CN113817927B - Method for efficiently preparing arsenic-alkene nanosheets - Google Patents

Method for efficiently preparing arsenic-alkene nanosheets Download PDF

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CN113817927B
CN113817927B CN202111175626.2A CN202111175626A CN113817927B CN 113817927 B CN113817927 B CN 113817927B CN 202111175626 A CN202111175626 A CN 202111175626A CN 113817927 B CN113817927 B CN 113817927B
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arsenic
additive
alkene
powder
organic solvent
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CN113817927A (en
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赵飞平
田金
赖心婷
柴立元
闵小波
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/04—Obtaining arsenic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention provides a method for efficiently preparing an arsenic alkene nano sheet, which comprises the following steps: dispersing arsenic powder and an additive in an organic solvent to obtain a premix; wherein the purity of the arsenic powder is not less than 99.999%, and the additive comprises one or more of sodium hydroxide, polyvinylpyrrolidone and sodium cholate; the organic solvent comprises N-methyl pyrrolidone; sequentially carrying out ultrasonic liquid-phase stripping treatment and centrifugal separation treatment on the premix, and taking supernatant after the centrifugal separation treatment, wherein the supernatant is dispersion liquid of arsenic alkene nano sheets; in addition, the additive in the present invention may also be polyvinylpyrrolidone alone, and the organic solvent may also include nitrogen-dimethylformamide. The preparation method provided by the invention can improve the yield and quality of the arsenic-alkene nano-sheets, and the arsenic-alkene nano-sheets with few layers can be prepared.

Description

Method for efficiently preparing arsenic-alkene nanosheets
Technical Field
The invention relates to the field of arsenic alkene materials, in particular to a method for efficiently preparing arsenic alkene nano-sheets.
Background
Two-dimensional materials such as graphene have been widely studied in the past few years because of their excellent properties in a wide range of applications such as electronics, catalysis, and biosensing. However, since graphene, silylene and germanene belong to zero band gap electronic structures, subsequent efficient application of two-dimensional materials is limited. Subsequently, researchers found that when the number of layers of the arsenic alkene nanosheets was reduced to two layers or even a single layer, the arsenic alkene had band gap structures of 0.37eV and 2.49eV, respectively, while the high carrier mobility, high strength, high photoelectric absorption capability, and the like exhibited by few layers of arsenic alkene made it to have great potential in transistor applications.
At present, the preparation of the arsenic alkene nano-sheets mostly adopts an ultrasonic liquid phase stripping method, although the process flow and the used equipment of the method are simple, the yield of the method is low, and few-layer arsenic alkene nano-sheets with regular shapes are difficult to obtain.
In view of the above, there is a need to provide a method for efficiently preparing arsenic alkene nano-sheets, which solves or at least alleviates the above-mentioned disadvantages of low yield and poor quality of arsenic alkene nano-sheets.
Disclosure of Invention
The invention mainly aims to provide a method for efficiently preparing an arsenic-alkene nano-sheet, and aims to solve the technical problems of low yield and poor quality of the arsenic-alkene nano-sheet in the prior art.
In order to achieve the above object, the present invention provides a method for efficiently preparing an arsenic alkene nanosheet, comprising:
dispersing arsenic powder and an additive in an organic solvent to obtain a premix; wherein the purity of the arsenic powder is not less than 99.999 percent, and the additive comprises one or more of sodium hydroxide, polyvinylpyrrolidone and sodium cholate; the organic solvent comprises N-methyl pyrrolidone;
and sequentially carrying out ultrasonic liquid phase stripping treatment and centrifugal separation treatment on the premix, and taking supernatant after the centrifugal separation treatment, wherein the supernatant is dispersion liquid of the arsenic-alkene nanosheets.
Further, the additive is one or two of the polyvinylpyrrolidone and the sodium cholate.
Further, the mass ratio of the arsenic powder to the additive is 100-250: 50-100.
Further, the sum of the mass of the arsenic powder and the additive is 150-350 mg-40 ml of the organic solvent.
Further, the ultrasonic liquid phase peeling treatment comprises: the pre-mixture was peeled off in an ultrasonic cell disruption instrument at power of 100-.
Further, the centrifugation process comprises: the dispersion was centrifuged at 8000rpm and 2000-.
