CN113322514A - Method for preparing (00l) preferred orientation low melting point bismuth film by molecular beam epitaxy technology - Google Patents
Method for preparing (00l) preferred orientation low melting point bismuth film by molecular beam epitaxy technology Download PDFInfo
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- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 121
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000001451 molecular beam epitaxy Methods 0.000 title claims abstract description 22
- 238000005516 engineering process Methods 0.000 title claims abstract description 12
- 230000008018 melting Effects 0.000 title description 2
- 238000002844 melting Methods 0.000 title description 2
- 239000000758 substrate Substances 0.000 claims abstract description 79
- 239000013078 crystal Substances 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 claims description 3
- 229910001632 barium fluoride Inorganic materials 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- -1 lanthanum aluminate Chemical class 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 1
- 230000003746 surface roughness Effects 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract 1
- 229920006395 saturated elastomer Polymers 0.000 abstract 1
- 239000010408 film Substances 0.000 description 62
- 239000010409 thin film Substances 0.000 description 12
- 230000005611 electricity Effects 0.000 description 6
- 230000007704 transition Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- CVOVFRILKMNGBC-UHFFFAOYSA-N 2-(3-oxo-4H-quinoxalin-2-yl)propanoic acid ethyl ester Chemical compound C1=CC=C2NC(=O)C(C(C)C(=O)OCC)=NC2=C1 CVOVFRILKMNGBC-UHFFFAOYSA-N 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/025—Epitaxial-layer growth characterised by the substrate
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a molecular beam epitaxy technology for preparing (00)l) A method for preferentially orienting a low-melting-point metal bismuth film belongs to the technical field of film preparation. The method is that high-purity metal bismuth is heated to a certain saturated vapor pressure, and a bismuth atom beam source is sprayed on a substrate to form a bismuth film with preferred orientation. The bismuth film prepared by the method has high (00)l) Preferred orientation, small surface roughness, accurately controllable film thickness, strong hydrophobicity, excellent transportation performance, low process cost and good repeatability, and can realize large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of film preparation, and particularly relates to a method for preparing a low-melting-point metal bismuth film by a molecular beam epitaxy technology.
Background
The semimetal bismuth (Bi) has unique physical properties and a carrier density of about 3 x 1017cm-3、10-3meThe effective mass, 30nm mean free path, highly anisotropic fermi surface and small band overlap at low temperature (38 meV) are one of the most important areas of research in condensed state physics. There are many potential applications in modern industries, including superconducting devices, giant magnetoresistive devices, thermoelectric devices, and the like. In addition, two-dimensional bismuth thin films are also the most promising candidates for the fabrication of low temperature spin hall devices.
The preparation of the bismuth film has a plurality of methods such as molecular beam epitaxy, flash evaporation, electron beam evaporation, magnetron sputtering, pulsed laser deposition and the like, wherein the molecular beam epitaxy is a method for preparing the bismuth film with better quality and surface smoothness at present. The performance of the semi-metal material depends on the shape and structure of the crystal, and in the deposition process, the substrate temperature, the growth rate and the deposition time are basic parameters influencing the quality of the film, and determine the growth mode, the surface appearance, the texture and the like of the film. However, the research on the growth area prepared by the low-melting-point bismuth film molecular beam epitaxy technology is few, and the structural area model of the low-melting-point bismuth film needs to be further researched. Therefore, the method has more important significance for preparing the preferred orientation bismuth film by utilizing the molecular beam epitaxy technology.
Disclosure of Invention
The invention aims to solve the problem that the prior low-melting-point bismuth film is controllable in preferred orientation growth, and provides a method for preparing a low-melting-point preferred orientation bismuth film by utilizing a molecular epitaxy technology.
The invention provides a method for preparing a low-melting-point preferred orientation bismuth film by utilizing a molecular beam epitaxy technology, which comprises the following steps of:
1) transferring the substrate to a growth chamber of a molecular beam epitaxy system;
2) the pressure of the growth chamber is less than 5.0 multiplied by 10-6Pa starting a reflection high-energy electron diffractometer to observe the substrate diffraction fringes;
3) controlling the deposition rate of the bismuth film by adjusting the temperature of a bismuth beam source and the temperature of a substrate;
4) adjusting the temperature of the bismuth beam source furnace to between 450 ℃ and 600 ℃, and adjusting the temperature of the substrate to between 18 and 150 ℃;
5) opening a bismuth beam source furnace and a substrate shutter baffle to enable bismuth beams to be sprayed onto the heated substrate;
6) and after the bismuth film continuously grows for 0.5-48 hours, closing the bismuth beam source furnace and the substrate shutter baffle, and reducing the temperature of the bismuth beam source furnace and the substrate to room temperature to obtain the preferred orientation bismuth film.
