CN111790904A - Method for preparing bismuth-alkene nanosheets by liquid-phase laser irradiation method - Google Patents
Method for preparing bismuth-alkene nanosheets by liquid-phase laser irradiation method Download PDFInfo
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- CN111790904A CN111790904A CN202010447521.7A CN202010447521A CN111790904A CN 111790904 A CN111790904 A CN 111790904A CN 202010447521 A CN202010447521 A CN 202010447521A CN 111790904 A CN111790904 A CN 111790904A
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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 method for preparing bismuth-alkene nanosheets by adopting a liquid-phase laser irradiation method, which is characterized by comprising the following steps: the method specifically comprises the following steps: step 1: preheating a laser, and step 2: preparing a reaction solution required by liquid-phase laser irradiation, and step 3: stirring the reaction solution to fully dissolve the reaction solution, and carrying out step 4: adjusting the light path to enable the laser light path to vertically shoot to the central position of the reaction solution, and 5: introducing protective gas above the reaction solution, and step 6: turning on laser, adjusting the voltage of the laser to the target laser energy, continuously irradiating the reaction solution with the laser for a period of time, and 7: and (5) turning off the laser, and step 8: centrifuging the reaction solution after the irradiation is finished, and carrying out step 9: collecting the centrifuged supernatant to obtain the finished product. The device is simple, the result repeatability is strong, the environment is friendly, the prepared bismuth alkene nanosheet has the optical limiting effect, and the application of bismuth alkene in the field of laser protection is promoted.
Description
Technical Field
The invention relates to a method for preparing a bismuth-alkene nanosheet by adopting a liquid-phase laser irradiation method, and belongs to the technical field of novel nano materials.
Background
The nonlinear optical limiting effect refers to the phenomenon that the transmission light intensity of a material under low light intensity linearly increases along with the increase of the incident light intensity, and when the light intensity reaches a certain threshold value, the transmission light intensity deviates from linearity, and the transmissivity is reduced. In recent years, materials based on nonlinear optical amplitude limiting effect have great application potential in the field of laser protection materials due to the advantages of wide protection wave band, low amplitude limiting threshold, fast response, large nonlinear coefficient, high damage threshold and the like, and are widely concerned by researchers.
The nonlinear optical limiting materials studied in the early stage mainly focus on fullerene, carbon nanotube, porphyrin, phthalocyanine and the like, but with the rapid development of nanotechnology, the contribution of nanomaterials to the field of laser protection is gradually increased. In recent years, VA group simple substance two-dimensional materials such as arsene, stibene, bismuth ene and the like have attracted research interest due to the characteristics of high carrier mobility, tunable band gap, good nonlinear optical response and the like. The bismuth alkene has electron transport, semimetal bonding, spin-orbit interaction and excellent stability, so that the bismuth alkene has a wide market in the application of electronic devices. Recent studies have found that bismuthylenes are also applicable in the field of optics. For example, a joint team consisting of guo and tensile break found that the bismuth alkene nanoplatelets prepared by the ultrasonic chemical stripping method have a nonlinear optical response phenomenon. The bismuth-alkene nano-sheet has a saturated absorption phenomenon in a near-infrared region of 1.55 mu m and can be used as a saturated absorber. After the bismuth-alkene tapered device is introduced into a mode-locked fiber laser, soliton pulse laser operation can be achieved. The research shows that the bismuth alkene has the unique advantages of wide working wavelength, good stability, easy integration with an optical fiber system and the like, is expected to replace a semiconductor saturable absorber mirror and a carbon nano tube in the near future, and becomes a novel laser pulse shaping material. However, currently, studies on optical properties of bismuth-alkene are still relatively rare, especially in the field of optical limiting.
Despite the many excellent properties of bismuthenes, challenges remain with respect to the preparation of two-dimensional bismuthenes. The existing methods for synthesizing the bismuth alkene include molecular beam epitaxy, solvothermal methods and ultrasonic chemical stripping methods. Molecular beam epitaxy is a common method for preparing high-quality two-dimensional bismuth thin films, but the expensive equipment cost and strict lattice matching requirements limit the industrial development of the high-quality two-dimensional bismuth thin films. The solvothermal method for preparing bismuth nanocrystals is generally of low quality and is easy to introduce impurity atoms. The ultrasonic chemical stripping method has the problem of long time consumption, and is not beneficial to the efficient preparation of the bismuth alkene. Therefore, it is necessary to find a simple and economical method for efficiently preparing high-quality two-dimensional bismuth alkene.
