 or 30 min.
Optionally, the rotation speed of the low-speed centrifugation is 6000-7000 rpm.
And the precipitate (namely the bismuth alkene nano sheet) obtained after the low-speed centrifugation can be re-dispersed into a second solvent to obtain a solution containing the bismuth alkene nano sheet. Optionally, the second solvent comprises one or more of N-methylpyrrolidone (NMP), Dimethylformamide (DMF), dimethyl sulfoxide (DMSO), acetone, tetrahydrofuran, anhydrous ethanol, methanol, and isopropanol.
In the invention, the first water bath ultrasound of the bismuth powder dispersion liquid is to initially break the bismuth powder by the ultrasonic cavitation effect to partially dissolve the bismuth powder in the organic solvent, thereby avoiding the loss of a probe type ultrasonic instrument by directly adopting probe type ultrasound and prolonging the ultrasonic time; the probe type ultrasonic treatment is to crush and strip a large amount of bismuth powder which is crushed preliminarily into bismuth alkene with a lamellar structure, so that the bismuth alkene is dissolved into an organic solvent in a large amount; and finally, the stripped bismuth-alkene layered material can be further smashed into smaller particles by the aid of second water bath ultrasound to obtain bismuth-alkene nanosheets, and agglomeration is further avoided, so that subsequent centrifugal purification treatment can be conveniently carried out.
According to the preparation method of the bismuth alkene nanosheet, provided by the invention, the bismuth powder is stripped through a liquid phase stripping method combining probe ultrasound and water bath ultrasound through a synergistic effect, the method is simple in process and easy to operate, the yield is high, the method has obvious advantages compared with the existing mechanical stripping method, the existing chemical vapor deposition method and the like, the bismuth alkene nanosheet with controllable size and good monodispersity can be obtained, and the low-cost industrial production is easy to realize. The method lays a foundation for the application of the bismuth-alkene nanosheets in the field of biomedicine.
In a second aspect, the invention also provides a bismuth-alkene nano sheet prepared by the preparation method. The thickness of the bismuth-alkene nano-sheet is less than 20nm, and the transverse dimension of the bismuth-alkene nano-sheet is 100 nm-10 mu m. Wherein, the transverse dimension refers to the length or width of the bismuth alkene nanometer sheet.
Optionally, the lateral dimension of the bismuth-alkene nano-sheet is 200 nm-10 μm. For example 300nm, 500nm, 800nm, 1 μm, 2 μm, 5 μm, 8 μm or 10 μm.
Optionally, the lateral dimension of the bismuth-alkene nano-sheet is 500 nm-10 μm.
Optionally, the lateral dimension of the bismuth-alkene nano-sheet is 1 μm to 10 μm.
The bismuth alkene nano-sheets comprise a layer of bismuth alkene or a plurality of layers of single-layer bismuth alkene which are repeatedly stacked in the direction vertical to the plane of the bismuth alkene.
Optionally, the thickness of the bismuth alkene nanoplatelets is 0.3-15 nm.
Optionally, the bismuth-alkene nano-sheet is 1-64 atomic layers thick. I.e. from 1 to 64 individual layers of bismuth-alkene stack. Further optionally, the bismuth-alkene nanoplatelets have a thickness of
Optionally, the bismuth alkene nanosheets are formed by stacking 1-10 layers of bismuth alkenes. The thickness of the bismuth-alkene nano-sheet is 0.3-3 nm.
Optionally, the shape of the bismuth alkene nanoplatelets includes, but is not limited to, square, circular, triangular, polygonal, and the like.
The bismuth-alkene nanosheets provided by the invention are regular in shape, uniform in size, good in dispersity and low in toxicity, and are convenient to use in the fields of preparation of optics, electrics, biomedicine (such as preparation of photothermal treatment medicines and optical marking medicines).
Advantages of embodiments of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of embodiments of the invention.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of a bismuth-alkene nanosheet made by an embodiment of the present invention;
FIG. 2 shows the result of Atomic Force Microscope (AFM) analysis of bismuth-alkene nanoplates prepared by an embodiment of the present invention;
FIG. 3 is a Raman spectrum of a bismuth-alkene nanosheet prepared according to an embodiment of the present invention;
fig. 4 is an ultraviolet-visible-near infrared absorption spectrum diagram of a bismuth-alkene nanosheet prepared in an NMP solvent according to an embodiment of the present invention.
Detailed Description
While the following is a description of the preferred embodiments of the present invention, it should be noted that those skilled in the art can make various modifications and improvements without departing from the principle of the embodiments of the present invention, and such modifications and improvements are considered to be within the scope of the embodiments of the present invention.
The following examples are intended to illustrate the invention in more detail. The embodiments of the present invention are not limited to the following specific examples. The present invention can be modified and implemented as appropriate within the scope of the main claim.
