CN114990358A - Arsenic-doped alkene nanosheet, and preparation method and application thereof - Google Patents

Arsenic-doped alkene nanosheet, and preparation method and application thereof Download PDF

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CN114990358A
CN114990358A CN202210383646.7A CN202210383646A CN114990358A CN 114990358 A CN114990358 A CN 114990358A CN 202210383646 A CN202210383646 A CN 202210383646A CN 114990358 A CN114990358 A CN 114990358A
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arsenic
doped
treatment
precursor
alkene
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CN114990358B (en
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赵飞平
田金
王伟杰
柴立元
闵小波
刘振兴
梁彦杰
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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
    • H01L31/0264—Inorganic materials
    • H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
    • H01L31/0321—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 characterised by the doping material
    • 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 preparation method of an arsenic-doped alkene nanosheet, which comprises the following steps: s1, calcining the dopant, the transmission agent and the simple substance arsenic by adopting a gas phase transmission method to obtain a precursor; wherein the dopant is elemental bismuth or elemental tellurium; the transmission agent is elementary iodine or iodide; and S2, sequentially carrying out soaking treatment, grinding treatment, dispersing treatment, ultrasonic liquid phase stripping treatment and solid-liquid separation treatment on the precursor to obtain a supernatant, wherein the supernatant is a dispersion containing the arsenic-doped alkene nanosheets. According to the invention, the modification of the arsenic-doped graphene nanosheet is completed, the arsenic-doped graphene nanosheet material is effectively obtained, new elements are doped into the arsenic-doped graphene nanosheet, and the arsenic-doped graphene nanosheet material can keep a lamellar structure; and when the doped arsenic alkene nano sheet is thicker, the doped arsenic alkene nano sheet still has a band gap, so that the application of the doped arsenic alkene nano sheet as a semiconductor material is facilitated.

Description

Arsenic-doped alkene nanosheet, and preparation method and application thereof
Technical Field
The invention relates to an arsenic alkene material, in particular to an arsenic alkene-doped nanosheet, and a preparation method and application thereof.
Background
The III-V group element two-dimensional material is widely researched in the last decade due to the characteristics of quantum-constrained electronic band structure, adjustable band gap along with the number of layers, excellent electron transfer performance and the like. However, to date, all reported two-dimensional semiconductors have a characteristic bandgap of less than 2.0eV, which greatly limits their applications, particularly in optoelectronic devices that are photoresponsive in the blue and ultraviolet range.
Researchers find that the single-layer arsenic alkene nanosheet material in the V-group element has the advantages of super large band gap, super high carrier mobility, super large on-off ratio and the like, and is expected to make up for the defects of other materials in semiconductor application; however, the arsenic alkene nano-sheet has special layer number dependency, that is, when the layer number of the arsenic alkene nano-sheet is more than or equal to three layers, the nano-sheet material presents a gapless structure, thereby greatly limiting the application value of the arsenic alkene nano-sheet.
In order to improve the performance and the applicability of the arsenic-olefin nanosheet, the arsenic-olefin nanosheet needs to be doped and modified to make up for the defects of the traditional arsenic-olefin nanosheet, so that the layer number of the arsenic-olefin nanosheet is still in a band gap structure when the layer number is more than or equal to three layers; however, no relevant preparation process of the arsenic-doped alkene nanosheet exists in the prior art so far, so that research on the arsenic-doped alkene nanosheet has not made a substantial breakthrough.
In view of the above, there is a need to provide an arsenic-doped alkene nanosheet, and a preparation method and an application thereof, so as to solve or at least alleviate the problems of poor performance of the arsenic-doped alkene nanosheet, inability to effectively obtain the arsenic-doped alkene nanosheet, and the like.
Disclosure of Invention
The invention mainly aims to provide an arsenic-doped alkene nanosheet, and a preparation method and application thereof, and aims to solve or at least relieve the problems that the arsenic-doped alkene nanosheet is poor in performance, cannot be effectively obtained and the like.