Disclosure of Invention
In order to solve the technical problem, the invention discloses a method for preparing a bismuth-alkene nanosheet by adopting a liquid-phase laser irradiation method, which specifically comprises the following steps:
step 1: the laser is preheated and the laser is heated,
step 2: preparing a reaction solution required by liquid-phase laser irradiation,
and step 3: the reaction solution is stirred to be fully dissolved,
and 4, step 4: adjusting the light path to make the laser light path vertically emit to the central position of the reaction solution,
and 5: introducing protective gas above the reaction solution,
step 6: turning on laser, regulating the voltage of laser to the target laser energy, continuously irradiating the reaction solution with the laser for a period of time,
and 7: the laser is turned off and the laser is turned off,
and 8: centrifuging the reaction solution after the irradiation is finished,
and step 9: collecting the centrifuged supernatant to obtain the finished product.
Further, the specific operation process in the step 1 is to select a laser as a pulse laser, set the laser wavelength to 1064nm, adjust the laser to be in a Q-Switch continuous pulse mode, set the pulse frequency to 10Hz, set the pulse width to 10ns, and keep the laser working and preheating for 30 min.
Further, the specific operation process in the step 2 is that the reaction vessel is a double-branch quartz beaker, and 0.5g of bismuth powder and 30mL of isopropanol solution are sequentially added into the double-branch quartz beaker.
Further, the specific operation process in the step 3 is that the reaction vessel containing the reaction solution is fixed on a magnetic stirring platform, a magnetic stirrer is placed in the reaction vessel, and the rotating speed of the magnetic stirrer is set to be 800r/min until the reaction solution is fully dissolved.
Further, the specific operation process in the step 4 is to arrange a reflector above the reaction solution, adjust the inclination angle of the reflector to 45 degrees, make the laser light path vertically emit into the reaction solution, and make the laser spot fall on the central position of the reaction solution.
Further, the specific operation process in the step 5 is that argon with the purity of more than 99.999 percent is introduced to the upper part of the liquid level in the double-branch quartz beaker through the double branches of the double-branch quartz beaker to be used as protective gas.
Further, the specific operation process in the step 6 is to turn on the laser, adjust the voltage of the laser to 100mJ, and continuously irradiate the reaction solution for 1h with the laser.
Further, the specific operation process of the step 8 is to centrifuge the reaction solution after the irradiation is finished, set the rotation speed of the centrifuge to 3000r/min, and centrifuge the time to 10 min.
Has the advantages that: the experimental device of the liquid phase laser irradiation method adopted by the invention is simple and easy, and the preparation process is simple; the experimental result has strong repeatability and is environment-friendly, and the preparation method has controllable process; the method can efficiently prepare the two-dimensional bismuth-alkene nanosheet, and the prepared bismuth-alkene nanosheet has a light amplitude limiting effect, so that the application of bismuth-alkene in the field of laser protection is promoted.
Drawings
FIG. 1 is a schematic view of an experimental setup of the present invention,
FIG. 2 is a schematic view of a Z-scan experimental apparatus in an embodiment of the present invention,
FIG. 3 is a TEM representation of the bismuth alkene nanoplatelets of the present invention,
FIG. 4 is a graph of the results of Z-scan testing of the inventive bismuth alkene nanoplates,
reference numerals: 1-laser, 2-reflector, 3-double-branch quartz beaker, 4-argon, 5-magnetic stirrer, 6-reaction solution, 7-bismuth powder, 8-magnetic stirring table, 9-optical attenuator, 10-spectroscope, 11-focusing mirror, 12-cuvette, 13-opening, 14-second energy meter, 15-first energy meter and 16-inching translation device.
Detailed Description
The present invention is further illustrated by the following figures and specific examples, which are to be understood as illustrative only and not as limiting the scope of the invention, which is to be given the full breadth of the appended claims and any and all equivalent modifications thereof which may occur to those skilled in the art upon reading the present specification.