Example 1
A preparation method of a bismuth alkene nanosheet comprises the following steps:
(1) taking a 250mL glass bottle of Sichuan cattle, filling 120mL NMP solvent, and then adding 120mg of 200-mesh (200 grains per square inch, namely the grain diameter is 0.074mm) bismuth powder to obtain a dispersion liquid of which the initial concentration of the bismuth powder is 1mg/mL (or called 1000 ppm);
(2) placing the glass bottle in the step (1) into a Xinzhi ultrasonic constant-temperature cleaning machine SBL-22DT, and carrying out water bath ultrasonic treatment for 3 hours at a constant temperature of 10 ℃ and 70% of the maximum power (600W) (namely, at a power of 420W);
after water bath ultrasonic treatment, placing the obtained solution in a BILON-1800Y (1800W maximum power) of a brown cell disruptor, and carrying out probe ultrasonic treatment for 24 hours at 4 ℃ with 60% power (1080W power) to obtain a first ultrasonic solution;
then putting the first ultrasonic liquid into a Xinzhi ultrasonic constant-temperature cleaning machine SBL-22DT, and carrying out secondary water bath ultrasonic treatment for 3 hours at the constant temperature of 10 ℃ and the power of 70% to obtain second ultrasonic liquid;
(3) and averagely dividing the second ultrasonic liquid into 4 parts, transferring the parts into 50mL centrifuge tubes, centrifuging the parts for 20 minutes at the rotating speed of 3000rpm (centrifugal force of 5000 g) by using a Hessi HR20MW centrifuge, transferring the obtained supernatant into 4 new 50mL centrifuge tubes respectively, centrifuging the parts for 20 minutes at the rotating speed of 7000rpm (centrifugal force of 11667 g), and collecting precipitates in the tubes to obtain the required bismuth-alkene nanosheets (about 71.4 mg).
According to calculation, in the example 1 of the invention, the yield of the bismuth alkene nano-sheets is 71.4mg/120 mg-59.5%.
Example 2
A preparation method of a bismuth alkene nanosheet comprises the following steps:
(1) taking a 500mL glass bottle of Sichuan cattle, filling 400mL NMP solvent, and then adding 200mg of 300-mesh bismuth powder to obtain a dispersion liquid with the initial concentration of the bismuth powder of 0.5 mg/mL;
(2) placing the glass bottle in the step (1) into a Xinzhi ultrasonic constant-temperature cleaning machine SBL-22DT, and carrying out water bath ultrasonic treatment for 2 hours at the constant temperature of 4 ℃ and the power of 480W;
after water bath ultrasound, placing the obtained solution in a BILON-1800Y (1800W maximum power) of a brown cell disruptor, and carrying out probe ultrasound for 15 hours at 75% power (namely 1350W power) to obtain first ultrasonic liquid;
then putting the first ultrasonic liquid into a Xinzhi ultrasonic constant-temperature cleaning machine SBL-22DT, and carrying out second water bath ultrasonic treatment for 3 hours at the power of 450W to obtain a second ultrasonic liquid;
(3) and averagely dividing the second ultrasonic solution into 4 parts, transferring the parts into 50mL centrifuge tubes, centrifuging the parts for 30 minutes at the rotating speed of 2000rpm by adopting a Hexie HR20MW centrifuge, transferring the obtained supernatant into 4 new 50mL centrifuge tubes respectively, centrifuging the parts for 25 minutes at the rotating speed of 6500rpm, and collecting precipitates in the tubes to obtain the desired bismuth alkene nanosheets (the yield is 65%).
Fig. 1 is a Scanning Electron Microscope (SEM) photograph of a bismuthylene nanoplate prepared according to an embodiment of the present invention. As can be seen from fig. 1, there are a number of distinct plate-like substances, namely bismuth alkene nanoplatelets. The obvious layered structure can be seen in an enlarged way, which shows that the required bismuth alkene nano-sheets can be stripped by adopting the preparation method of the invention. The transverse size of the bismuth alkene nano-sheet is 100 nm-10 μm, and one or more layers of single-layer bismuth alkene are repeatedly stacked in the direction vertical to the plane of the bismuth alkene nano-sheet to form a layered feather-like structure. The thickness of the bismuth-alkene nano-sheets is formed
Fig. 2 shows the analysis result of an Atomic Force Microscope (AFM) of the bismuth-alkene nanosheets prepared in the example of the present invention. A large number of sheet structures with a thickness of 3nm (Δ Z) exist in the figure, which illustrates that the preparation method provided by the present invention can successfully peel off and form a bismuth-alkene nanosheet, and the bismuth-alkene nanosheet is formed by stacking about 10 single-layer bismuth-alkene layers, i.e., the bismuth-alkene nanosheet is 10 bismuth atomic layers thick.
Fig. 3 is a raman graph of a bismuth-alkene nanosheet prepared in an embodiment of the present invention. 70cm at an excitation wavelength of 1064nm-1And 97cm-1(E each corresponding to Bi element)gAnd A1gVibration mode) are obvious, which indicates that the preparation method provided by the invention can be stripped to form the bismuth alkene nano-sheet.