The invention also provides another method for efficiently preparing an arsenic alkene nano sheet, which comprises the following steps:
dispersing arsenic powder and an additive in an organic solvent to obtain a premix; wherein the purity of the arsenic powder is not less than 99.999 percent, and the additive comprises polyvinylpyrrolidone; the organic solvent comprises nitrogen-dimethylformamide;
and sequentially carrying out ultrasonic liquid phase stripping treatment and centrifugal separation treatment on the premix, and taking supernatant after the centrifugal separation treatment, wherein the supernatant is dispersion liquid of the arsenic-alkene nanosheets.
Further, the mass ratio of the arsenic powder to the additive is 100-250: 50-100.
Further, the sum of the mass of the arsenic powder and the additive is 150-350 mg-40 ml of the organic solvent.
Further, the ultrasonic liquid phase peeling treatment includes: the pre-mixture was peeled off in an ultrasonic cell disruption instrument at power of 100-.
Compared with the prior art, the invention has the following advantages:
the invention can improve the yield and quality of the arsenic-alkene nano-sheets, and prepares the arsenic-alkene nano-sheets with few layers; by adding the arsenic powder and the additive into the organic solvent together, the additive can promote the subsequent ultrasonic liquid phase stripping, so that more few-layer arsenic alkene nano sheets are obtained; in addition, the additive is one or more of sodium hydroxide, polyvinylpyrrolidone and sodium cholate, and the organic solvent is N-methylpyrrolidone, so that the yield of the arsenic-alkene nanosheets can be improved by 27.22%, 58.83% and 88.89% respectively under the condition that the structural property of the arsenic-alkene nanosheets is not influenced; in addition, the additive is polyvinylpyrrolidone, the organic solvent is nitrogen-dimethylformamide, the yield of the arsenic-alkene nanosheets can be improved by 129.39%, the yield of the arsenic-alkene nanosheets is greatly improved, and the obtained arsenic-alkene nanosheets are more regular in appearance under the condition that the organic solvent is nitrogen-dimethylformamide. Moreover, the preparation method adopted by the invention is simple, has low cost and is convenient for large-scale popularization and use.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a Raman spectrum of an arsenic alkene nano-sheet prepared in comparative example 1 in the invention;
FIG. 2 is a comparison graph of Raman spectra of arsenic alkene nano-sheets prepared in comparative example 1 and example 6 in the invention;
FIG. 3 is an SEM image of an arsenene nanosheet prepared in example 6 of the present invention;
FIG. 4 is a TEM image of an arsenene nanosheet prepared in example 8 of the present invention.
The implementation, functional features and advantages of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
It should be noted that all the directional indicators (such as the upper and lower … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
In addition, the descriptions related to "first", "second", etc. in the present invention are only for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature.
Moreover, the technical solutions in the embodiments of the present invention may be combined with each other, but it is necessary to be able to be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent, and is not within the protection scope of the present invention. It should be noted that, for the sake of understanding, in the drawings of the present specification, NMP represents N-methylpyrrolidone, and DMF represents N-dimethylformamide.
The invention provides a method for efficiently preparing arsenic alkene nano-sheets, which comprises the following steps:
1. dispersing arsenic powder and an additive in an organic solvent to obtain a premix; wherein the additive comprises one or more of sodium hydroxide, polyvinylpyrrolidone and sodium cholate; the organic solvent comprises N-methyl pyrrolidone;
it should be noted that the arsenic powder is high-purity arsenic powder, the purity of the high-purity arsenic powder should be not less than 99.999%, in addition, as a preferred scheme, the additive is one or two of the polyvinylpyrrolidone and the sodium cholate, and specifically, only the sodium cholate may be selected as the additive.
In the process of dispersing the arsenic powder and the additive in the organic solvent, the mass ratio of the arsenic powder to the additive can be 100-. The sum of the mass of the arsenic powder and the additive is that the volume of the organic solvent can be 150-350 mg/40 ml; for example: 40mL of 150mg, 40mL of 200mg, 40mL of 250mg, 40mL of 300mg, and 40mL of 350mg, and a preferable ratio may be 350mg to 40 mL.
2. And sequentially carrying out ultrasonic liquid phase stripping treatment and centrifugal separation treatment on the premix, and taking supernatant after the centrifugal separation treatment, wherein the supernatant is dispersion liquid of the arsenic-alkene nanosheets.
The ultrasonic liquid phase stripping treatment comprises the following steps: stripping the pre-mixture in an ultrasonic cell disruption instrument with the power of 100-; the ultrasonic liquid phase stripping treatment is performed in a circulating cooling environment, generally at a temperature of minus one degree centigrade.
