CN115807211B - Preparation method and device of arsenic-phosphorus film material - Google Patents
Preparation method and device of arsenic-phosphorus film material Download PDFInfo
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- CN115807211B CN115807211B CN202310083671.8A CN202310083671A CN115807211B CN 115807211 B CN115807211 B CN 115807211B CN 202310083671 A CN202310083671 A CN 202310083671A CN 115807211 B CN115807211 B CN 115807211B
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Abstract
The invention provides a preparation method and a device of an arsenic-phosphorus film material. The preparation method of the arsenic-phosphorus thin film material comprises the steps of heating at 400-450 ℃ under vacuum condition to volatilize the black phosphorus-arsenic crystal, depositing the black phosphorus-arsenic crystal on a substrate, and forming the arsenic-phosphorus thin film material on the substrate; wherein the substrate is positioned above the black phosphorus arsenic crystal. The method is simple and easy to operate, and solves the problems that the arsenic-phosphorus thin film material in the prior art has small size, the thinnest thickness can only reach the micron level, the thickness is uncontrollable, the arsenic-phosphorus thin film material with large area and uniform thickness is difficult to obtain, or organic impurities are easy to introduce, and the like. The prepared arsenic-phosphorus film material can be used as a precursor for preparing a large-area black phosphorus-arsenic two-dimensional film, so that the material is applied to manufacturing of semiconductor devices.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a preparation method and a preparation device of an arsenic-phosphorus film material.
Background
With the advancement of technology, the current society is entering the "post-molar age" with the continued need for shrinking semiconductor device dimensions. With the discovery of two-dimensional materials such as graphene, black phosphorus and the like, the graphene-black phosphorus composite material is excellentThe properties of black phosphorus and arsenic have been paid more and more attention to in the field of semiconductor devices, and as a novel two-dimensional material, black phosphorus and arsenic have a moderately adjustable band gap structure (0.15-0.3 and eV), so that the spectral blank between the zero band gap of graphene and the relatively large band gap (5-6 and eV) of hexagonal boron nitride can be filled, and the response of a medium-long wave infrared region can be realized. Meanwhile, the black phosphorus arsenic has anisotropic photoelectric property and theoretical carrier mobility (14000 cm) higher than that of transition metal disulfide 2 V -1 s -1 ). Based on these excellent characteristics, some exciting applications of black phosphorus and arsenic have been reported, such as field effect transistors, photoconductors, mid-wave infrared photodetectors, silicon photon microheaters, lithium ion batteries, solar exciton batteries, lasers, and the like, and black phosphorus and arsenic are also considered as a very promising material for the mid-wave infrared photodetectors field.
However, direct preparation of a small-layer even single-layer large-area arsenic-phosphorus film material is not realized at present. The top-down method is the main stream method for preparing the arsenic-phosphorus two-dimensional material at present, namely, a block-shaped black phosphorus-arsenic crystal is synthesized by a chemical vapor transport method, and then the black phosphorus-arsenic crystal is stripped by various methods to obtain the arsenic-phosphorus two-dimensional material. However, the arsenic-phosphorus two-dimensional material obtained by stripping in any method has small size and thinnest thickness, can only reach the micron level, has uncontrollable thickness, or is easy to introduce organic impurities. In view of this, it is necessary to provide a method and apparatus for preparing an arsenic-phosphorus thin film material, so as to use this as a precursor to realize the synthesis of a large-area black phosphorus-arsenic two-dimensional thin film.
Disclosure of Invention
The invention mainly aims to provide a preparation method and a preparation device of an arsenic-phosphorus film material, and aims to solve the problems that the size of the arsenic-phosphorus film material in the prior art is small, the thinnest thickness can only reach a micron level, the thickness is uncontrollable, the arsenic-phosphorus film material with large area and uniform thickness is difficult to obtain, or organic impurities are easy to introduce and the like.
In order to achieve the above purpose, the invention provides a preparation method of an arsenic-phosphorus thin film material, which comprises the steps of heating at 400-450 ℃ under vacuum condition to volatilize black phosphorus-arsenic crystals, depositing the black phosphorus-arsenic crystals on a substrate, and forming the arsenic-phosphorus thin film material on the substrate; wherein the substrate is positioned above the black phosphorus arsenic crystal.