Examples
The schematic diagram of the experimental device of the invention is shown in fig. 1, and the method for preparing the bismuth-alkene nanosheets by adopting the liquid-phase laser irradiation method specifically comprises the following steps:
step 1: selecting a laser 1 as a pulse laser, setting the laser wavelength to be 1064nm, adjusting the laser 1 to be in a Q-Switch continuous pulse mode, setting the pulse frequency to be 10Hz and the pulse width to be 10ns, keeping the laser working preheating for 30min,
step 2: taking a reaction vessel as a double-branch quartz beaker 3, sequentially adding 0.5g of bismuth powder 7 and 30mL of isopropanol solution into the double-branch quartz beaker 3 to prepare a reaction solution 6 required by liquid-phase laser irradiation,
and step 3: fixing a reaction vessel filled with a reaction solution 6 on a magnetic stirring platform 8, putting a magnetic stirrer 5 into the reaction vessel, stirring the reaction solution 6 by setting the rotating speed of the magnetic stirrer 5 at 800r/min until the reaction solution 6 is fully dissolved,
and 4, step 4: a reflecting mirror 2 is arranged above the reaction solution 6, the inclination angle of the reflecting mirror 2 is adjusted to be 45 degrees so as to adjust the light path, the light path of the laser is vertically shot into the reaction solution 6, the laser spot is positioned at the central position of the reaction solution 6,
and 5: argon gas 4 with the purity of more than 99.999 percent is introduced to the upper part of the liquid surface in the double-branch quartz beaker 3 as protective gas through the double branches of the double-branch quartz beaker 3,
step 6: turning on the laser, adjusting the voltage of the laser 1 to the target laser energy of 100mJ, continuously irradiating the reaction solution with the laser for 6 hours,
and 7: the laser 1 is switched off and the laser is,
and 8: centrifuging the reaction solution 6 after the irradiation is finished, setting the rotating speed of a centrifuge to be 3000r/min and the centrifuging time to be 10min,
and step 9: collecting the centrifuged supernatant to obtain the finished product.
Performing TEM representation on the collected centrifuged supernatant, as shown in FIG. 3, and performing optical amplitude limiting performance test on the supernatant by using a Z-scan experimental apparatus, which is schematically shown in FIG. 2, and sequentially comprises a laser 1, an optical attenuator 9, a spectroscope 10 and a first energy meter 15 at the lower part thereof, a focusing mirror 11, a cuvette 12 and a jogging translation device 16 at the lower part thereof, an opening 13 and a second energy meter 14, specifically operating steps are as follows,
step a: the laser 1 is turned on for preheating, the parameters of the laser 1 are set as 532nm wavelength, 20Hz pulse frequency and 1.8ns pulse width,
step b: the computer-connected related equipment is opened up and comprises a jog translation device 16, a first energy meter 15 and a second energy meter 14,
step c: the required software is opened, the set relevant parameters comprise that the jog translation device 16 is reset, the moving distance is 80mm, the measuring ranges of the first energy meter 15 and the second energy meter 14 are Low1.735Ex104, the Triger level is 0.5%, the Fixed 50sample size, the Time interval,
step d: preparing a sample, sucking the collected supernatant by a needle syringe, injecting the supernatant into a cuvette 12 with a 1mm optical path,
step e: the cuvette 12 containing the sample is fixed by clamping means to a jogging translation device 16,
step f: the laser is turned on, the optical attenuator 9 is adjusted to control the incident laser energy to be 60 muJ,
step g: injecting a proper amount of isopropanol into the cuvette 12 to mix with the supernatant, adjusting the concentration of the sample so as to control the initial transmittance of the sample to be about 70%,
step h: the inching execution inching translation device 16 acquires data with the translation interval of 1mm each time,
step i: and (3) processing and analyzing the collected data, determining the position of a focal point as the origin of coordinates of the Z axis, and drawing a relation curve of the transmittance of the sample along with the change of the translation position of the Z axis, as shown in FIG. 4, proving that the prepared two-dimensional bismuth alkene nano-sheet has a good optical limiting effect.
The method for preparing the bismuth alkene by adopting the liquid-phase laser irradiation method has the advantages of simple experimental device, simple preparation process, strong repeatability and environmental friendliness, and is a controllable preparation method. The prepared two-dimensional bismuth-alkene nano-sheet also has good optical amplitude limiting effect, and further promotes the application of the bismuth-alkene nano-sheet in the field of laser protection.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A method for preparing bismuth-alkene nanosheets by adopting a liquid-phase laser irradiation method is characterized by comprising the following steps: the method specifically comprises the following steps:
step 1: the laser is preheated and the laser is heated,
step 2: preparing a reaction solution required by liquid-phase laser irradiation,
and step 3: the reaction solution is stirred to be fully dissolved,
and 4, step 4: adjusting the light path to make the laser light path vertically emit to the central position of the reaction solution,
and 5: introducing protective gas above the reaction solution,
step 6: turning on laser, regulating the voltage of laser to the target laser energy, continuously irradiating the reaction solution with the laser for a period of time,
and 7: the laser is turned off and the laser is turned off,
and 8: centrifuging the reaction solution after the irradiation is finished,
and step 9: collecting the centrifuged supernatant to obtain the finished product.