The substrate is glass, magnesium oxide single crystal, strontium titanate single crystal, lanthanum aluminate single crystal, aluminum oxide single crystal and barium fluoride single crystal.
The temperature of the bismuth beam source furnace in the step 4) is 450-600 ℃.
The temperature of the substrate in the step 4) is 18-150 ℃.
The film growth time in the step 6) is 0.5-48 hours.
The bismuth beam source uses high-purity metal bismuth.
The method has the advantages that:
the invention provides a method for preparing a low-melting-point preferred orientation bismuth film by a molecular beam epitaxy technology.
The bismuth film has the advantages of good repeatability, good smoothness, low surface roughness, large magnetoresistance effect, strong hydrophobicity and the like through the preparation of the preferred orientation bismuth film.
Drawings
FIG. 1 is an XRD pattern of the bismuth films prepared in examples 1 and 2;
FIG. 2 is an AFM image of the bismuth film prepared in example 1;
FIG. 3 is a RT curve of the bismuth film prepared in example 1;
FIG. 4 is the MR curve of the bismuth film prepared in example 1;
FIG. 5 is a photograph showing the contact angle of the bismuth thin film prepared in example 1.
Detailed Description
The invention is described in detail below with reference to specific examples, but the scope of the invention is not limited to the examples:
example 1
1) Using a glass substrate as a substrate for preparing the bismuth film, putting the substrate into a treatment chamber, and conveying the substrate to a growth chamber of a molecular beam epitaxy system;
2) the pressure of the growth chamber is less than 5.0 multiplied by 10-6Pa, preheating the substrate;
3) adjusting the temperature of a bismuth beam source furnace to 560 ℃ and the temperature of a substrate to 70 ℃;
4) opening a bismuth beam source furnace and a substrate shutter baffle to enable bismuth beams to be sprayed on the heated substrate and deposited for 3 hours;
5) starting a reflection high-energy electron diffractometer to observe diffraction stripes of the film, wherein the stripes are clear and sharp to indicate that the grown bismuth film has good quality and smooth surface;
6) closing the bismuth beam source furnace and the substrate shutter baffle, and reducing the temperature of the bismuth beam source furnace and the substrate to room temperature to obtain a film sample;
7) taking out a bismuth film sample, and carrying out phase, electricity and wettability tests, wherein the results show that: obtain (00)1) High magnetic resistance effect of preferred orientation bismuth filmLow surface roughness, high hydrophobicity.
Example 2
1) The magnesium oxide substrate is used as a substrate for preparing the bismuth film and is placed in a treatment chamber to be conveyed to a growth chamber of a molecular beam epitaxy system;
2) the pressure of the growth chamber is less than 5.0 multiplied by 10-6Pa, preheating the substrate, and starting a reflection high-energy electron diffractometer to observe diffraction fringes of the substrate;
3) adjusting the temperature of a bismuth beam source furnace to 560 ℃ and the temperature of a substrate to 70 ℃;
4) opening a bismuth beam source furnace and a substrate shutter baffle to enable bismuth beams to be sprayed on the heated substrate and deposited for 3 hours;
5) starting a reflection high-energy electron diffractometer to observe diffraction stripes of the film, wherein the stripes are clear and sharp to indicate that the grown bismuth film has good quality and smooth surface;
6) closing the bismuth beam source furnace and the substrate shutter baffle, and reducing the temperature of the bismuth beam source furnace and the substrate to room temperature to obtain a film sample;
7) taking out a bismuth film sample, and carrying out phase, electricity and wettability tests, wherein the results show that: obtain (00)1) Preferred orientation bismuth film, large magnetoresistance effect, low surface roughness, and high hydrophobicity.
Example 3
1) The strontium titanium oxide substrate is used as a substrate for preparing the bismuth film and is placed in a treatment chamber to be conveyed to a growth chamber of a molecular beam epitaxy system;
2) the pressure of the growth chamber is less than 5.0 multiplied by 10-6Pa, preheating the substrate, and starting a reflection high-energy electron diffractometer to observe diffraction fringes of the substrate;
3) adjusting the temperature of a bismuth beam source furnace to 490 ℃ and the temperature of a substrate to 30 ℃;
4) opening a bismuth beam source furnace and a substrate shutter baffle to enable bismuth beams to be sprayed on the heated substrate and deposited for 3 hours;
5) starting a reflection high-energy electron diffractometer to observe diffraction stripes of the film, wherein the stripes are clear and sharp to indicate that the grown bismuth film has good quality and smooth surface;
6) closing the bismuth beam source furnace and the substrate shutter baffle, and reducing the temperature of the bismuth beam source furnace and the substrate to room temperature to obtain a film sample;
7) taking out a bismuth film sample, and carrying out phase, electricity and wettability tests, wherein the results show that: obtain (00)1) Preferred orientation bismuth film, large magnetoresistance effect, low surface roughness, and high hydrophobicity.