In order to achieve the purpose, the invention provides a preparation method of an arsenic-doped alkene nano sheet, which comprises the following steps:
s1, calcining the dopant, the simple substance arsenic and the transmission agent by adopting a gas phase transmission method to obtain a precursor;
wherein the dopant comprises elemental bismuth or elemental tellurium; the transmission agent comprises elemental iodine or iodide;
s2, sequentially carrying out soaking treatment, grinding treatment, dispersing treatment, ultrasonic liquid phase stripping treatment and solid-liquid separation treatment on the precursor to obtain a supernatant, wherein the supernatant is a dispersion containing the arsenic-doped alkene nanosheets;
wherein the soaking treatment comprises: soaking the precursor into a first organic solvent;
the grinding treatment comprises the following steps: drying and grinding the soaked precursor in sequence to obtain precursor powder;
the dispersion treatment comprises: dispersing the precursor powder into a second organic solvent.
Further, in the step S1, the molar ratio of the dopant, the elemental arsenic and the transport agent is 1-10: 50: 0.5-1.
Further, in the step S1, the operation process of the gas phase transport method includes: and placing the dopant, the simple substance arsenic and the transmission agent in a quartz tube, then placing the quartz tube in a double-temperature-zone tube furnace after vacuum sealing, and calcining under a set temperature field.
Further, the temperature field adopted by the gas phase transmission method is 500-550 ℃ or 550-600 ℃; the calcination time is 0.5-3 h.
Further, the operation process of the gas phase transmission method also comprises the following steps: and after the calcination is finished, reducing the temperature in the quartz tube to room temperature at a cooling rate of 0.5-5 ℃/min.
Further, in the step S2, the first organic solvent and the second organic solvent each include nitrogen-methyl pyrrolidone;
in the dispersion treatment, the mass-to-volume ratio of the precursor powder to the second organic solvent is 100-400mg:40 ml.
Further, the power of the ultrasonic liquid phase stripping treatment is 100-130W, and the treatment time of the ultrasonic liquid phase stripping treatment is 15-18 h.
Further, the purity of the simple substance arsenic is not less than 99.999%; the purity of the simple substance bismuth or the simple substance tellurium is not less than 99.99 percent; the duration of the soaking treatment is 1-3 days.
The invention also provides an arsenic-doped alkene nanosheet, which is prepared by the preparation method.
The invention also provides an application of the doped arsenic-doped alkene nano sheet as a semiconductor material.
Compared with the prior art, the invention has the following advantages:
according to the invention, the modification of the arsenic-doped graphene nanosheet is completed, the arsenic-doped graphene nanosheet material is effectively obtained, new elements are doped into the arsenic-doped graphene nanosheet, and the arsenic-doped graphene nanosheet material can keep a lamellar structure; and when the arsenic-doped alkene nano sheet is thicker and is multi-layered, the arsenic-doped alkene nano sheet still has a band gap, so that the application of the arsenic-doped alkene nano sheet as a semiconductor material is facilitated.
Specifically, bismuth and tellurium are selected as doping elements, iodine is selected as a transmission agent, and a precursor of the arsenic-doped alkene nanosheet is successfully synthesized by a gas phase transmission method, so that the doping material is ensured to be still in a lamellar structure, and the arsenic-doped alkene nanosheet can be conveniently obtained by a subsequent ultrasonic liquid phase stripping method. Moreover, the preparation method adopted by the invention is simple and 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 TEM and AFM images of arsine nanoplatelets of comparative example 1;
FIG. 2 is an optical photograph of the precursor of example 1 and a TEM image of bismuth-doped arsenene nanoplates; wherein (a) is an optical photograph of the precursor in example 1; (b) is a TEM image of the bismuth-doped arsene nanoplatelets of example 1;
FIG. 3 is a mapping diagram of the elements of bismuth-doped arsalene nanosheets of example 1;
FIG. 4 is an optical photograph of the precursor of example 2 and a TEM image of a tellurium-doped arsenene nanoplate; wherein (a) is an optical photograph of the precursor in example 2; (b) is a TEM image of the tellurium doped arsenene nanoplates of example 2;
FIG. 5 is a mapping diagram of the elements of the tellurium-doped arsenene nanosheets of example 2;
FIG. 6 is an optical photograph of bismuth-doped arsalene nanoplatelets from examples 3-5;
FIG. 7 is an optical photograph of the tellurium-doped arsenene nanoplates of examples 6-7.
