CN112028034A - Preparation method of selenium nanosheet - Google Patents
Preparation method of selenium nanosheet Download PDFInfo
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- CN112028034A CN112028034A CN202011024253.4A CN202011024253A CN112028034A CN 112028034 A CN112028034 A CN 112028034A CN 202011024253 A CN202011024253 A CN 202011024253A CN 112028034 A CN112028034 A CN 112028034A
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 108
- 239000011669 selenium Substances 0.000 title claims abstract description 108
- 239000002135 nanosheet Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 116
- 238000005119 centrifugation Methods 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 40
- CYRGZAAAWQRSMF-UHFFFAOYSA-N aluminium selenide Chemical compound [Al+3].[Al+3].[Se-2].[Se-2].[Se-2] CYRGZAAAWQRSMF-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000523 sample Substances 0.000 claims abstract description 29
- 239000002270 dispersing agent Substances 0.000 claims abstract description 28
- 238000005530 etching Methods 0.000 claims abstract description 28
- 239000002244 precipitate Substances 0.000 claims abstract description 27
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 239000007791 liquid phase Substances 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000002055 nanoplate Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- 238000002604 ultrasonography Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002064 nanoplatelet Substances 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000004299 exfoliation Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 14
- 238000005406 washing Methods 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 206010028980 Neoplasm Diseases 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000012221 photothermal agent Substances 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007626 photothermal therapy Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000012202 endocytosis Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011275 oncology therapy Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a preparation method of selenium nanosheets, which comprises the following steps: etching: providing a hydrofluoric acid solution with the mass fraction of 5% -20%, adding aluminum selenide into the hydrofluoric acid solution to obtain a hydrofluoric acid mixed system, transferring the hydrofluoric acid mixed system to a place with the temperature of 50-80 ℃, stirring for 1-5 hours, performing primary centrifugation on the hydrofluoric acid mixed system after stirring, and collecting precipitates; liquid phase stripping: adding the precipitate into a dispersing agent, and then carrying out ultrasonic treatment on the dispersing agent for 4-24 hours by using a probe, wherein the ultrasonic power of the probe is 200-400W, and the temperature of the dispersing agent in the ultrasonic process of the probe is not more than 25 ℃; centrifugally collecting selenium nanosheets: and performing secondary centrifugation on the dispersant subjected to the ultrasonic treatment, collecting supernatant to obtain selenium nanosheet dispersion liquid, performing tertiary centrifugation on the selenium nanosheet dispersion liquid, and collecting precipitates to obtain the selenium nanosheets. The preparation method of the selenium nanosheet has the advantages of low cost, high yield and the like.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of a selenium nanosheet.
Background
Photothermal therapy is a cancer therapy developed in recent years with little side effect and high efficiency, and the therapeutic mechanism of the photothermal therapy is mainly that a photothermal agent is used to generate local high temperature under the irradiation of near-infrared laser to kill cancer cells. The laser with the wavelength of 808nm has less damage to tissues, and water and protein substances have weaker absorption capacity, so the laser with the wavelength of 808nm can penetrate through human tissues more deeply, and the laser with the wavelength is generally selected as a light source for treatment. The two-dimensional material has small size and large specific surface area, and can enter tumor cells through endocytosis of the cells, so that the two-dimensional material has wide prospect in application to a photo-thermal agent.
Selenium is a famous anticancer element, and the nano photothermal agent prepared by utilizing the selenium has great application prospect in the field of tumor treatment. However, selenium is a non-layered material, and the general preparation method is difficult to obtain two-dimensional selenium nanosheets in large batch. Although there is a research on the preparation of selenium nanosheets by chemical vapor deposition and other methods, such methods are harsh in conditions and low in yield, and are difficult to apply to the market quickly. The common liquid phase stripping method is also utilized to prepare the selenium nanosheet, and the nanosheet is large in thickness and difficult to exert the advantages of a two-dimensional material.