Further, the vacuum degree of the vacuum condition<10 -6 pa。
Further, the deposition time is 10-180 s.
Further, the substrate is in a rotated state.
Further, the distance between the substrate and the black phosphorus arsenic crystal is 30-100 cm.
The invention also provides the arsenic phosphorus thin film material prepared by the preparation method of any one of the arsenic phosphorus thin film materials.
The invention also provides a device for the preparation method of the arsenic phosphorus film material according to any one of the above, which comprises a vacuum bell jar and a vacuum cavity; the vacuumizing mechanism is communicated with the vacuum cavity of the vacuum bell jar; the evaporation chamber is arranged in the vacuum chamber and is used for placing and heating the black phosphorus arsenic crystals; the deposition table is arranged in the vacuum cavity and is positioned above the evaporation cavity so as to support the substrate.
Further, the deposition station is a rotary stage to rotate the substrate during deposition in the preparation of the arsenic phosphorus thin film material.
Further, the distance between the deposition table and the base of the evaporation chamber is 30-100 cm.
The invention has the beneficial effects that:
first, the invention provides an arsenic-phosphorus thin film material, wherein the thickness of the arsenic-phosphorus thin film material is less than 50nm. The arsenic-phosphorus film material is uniform, large in area and high in purity; can be used as a precursor for preparing a large-area black phosphorus arsenic two-dimensional film, thereby being applied to the manufacture of semiconductor devices.
In addition, by the preparation method of the arsenic-phosphorus thin film material, the black phosphorus-arsenic crystals are volatilized by heating under the vacuum condition and deposited on the substrate, and the arsenic-phosphorus thin film material is formed on the substrate, so that the defects of small size, uncontrollable thickness and easiness in introducing organic impurities in the preparation of the two-dimensional material in the prior art are overcome. The preparation method is simple, and the prepared film has high purity, the thickness reaches nano-scale uniformity and controllability, and the area is not limited to meet the requirements.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an apparatus used in a method for preparing an arsenic phosphorus thin film material;
FIG. 2 is a schematic diagram of the arsenic phosphorus thin film material obtained in example 1;
FIG. 3 is a schematic representation of the arsenic phosphorus thin film material obtained in example 2;
FIG. 4 is a schematic diagram of the arsenic phosphorus thin film material obtained in example 3;
FIG. 5 is a Transmission Electron Microscope (TEM) image of the arsenic phosphorus thin film material obtained in example 1;
FIG. 6 is a transmission electron microscope (TEM-EDS) diagram of the arsenic phosphorus thin film material obtained in example 1;
FIG. 7 is a Raman spectrum (Raman) comparison chart of the arsenic phosphorus thin-film materials obtained in examples 1 to 3;
FIG. 8 is an Atomic Force Microscope (AFM) image of the arsenic phosphorus thin film material obtained in example 2;
FIG. 9 is a graph of the height statistics of the white dashed area in an Atomic Force Microscope (AFM) image of the arsenic phosphorus thin film material obtained in example 2;
FIG. 10 is an Atomic Force Microscope (AFM) image of the two-dimensional material obtained in comparative example 1.
The achievement of the object, functional features and advantages of the present invention will be further described with reference to the drawings in connection with the embodiments.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
It should be noted that the following embodiments and features in the embodiments may be combined with each other without conflict. It is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention.
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 to which this invention belongs, and any method, apparatus, or material of the prior art similar or equivalent to the methods, apparatus, or materials described in the examples of this invention may be used to practice the invention. It should be appreciated by those skilled in the art that for one of the purposes of this specification, an "Element type" may be denoted as an Element type, and a "Content" may be denoted as the atomic ratio of the arsenic-phosphorus thin film material without affecting the actual understanding of the technical solution of this application.
Where numerical ranges are provided in the examples, it is understood that unless otherwise stated herein, both endpoints of each numerical range and any number between the two endpoints are significant both in the numerical range. The test methods in the following examples, in which specific conditions are not noted, are generally conducted under conventional conditions or under conditions recommended by the respective manufacturers. The materials or reagents required in the examples below are commercially available unless otherwise specified.