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.
Moreover, the technical solutions in the embodiments of the present invention may be combined with each other, but it is necessary to be based on the realization of the technical solutions by those skilled in the art, and when the technical solutions are contradictory to each other or cannot be realized, such a combination of the technical solutions should not be considered to exist, and is not within the protection scope claimed by the present invention.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs and are intended to be open ended, i.e., to include any methods, devices, and materials similar or equivalent to those described in the examples.
The invention provides a preparation method of an arsenic-doped alkene nanosheet, which is characterized by comprising the following steps:
s1, weighing the dopant, the simple substance arsenic and the transport agent into a quartz tube according to a required proportion, then carrying out vacuum sealing on the quartz tube, and synthesizing the precursor doped with the arsenic-alkene nano-sheet by using a gas phase transport method.
Wherein the molar ratio of the dopant, the elemental arsenic (arsenic chunk) and the transport agent can be 1-10: 50: 0.5-1.
The dopant comprises simple substance bismuth or simple substance tellurium, and specifically can be bismuth powder or tellurium powder; the transmission agent comprises elementary iodine or iodide, and particularly, the iodide can be tin iodide; to reduce the introduction of impurities, the iodide may also be bismuth iodide or tellurium iodide.
It is noted that the arsenic lumps used in the present invention have a purity of not less than 99.999%; the purity of the bismuth powder or the tellurium powder used by the invention is not less than 99.99%.
As one of the preferable options, bismuth powder, arsenic nuggets and tin iodide may be calcined at a molar ratio of 3:50: 1.
As another preferred option, tellurium powder, arsenic nuggets and tin iodide may be calcined at a molar ratio of 3:50: 0.5.
As an illustration of the gas phase transport method: the gas phase transmission method is that the dopant, the arsenic block and the transmission agent are subjected to gas phase transmission in a closed vacuum environment; the process can be carried out under the protection of a protective gas, and the gas phase transport method can be generally carried out in a two-temperature zone tube furnace.
The gas phase transport process can be understood in particular as: due to the existence of the calcining temperature, the dopant, the transport agent and the arsenic block are converted into gas phase in the calcining process; wherein, according to the set temperature field, the gas phase substance circulates in the reaction vessel due to the temperature difference and the existence of the transmission agent, namely, the gas phase substance migrates from the high temperature area to the low temperature area, and finally is crystallized and deposited in the low temperature area after being cooled.
It is understood that the calcining temperature range formed by the low temperature zone and the high temperature zone can be called as a temperature field; in addition, in the cooling process after the calcination is finished, the cooling rates of the low-temperature area and the high-temperature area can be kept consistent, so that the temperature difference exists continuously until the two ends are cooled to the room temperature.
For the invention, the temperature field of the gas phase transmission can be 500-550 ℃ or 550-600 ℃, and the preferable temperature field can be 550-600 ℃, that is, the calcination temperature of the low temperature region is set to be 550 ℃, and the calcination temperature of the high temperature region is set to be 600 ℃; the calcination time period may be 0.5 to 3 hours, and preferably, may be 2 hours. In addition, after the calcination is completed, the temperature in the reaction vessel can be controlled to be reduced to the room temperature at a cooling rate of 0.5-5 ℃/min, and the preferred cooling rate can be 1 ℃/min.
Taking bismuth doping as an example, the specific process for synthesizing and preparing the arsenic-doped alkene nanosheet precursor by using a dual-temperature-zone tube furnace CVT (gas phase transport) method can be as follows: adding simple substance bismuth, simple substance arsenic and a transmission agent into a quartz tube according to a preset proportion, placing the quartz tube into a double-temperature-zone tube furnace after vacuum sealing, and introducing argon gas as protective gas after the quartz tube is installed in the double-temperature-zone tube furnace. Setting the temperature of one end of the double-temperature-zone tubular furnace to be 550 ℃ and the temperature of the other end of the double-temperature-zone tubular furnace to be 600 ℃; and after 2h, respectively heating the temperature of the low-temperature area and the high-temperature area from the room temperature to a set temperature, preserving the heat for 2h at the temperature, then cooling to the room temperature at a cooling speed of 1 ℃/min, finally taking the quartz tube out to a glove box, breaking the quartz tube in the glove box, and collecting the precursor of the bismuth-doped arsenene nanosheet at one side corresponding to the lower temperature.