The centrifugation treatment comprises: the dispersion was centrifuged at 8000rpm and 2000-. The specific rotating speed can be 2000rmp, and the centrifugation time can be 30 min.
The invention also provides another method for efficiently preparing an arsenic alkene nano sheet, which comprises the following steps:
1. dispersing arsenic powder and an additive in an organic solvent to obtain a premix; wherein the additive comprises polyvinylpyrrolidone; the organic solvent comprises nitrogen-dimethylformamide;
2. and sequentially carrying out ultrasonic liquid phase stripping treatment and centrifugal separation treatment on the premix, and taking supernatant after the centrifugal separation treatment, wherein the supernatant is dispersion liquid of the arsenic-alkene nanosheets.
It is to be noted that, in the method, the arsenic powder is also high-purity arsenic powder, the purity of the high-purity arsenic powder should be not less than 99.999%, and the mass ratio of the arsenic powder to the additive can also be 100-. The sum of the mass of the arsenic powder and the additive is that the volume of the organic solvent can also be 150-350 mg-40 ml; for example: 40mL of 150mg, 40mL of 200mg, 40mL of 250mg, 40mL of 300mg, and 40mL of 350mg, and a preferable ratio may be 350mg to 40 mL.
The ultrasonic liquid phase exfoliation treatment may also include: stripping the pre-mixture in an ultrasonic cell disruption instrument with the power of 100-; the preferred stripping time is 16.5 h. The ultrasonic liquid phase stripping treatment is performed in a circulating cooling environment, generally at a temperature of minus one degree centigrade.
The centrifugation treatment may also include: the dispersion was centrifuged at 8000rpm for 15-30min at 2000-.
It should be understood that, in the present invention, it is required to rely on the conventional ultrasonic liquid phase stripping treatment, since the elemental arsenic powder is a crystal with a significant layered structure, bubbles and cavities generated in the solution by the ultrasonic waves are broken to generate high energy impact, which leads to the dissociation between three-dimensional layered crystals, and thus a single-layer or few-layer nanosheet material can be generated.
However, it should be noted that the present invention is further improved on the basis of the traditional ultrasonic liquid phase stripping, i.e. specific additives are introduced in both methods, and in the second method, organic solvent is also changed, and by means of the added additives and the changed organic solvent, the acting force between crystal layers is weakened and the interlayer spacing thereof is increased, thereby effectively assisting the liquid phase ultrasonic stripping process.
To facilitate a further understanding of the invention, reference will now be made to the following examples:
comparative example 1
Adding 250mg of high-purity arsenic powder into 40mL of nitrogen-methyl pyrrolidone solvent, carrying out ultrasonic liquid phase stripping for a preset time at-1 ℃, wherein the preset time is 12-24h, centrifuging dispersion liquid obtained after stripping at 2000rpm, taking supernatant liquid, and finally obtaining the arsenic alkene nanosheet.
Example 1
Adding 250mg of high-purity arsenic powder and 100mg of sodium hydroxide into 40mL of nitrogen-methyl pyrrolidone solvent, carrying out ultrasonic liquid phase stripping for 18h at the temperature of-1 ℃, centrifuging dispersion liquid obtained after stripping at 2000rpm, taking supernatant liquid, and finally obtaining the arsenic-alkene nanosheet.
Example 2
Adding 250mg of high-purity arsenic powder and 100mg of ascorbic acid into 40mL of nitrogen-methyl pyrrolidone solvent, carrying out ultrasonic liquid phase stripping for 18h at the temperature of-1 ℃, centrifuging dispersion liquid obtained after stripping at the speed of 2000rpm, taking supernatant liquid, and finally obtaining the arsenic-alkene nanosheet.
Example 3
Adding 250mg of high-purity arsenic powder and 100mg of polyvinylpyrrolidone into 40mL of nitrogen-methyl pyrrolidone solvent, carrying out ultrasonic liquid phase stripping for 18h at the temperature of-1 ℃, centrifuging dispersion liquid obtained after stripping at the speed of 2000rpm, taking supernatant liquid, and finally obtaining the arsenic-alkene nanosheet.
Example 4
Adding 250mg of high-purity arsenic powder and 100mg of sodium cholate into 40mL of nitrogen-methyl pyrrolidone solvent, carrying out ultrasonic liquid phase stripping for 18h at the temperature of-1 ℃, centrifuging dispersion liquid obtained after stripping at the speed of 2000rpm, taking supernatant liquid, and finally obtaining the arsenic-alkene nanosheet.