Disclosure of Invention
In view of the above, the invention provides a method for preparing selenium nanosheets, which solves the problems of low yield, large thickness, severe conditions, complex preparation process and the like in the preparation process of the selenium nanosheets.
The invention provides a preparation method of selenium nanosheets, which comprises the following steps:
etching: providing a hydrofluoric acid solution with the mass fraction of 5% -20%, adding aluminum selenide into the hydrofluoric acid solution to obtain a hydrofluoric acid mixed system, transferring the hydrofluoric acid mixed system to a place with the temperature of 50-80 ℃, stirring for 1-5 hours, performing primary centrifugation on the hydrofluoric acid mixed system after stirring, and collecting precipitates;
liquid phase stripping: adding the precipitate into a dispersing agent, and then carrying out ultrasonic treatment on the dispersing agent for 4-24 hours by using a probe, wherein the ultrasonic power of the probe is 200-400W, and the temperature of the dispersing agent in the ultrasonic process of the probe is not more than 25 ℃;
centrifugally collecting selenium nanosheets: and performing secondary centrifugation on the dispersant subjected to the ultrasonic treatment, collecting supernatant to obtain selenium nanosheet dispersion liquid, performing tertiary centrifugation on the selenium nanosheet dispersion liquid, and collecting precipitates to obtain the selenium nanosheets.
Preferably, the thickness of the selenium nanosheet is 1-10 nm, and the size of the selenium nanosheet is 50-300 nm.
Preferably, in the etching process, the aluminum selenide is aluminum selenide powder, the fineness of the aluminum selenide powder is more than 200 meshes, and the mass fraction of hydrofluoric acid in the hydrofluoric acid solution is 10%.
Preferably, in the etching process, the concentration of the aluminum selenide in the hydrofluoric acid mixed system is 1-100 mg/ml.
Preferably, in the etching process, the hydrofluoric acid mixed system is transferred to the temperature of 60-70 ℃ and stirred for 1.5-2.5 h;
the rotating speed of the primary centrifugation is 5000-10000 rpm, and the time of the primary centrifugation is 5-20 min.
Preferably, in the liquid phase stripping process, the mass-to-volume ratio of the precipitate to the dispersing agent is 2-20 mg/ml, and the dispersing agent is isopropanol or deionized water.
Preferably, in the liquid phase stripping process, the ultrasonic time of the probe is 5-10 h, the ultrasonic power of the probe is 280-320W, and the temperature of the dispersing agent in the probe ultrasonic process is 10-15 ℃.
Preferably, in the process of centrifugally collecting the selenium nanosheets, the rotation speed of the secondary centrifugation is 2500-4000 rpm, and the time of the secondary centrifugation is 15-30 min.
Preferably, in the process of centrifugally collecting the selenium nanosheets, the rotating speed of the three-stage centrifugation is 8000-15000 rpm, and the time of the three-stage centrifugation is 5-10 min.
The preparation method of the selenium nanosheet comprises an etching step, a liquid-phase stripping step and a step of centrifugally collecting the selenium nanosheet. In the etching step, hydrofluoric acid is used for etching metal aluminum in the aluminum selenide, the aluminum selenide is initially stripped through etching the aluminum selenide, and the multilayer microstructure of selenium is obtained through centrifugally collecting and precipitating. In the liquid phase stripping step, the multilayer microstructure of the selenium after the primary stripping is further stripped by means of a liquid phase stripping process, and the few-layer nanosheet of the selenium is obtained. And finally, completely realizing the separation of the target selenium nanosheet generated by stripping from the multilayer microstructure of the selenium which is not effectively stripped through a two-step separation method, namely removing the multilayer microstructure of the selenium which is not effectively stripped through two-stage centrifugation to obtain a supernatant part containing the target selenium nanosheet, and collecting the target selenium nanosheet through three-stage centrifugation.