Wherein the temperature is increased from room temperature to 550 ℃ and 600 ℃ in order to change the gasification of the raw material in the quartz tube into a gaseous state; the heat preservation at 550 ℃ and 600 ℃ is used for fully gasifying and transferring the raw materials from a high-temperature area to a low-temperature area; the cooling is to make the raw material crystallize and deposit at the low temperature end.
And S2, sequentially carrying out soaking treatment, grinding treatment, dispersing treatment, ultrasonic liquid phase stripping treatment and solid-liquid separation treatment on the precursor to obtain a supernatant, wherein the supernatant is a dispersion containing the arsenic-doped alkene nanosheets.
Wherein the soaking treatment comprises: soaking the precursor into a first organic solvent; the duration of the soaking treatment may be 1 to 3 days.
The grinding treatment comprises the following steps: and drying and grinding the precursor after soaking treatment in sequence to obtain precursor powder.
The dispersion treatment comprises: dispersing the precursor powder into a second organic solvent. Wherein the mass-volume ratio of the precursor powder to the second organic solvent can be 100-400mg:40ml, preferably 200mg:40 ml. The first organic solvent and the second organic solvent may both be nitrogen-methyl pyrrolidone solvents.
The ultrasonic liquid phase stripping treatment comprises the following steps: dispersing the precursor powder to a second organic solvent to obtain a mixed solution; stripping the mixed solution 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-one centigrade.
The solid-liquid separation treatment comprises the following steps: and centrifuging the mixed solution subjected to the ultrasonic liquid-phase stripping treatment for 30min at the rotating speed of 2000 rpm.
As an explanation of the above embodiment:
the invention mainly relates to a two-step method for preparing an arsenic-doped alkene nano sheet, which comprises the steps of preparing a precursor of the arsenic-doped alkene nano sheet and stripping the precursor. The preparation of the precursor is mainly that under a certain temperature, raw materials are fully mixed under the condition of being in a gaseous state, and doping elements enter a structure of simple substance arsenic and finally form the doping precursor through crystallization and deposition. And the stripping of the precursor is mainly to break the layered structure of the precursor by utilizing bubbles and holes generated in the ultrasonic process, and finally disperse the layered structure into few layers of arsenic-doped alkene nanosheets.
In order to obtain a high-performance material, the invention further provides an arsenic-doped alkene nano sheet prepared by the preparation method according to any embodiment.
In order to improve the application value of the doped arsenic-alkene nano-sheet, the invention also provides an application of the doped arsenic-alkene nano-sheet as a semiconductor material.
To facilitate a further understanding of the above embodiments, the following is illustrated:
comparative example 1
1. Adding 200mg of simple substance arsenic powder into 40ml of nitrogen-methyl pyrrolidone solvent to obtain a mixed solution;
2. ultrasonic liquid phase stripping (100-130W) is carried out on the mixed solution for 16.5h under the condition of-1 ℃, and the mixed solution is centrifuged for 30min under the condition of 2000rpm after stripping; taking the supernatant to finally obtain the dispersion liquid of the arsenic-alkene nano sheets.
In the comparative example, the thickness of the arsenic alkene nano-sheet is 10nm, the number of layers is about 30, and the arsenic alkene nano-sheet does not have a band gap, and a TEM image and an AFM image thereof are shown in FIG. 1.