Example 5
Adding 250mg of high-purity arsenic powder and 100mg of sodium deoxycholate into 40mL of nitrogen-methyl pyrrolidone solvent, carrying out ultrasonic liquid phase stripping for 18h at the temperature of-1 ℃, centrifuging dispersion liquid obtained after stripping at 2000rpm, taking supernatant liquid, and finally obtaining the arsenic-alkene nanosheet.
Example 6
Adding 250mg of high-purity arsenic powder into 40mL of nitrogen-dimethylformamide, carrying out ultrasonic liquid phase stripping for 16.5h at the temperature of-1 ℃, centrifuging dispersion liquid obtained after stripping at 2000rpm, taking supernatant liquid, and finally obtaining the arsenic alkene nanosheet.
Example 7
Adding 250mg of high-purity arsenic powder and 100mg of sodium cholate into 40mL of nitrogen-dimethyl formamide, carrying out ultrasonic liquid phase stripping for 16.5h at the temperature of-1 ℃, centrifuging dispersion liquid obtained after stripping at the speed of 2000rpm, taking supernatant liquid, and finally obtaining the arsenic-alkene nanosheet.
Example 8
Adding 250mg of high-purity arsenic powder and 100mg of polyvinylpyrrolidone into 40mL of nitrogen-dimethylformamide, carrying out ultrasonic liquid phase stripping for 16.5h at the temperature of-1 ℃, centrifuging dispersion liquid obtained after stripping at the speed of 2000rpm, taking supernatant liquid, and finally obtaining the arsenic alkene nanosheet.
Example 9
Description of the data:
1. the yield data for the 18h arsenic olefin nanoplatelets stripped in comparative example 1 was taken and compared to the data for examples 1-5 and is detailed in the following table:
group of Reaction conditions Yield (%) Yield increase (%)
Comparative example 1 N-methylpyrrolidone 11.61 Is free of
Example 1 N-methyl pyrrolidone + sodium hydroxide 14.77 27.22
Example 2 N-methylpyrrolidone + ascorbic acid Is free of Is composed of
Example 3 N-methylpyrrolidone + polyvinylpyrrolidone 18.44 58.83
Example 4 N-methyl pyrrolidone + sodium cholate 21.93 88.89
Example 5 N-methyl pyrrolidone + sodium deoxycholate 10.02 -13.7
As can be seen from the above table, the yields of the arsenic alkene nanoplatelets of examples 1, 3 and 4 are all higher than that of comparative example 1, while the additive used in example 1 is sodium hydroxide, the additive used in example 3 is polyvinylpyrrolidone and the additive used in example 4 is sodium cholate. Therefore, the yield of arsenic alkene stripping can be improved by adding sodium hydroxide, polyvinylpyrrolidone or sodium cholate, and the effects of polyvinylpyrrolidone and sodium cholate are particularly prominent.
2. The yield data of the arsenic alkene nanosheets stripped for 16.5h in comparative example 1 is taken and compared with the data of examples 6-8, and the comparison data is detailed in the following table:
group of Reaction conditions Yield (%) Yield increase (%)
Comparative example 1 N-methylpyrrolidone 12.35 Is free of
Example 6 N-dimethylformamide 18.03 45.99
Example 7 N-dimethylformamide + sodium cholate 8.9 -27.94
Example 8 Nitrogen-nitrogen-dimethyl formamide + polyvinylpyrrolidone 28.33 129.39
It should be noted that in the present invention, the data used in examples 1 to 5 correspond to a stripping time of 18h, while the data used in examples 6 to 8 correspond to a stripping time of 16.5h, mainly because the stripping time of 18h was selected in the early stage of the experiment, but when the organic solvent was changed to nitrogen-dimethylformamide, the stripping time of 18h did not well reflect the function of nitrogen-dimethylformamide in the preparation process of arsenic-containing nanosheets, and therefore the experimental scheme of 16.5h was used for the exploration.
As can be seen from the above table, both examples 6 and 8 can improve the yield of the arsenic-alkene nanosheets, wherein example 6 changes the organic solvent, and replaces the organic solvent with the nitrogen-dimethylformamide, and example 8 adds polyvinylpyrrolidone as an additive on the basis of replacing the organic solvent, so as to further improve the yield of the arsenic-alkene nanosheets.
