CN115807211A - Preparation method and device of arsenic-phosphorus thin film material - Google Patents
Preparation method and device of arsenic-phosphorus thin film material Download PDFInfo
- Publication number
- CN115807211A CN115807211A CN202310083671.8A CN202310083671A CN115807211A CN 115807211 A CN115807211 A CN 115807211A CN 202310083671 A CN202310083671 A CN 202310083671A CN 115807211 A CN115807211 A CN 115807211A
- Authority
- CN
- China
- Prior art keywords
- arsenic
- phosphorus
- film material
- thin film
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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 and a device of an arsenic-phosphorus thin film material. The preparation method of the arsenic-phosphorus thin film material comprises the steps of heating at 400-450 ℃ under a 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 size of the arsenic-phosphorus thin film material is small, the thinnest thickness can only reach 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 in the prior art. 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 preparation method is applied to the manufacture of semiconductor devices.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a preparation method and a device of an arsenic-phosphorus thin film material.
Background
With the progress of technology, the society is now entering the "post-mortal era", which is accompanied by the demand for the continuous reduction of the size of semiconductor devices. With the discovery of two-dimensional materials such as graphene and black phosphorus, the excellent performance and the huge potential of the two-dimensional materials in the field of semiconductor devices are paid more and more attention, and as a novel two-dimensional material, black phosphorus and arsenic have a moderately adjustable band gap structure (0.15-0.3 eV), can fill the spectrum blank between the zero band gap of graphene and the relatively large band gap (5-6 eV) of hexagonal boron nitride, and realize the response of a medium-long wave infrared region. Meanwhile, the black phosphorus arsenic has anisotropic photoelectric characteristics and higher theoretical carrier mobility (14000 cm) than transition metal disulfide 2 V -1 s -1 ). Based on these excellent properties, some exciting applications of black phosphorus arsenic have been reported, such as field effect transistors, photoconductors, mid-wave infrared photodetectors, silicon photonic micro-heaters, lithium ion batteries, solar excitonic batteries, lasers, etc., which are also considered as a promising material in the mid-wave infrared photodetection field.
However, the direct preparation of the arsenic-phosphorus thin film material with few layers or even a single layer and large area is not realized at present. The top-down method is the mainstream method for preparing the arsenic-phosphorus two-dimensional material at present, namely, a blocky black phosphorus-arsenic crystal is synthesized by a chemical vapor transport method, and then the blocky black phosphorus-arsenic crystal is stripped by various methods to obtain the arsenic-phosphorus two-dimensional material. However, in any method, the size of the arsenic-phosphorus two-dimensional material obtained by stripping is small, the thickness can only reach micron level at the thinnest, the thickness is not controllable, or organic impurities are easily introduced. Therefore, there is a need for a method and an apparatus for preparing an arsenic-phosphorus thin film material, which is used as a precursor to synthesize a large-area black phosphorus-arsenic two-dimensional thin film.
Disclosure of Invention
The invention mainly aims to provide a preparation method and a device of an arsenic-phosphorus thin film material, and aims to solve the problems that the size of the arsenic-phosphorus thin film material is small, the thinnest thickness of the arsenic-phosphorus thin film material can only reach micron level, the thickness is uncontrollable, the arsenic-phosphorus thin film material with large area and uniform thickness is difficult to obtain, organic impurities are easy to introduce and the like in the prior art.
In order to achieve the purpose, the invention provides a preparation method of an arsenic-phosphorus film material, which comprises the steps of heating at 400 to 450 ℃ under a vacuum condition to volatilize black phosphorus-arsenic crystals, depositing the black phosphorus-arsenic crystals on a substrate, and forming the arsenic-phosphorus film material on the substrate; wherein the substrate is positioned above the black phosphorus arsenic crystal.
Further, the degree of vacuum of the vacuum condition<10 -6 pa。
Further, the deposition time is 10 to 180s.
Further, the substrate is in a rotated state.
Further, the distance between the substrate and the black phosphorus arsenic crystal is 30 to 100cm.
The invention also provides an arsenic-phosphorus thin film material prepared by the preparation method of the arsenic-phosphorus thin film material.
The invention also provides a device used in the preparation method of the arsenic-phosphorus thin film material, which comprises a vacuum bell jar and a vacuum cavity, wherein the vacuum bell jar is provided with the 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 used for placing and heating the black phosphorus arsenic crystal; and the deposition table is arranged in the vacuum cavity and positioned above the evaporation chamber so as to support the substrate.