The preparation method of the selenium nanosheet can prepare the high-quality ultrathin nanosheet with small thickness, large transverse size and large surface area, the nanosheet has good biocompatibility, environmental stability and high photo-thermal conversion rate, the heating effect is good, the photo-thermal stability is high, and the preparation method can be applied to preparation of photo-thermal preparations for tumor treatment. The preparation method of the selenium nanosheet has the advantages of simple and repeatable preparation process, is lower in cost and higher in yield compared with the traditional preparation method, and can be directly applied to large-scale industrial production.
Advantages 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
In order to more clearly illustrate the contents of the present invention, a detailed description thereof will be given below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is an SEM image of aluminum selenide powder before etching;
fig. 2 is an SEM image of aluminum selenide powder after etching;
fig. 3 is an XRD spectrum of selenium nanosheet and selenium powder prepared in example 1 of the present invention;
FIG. 4 is an AFM spectrum of selenium nanoplates prepared in example 1;
fig. 5 is a graph showing photothermal effects of the selenium nanoplates prepared in example 1.
Detailed Description
While the following is a description of the preferred embodiments of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
The invention provides a preparation method of selenium nanosheets, which comprises the following steps:
etching: providing a hydrofluoric acid solution with the mass fraction of 5% -20%, adding aluminum selenide into the hydrofluoric acid solution to obtain a hydrofluoric acid mixed system, transferring the hydrofluoric acid mixed system to a place with the temperature of 50-80 ℃, stirring for 1-5 hours, performing primary centrifugation on the hydrofluoric acid mixed system after stirring, and collecting precipitates;
liquid phase stripping: adding the precipitate into a dispersing agent, and then carrying out ultrasonic treatment on the dispersing agent for 4-24 hours by using a probe, wherein the ultrasonic power of the probe is 200-400W, and the temperature of the dispersing agent in the ultrasonic process of the probe is not more than 25 ℃;
centrifugally collecting selenium nanosheets: and performing secondary centrifugation on the dispersant subjected to the ultrasonic treatment, collecting supernatant to obtain selenium nanosheet dispersion liquid, performing tertiary centrifugation on the selenium nanosheet dispersion liquid, and collecting precipitates to obtain the selenium nanosheets.
Further, the thickness of the selenium nanosheet is 1-10 nm, and the size of the selenium nanosheet is 50-300 nm.
Further, in the etching process, the aluminum selenide is aluminum selenide powder, the fineness of the aluminum selenide powder is more than 200 meshes, and the mass fraction of hydrofluoric acid in the hydrofluoric acid solution is 10%.
Further, in the etching process, in the hydrofluoric acid mixed system, the concentration of the aluminum selenide is 1-100 mg/ml.
Further, in the etching process, transferring the hydrofluoric acid mixed system to a temperature of 60-70 ℃ and stirring for 1.5-2.5 h;
the rotating speed of the primary centrifugation is 5000-10000 rpm, and the time of the primary centrifugation is 5-20 min.
Further, in the liquid phase stripping process, the mass-to-volume ratio of the precipitate to the dispersing agent is 2-20 mg/ml, and the dispersing agent is isopropanol or deionized water.
Further, in the liquid phase stripping process, the ultrasonic time of the probe is 5-10 hours, the ultrasonic power of the probe is 280-320W, and the temperature of the dispersing agent in the probe ultrasonic process is 10-15 ℃.
Further, in the process of centrifugally collecting the selenium nanosheets, the rotation speed of the secondary centrifugation is 2500-4000 rpm, and the time of the secondary centrifugation is 15-30 min.
Further, in the process of centrifugally collecting the selenium nanosheets, the rotating speed of the three-stage centrifugation is 8000-15000 rpm, and the time of the three-stage centrifugation is 5-10 min.