Example 4
1) Using a lanthanum aluminate substrate as a substrate for preparing a bismuth film, and transferring the substrate to a growth chamber of a molecular beam epitaxy system in a treatment chamber;
2) the pressure of the growth chamber is less than 5.0 multiplied by 10-6Pa, preheating the substrate, and starting a reflection high-energy electron diffractometer to observe diffraction fringes of the substrate;
3) adjusting the temperature of a bismuth beam source furnace to 520 ℃ and the temperature of a substrate to 100 ℃;
4) opening a bismuth beam source furnace and a substrate shutter baffle to enable bismuth beams to be sprayed on the heated substrate and deposited for 3 hours;
5) starting a reflection high-energy electron diffractometer to observe diffraction stripes of the film, wherein the stripes are clear and sharp to indicate that the grown bismuth film has good quality and smooth surface;
6) closing the bismuth beam source furnace and the substrate shutter baffle, and reducing the temperature of the bismuth beam source furnace and the substrate to room temperature to obtain a film sample;
7) taking out a bismuth film sample, and carrying out phase, electricity and wettability tests, wherein the results show that: obtain (00)1) Preferred orientation bismuth film, large magnetoresistance effect, low surface roughness, and high hydrophobicity.
Example 5
1) An aluminum oxide substrate is used as a substrate for preparing the bismuth film and is placed in a disposal chamber to be conveyed to a growth chamber of a molecular beam epitaxy system;
2) the pressure of the growth chamber is less than 5.0 multiplied by 10-6Pa, preheating the substrate, and starting a reflection high-energy electron diffractometer to observe diffraction fringes of the substrate;
3) adjusting the temperature of a bismuth beam source furnace to 510 ℃ and the temperature of a substrate to 120 ℃;
4) opening a bismuth beam source furnace and a substrate shutter baffle to enable bismuth beams to be sprayed on the heated substrate and deposited for 3 hours;
5) starting a reflection high-energy electron diffractometer to observe diffraction stripes of the film, wherein the stripes are clear and sharp to indicate that the grown bismuth film has good quality and smooth surface;
6) closing the bismuth beam source furnace and the substrate shutter baffle, and reducing the temperature of the bismuth beam source furnace and the substrate to room temperature to obtain a film sample;
7) taking out a bismuth film sample, and carrying out phase, electricity and wettability tests, wherein the results show that: obtain (00)1) Preferred orientation bismuth film, large magnetoresistance effect, low surface roughness, and high hydrophobicity.
Example 6
1) A barium fluoride substrate is used as a substrate for preparing the bismuth film and is placed in a treatment chamber to be conveyed to a growth chamber of a molecular beam epitaxy system;
2) the pressure of the growth chamber is less than 5.0 multiplied by 10-6Pa, preheating the substrate, and starting a reflection high-energy electron diffractometer to observe diffraction fringes of the substrate;
3) adjusting the temperature of a bismuth beam source furnace to 570 ℃ and the temperature of a substrate to 90 ℃;
4) opening a bismuth beam source furnace and a substrate shutter baffle to enable bismuth beams to be sprayed on the heated substrate and deposited for 3 hours;
5) starting a reflection high-energy electron diffractometer to observe diffraction stripes of the film, wherein the stripes are clear and sharp to indicate that the grown bismuth film has good quality and smooth surface;
6) closing the bismuth beam source furnace and the substrate shutter baffle, and reducing the temperature of the bismuth beam source furnace and the substrate to room temperature to obtain a film sample;
7) taking out a bismuth film sample, and carrying out phase, electricity and wettability tests, wherein the results show that: obtain (00)1) Preferred orientation bismuth film, large magnetoresistance effect, low surface roughness, and high hydrophobicity.
FIG. 1 is an XRD pattern of bismuth films grown on glass and magnesium oxide substrates of examples 1 and 2, in which only strong and sharp bismuth (00) is presentl) The diffraction peak of the surface is free of other crystal faces and diffraction peaks of impurity phases, which shows that the bismuth film has high purity and the growth orientation is along (00)l) And (4) growing in a preferred orientation.
Fig. 2 is an AFM image of the bismuth thin film grown on the glass substrate of example 1, and the image shows that the bismuth thin film structure is continuous, has a flat and smooth surface, and has a root mean square surface roughness of 1.96 nm.
Fig. 3 is an RT curve of the bismuth thin film grown on glass according to example 1, and the resistance of the bismuth thin film exhibits good semiconductor characteristics in a range of 54K to 300K, indicating that the resistance temperature relationship of the thin film shows semiconductor state characteristics at this time. With further temperature decrease, the sheet resistance temperature relationship is characterized by a metallic state, which is represented by a transition from a semiconductor state to a metallic state. The transition process exhibits a higher transition temperature. The transition temperature of the film was 54K.