In order to solve the problems that the arsenic-phosphorus thin film material in the prior art has small size, thinnest thickness, only micron-sized thickness and uncontrollable thickness, is difficult to obtain the arsenic-phosphorus thin film material with large area and uniform thickness, or organic impurities are easy to introduce, and the like, the invention provides a preparation method of the arsenic-phosphorus thin film material, which comprises the steps of heating at 400-450 ℃ under vacuum condition to volatilize black phosphorus arsenic crystals, depositing the black phosphorus arsenic crystals on a substrate, and forming the arsenic-phosphorus thin film material on the substrate; wherein the substrate is positioned above the black phosphorus arsenic crystal.
Specifically, under vacuum condition, heating the black phosphorus arsenic crystal at 400-450 ℃, and when the heating temperature exceeds the volatilization point, volatilizing the black phosphorus arsenic crystal upwards into black phosphorus arsenic vapor. When the temperature is controlled within the temperature range of 400-450 ℃, slow volatilization of black phosphorus arsenic crystals can be realized, and further controllable preparation of the film thickness is realized. Meanwhile, the size and thickness of the arsenic-phosphorus thin film material formed by depositing black phosphorus-arsenic vapor on the substrate from bottom to top can be controlled by regulating the area and the deposition time of the substrate. Overcomes the defects of small size, uncontrollable thickness and easy introduction of organic impurities in the prior art for preparing the two-dimensional material.
Illustratively, black phosphorus arsenic crystals may be obtained by calcining ash arsenic (As), red phosphorus (P) and an iodine-based additive in a vapor phase synthesis process. Wherein, the mass ratio of the gray arsenic (As), the red phosphorus (P) and the iodine-based additive can be 22:9:2-4; the iodine-based additive may be antimony iodide (SbI) 3 ) Tantalum iodide (TaI) 5 ) Or bismuth iodide (BiI) 3 ) The method comprises the steps of carrying out a first treatment on the surface of the The calcination temperature is 480-520 ℃.
Specifically, placing the ash arsenic (As), red phosphorus (P) and an iodine-based additive in a quartz tube according to the mass ratio of 22:9:2-4, vacuum sealing the quartz tube, placing the quartz tube in a double-temperature-zone tube furnace, and heating both a high-temperature zone and a low-temperature zone to respective set temperatures so As to calcine the ash arsenic, red phosphorus and iodine-based additive in a set temperature field. The high temperature region can be understood as a high temperature reaction region, the low temperature region can be understood as a low temperature deposition region, and the temperature field is formed by the high temperature region and the low temperature region together; in the reaction process, after the temperatures of the high-temperature area and the low-temperature area are stable, the temperature of the high-temperature area is not lower than 550 ℃, and the temperature of the low-temperature area is 450-530 ℃; illustratively, the temperature of the high temperature region may be 550-600 ℃; the temperature in the low temperature region may be 480 to 520 ℃.
Further, the degree of vacuum of the vacuum condition<10 -6 pa. To achieve the condition approaching vacuum, thereby reducing air molecules and targets in the evaporation processThe collision between gaseous molecules realizes the preparation of uniform films.
Further, the deposition time is 10-180 s. And (3) controlling the deposition time to be 10-180 s to obtain the arsenic-phosphorus film material with the thickness of less than 50nm.
Further, the substrate is in a rotated state. The substrate material may be in particular silicon (Si)/silicon dioxide (SiO 2 ) Sheet, mica sheet (KAl) 2 (AlSi 3 O 10 )(OH) 2 ) Or fluorogenic mica flakes (KMg) 3 (AlSi 3 O 10 )F 2 ). The substrate in a rotating state drives gas molecules to rotate by utilizing centrifugal force, the aggregation degree of the gas molecules is reduced by utilizing the centrifugal effect at high rotating speed, the gas molecules are dispersed by pressure difference generated by the action of the gas molecules and fluidization airflow, the uniformity of gas molecule distribution is improved, and the uniform deposition of black phosphorus and arsenic vapor on the substrate in the deposition process is facilitated.
Further, the distance between the substrate and the black phosphorus arsenic crystal is 30-100 cm. The distance between the substrate and the black phosphorus arsenic crystal is controlled within the range of 30-100 cm so as to ensure the effectiveness and uniformity of deposition.