Further, the deposition stage 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 cabin is 30 to 100cm.
The invention achieves the following beneficial effects:
firstly, the invention provides an arsenic-phosphorus thin film material, and the thickness of the arsenic-phosphorus thin film material is less than 50nm. The arsenic-phosphorus thin 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, according to the preparation method of the arsenic-phosphorus thin film material, the black phosphorus-arsenic crystal is volatilized by heating under the vacuum condition and is deposited on the substrate, and the arsenic-phosphorus thin film material is formed on the substrate, so that the defects that the two-dimensional material prepared by the prior art is small in size, uncontrollable in thickness and easy to introduce organic impurities are overcome. The preparation method is simple, and the prepared film has high purity, uniform and controllable thickness reaching a nanometer level, and is not limited in area to meet the requirements.
Drawings
In order to more clearly illustrate the embodiments or technical solutions of the present invention, the drawings used in the embodiments or technical solutions of 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 schematic diagram of an apparatus used in a method for preparing an arsenic-phosphorus thin film material;
FIG. 2 is a diagram showing an embodiment of the As-P thin film material obtained in example 1;
FIG. 3 is a diagram showing an embodiment of the As-P thin film material obtained in example 2;
FIG. 4 is a schematic representation of the As-P thin film material obtained in example 3;
FIG. 5 is a Transmission Electron Microscope (TEM) image of the As-P thin film material obtained in example 1;
FIG. 6 is a transmission electron microscopy (TEM-EDS) image of the As-P thin film material obtained in example 1;
FIG. 7 is a comparison graph of Raman spectra (Raman) of the As-P thin film materials obtained in examples 1-3;
FIG. 8 is an Atomic Force Microscope (AFM) image of the As-P thin film material obtained in example 2;
FIG. 9 is a graph of a high level statistic of white dashed areas in an Atomic Force Microscope (AFM) image of the As-P 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 implementation, functional features and advantages of the present invention will be further described 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 inventive efforts based on the embodiments of the present invention, are within the scope of protection of the present invention.
It should be noted that the features in the following embodiments and examples may be combined with each other without conflict. It is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present 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 the description of the present invention, and any methods, apparatuses, and materials similar or equivalent to those described in the examples of the present invention may be used to practice the present invention. It should be understood by those skilled in the art that for the purpose of this document, "Element type" can be expressed as Element type and "Content (atom%)" can be expressed as atomic ratio in the arsenic-phosphorous thin film material without affecting the practical understanding of the technical solution of the present application.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any number between the two endpoints are optional unless otherwise specified in the invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers. The materials or reagents required in the following examples are commercially available unless otherwise specified.
In order to solve the problems that the size of an arsenic-phosphorus film material is small, the thickness can only reach a micron level when the arsenic-phosphorus film material is thinnest, 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 the prior art, the invention provides a preparation method of the arsenic-phosphorus film material, wherein under the vacuum condition, black phosphorus arsenic crystals are volatilized by heating at 400 to 450 ℃, and are deposited on a substrate to form the arsenic-phosphorus film material on the substrate; wherein the substrate is positioned above the black phosphorus arsenic crystal.
Specifically, under the vacuum condition, the black phosphorus arsenic crystal is heated at the temperature of 400-450 ℃, and when the heating temperature exceeds the volatilization point, the black phosphorus arsenic crystal volatilizes upwards to form black phosphorus arsenic vapor. When the temperature is controlled within the range of 400 to 450 ℃, the slow volatilization of the black phosphorus arsenic crystal can be realized, and the controllable preparation of the film thickness can be further realized. Meanwhile, the size and the thickness of the arsenic-phosphorus film material formed by depositing black phosphorus and 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 preparation of two-dimensional materials in the prior art.
Illustratively, the black arsenic-phosphorus crystal may be obtained by calcining gray arsenic (As), red phosphorus (P) and an iodine-based additive in a gas phase synthesis method. Wherein the mass ratio of the ash arsenic (As), the red phosphorus (P) and the iodine-based additive can be 22: 9: 2 to 4; the iodine-based additive may specifically be antimony iodide (SbI) 3 ) Tantalum iodide (TaI) 5 ) Or bismuth iodide (BiI) 3 ) (ii) a The calcination temperature is 480 to 520 ℃.