Example 1
1. 62.694mg of bismuth powder, 374.6mg of arsenic block and 62.622mg of tin iodide (i.e. molar ratio Bi: As: SnI) 4 Adding the bismuth doped arsenic alkene nanosheet into a quartz tube at a ratio of 3:50:1), sealing in vacuum, calcining at the temperature of 550-600 ℃ for 2h, and then cooling to room temperature at a speed of 1 ℃/min to obtain a precursor of the bismuth doped arsenic alkene nanosheet;
2. soaking 200mg of the precursor in 40mL of nitrogen-methyl pyrrolidone solvent for three days, taking out, drying and grinding to obtain precursor powder; adding the precursor powder into 40ml of nitrogen-methyl pyrrolidone solvent to obtain a mixed solution;
3. ultrasonic liquid phase stripping (100-130W) is carried out on the mixed solution for 16.5h under the condition of-1 ℃, and the mixed solution is centrifuged for 30min under the condition of 2000rpm after stripping; and taking the supernatant to finally obtain the dispersion liquid of the bismuth-doped arsenic-alkene nanosheets.
In the embodiment, the thickness of the bismuth-doped arsenene nanosheet is within the range of 20nm-40nm, the band gap is 2.13eV, an optical photograph of the precursor and a TEM of the bismuth-doped arsenene nanosheet are shown in FIG. 2, and element mapping of the bismuth-doped arsenene nanosheet is shown in FIG. 3.
The method proves that the precursor still presents a layered structure after the Bi element is doped, the material after the precursor is stripped is in a nanosheet shape, the element mapping graph also proves the effective doping of the Bi element, and the Bi-doped arsenic-alkene nanosheet can be successfully prepared by the method, and the band gap of the Bi-doped arsenic-alkene nanosheet is 2.13 eV.
Example 2
1. 38.28mg of tellurium powder, 374.6mg of arsenic block and 31.311mg of tin iodide (i.e. molar ratio Te: As: SnI) 4 3:50:0.5), adding the mixture into a quartz tube, sealing in vacuum, calcining at the temperature of 550-600 ℃ for 2h, and then cooling to room temperature at the speed of 1 ℃/min to obtain a precursor of the tellurium-doped arsenic-alkene nanosheet;
2. soaking 200mg of the precursor in 40mL of nitrogen-methyl pyrrolidone solvent for three days, taking out, drying and grinding to obtain precursor powder; adding the precursor powder into 40ml of nitrogen-methyl pyrrolidone solvent to obtain a mixed solution;
3. ultrasonic liquid phase stripping (100-; and taking the supernatant to finally obtain the dispersion liquid of the tellurium-doped arsenic-alkene nanosheets.
In this embodiment, the thickness of the tellurium-doped arsenic-ene nanosheets is within the range of 40nm to 50nm, the band gap is 1.96eV, the optical photograph of the precursor and the TEM of the tellurium-doped arsenic-ene nanosheets are shown in FIG. 4, and the element mapping of the tellurium-doped arsenic-ene nanosheets is shown in FIG. 5.
The method proves that the precursor still presents a layered structure after the Te element is doped, the material stripped from the precursor is in the shape of a nanosheet, the element mapping graph also proves the effective doping of the Te element, and the method can successfully prepare the Te-doped arsenene nanosheet with the band gap of 1.96 eV.
The following are other examples of the present invention:
example 3
1. 62.694mg of bismuth powder, 374.6mg of arsenic block and 62.622mg of tin iodide (i.e. molar ratio Bi: As: SnI) 4 Adding the bismuth doped arsenic alkene nanosheet into a quartz tube at a ratio of 3:50:1), sealing in vacuum, calcining at the temperature of 550-600 ℃ for 30min, and then cooling to room temperature at a speed of 1 ℃/min to obtain a precursor of the bismuth doped arsenic alkene nanosheet; the optical photo of the precursor is shown in fig. 6, and the shape of the precursor is granular;
2. soaking 200mg of the precursor in 40mL of nitrogen-methyl pyrrolidone solvent for three days, taking out, drying and grinding to obtain precursor powder, and adding the precursor powder into 40mL of nitrogen-methyl pyrrolidone solvent to obtain a mixed solution;
3. and (2) carrying out ultrasonic liquid phase stripping (100-.