The invention provides an arsenic-phosphorus thin film material prepared by the preparation method of any one of the arsenic-phosphorus thin film materials. Specifically, the thickness of the resulting arsenic-phosphorus thin film material can be controlled to be on the order of nanometers, for example, an arsenic-phosphorus thin film material having a thickness of <50nm.
The invention also provides a device for the preparation method of the arsenic phosphorus film material according to any one of the above, which comprises a vacuum bell jar 2 with a vacuum cavity (not shown); the vacuumizing mechanism is communicated with the vacuum cavity of the vacuum bell jar 2; an evaporation chamber (not shown) disposed in the vacuum chamber for placing and heating the black arsenic phosphate crystal; the deposition table is arranged in the vacuum cavity and is positioned above the evaporation chamber to support the substrate 4.
Further, the deposition station is a rotary stage 3 to put the substrate 4 in rotation during deposition in the preparation of the arsenic phosphorus thin film material. Specifically, the rotation speed of the substrate 4 can be controlled by adjusting the digital display workbench 1, so that the black phosphorus arsenic vapor is uniformly formed into a film in the deposition process.
Illustratively, referring to fig. 1, a vacuum bell jar 2 is connected to a connection base (not shown) of a vacuum pumping mechanism, and a chamber formed by the connection base and the vacuum bell jar 2 is a vacuum chamber. The vacuumizing mechanism comprises a connecting seat, a corrugated pipe 9 and a vacuum pump 10 which is connected to the connecting seat by means of the corrugated pipe 9 and is far away from one side of the vacuum cavity. A tungsten boat 6, a tungsten wire 7 and a heating electrode 8 for supplying heat to the tungsten boat 6 are arranged at the lower part of the vacuum cavity. A deposition station (not shown) is disposed in the upper portion of the vacuum chamber, and specifically includes a rotary stage 3 for cooperation therewith, a clamping plate (not shown) disposed on the rotary stage 3, and a baffle plate 5 for fixing the substrate 4 to collect the vaporized material (e.g., black phosphorus arsenic vapor). The chamber formed between the baffle plate 5 and the tungsten boat 6 is an evaporation chamber. The digital display workbench 1 is connected with a connecting seat of the vacuumizing mechanism so as to regulate and control various parameters in the specific preparation process.
The specific working mode of the device used in the preparation method of the arsenic-phosphorus film material is that black phosphorus-arsenic crystals are placed in a tungsten boat 6, a tungsten wire 7 is used for fixing the position, and a substrate 4 is fixed on a rotary objective table 3 by a clamping piece; then the vacuumizing time is controlled to be 10-60 min through the vacuum pump 10 and the digital display workbench 1 in a cooperative mode, so that the vacuum degree in the vacuum cavity is ensured to be less than 10-6 pa; after the vacuum degree is ensured to meet the requirement, the evaporation temperature, the heating time, the preheating time, the deposition time and the like can be controlled by the digital display workbench 1 so as to realize the volatilization of black phosphorus arsenic crystals and the controllable preparation of the arsenic phosphorus film.
Further, the distance between the deposition table and the base of the evaporation chamber is 30-100 cm. Specifically, referring to fig. 1, the distance between the rotary stage 3 and the tungsten boat 6 is 30 to 100cm.
For a further understanding of the present invention, an illustration is now given:
the black arsenic and phosphorus crystals used in examples 1 to 3 and comparative example 1 were prepared in a laboratory by the following method:
440 mg gray arsenic (As), 180 mg red phosphorus (P) and 16 mg antimony iodide (SbI) were weighed with an electronic ten-thousandth balance in a glove box under argon atmosphere 3 ) In quartzIn the tube, one end of the quartz tube is plugged by a plug, then the quartz tube is sealed by a vacuum valve, then the interior of the quartz tube is vacuumized by a tube sealing machine, and the quartz tube is sealed by an oxyhydrogen machine. Horizontally placing the quartz tube subjected to tube sealing into a double-temperature-zone tube furnace, and performing gas phase synthesis reaction after setting the temperature of the double-temperature zone; wherein the temperature of the high temperature reaction zone is 550 ℃, and the temperature of the low temperature deposition zone is 500 ℃. After the reaction of 20 h is kept, the temperature is reduced to 75 ℃ -25 ℃ through 2h synchronous cooling (namely, the temperature of a high-temperature reaction area is reduced to 75 ℃ and the temperature of a low-temperature deposition area is reduced to 25 ℃), and finally, the black phosphorus arsenic crystal is obtained after natural cooling to room temperature.