Specifically, ash arsenic (As), red phosphorus (P) and an iodine-based additive are placed in a quartz tube according to the mass ratio of 22: 9: 2 to 4, the quartz tube is placed in a two-temperature-zone tube furnace after being subjected to vacuum sealing, and then a high-temperature area and a low-temperature area are heated to respective set temperatures, so that the ash arsenic, the red phosphorus and the iodine-based additive are calcined in the set temperature fields. The high-temperature area can be understood as a high-temperature reaction area, the low-temperature area can be understood as a low-temperature deposition area, and the temperature field is formed by the high-temperature area and the low-temperature area; in the reaction process, when 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 to 600 ℃; the temperature of the low-temperature region may be 480 to 520 ℃.
Further, degree of vacuum condition<10 -6 pa. So as to realize the condition of approaching vacuum, thereby reducing the collision between air molecules and target gaseous molecules in the evaporation process and realizing the preparation of uniform films.
Further, the deposition time is 10 to 180s. And controlling the deposition time to be 10 to 180s to obtain the arsenic-phosphorus film material with the thickness of less than 50nm.
Further, the substrate is in a rotated state. The material of the substrate may be silicon (Si)/silicon dioxide (SiO) 2 ) Sheet, mica sheet (KAl) 2 (AlSi 3 O 10 )(OH) 2 ) Or fluorine crystal mica flake (KMg) 3 (AlSi 3 O 10 )F 2 ). The substrate in a rotating state drives gas molecules to rotate by using centrifugal force, the agglomeration degree of the gas molecules is reduced by using the centrifugal action at high rotating speed, the gas molecules are dispersed by using the pressure difference generated by the action of the gas molecules and the fluidized gas flow, the distribution uniformity of the gas molecules is improved, and the black phosphorus and arsenic vapor is favorably and uniformly deposited on the substrate in the deposition process.
Further, the distance between the substrate and the black phosphorus arsenic crystal is 30 to 100cm. And controlling the distance between the substrate and the black arsenic phosphate crystal within the range of 30 to 100cm to ensure the effectiveness and uniformity of deposition.
The invention provides an arsenic-phosphorus thin film material prepared by the preparation method of the arsenic-phosphorus thin film material. Specifically, the thickness of the obtained arsenic-phosphorus thin film material can be controlled in a nanometer scale, for example, the thickness of the arsenic-phosphorus thin film material is less than 50nm.
The invention also provides a device used in the preparation method of the arsenic-phosphorus thin film material, 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) arranged in the vacuum chamber and used for placing and heating the black phosphorus arsenic crystal; and the deposition table is arranged in the vacuum chamber and positioned above the evaporation chamber so as to support the substrate 4.
Further, the deposition stage is a rotary stage 3 to rotate the substrate 4 during deposition in the preparation of the arsenic-phosphorous 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 and arsenic vapor can be uniformly formed into a film in the deposition process.
Exemplarily, referring to fig. 1, the vacuum bell 2 is connected to a connection seat (not shown) of the vacuum pumping mechanism, and a chamber formed by the connection seat and the vacuum bell 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 virtue of the corrugated pipe 9 and is far away from one side of the vacuum cavity. The lower part of the vacuum cavity is provided with a tungsten boat 6, a tungsten filament 7 and a heating electrode 8 for supplying heat to the tungsten boat 6. In the upper part of the vacuum chamber, a deposition stage (not shown) is provided, which comprises a rotating stage 3, a clamping piece (not shown) on the rotating stage 3 and a baffle 5 for fixing a substrate 4 for collecting the evaporated material (such as black phosphorus and arsenic vapor). The chamber formed between the baffle 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 device used in the preparation method of the arsenic-phosphorus thin film material can work in a specific mode that black phosphorus-arsenic crystals are placed in a tungsten boat 6, a tungsten filament 7 is used for fixing the position, and a substrate 4 is fixed on a rotary object stage 3 by a clamping piece; then cooperatively controlling the vacuumizing time to be 10 to 60min through a vacuum pump 10 and a digital display workbench 1 so as to ensure that the vacuum degree in the vacuum cavity is 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 through the digital display workbench 1, so that volatilization of black phosphorus arsenic crystals and controllable preparation of the arsenic-phosphorus film are realized.