Example 1
A preparation method of selenium nanosheets comprises the following steps:
etching: 15ml of hydrofluoric acid solution with the mass fraction of 10% is provided, 100mg of aluminum selenide with the fineness of 200 meshes is added into the hydrofluoric acid solution, and a hydrofluoric acid mixed system is obtained. And transferring the hydrofluoric acid mixed system to a temperature of 65 ℃ and stirring for 2 hours, wherein the hydrofluoric acid etches aluminum in the aluminum selenide in the stirring process, so that the multilayer microstructure of the selenium subjected to primary stripping is obtained. And after etching is finished, centrifuging the hydrofluoric acid mixed system at 7500rpm for 10min, collecting precipitates after centrifugation, washing the precipitates with deionized water for three times, and drying after washing is finished. The step can effectively remove the residual hydrofluoric acid, prevent the residual hydrofluoric acid from influencing the subsequent liquid phase stripping process, and is also beneficial to maintaining the stability of the selenium nanosheet.
Liquid phase stripping: and dissolving the dried multilayer microstructure of the selenium in isopropanol again, stirring and dispersing to prepare a dispersion liquid with the concentration of 7.5 mg/ml. Treating the dispersion with ultrasonic probe for 7.5h, wherein the power of ultrasonic probe is 280W, and the temperature of the dispersion is maintained at 15 deg.C during ultrasonic probe treatment.
Centrifugally collecting selenium nanosheets: and (3) firstly carrying out secondary centrifugation on the dispersant subjected to the ultrasonic treatment, wherein the rotation speed of the secondary centrifugation is 3000rpm, the time of the secondary centrifugation is 20min, and collecting supernatant (at this time, the supernatant contains stripped high-quality ultrathin selenium nanosheets) after the secondary centrifugation is finished, so as to obtain the selenium nanosheet dispersion liquid. And further carrying out three-stage centrifugation on the selenium nanosheet dispersion, wherein the rotation speed of the three-stage centrifugation is 12000rpm, the time of the three-stage centrifugation is 8min, removing the supernatant and collecting the precipitate, wherein the precipitate is high-quality ultrathin selenium nanosheets.
As shown in fig. 1, the SEM image of the aluminum selenide powder before etching, and as shown in fig. 2, the SEM image of the aluminum selenide powder after etching. In comparison with fig. 1, fig. 2 clearly shows the etching trace, the middle block has been etched to have an accordion shape, aluminum has been reacted by hydrofluoric acid, and the rest is stacked selenium nanosheets, which can be subsequently stripped by probe ultrasound.
As shown in fig. 3, the selenium nanoplate prepared in example 1 has the same XRD as the commercially available selenium powder, which indicates that the preparation method of the selenium nanoplate of the present invention can prepare the selenium nanoplate. The selenium nanoplate prepared in example 1 is further subjected to an AFM test, and as shown in FIG. 4, the thickness of the selenium nanoplate prepared in example 1 is 2 to 3nm, and the size of the selenium nanoplate prepared in example 1 is 50 to 300 nm.
The selenium nanosheet prepared in example 1 was further applied to a photothermal test. Preparing 0.1mg/ml selenium nanosheet aqueous solution, placing 1ml into a quartz cuvette, and irradiating the selenium solution in the cuvette by using laser with the wavelength of 808nm and the power density of 1W/cm2, so as to test the photo-thermal performance of the selenium solution by using a thermocouple thermodetector. As shown in fig. 5, the photo-thermal effect diagram of the selenium nanosheet is shown, and the selenium nanosheet can be rapidly heated to 50-60 ℃ by performing 808nm laser irradiation for six consecutive times, which confirms that the selenium nanosheet prepared in this embodiment 1 has good heating effect and photo-thermal stability.