Example 1
50mg black phosphorus arsenic crystals are weighed and placed in a tungsten boat 6 of a device used in the preparation method of the arsenic phosphorus thin film material shown in fig. 1, the tungsten wires 7 are used for fixing the positions, and meanwhile, a substrate 4 is fixed on a rotary object stage 3 by using clamping pieces. The vacuum bell jar 2 is covered, the joint of the vacuum bell jar 2 and the connecting seat is sealed by transparent gel, and then the vacuum pump 10 is turned on to vacuumize the vacuum cavity. Wherein the vacuumizing time is 30 min, and the vacuum degree of the vacuum chamber is the same as that of the vacuum chamber<10 -6 pa. The material of the substrate 4 is silicon (Si)/silicon dioxide (SiO) 2 ) The sheet, substrate 4, was 1cm by 1cm in size.
Setting the heating temperature of the evaporation chamber to 450 ℃ through the digital display workbench 1; the deposition time period was 10s. An arsenic-phosphorus thin film material of 1cm x 1cm and even thickness of 5nm was obtained, and a physical diagram is shown in fig. 2.
Characterizing the obtained arsenic-phosphorus thin film material, wherein a TEM image of the arsenic-phosphorus thin film material is shown in FIG. 5; a TEM-EDS diagram of the arsenic phosphorus thin film material is shown in fig. 6. From the observation of fig. 6, it is found that, in addition to copper (Cu) and carbon (C) carried by the TEM copper mesh for carrying the object and oxygen (O) caused by oxidation of a part of the sample, the sample only had signal peaks of arsenic (As) and phosphorus (P) elements, indicating that the thin film had an ultra-high purity, and the atomic ratio of arsenic to phosphorus in the TEM-EDS results of table 1 could be obtained by conversion of the peak intensities, and from table 1, the atomic ratio of arsenic to phosphorus in the thin film was about 2.28.
TABLE 1 atomic ratio of arsenic to phosphorus in TEM-EDS results
| Element type | As | P |
| Content (atom%) | 69.48 | 30.52 |
Example 2
Compared to example 1, only the heating temperature and the deposition period were changed, namely:
the heating temperature of the evaporation chamber is set to 420 ℃ through the digital display workbench 1; the deposition time period was 60s. An arsenic-phosphorus thin film material with the thickness of 1cm and the thickness of 15nm is obtained, and a physical diagram is shown in figure 3.
Example 3
Compared to example 1, only the heating temperature and the deposition period were changed, namely:
the heating temperature of the evaporation chamber is set to 400 ℃ through the digital display workbench 1; the deposition duration was 180s. An arsenic-phosphorus thin film material with a thickness of 1cm by 1cm and a thickness of 45nm is obtained, and a physical diagram is shown in fig. 4.
Comparative example 1
Weighing 50mg of black phosphorus arsenic crystal, directly covering the surface of black phosphorus arsenic crystal with transparent adhesive tape to make it closely adhere, then carefully tearing off the adhesive tape with forceps, repeating for 3-5 times, and adhering the adhesive tape to silicon (Si)/silicon dioxide (SiO) 2 ) On the sheet, after waiting for 15 min, the tape was carefully torn off with tweezers to remove the silicon (Si)/silicon dioxide (SiO) 2 ) The sheet was observed under an optical microscope, and the results are shown in FIG. 10. The results according to FIG. 10 show that the resulting two-dimensional material is non-uniform in thickness, has a fracture and is far away in areaFar less than 1cm by 1cm.
Analytical example 1
Characterization analysis of the As-P thin film materials obtained in examples 1-3
1. A physical diagram of the arsenic phosphorus thin film material obtained in example 1 is shown in FIG. 2; a physical diagram of the arsenic phosphorus thin film material obtained in example 2 is shown in FIG. 3; a physical diagram of the arsenic phosphorus thin film material obtained in example 3 is shown in FIG. 4.