Further, the distance between the deposition table and the base of the evaporation chamber is 30 to 100cm. 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 invention, reference will now be made to the following examples:
the black arsenic phosphate crystals used in examples 1 to 3 and comparative example 1 were prepared in the laboratory by the following method:
440 mg of gray arsenic (As), 180 mg of red phosphorus (P) and 16 mg of antimony iodide (SbI) were weighed in a glove box under an argon atmosphere with a ten-thousandth electronic balance 3 ) In the quartz tube, one end of the quartz tube is plugged by a plug, then the quartz tube is sealed by a vacuum valve, then 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 after the tube sealing into a double-temperature-zone tube furnace, and setting the temperature of the double-temperature zone and then carrying out gas-phase synthesis reaction; wherein the temperature of the high-temperature reaction area is 550 ℃, and the temperature of the low-temperature deposition area is 500 ℃. After the reaction is kept for 20 hours, the temperature is reduced to 75-25 ℃ through synchronous temperature reduction for 2 hours (namely, the temperature in a high-temperature reaction area is reduced to 75 ℃, the temperature in a low-temperature deposition area is reduced to 25 ℃), and finally, the mixture is naturally cooled to room temperature to obtain black phosphorus arsenic crystals.
Example 1
50mg of black phosphorus arsenic crystal is 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 figure 1, a tungsten filament 7 is used for fixing the position, and a substrate 4 is fixed on a rotary object stage 3 by a clamping piece. The vacuum bell 2 is closed and the junction of the vacuum bell 2 and the connection socket is sealed with transparent gel, and then the vacuum pump 10 is turned on and the vacuum chamber is evacuated to vacuum. Wherein the vacuum pumpingThe empty time is 30 min, the vacuum degree of the vacuum chamber<10 -6 pa. The material of the substrate 4 is silicon (Si)/silicon dioxide (SiO) 2 ) Pieces, base 4 size 1cm x 1cm.
The heating temperature of the evaporation chamber is set to be 450 ℃ through a digital display workbench 1; the deposition time was 10s. The obtained arsenic-phosphorus thin film material is 1cm by 1cm and the thickness is uniform and 5nm, and the physical diagram is shown in figure 2.
The obtained arsenic-phosphorus thin film material is characterized, and a TEM image of the arsenic-phosphorus thin film material is shown in FIG. 5; the TEM-EDS diagram of the arsenic-phosphorus thin film material is shown in FIG. 6. As can be seen from fig. 6, except for copper (Cu) and carbon (C) carried by the TEM copper mesh for carrying the article and oxygen (O) caused by oxidation of a part of the sample, only signal peaks of arsenic (As) and phosphorus (P) elements exist in the sample, indicating that the film has an ultra-high purity, and As a result of conversion of peak intensity, the atomic ratio of arsenic to phosphorus in the TEM-EDS results of table 1 can be obtained, and As can be seen from table 1, the atomic ratio of arsenic to phosphorus in the film is about 2.28.
TABLE 1 TEM-EDS results for arsenic to phosphorus atomic ratio
| Element type | As | P |
| Content (atom%) | 69.48 | 30.52 |
Example 2
Compared to example 1, only the heating temperature and the deposition duration were varied, namely:
the heating temperature of the evaporation chamber is set to be 420 ℃ through the digital display workbench 1; the deposition time was 60s. The obtained arsenic-phosphorus thin film material is 1 cm-1 cm and the thickness is uniform and 15nm, and the physical diagram is shown in figure 3.
Example 3
Compared to example 1, only the heating temperature and the deposition time were varied, namely:
the heating temperature of the evaporation chamber is set to be 400 ℃ through a digital display workbench 1; the deposition time was 180s. The obtained arsenic-phosphorus thin film material is 1cm by 1cm and has a uniform thickness of 45nm, and the physical diagram is shown in FIG. 4.
Comparative example 1
Weighing 50mg of black phosphorus arsenic crystal, directly covering the black phosphorus arsenic crystal with transparent adhesive tape to make it closely adhere, carefully tearing off the adhesive tape with tweezers, 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 peeled off with tweezers, and the silicon (Si)/silicon dioxide (SiO) was applied 2 ) The sheet was observed under an optical microscope, and the results are shown in FIG. 10. The results in fig. 10 show that the resulting two-dimensional material was non-uniform in thickness, had fractures, and had an area far below 1cm x 1cm.
Analytical example 1
Characterization analysis was performed on the As-P thin film materials obtained in examples 1 to 3
1. The physical diagram of the arsenic-phosphorus thin film material obtained in example 1 is shown in FIG. 2; the physical diagram of the arsenic-phosphorus thin film material obtained in example 2 is shown in FIG. 3; FIG. 4 shows a schematic diagram of the As-P thin film material obtained in example 3.