Fig. 4 is an MR curve of the bismuth thin film grown on glass according to example 1, which shows that the bismuth thin film exhibits a linear magnetoresistance with increasing magnetic field, and has a magnetoresistance effect of 21% at a temperature of T =300K and a magnetic field of B = 9T.
Fig. 5 is a photograph of the contact angle of the bismuth thin film grown on glass of example 1, the contact angle of the bismuth thin film having 112 °, indicating strong hydrophobicity of the bismuth thin film.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A method for preparing a low-melting-point preferred orientation bismuth film by utilizing a molecular beam epitaxy technology is characterized by comprising the following steps of:
1) transferring the substrate to a growth chamber of a molecular beam epitaxy system;
2) the pressure of the growth chamber is less than 5.0 multiplied by 10-6Pa starting a reflection high-energy electron diffractometer to observe the substrate diffraction fringes;
3) controlling the deposition rate of the bismuth film by adjusting the temperature of a bismuth beam source and the temperature of a substrate;
4) adjusting the temperature of the bismuth beam source furnace to between 450 ℃ and 600 ℃, and adjusting the temperature of the substrate to between 18 and 150 ℃;
5) opening a bismuth beam source furnace and a substrate shutter baffle to enable bismuth beams to be sprayed onto the heated substrate;
6) and after the bismuth film continuously grows for 0.5-48 hours, closing the bismuth beam source furnace and the substrate shutter baffle, and reducing the temperature of the bismuth beam source furnace and the substrate to room temperature to obtain the preferred orientation bismuth film.
2. The method for preparing a low-melting-point preferred orientation bismuth film by using the molecular beam epitaxy technique as claimed in claim 1, wherein the substrate is glass, a single crystal of magnesium oxide, a single crystal of strontium titanate, a single crystal of lanthanum aluminate, a single crystal of aluminum oxide, and a single crystal of barium fluoride.
3. The method as claimed in claim 1, wherein the temperature of the bismuth beam source furnace in step 4) is 450-600 ℃.
4. The method for preparing a low-melting-point preferentially oriented bismuth film by using the molecular beam epitaxy technology as claimed in claim 1, wherein the substrate temperature in the step 4) is 18-150 ℃.
5. The method for preparing a low-melting-point preferentially oriented bismuth film by using the molecular beam epitaxy technology as claimed in claim 1, wherein the film growth time of the step 6) is 0.5-48 hours.
6. The method of claim 1, wherein the bismuth beam source uses bismuth as a high purity material.
7. The method of claim 1, wherein the bismuth film has a large magnetoresistance effect and high hydrophobicity.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115233302A (en) * | 2022-06-14 | 2022-10-25 | 沈阳大学 | Preparation method for semi-metal Bi ultrathin film with transparent conductivity and hydrophobicity |
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|---|---|---|---|---|
| AU4086189A (en) * | 1988-08-29 | 1990-03-01 | Sumitomo Electric Industries, Ltd. | Process for preparing a bismuth-type superconducting thin film |
| WO2000037715A1 (en) * | 1998-11-18 | 2000-06-29 | The Johns Hopkins University | Bismuth thin film structure and method of construction |
| US20040179309A1 (en) * | 2003-03-14 | 2004-09-16 | Korea Institute Of Science And Technology | Method for fabricating Bi thin film and device using the same |
| CN107146761A (en) * | 2017-05-05 | 2017-09-08 | 电子科技大学 | The yttrium iron garnet of a kind of large magneto-optical effect/bismuth heterofilm and preparation method thereof |
-
2021
- 2021-05-24 CN CN202110562374.2A patent/CN113322514A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU4086189A (en) * | 1988-08-29 | 1990-03-01 | Sumitomo Electric Industries, Ltd. | Process for preparing a bismuth-type superconducting thin film |
| WO2000037715A1 (en) * | 1998-11-18 | 2000-06-29 | The Johns Hopkins University | Bismuth thin film structure and method of construction |
| US20040179309A1 (en) * | 2003-03-14 | 2004-09-16 | Korea Institute Of Science And Technology | Method for fabricating Bi thin film and device using the same |
| CN107146761A (en) * | 2017-05-05 | 2017-09-08 | 电子科技大学 | The yttrium iron garnet of a kind of large magneto-optical effect/bismuth heterofilm and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张忠阳: "硅基InSb薄膜外延集成生长研究", 中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115233302A (en) * | 2022-06-14 | 2022-10-25 | 沈阳大学 | Preparation method for semi-metal Bi ultrathin film with transparent conductivity and hydrophobicity |
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