2. The method for preparing bismuth-alkene nano-sheets by adopting the liquid-phase laser irradiation method according to claim 1, which is characterized in that: the specific operation process of the step 1 is that a laser is selected as a pulse laser, the laser wavelength is set to be 1064nm, the laser is adjusted to be in a Q-Switch continuous pulse mode, the pulse frequency is 10Hz, the pulse width is 10ns, and the laser is kept to work and preheat for 30 min.
3. The method for preparing bismuth-alkene nano-sheets by adopting the liquid-phase laser irradiation method according to claim 1, which is characterized in that: the specific operation process of the step 2 is that the reaction vessel is a double-branch quartz beaker, and 0.5g of bismuth powder and 30mL of isopropanol solution are sequentially added into the double-branch quartz beaker.
4. The method for preparing bismuth-alkene nano-sheets by adopting the liquid-phase laser irradiation method according to claim 1, which is characterized in that: and 3, fixing the reaction container filled with the reaction solution on a magnetic stirring table, putting a magnetic stirrer into the reaction container, and setting the rotating speed of the magnetic stirrer to be 800r/min until the reaction solution is fully dissolved.
5. The method for preparing bismuth-alkene nano-sheets by adopting the liquid-phase laser irradiation method according to claim 1, which is characterized in that: and 4, specifically, arranging a reflector above the reaction solution, adjusting the inclination angle of the reflector to be 45 degrees, enabling the laser light path to vertically shoot into the reaction solution, and enabling the laser light spot to fall on the central position of the reaction solution.
6. The method for preparing bismuth-alkene nano-sheets by adopting the liquid-phase laser irradiation method according to claim 3, which is characterized in that: and 5, specifically, introducing argon with the purity of more than 99.999 percent as protective gas above the liquid level in the double-branch quartz beaker through the double branches of the double-branch quartz beaker.
7. The method for preparing bismuth-alkene nano-sheets by adopting the liquid-phase laser irradiation method according to claim 1, which is characterized in that: and 6, turning on the laser, adjusting the voltage of the laser to 100mJ, and continuously irradiating the reaction solution for 1h by the laser.
8. The method for preparing bismuth-alkene nano-sheets by adopting the liquid-phase laser irradiation method according to claim 1, which is characterized in that: and 8, centrifuging the reaction solution after the irradiation is finished, wherein the rotating speed of a centrifuge is set to 3000r/min, and the centrifuging time is set to 10 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109238974A (en) * | 2018-08-30 | 2019-01-18 | 南京理工大学 | A kind of preparation method of blind type deep ultraviolet plasma resonance nano particle |
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| CN108145171A (en) * | 2017-12-26 | 2018-06-12 | 深圳大学 | A kind of bismuth alkene nanometer sheet and preparation method thereof |
| CN108284220A (en) * | 2017-12-26 | 2018-07-17 | 深圳大学 | A kind of bismuth alkene nanometer sheet and preparation method thereof |
| CN110480021A (en) * | 2019-08-07 | 2019-11-22 | 南京理工大学 | A method of antimony alkene nanometer sheet is prepared using liquid laser irradiation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108145171A (en) * | 2017-12-26 | 2018-06-12 | 深圳大学 | A kind of bismuth alkene nanometer sheet and preparation method thereof |
| CN108284220A (en) * | 2017-12-26 | 2018-07-17 | 深圳大学 | A kind of bismuth alkene nanometer sheet and preparation method thereof |
| CN110480021A (en) * | 2019-08-07 | 2019-11-22 | 南京理工大学 | A method of antimony alkene nanometer sheet is prepared using liquid laser irradiation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109238974A (en) * | 2018-08-30 | 2019-01-18 | 南京理工大学 | A kind of preparation method of blind type deep ultraviolet plasma resonance nano particle |
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