It should be noted that, the visual observation color development effects of examples 1 to 3 differ depending on the film formation thickness, and specifically correspond to fig. 2 to 4, respectively; and the two shaded areas at the lower part in the figures 2 to 4 are the areas without film formation, which are generated by the covering of the clamping pieces during the preparation. As can be seen from FIGS. 2 to 4, the thickness of the As-P thin film materials obtained in examples 1 to 3 was uniform and almost no impurities were observed.
2. The comparative Raman spectra (Raman) of the arsenic-phosphorus thin film materials obtained in examples 1 to 3 are shown in FIG. 7. As can be seen from the observation of FIG. 7, the Raman spectrum shows distinct arsenic and phosphorus vibration peaks and strong peaks depending on the thickness variation of the film.
3. An Atomic Force Microscope (AFM) image of the arsenic-phosphorus thin film material obtained in example 2 is shown in fig. 8, and it can be seen from fig. 8 that the thickness of the thin film material is uniform and has no significant height fluctuation, and the color difference region at the bottom right corner is a clip blocking region (i.e., no deposition product) during deposition; the result of analyzing the overall height of the material covering the substrate 4 by the white dotted line region is shown in fig. 9, and it can be seen from fig. 9 that the height difference between the height of the micro-radiation undulation and the tail end (the height of the substrate 4) in fig. 9 is about 15nm of the thickness of the thin film material, and other embodiments may sequentially obtain the thickness data according to the AFM result in the same manner.
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 or other related technical fields directly/indirectly applied under the technical idea of the present invention are included in the technical scope of the present invention.
Claims (8)
1. The preparation method of the arsenic-phosphorus thin film material is characterized by heating at 400 to 450 ℃ under a 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.
2. The method of claim 1, wherein the vacuum is applied under vacuum<10 -6 pa。
3. The method for preparing the arsenic-phosphorus thin film material as claimed in claim 1, wherein the deposition time is 10 to 180s.
4. The method of claim 1, wherein the substrate is rotated.
5. The method for preparing the arsenic-phosphorus thin film material as claimed in claim 1, wherein the distance between the substrate and the black phosphorus-arsenic crystal is 30 to 100cm.
6. An apparatus used in the method for preparing the arsenic-phosphorus thin film material according to any one of claims 1 to 5, comprising:
a vacuum bell jar having 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 cavity and used for placing and heating the black phosphorus arsenic crystal;
and the deposition table is arranged in the vacuum cavity and positioned above the evaporation chamber so as to support the substrate.
7. The apparatus of claim 6, wherein the deposition stage is a rotary stage for rotating the substrate during deposition in the preparation of the As-P thin film material.
8. The apparatus for preparing As-P thin film material according to claim 6, wherein the distance between the deposition table and the base of the evaporation chamber is 30-100 cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310083671.8A CN115807211B (en) | 2023-02-08 | 2023-02-08 | Preparation method and device of arsenic-phosphorus film material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310083671.8A CN115807211B (en) | 2023-02-08 | 2023-02-08 | Preparation method and device of arsenic-phosphorus film material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115807211A true CN115807211A (en) | 2023-03-17 |
| CN115807211B CN115807211B (en) | 2023-05-05 |
Family
ID=85487710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310083671.8A Active CN115807211B (en) | 2023-02-08 | 2023-02-08 | Preparation method and device of arsenic-phosphorus film material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115807211B (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107447193A (en) * | 2016-11-14 | 2017-12-08 | 深圳大学 | A kind of black phosphorus film and preparation method thereof |
| CN108538707A (en) * | 2018-03-05 | 2018-09-14 | 南京航空航天大学 | A kind of two dimension black phosphorus crystal preparation method |
| 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 |
| 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 |
| CN111020487A (en) * | 2019-11-21 | 2020-04-17 | 华中科技大学 | Method for preparing film of quasi-one-dimensional structure material with controllable orientation |
| CN111285339A (en) * | 2020-03-15 | 2020-06-16 | 湖北中科墨磷科技有限公司 | Sn (tin)3P4Preparation method of induced two-dimensional black phosphorus crystal |
| CN111334780A (en) * | 2020-03-02 | 2020-06-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus film, preparation method and application thereof |