Example 4
1. 62.694mg of bismuth powder, 374.6mg of arsenic block and 62.622mg of tin iodide (i.e. molar ratio Bi: As: SnI) 4 Adding the bismuth doped arsenic nano sheet into a quartz tube at a ratio of 3:50:1), vacuum sealing, calcining at the temperature of 550-600 ℃ for 2h, and then cooling to room temperature at the speed of 5 ℃/min to obtain a precursor of the bismuth doped arsenic nano sheet; the optical photo of the precursor is shown in fig. 6, and the shape of the precursor is granular;
2. soaking 200mg of the precursor in 40mL of nitrogen-methyl pyrrolidone solvent for three days, taking out, drying and grinding to obtain precursor powder, and finally adding the precursor powder into 40mL of nitrogen-methyl pyrrolidone solvent to obtain a mixed solution;
3. and (2) carrying out ultrasonic liquid phase stripping (100-130W) on the mixed solution for 16.5h at the temperature of-1 ℃, centrifuging the stripped mixed solution for 30min at 2000rpm, and taking supernatant to finally obtain the dispersion liquid of the bismuth-doped arsenic-alkene nanosheet.
Example 5
1. 41.796mg of bismuth powder, 374.6mg arsenic block and 62.622mg tin iodide (i.e. molar ratio Bi: As: SnI) 4 Adding the bismuth doped arsenic alkene nanosheet into a quartz tube at a ratio of 2:50:1), sealing in vacuum, calcining at the temperature of 550-600 ℃ for 2h, and then cooling to room temperature at a speed of 1 ℃/min to obtain a precursor of the bismuth doped arsenic alkene nanosheet; the optical photo of the precursor is shown in fig. 6, and the shape of the precursor is granular;
2. soaking 200mg of the precursor in 40mL of nitrogen-methyl pyrrolidone solvent for three days, taking out, drying and grinding to obtain precursor powder, and finally adding the precursor powder into 40mL of nitrogen-methyl pyrrolidone solvent to obtain mixed solution;
3. and (2) carrying out ultrasonic liquid phase stripping (100-.
Example 6
1. 38.28mg of tellurium powder, 374.6mg of arsenic block and 62.622mg of tin iodide (i.e. the molar ratio Te: As: SnI) 4 Adding the tellurium-doped arsenic alkene nanosheet into a quartz tube at a ratio of 3:50:1), sealing in vacuum, calcining at the temperature of 550-600 ℃ for 2h, and then cooling to room temperature at a speed of 1 ℃/min to obtain a precursor of the tellurium-doped arsenic alkene nanosheet; the optical photo of the precursor is shown in fig. 7, the surface of the precursor is covered with black and orange blocks in irregular shapes;
2. soaking 200mg of the precursor in 40mL of nitrogen-methyl pyrrolidone solvent for three days, taking out, drying and grinding to obtain precursor powder, and finally adding the precursor powder into 40mL of nitrogen-methyl pyrrolidone solvent to obtain mixed solution;
3. and (2) carrying out ultrasonic liquid phase stripping (100-.
Example 7
1. 38.28mg of tellurium powder, 374.6mg of arsenic block and 31.311mg of tin iodide (i.e. molar ratio Te: As: SnI) 4 2:50:1), adding the mixture into a quartz tube, sealing the quartz tube in vacuum, calcining the mixture at the temperature of 550-600 ℃ for 2 hours, and then cooling the mixture to room temperature at the speed of 1 ℃/min to obtain telluriumDoping a precursor of an arsenic-alkene nano sheet; the optical photo of the precursor is shown in fig. 7, and the precursor presents a block body with an irregular shape;
2. soaking 200mg of the precursor in 40mL of nitrogen-methyl pyrrolidone solvent for three days, taking out, drying and grinding to obtain precursor powder, and finally adding the precursor powder into 40mL of nitrogen-methyl pyrrolidone solvent to obtain mixed solution;
3. and (2) carrying out ultrasonic liquid phase stripping (100-.
In summary, in the above technical solutions of the present invention, the above are only preferred embodiments of the present invention, and the technical scope of the present invention is not limited thereby, and all equivalent structural changes made by using the contents of the specification and the drawings of the present invention or other related technical fields directly/indirectly applied thereto are included in the scope of the present invention.