It should be noted that, because of different film thickness, the visual observation of the color development effects in examples 1 to 3 are different, and correspond to fig. 2 to 4, respectively; and the lower two shaded areas in fig. 2-4 are non-film-forming areas due to clip coverage during manufacturing. As can be seen from the observation of FIGS. 2 to 4, the arsenic phosphorus thin film materials obtained in examples 1 to 3 are uniform in thickness and almost free of impurities.
2. A comparison of Raman spectra (Raman) of the arsenic phosphorus thin film materials obtained in examples 1 to 3 is shown in FIG. 7. From the observation of fig. 7, the raman spectrum showed distinct arsenic and phosphorus vibrational peaks, as well as strong peaks depending on the film thickness variation.
3. An Atomic Force Microscope (AFM) image of the arsenic phosphorus thin film material obtained in example 2 is shown in fig. 8, and as can be seen from fig. 8, the thickness of the thin film material is uniform, no obvious height fluctuation exists, and the color difference area at the lower right corner is the blocking area of the clamping piece during deposition (i.e. no deposition product exists); as a result of analyzing the overall height of the material covered on the substrate 4 with the white dotted line area, as shown in fig. 9, it can be seen from fig. 9 that the difference between the height of the micro-spoke fluctuation and the height of the tail end (the height of the position of the substrate 4) in fig. 9 is the thickness of the thin film material is about 15 a nm a, and other embodiments can similarly obtain thickness data according to the AFM result.
In summary, the above embodiments of the present invention are only preferred embodiments of the present invention, and therefore, the scope of the present invention is not limited by the above embodiments, and all equivalent structural changes made by the description and the accompanying drawings under the technical concept of the present invention, or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (7)
1. A preparation method of an arsenic-phosphorus thin film material is characterized in that under the vacuum condition, heating is carried out at 400-450 ℃ to volatilize black phosphorus-arsenic crystals, the black phosphorus-arsenic crystals are deposited on a substrate, and the arsenic-phosphorus thin film material is formed on the substrate;
wherein the substrate is positioned above the black phosphorus arsenic crystal; the substrate is in a rotated state.
2. The method for preparing an arsenic phosphorus thin film material according to claim 1, wherein the vacuum degree of the vacuum condition<10 -6 pa。
3. The method for preparing the arsenic phosphorus thin film material according to claim 1, wherein the deposition time is 10-180 s.
4. The method for preparing an arsenic phosphorus thin film material according to claim 1, wherein a distance between the substrate and the black phosphorus arsenic crystal is 30-100 cm.
5. Use of a preparation device of an arsenic phosphorus thin film material in the preparation method of the arsenic phosphorus thin film material according to any one of claims 1 to 4, wherein the preparation device comprises:
a vacuum bell having a vacuum chamber;
the vacuumizing mechanism is communicated with the vacuum cavity of the vacuum bell jar;
the evaporation chamber is arranged in the vacuum chamber and is used for placing and heating the black phosphorus arsenic crystals;
the deposition table is arranged in the vacuum cavity and is positioned above the evaporation cavity so as to support the substrate.
6. The use of claim 5, wherein the deposition station is a rotary stage to rotate the substrate during deposition in the preparation of the arsenic phosphorus thin film material.
7. The use according to claim 5, wherein the distance between the deposition station and the base of the evaporation chamber is 30-100 cm.
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| CN107447193A (en) * | 2016-11-14 | 2017-12-08 | 深圳大学 | A kind of black phosphorus film and preparation method thereof |
| CN108538707B (en) * | 2018-03-05 | 2020-04-24 | 南京航空航天大学 | Preparation method of two-dimensional black phosphorus crystal |
| CN109913946A (en) * | 2018-04-18 | 2019-06-21 | 清华-伯克利深圳学院筹备办公室 | A kind of method that vapor transportation method prepares black arsenic phosphorus monocrystalline |
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| CN111020487B (en) * | 2019-11-21 | 2021-02-26 | 华中科技大学 | Method for preparing film of quasi-one-dimensional structure material with controllable orientation |
| CN110878425A (en) * | 2019-12-06 | 2020-03-13 | 深圳市中科墨磷科技有限公司 | Method for rapidly preparing high-quality two-dimensional black phosphorus crystal by seed crystal induction |
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