Example 2
A preparation method of selenium nanosheets comprises the following steps:
etching: providing 20ml of hydrofluoric acid solution with the mass fraction of 5%, and adding 100mg of aluminum selenide with the fineness of 300 meshes into the hydrofluoric acid solution to obtain a hydrofluoric acid mixed system. And transferring the hydrofluoric acid mixed system to a temperature of 80 ℃ and stirring for 5 hours, wherein the hydrofluoric acid etches aluminum in the aluminum selenide in the stirring process, so that the multilayer microstructure of the selenium subjected to primary stripping is obtained. And after etching is finished, centrifuging the hydrofluoric acid mixed system at 10000rpm for 5min, collecting precipitates after centrifugation, washing the precipitates with deionized water for three times, and drying after washing is finished. The step can effectively remove the residual hydrofluoric acid, prevent the residual hydrofluoric acid from influencing the subsequent liquid phase stripping process, and is also beneficial to maintaining the stability of the selenium nanosheet.
Liquid phase stripping: and dissolving the dried multilayer microstructure of the selenium in isopropanol again, stirring and dispersing to prepare a dispersion liquid with the concentration of 20 mg/ml. Treating the dispersion with ultrasonic probe with power of 200W for 10h, and maintaining the temperature of the dispersion at 25 deg.C during the ultrasonic treatment.
Centrifugally collecting selenium nanosheets: and (3) firstly carrying out secondary centrifugation on the dispersant subjected to the ultrasonic treatment, wherein the rotation speed of the secondary centrifugation is 2500rpm, the time of the secondary centrifugation is 30min, and collecting supernatant (at the moment, the supernatant contains stripped high-quality ultrathin selenium nanosheets) after the secondary centrifugation is finished, so as to obtain the selenium nanosheet dispersion liquid. And further carrying out three-stage centrifugation on the selenium nanosheet dispersion, wherein the rotation speed of the three-stage centrifugation is 15000rpm, the time of the three-stage centrifugation is 5min, removing the supernatant and collecting the precipitate, wherein the precipitate is high-quality ultrathin selenium nanosheets.
Example 3
A preparation method of selenium nanosheets comprises the following steps:
etching: 10ml of hydrofluoric acid solution with the mass fraction of 20% is provided, 500mg of aluminum selenide with the fineness of 400 meshes is added into the hydrofluoric acid solution, and a hydrofluoric acid mixed system is obtained. And transferring the hydrofluoric acid mixed system to a temperature of 50 ℃ and stirring for 1h, wherein the hydrofluoric acid etches aluminum in the aluminum selenide in the stirring process, so that the multilayer microstructure of the selenium subjected to primary stripping is obtained. And after etching is finished, centrifuging the hydrofluoric acid mixed system at 5000rpm for 20min, collecting precipitates after centrifugation, washing the precipitates with deionized water for three times, and drying after washing is finished. The step can effectively remove the residual hydrofluoric acid, prevent the residual hydrofluoric acid from influencing the subsequent liquid phase stripping process, and is also beneficial to maintaining the stability of the selenium nanosheet.
Liquid phase stripping: and dissolving the dried multilayer microstructure of the selenium in isopropanol again, stirring and dispersing to prepare a dispersion liquid with the concentration of 2 mg/ml. Treating the dispersion with probe ultrasound for 5h, wherein the power of probe ultrasound is 400W, and the temperature of the dispersion is maintained at 10 ℃ in the probe ultrasound process.
Centrifugally collecting selenium nanosheets: and (3) firstly carrying out secondary centrifugation on the dispersant subjected to the ultrasonic treatment, wherein the rotation speed of the secondary centrifugation is 4000rpm, the time of the secondary centrifugation is 15min, and collecting supernatant (at the moment, the supernatant contains stripped high-quality ultrathin selenium nanosheets) after the secondary centrifugation is finished, so that the selenium nanosheet dispersion liquid is obtained. And further carrying out three-stage centrifugation on the selenium nanosheet dispersion, wherein the rotation speed of the three-stage centrifugation is 8000rpm, the time of the three-stage centrifugation is 10min, removing the supernatant, and collecting the precipitate, wherein the precipitate is the high-quality ultrathin selenium nanosheet.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. A preparation method of selenium nanosheets is characterized by comprising the following steps:
etching: providing a hydrofluoric acid solution with the mass fraction of 5% -20%, adding aluminum selenide into the hydrofluoric acid solution to obtain a hydrofluoric acid mixed system, transferring the hydrofluoric acid mixed system to a place with the temperature of 50-80 ℃, stirring for 1-5 hours, performing primary centrifugation on the hydrofluoric acid mixed system after stirring, and collecting precipitates;
liquid phase stripping: adding the precipitate into a dispersing agent, and then carrying out ultrasonic treatment on the dispersing agent for 4-24 hours by using a probe, wherein the ultrasonic power of the probe is 200-400W, and the temperature of the dispersing agent in the ultrasonic process of the probe is not more than 25 ℃;
centrifugally collecting selenium nanosheets: and performing secondary centrifugation on the dispersant subjected to the ultrasonic treatment, collecting supernatant to obtain selenium nanosheet dispersion liquid, performing tertiary centrifugation on the selenium nanosheet dispersion liquid, and collecting precipitates to obtain the selenium nanosheets.
2. A method of making selenium nanoplatelets as in claim 1 wherein the thickness of the selenium nanoplatelets is from 1 to 10nm and the size of the selenium nanoplatelets is from 50 to 300 nm.
3. A method of producing selenium nanoplates as in claim 1, wherein during etching, the aluminum selenide is an aluminum selenide powder, the fineness of the aluminum selenide powder is 200 mesh or more, and the mass fraction of hydrofluoric acid in the hydrofluoric acid solution is 10%.
4. A method of making selenium nanoplates as in claim 1, wherein during etching, the concentration of aluminum selenide in the hydrofluoric acid mixed system is 1-100 mg/ml.
5. A method for preparing selenium nanoplate as claimed in claim 1 wherein in the etching process, the hydrofluoric acid mixed system is transferred to 60-70 ℃ and stirred for 1.5-2.5 h;
the rotating speed of the primary centrifugation is 5000-10000 rpm, and the time of the primary centrifugation is 5-20 min.
6. A method of preparing selenium nanoplates as in claim 1, wherein the mass to volume ratio of the precipitate to a dispersant is 2-20 mg/ml during liquid phase exfoliation, the dispersant being isopropanol or deionized water.
7. The preparation method of selenium nanosheets as claimed in claim 1, wherein the probe ultrasound time is 5-10 h, the probe ultrasound power is 280-320W, and the dispersant temperature is 10-15 ℃ during the probe ultrasound process, in the liquid phase stripping process.
8. The method for preparing selenium nanosheets of claim 1, wherein during centrifugation collection of the selenium nanosheets, the rotation speed of the secondary centrifugation is 2500-4000 rpm, and the time of the secondary centrifugation is 15-30 min.
9. The method for preparing selenium nanosheets of claim 1, wherein the rotation speed of the three-stage centrifugation is 8000 to 15000rpm and the time of the three-stage centrifugation is 5 to 10min during the centrifugation and collection of the selenium nanosheets.
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| CN114988373A (en) * | 2022-06-28 | 2022-09-02 | 安徽大学 | Quasi-two-dimensional selenium nanosheet and preparation method thereof |
| CN115947316A (en) * | 2023-01-09 | 2023-04-11 | 合肥工业大学 | Selenium disulfide nanosheet and application thereof in preparation of photo-thermal agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114988373A (en) * | 2022-06-28 | 2022-09-02 | 安徽大学 | Quasi-two-dimensional selenium nanosheet and preparation method thereof |
| CN114988373B (en) * | 2022-06-28 | 2024-03-01 | 安徽大学 | Quasi two-dimensional selenium nano-sheet and preparation method thereof |
| CN115947316A (en) * | 2023-01-09 | 2023-04-11 | 合肥工业大学 | Selenium disulfide nanosheet and application thereof in preparation of photo-thermal agent |
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