Claims (10)

1. A preparation method of an arsenic-doped alkene nano sheet is characterized by comprising the following steps:
s1, calcining the dopant, the simple substance arsenic and the transmission agent by adopting a gas phase transmission method to obtain a precursor;
wherein the dopant comprises elemental bismuth or elemental tellurium; the transport agent comprises elemental iodine or iodide;
s2, sequentially carrying out soaking treatment, grinding treatment, dispersing treatment, ultrasonic liquid phase stripping treatment and solid-liquid separation treatment on the precursor to obtain a supernatant, wherein the supernatant is a dispersion containing the arsenic-doped alkene nanosheets;
wherein the soaking treatment comprises: soaking the precursor into a first organic solvent;
the grinding treatment comprises the following steps: drying and grinding the soaked precursor in sequence to obtain precursor powder;
the dispersion treatment comprises: dispersing the precursor powder into a second organic solvent.
2. The method according to claim 1, wherein in the step S1, the molar ratio of the dopant, the elemental arsenic and the transport agent is 1-10: 50: 0.5-1.
3. The method according to claim 1, wherein in the step S1, the operation process of the gas phase transport method includes: and placing the dopant, the elemental arsenic and the transport agent in a quartz tube, then placing the quartz tube in a double-temperature-zone tube furnace after vacuum sealing, and calcining under a set temperature field.
4. The method as claimed in claim 3, wherein the temperature field used in the gas phase transport method is 500-550 ℃ or 550-600 ℃; the calcination time is 0.5-3 h.
5. The method of claim 3, wherein the gas phase transport process further comprises: and after the calcination is finished, reducing the temperature in the quartz tube to room temperature at a cooling rate of 0.5-5 ℃/min.
6. The production method according to claim 1, characterized in that, in the step S2, the first organic solvent and the second organic solvent each include nitrogen-methylpyrrolidone;
in the dispersion treatment, the mass-to-volume ratio of the precursor powder to the second organic solvent is 100-400mg:40 ml.
7. The preparation method as claimed in claim 1, wherein the power of the ultrasonic liquid phase stripping treatment is 100-130W, and the treatment time of the ultrasonic liquid phase stripping treatment is 15-18 h.
8. The method according to any one of claims 1 to 7, wherein the elemental arsenic has a purity of not less than 99.999%; the purity of the simple substance bismuth or the simple substance tellurium is not less than 99.99 percent; the duration of the soaking treatment is 1-3 days.
9. Arsenic-doped alkene nanosheets, characterized in that they have been prepared by a process according to any one of claims 1 to 8.
10. Use of a doped arsalene nanoplatelet of claim 9 as a semiconductor material.
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Publication number Priority date Publication date Assignee Title
US3392066A (en) * 1963-12-23 1968-07-09 Ibm Method of vapor growing a homogeneous monocrystal
JPS6042819A (en) * 1983-06-08 1985-03-07 ステンカ−・コ−ポレ−シヨン Foam semiconductor doping agent carrier
CN108145171A (en) * 2017-12-26 2018-06-12 深圳大学 A kind of bismuth alkene nanometer sheet and preparation method thereof
CN112008086A (en) * 2020-08-25 2020-12-01 沈阳航空航天大学 Antimonene nanosheet effectively stripped through physical modification and preparation method thereof
CN113817927A (en) * 2021-10-09 2021-12-21 中南大学 Method for efficiently preparing arsenic-alkene nanosheets

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3392066A (en) * 1963-12-23 1968-07-09 Ibm Method of vapor growing a homogeneous monocrystal
JPS6042819A (en) * 1983-06-08 1985-03-07 ステンカ−・コ−ポレ−シヨン Foam semiconductor doping agent carrier
CN108145171A (en) * 2017-12-26 2018-06-12 深圳大学 A kind of bismuth alkene nanometer sheet and preparation method thereof
CN112008086A (en) * 2020-08-25 2020-12-01 沈阳航空航天大学 Antimonene nanosheet effectively stripped through physical modification and preparation method thereof
CN113817927A (en) * 2021-10-09 2021-12-21 中南大学 Method for efficiently preparing arsenic-alkene nanosheets

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