In addition, for the convenience of understanding, the raman spectrum of the arsenic alkene nano-sheet prepared by different stripping time in comparative example 1 is shown in fig. 1, and the shift of the peak in the graph can be used for proving that the arsenic alkene nano-sheet is effectively prepared; as (5N) in the figure represents the Raman spectrum of the arsenic powder, 5N represents that the purity of the arsenic powder is 99.999 percent and SiO 2 Representing the Raman spectrum of the substrate, 12h, 15h, 18h, 21h and 24h in the graph correspond to the Raman spectrum of the arsenic alkene nano-sheet obtained after stripping for corresponding time.
In addition, a comparison graph of the raman spectra of comparative example 1 and example 6 is shown in fig. 2, wherein 16.5h-NMP in fig. 2 represents the raman spectrum corresponding to the peeling of 16.5h in comparative example 1, 18h-NMP represents the raman spectrum corresponding to the peeling of 18h in comparative example 1, and 16.5h-DMF represents the raman spectrum corresponding to the peeling of 16.5h in example 6, it is to be understood that the raman spectrum of the substrate is not included in fig. 2; by comparing the shift degrees of the peaks in the graph, the method can be used for explaining that two different organic solvents can realize the effective preparation of the arsenic alkene nano-sheet.
In order to facilitate the visual observation of the arsenic-alkene nano-sheets in the invention, the arsenic-alkene nano-sheets prepared in example 6 are shown in fig. 3; the arsine nanoplatelets prepared in example 8 are shown in fig. 4, and DMF shown in fig. 3 and 4 is used only to distinguish organic solvents. It can be seen that example 6 and example 8 both successfully produce regular-shaped arsenic-alkene nanosheets, but the scheme in example 8 can further improve the production yield of arsenic-alkene nanosheets by combining the yield data of example 6 and example 8.
In the above technical solutions, the above are only preferred embodiments of the present invention, and the technical scope of the present invention is not limited thereby, and all the technical concepts of the present invention include the claims of the present invention, which are directly or indirectly applied to other related technical fields by using the equivalent structural changes made in the content of the description and the drawings of the present invention.

Claims (6)

1. A method for efficiently preparing an arsenic alkene nano-sheet is characterized by comprising the following steps:
dispersing arsenic powder and an additive in an organic solvent to obtain a premix; wherein the purity of the arsenic powder is not less than 99.999 percent, and the additive comprises one or more of sodium hydroxide, polyvinylpyrrolidone and sodium cholate; the organic solvent comprises N-methyl pyrrolidone;
the mass ratio of the arsenic powder to the additive is 100-;
and sequentially carrying out ultrasonic liquid phase stripping treatment and centrifugal separation treatment on the premix, and taking supernatant after the centrifugal separation treatment, wherein the supernatant is dispersion liquid of the arsenic-alkene nanosheets.
2. The method for efficiently preparing arsenic alkene nano sheets as claimed in claim 1, wherein the additive is one or both of the polyvinylpyrrolidone and the sodium cholate.
3. The method for efficiently preparing arsenic alkene nanoplatelets as in claim 1, wherein the ultrasonic liquid phase exfoliation treatment comprises: the pre-mixture was peeled off in an ultrasonic cell disruption instrument at power of 100-.
4. The method for efficiently preparing arsenic alkene nanoplatelets as in any of the claims 1-3, wherein the centrifugation process comprises: the dispersion was centrifuged at 8000rpm and 2000-.
5. A method for efficiently preparing an arsenic alkene nano-sheet is characterized by comprising the following steps:
dispersing arsenic powder and an additive in an organic solvent to obtain a premix; wherein the purity of the arsenic powder is not less than 99.999 percent, and the additive comprises polyvinylpyrrolidone; the organic solvent comprises nitrogen-dimethylformamide;
the mass ratio of the arsenic powder to the additive is 250:50-100, and the sum of the mass of the arsenic powder and the additive is 150-350 mg-40 ml;
and sequentially carrying out ultrasonic liquid-phase stripping treatment and centrifugal separation treatment on the premix, and taking supernatant after the centrifugal separation treatment, wherein the supernatant is dispersion liquid of arsenic alkene nano sheets.
6. The method for efficiently preparing arsenic alkene nanoplatelets as in claim 5, wherein the ultrasonic liquid phase exfoliation treatment comprises: the pre-mixture was peeled off in an ultrasonic cell disruption instrument at power of 100-.
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