Fig. 4 is an ultraviolet-visible-near infrared absorption spectrum diagram of a bismuth-alkene nanosheet prepared in an NMP solvent according to an embodiment of the present invention. As can be seen from FIG. 4, the bismuth-alkene nanosheets provided by the invention all show obvious absorption characteristics in the region of 300-1100 nm.
To highlight the beneficial effects of the invention, the invention also provides the following comparative examples for example 1:
comparative example 1 differs from example 1 in that: in the step (2), performing probe ultrasound for 24 hours by using a brown cell disruptor;
comparative example 2 differs from example 1 in that: in the step (2), firstly, carrying out probe ultrasonic treatment by using a BIRAN cell disruptor, and then carrying out water bath ultrasonic treatment;
comparative example 3 differs from example 1 in that: in the step (2), water bath ultrasound is firstly carried out, then probe type ultrasound is carried out, and secondary water bath ultrasound is carried out after probe type ultrasound is not carried out.
The lateral dimension of the product prepared by the comparative example 1 is mainly more than 1 μm compared with that of the bismuth-alkene nano-sheets prepared by the example 1, and the yield of the bismuth-alkene nano-sheets is 63.9mg/120 mg-53.25%.
The product prepared by the comparative example 2 has the yield of the bismuth alkene nano sheets of 67.8mg/120 mg-56.5% compared with the product prepared by the example 1. Among them, there are also contained nanosheets having a lateral dimension of 1 μm or more.
The product prepared by the comparative example 3 has a yield of 68.2mg/120 mg-56.83% compared with that of the product prepared by the example 1. And the product of comparative example 3 was dispersed in an organic solvent and allowed to stand for 6 hours with a slight amount of agglomeration.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
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| CN108284220B (en) * | 2017-12-26 | 2021-01-05 | 深圳大学 | Bismuth-alkene nanosheet and preparation method thereof |
| US11623873B2 (en) * | 2018-12-06 | 2023-04-11 | Purdue Research Foundation | Substrate-free crystalline 2D bismuthene |
| CN112792350B (en) * | 2019-10-25 | 2022-04-19 | 中国科学院福建物质结构研究所 | Antimony and/or bismuth nanosheet, stibene and/or bislimonene and preparation method and application thereof |
| CN110982900B (en) * | 2019-12-13 | 2023-10-03 | 深圳瀚光科技有限公司 | Biosensor based on bismuth alkene nanosheet fluorescence quenching, miRNA detection kit and application |
| CN111790904A (en) * | 2020-05-25 | 2020-10-20 | 南京理工大学 | A method for preparing bismuthene nanosheets by liquid-phase laser irradiation |
| CN112618715B (en) * | 2021-01-06 | 2023-03-14 | 浙江理工大学 | Preparation method of drug-loaded photothermal photodynamic nanoparticles based on electrostatic adsorption |
| CN112846199B (en) * | 2021-01-08 | 2022-09-09 | 新乡医学院 | Method for preparing ultrathin bismuth-alkene nanosheets by heating, freezing, grinding and ultrasonic |
| CN114147211B (en) * | 2021-12-07 | 2024-01-30 | 合肥工业大学 | Copper-tin bimetal alkene nanosheet and preparation method thereof |
| WO2023224579A1 (en) * | 2022-05-20 | 2023-11-23 | Koc Universitesi | Bismuthene as a versatile photocatalyst operating under variable conditions for the photoredox c–h bond functionalization |
| CN116947021A (en) * | 2023-09-07 | 2023-10-27 | 吉林大学 | A method for preparing N-doped carbon nanosheets by carbonizing organic solvent NMP with an ultrasonic crusher |
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| US6872330B2 (en) * | 2002-05-30 | 2005-03-29 | The Regents Of The University Of California | Chemical manufacture of nanostructured materials |
| CN102674476A (en) * | 2012-05-17 | 2012-09-19 | 哈尔滨工业大学 | Chemical preparation method of magnetic graphene |
| US9108275B2 (en) * | 2012-10-10 | 2015-08-18 | Federal-Mogul Corporation | Bi-material strip and a method of bonding strips of different materials together |
| CN104591181B (en) * | 2015-02-13 | 2016-09-21 | 山东大学 | A kind of method utilizing nanoscale twins stripping to prepare Two-dimensional Composites |
| CN104843695A (en) * | 2015-05-26 | 2015-08-19 | 山东大学 | Method for preparing two-dimensional nanosheet material through all-directional ultrasonic agitation process |
| CN105600760B (en) * | 2015-12-25 | 2018-01-23 | 湖北中科墨磷科技有限公司 | A kind of small size black phosphorus piece and preparation method thereof |
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| CN107234244B (en) * | 2017-06-23 | 2019-10-18 | 南京理工大学 | A preparation method of large-yield antimonene quantum dots by ultrasonic liquid phase exfoliation |
| CN107275628B (en) * | 2017-07-19 | 2019-10-25 | 华中科技大学 | A kind of preparation method of two-dimensional bismuthene and lithium-ion battery |
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2018
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| Publication number | Publication date |
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| WO2019128247A1 (en) | 2019-07-04 |
| CN108284220A (en) | 2018-07-17 |
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