| US20200207623A1 (en) * | 2018-12-26 | 2020-07-02 | Government Of The United States, As Represented By The Secretary Of The Air Force | Method and apparatus for producing a nanometer thick film of black phosphorus |
| CN113668053A (en) * | 2021-10-25 | 2021-11-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus film reaction device and black phosphorus film preparation method |
| CN113737279A (en) * | 2021-09-13 | 2021-12-03 | 中南大学 | Preparation method of black phosphorus arsenic crystal |
| CN114293146A (en) * | 2022-03-07 | 2022-04-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus and preparation method and application thereof |
-
2023
- 2023-02-08 CN CN202310083671.8A patent/CN115807211B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107447193A (en) * | 2016-11-14 | 2017-12-08 | 深圳大学 | A kind of black phosphorus film and preparation method thereof |
| CN108538707A (en) * | 2018-03-05 | 2018-09-14 | 南京航空航天大学 | A kind of two dimension black phosphorus crystal preparation method |
| 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 |
| US20200207623A1 (en) * | 2018-12-26 | 2020-07-02 | Government Of The United States, As Represented By The Secretary Of The Air Force | Method and apparatus for producing a nanometer thick film of black phosphorus |
| CN111020487A (en) * | 2019-11-21 | 2020-04-17 | 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 |
| CN111334780A (en) * | 2020-03-02 | 2020-06-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus film, preparation method and application thereof |
| CN111285339A (en) * | 2020-03-15 | 2020-06-16 | 湖北中科墨磷科技有限公司 | Sn (tin)3P4Preparation method of induced two-dimensional black phosphorus crystal |
| CN113737279A (en) * | 2021-09-13 | 2021-12-03 | 中南大学 | Preparation method of black phosphorus arsenic crystal |
| CN113668053A (en) * | 2021-10-25 | 2021-11-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus film reaction device and black phosphorus film preparation method |
| CN114293146A (en) * | 2022-03-07 | 2022-04-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Black phosphorus and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115807211B (en) | 2023-05-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Sun et al. | Chemical vapour deposition | |
| CN102191476B (en) | Method for preparing sulfur-doped graphene films | |
| CN110155959B (en) | Method for preparing two-dimensional transition metal alloy chalcogenide by limited-area chemical vapor deposition | |
| Chaudhari et al. | Heteroepitaxial silicon film growth at 600° C from an Al–Si eutectic melt | |
| CN110565052B (en) | Preparation method of two-dimensional tungsten sulfide-based vertical heterostructure material | |
| CN113957527B (en) | Preparation of two-dimensional nano Cs 3 Cu 2 I 5 Method for producing crystalline material and use thereof | |
| CN113026096B (en) | Two-dimensional semiconductor material SnSe2Method for producing single crystal | |
| CN111960388B (en) | Method for preparing large-area two-dimensional molybdenum diselenide thin film with different layer numbers and application | |
| CN110980659A (en) | Tungsten ditelluride grown by using new raw material and preparation method thereof | |
| CN112875655A (en) | Non-laminated two-dimensional Cr2Se3Preparation method and application of nanosheet | |
| CN112456452B (en) | Preparation method of germanium diselenide nano material | |
| Liu et al. | Preparation of CdS nanorods on silicon nanopillars surface by hydrothermal method | |
| CN111392685B (en) | Two-dimensional self-assembled M1/M2-VO 2 Homojunction nanosheet and preparation method thereof | |
| CN114232101A (en) | Single-layer P-type semiconductor phase vanadium diselenide single crystal and salt-assisted growth method thereof and back gate field effect transistor | |
| Liu et al. | Colloidal synthesis and characterization of single-crystalline Sb 2 Se 3 nanowires | |
| CN107915496A (en) | A kind of preparation method of large-area two-dimensional organic-inorganic perovskite thin film | |
| CN113718227B (en) | Two-dimensional layered ternary compound and preparation method thereof | |
| Mahdhi et al. | Physical properties of metal-doped ZnO thin films prepared by RF magnetron sputtering at room temperature | |
| Verma et al. | Heat-up and gram-scale synthesis of Cu-poor CZTS nanocrystals with controllable compositions and shapes | |
| CN105399061A (en) | Preparation method for one-dimensional SnSe monocrystal nanowire | |
| CN115807211B (en) | Preparation method and device of arsenic-phosphorus film material | |
| CN115341273B (en) | Preparation of large-size two-dimensional thermoelectric material bismuth telluride single crystal | |
| CN115385378B (en) | Preparation method and application of two-dimensional double-layer tungsten sulfide homojunction | |
| CN113104885B (en) | Non-lamellar Sn 2 P 2 S 6 Preparation method of nanosheet and application of nanosheet in field of photocatalytic hydrogen evolution | |
| CN114808140B (en) | Two-dimensional monocrystalline ferroferric oxide nano material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |