CN115125513A - Preparation method of transition metal chalcogenide film - Google Patents
Preparation method of transition metal chalcogenide film Download PDFInfo
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- CN115125513A CN115125513A CN202210959994.4A CN202210959994A CN115125513A CN 115125513 A CN115125513 A CN 115125513A CN 202210959994 A CN202210959994 A CN 202210959994A CN 115125513 A CN115125513 A CN 115125513A
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- transition metal
- metal chalcogenide
- thin film
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a preparation method of a transition metal chalcogenide film, which comprises the following steps: placing a target substrate in a chemical vapor deposition cavity, wherein a deposition surface of the target substrate faces to a raw material conveying direction, a preset angle is formed between the deposition surface and a horizontal plane, and the preset angle is larger than 0 degree; and conveying a sulfur source and a transition metal source to the deposition surface to form a transition metal chalcogenide film with preset layer number distribution and preset coverage rate on the surface of the deposition surface. The preparation method of the transition metal chalcogenide film can controllably modulate the concentration of the precursor near the target substrate by changing the inclination angle of the target substrate, can effectively control the coverage rate and the layer number of the transition metal chalcogenide film, and is favorable for expanding the application of the transition metal chalcogenide.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and relates to a preparation method of a transition metal chalcogenide film.
Background
Since the discovery of graphene in 2004, graphene draws extensive attention of researchers by virtue of excellent physicochemical properties, but the zero band gap of graphene limits further application of graphene in the field of photoelectricity. Thus, scientists are motivated to explore two-dimensional materials. Among them, transition metal chalcogenide (TMDS) has advantages of large specific surface area, variation of band gap size and species with the number of layers of thin film, spin-orbit coupling for nanoelectronic and nanophotonics applications, etc., and provides great opportunities for optoelectronic devices and photonic applications.
However, it is a technical difficulty to obtain TMDS with good uniformity and controllable layer number. In view of the difficulty in controlling the number of layers, morphology, etc. of thin films by conventional mechanical stripping methods, more and more methods are used in the field of two-dimensional material preparation. Among them, Chemical Vapor Deposition (CVD) is often used to prepare TMDS materials due to its advantages such as simple apparatus and controllable number of layers.
However, the CVD method reported so far usually has a gas flow direction fixed from upstream to downstream, and the target substrate is horizontally placed on a downstream quartz boat. This can result in precursor concentrations near the target substrate that are difficult to control and can severely impact film quality. Although there are few reports that the number of layers of the thin film can be adjusted by adjusting the conditions of temperature, growth time, gas flow, pressure, etc., the process is complicated and the number of layers and the coverage rate of the thin film are difficult to control. This can severely limit the application of TMDCS films.
Therefore, how to improve the preparation method of the transition metal chalcogenide thin film to facilitate the control of the precursor concentration and improve the film quality becomes an important technical problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides a method for preparing a transition metal chalcogenide thin film, which is used to solve the problem of difficult adjustment of the concentration of the precursor in the conventional chemical vapor deposition method.
To achieve the above and other related objects, the present invention provides a method for preparing a transition metal chalcogenide thin film, which comprises the following steps, as a typical example:
placing a target substrate in a chemical vapor deposition chamber, wherein a deposition surface of the target substrate faces the raw material conveying direction, a preset angle is formed between the deposition surface and a horizontal plane, and the preset angle is larger than 0 degree;
and conveying a sulfur source and a transition metal source to the deposition surface to form a transition metal chalcogenide film with preset layer number distribution and preset coverage rate on the surface of the deposition surface.
Optionally, the transition metal source comprises a tungsten source and the transition metal chalcogenide film comprises a tungsten disulfide film, or the transition metal source comprises a molybdenum source and the transition metal chalcogenide film comprises a molybdenum disulfide film.
Optionally, the preset angle is in the range of 10 ° to 90 °.
Alternatively, the predetermined angle is set to 15 ° to 40 ° so that an area ratio of a single layer film in the transition metal chalcogenide film is greater than 50%.
Optionally, the preset angle is set to 45 ° to 75 ° so that the coverage of the transition metal chalcogenide thin film with respect to the deposition surface is greater than 70%.
Alternatively, the predetermined angle is set to 45 ° to 75 ° so that an area ratio of a multi-layer thin film in the transition metal chalcogenide thin film is greater than 80%.
Optionally, the predetermined angle is set to 80 ° to 90 ° so that an area ratio of a multi-layer thin film in the transition metal chalcogenide thin film is greater than 90%.
Optionally, the chemical vapor deposition chamber includes a first heating area and a second heating area, the first heating area and the second heating area are sequentially disposed along the raw material conveying direction, the sulfur source is obtained by placing sulfur powder in the first heating area and heating and gasifying, and the transition metal source is obtained by placing transition metal oxide powder in the second heating area and heating and gasifying.
Optionally, the target substrate is held by a holding device so that the deposition surface and a horizontal surface form the preset angle.
Optionally, the clamping device includes a quartz boat, the quartz boat includes a receiving groove with an upward opening, and a groove wall of the receiving groove is provided with a clamping groove for clamping the target substrate.
Optionally, the target substrate includes a silicon layer and a silicon dioxide layer stacked, and the target substrate has one surface of the silicon dioxide layer as the deposition surface.
As described above, in the method for preparing a transition metal chalcogenide film according to the present invention, a target substrate is placed in a chemical vapor deposition chamber, a deposition surface of the target substrate faces a raw material conveying direction, a preset angle is formed between the deposition surface and a horizontal plane, and the preset angle is greater than 0 °; and conveying a sulfur source and a transition metal source to the deposition surface to form a transition metal chalcogenide film with preset layer number distribution and preset coverage rate on the surface of the deposition surface. The method can controllably modulate the concentration of the precursor near the target substrate by changing the inclination angle of the target substrate, can effectively control the coverage rate and the layer number of the transition metal chalcogenide film, and is favorable for expanding the application of the transition metal chalcogenide.
Drawings
FIG. 1 is a process flow diagram illustrating a method for forming a transition metal chalcogenide thin film according to the present invention.
FIG. 2 is a schematic view showing a chemical vapor deposition apparatus using a quartz tube as a deposition chamber.
FIG. 3 is a schematic view of a target substrate horizontally placed on a quartz boat.
Fig. 4 shows a schematic view of a deposition surface of a target substrate at an angle of 30 ° to the horizontal.
Fig. 5 shows a schematic view of the deposition surface of a target substrate at an angle of 60 ° to the horizontal.
Fig. 6 shows a schematic view of a deposition surface of a target substrate at an angle of 90 ° to the horizontal.
Figure 7 shows an optical microscope image of a tungsten disulfide film obtained when the target substrate was placed horizontally on a quartz boat.
Figure 8 shows an optical microscope image of a tungsten disulfide film obtained at an angle of 30 ° between the deposition surface of the target substrate and the horizontal plane.
Figure 9 shows an optical microscope photograph of a tungsten disulfide film obtained at an angle of 60 deg. between the deposition surface of the target substrate and the horizontal plane.
Figure 10 shows an optical microscope image of a tungsten disulfide film obtained at a 90 deg. angle between the deposition surface of the target substrate and the horizontal plane.
Description of the element reference numerals
S1-S2 steps
1 Quartz tube
2 first heating zone
3 second heating zone
4 Sulfur powder
5 transition metal oxide powder
6 target substrate
7 card slot
8 first quartz boat
9 second Quartz boat
Detailed Description
The following embodiments of the present invention are provided by way of specific examples, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure herein. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Please refer to fig. 1 to 10. It should be noted that the drawings provided in this embodiment are only for schematically illustrating the basic idea of the present invention, and the components related to the present invention are only shown in the drawings and not drawn according to the number, shape and size of the components in actual implementation, and the form, quantity and proportion of each component in actual implementation may be arbitrarily changed, and the component layout may be more complicated.
The present invention provides a method for preparing a transition metal chalcogenide thin film, referring to fig. 1, which is a process flow diagram of the method, comprising the following steps:
s1: placing a target substrate in a chemical vapor deposition chamber, wherein a deposition surface of the target substrate faces the raw material conveying direction, a preset angle is formed between the deposition surface and a horizontal plane, and the preset angle is larger than 0 degree;
s2: and conveying a sulfur source and a transition metal source to the deposition surface to form a transition metal chalcogenide film with preset layer number distribution and preset coverage rate on the surface of the deposition surface.
Specifically, the concentration of the precursor near the target substrate can be controllably modulated by changing the inclination angle of the target substrate, so that the purposes of controlling the coverage rate and the number of layers of the transition metal chalcogenide film are achieved, and the method is simple and effective.
As an example, the target substrate includes a silicon layer and a silicon dioxide layer stacked, and the target substrate has one surface of the silicon dioxide layer as the deposition surface.
As an example, the chemical vapor deposition apparatus adopted by the present invention may be a tube furnace or other suitable apparatus, please refer to fig. 2, which is a schematic diagram of a chemical vapor deposition apparatus adopting a quartz tube 1 as a deposition chamber, and includes a first heating region 2 and a second heating region 3, where the first heating region 2 and the second heating region 3 are sequentially arranged along the raw material conveying direction, the sulfur source is obtained by placing sulfur powder 4 in the first heating region 2 and heating and gasifying, and the transition metal source is obtained by placing transition metal oxide powder 5 in the second heating region 3 and heating and gasifying.
By way of example, the transition metal source includes, but is not limited to, a tungsten source or a molybdenum source, and correspondingly, the transition metal chalcogenide film includes, but is not limited to, a tungsten disulfide film or a molybdenum disulfide film.
As an example, the sulfur powder 4 is high-purity sulfur powder, the sulfur powder 4 is placed in a first quartz boat 8 in the quartz tube 1, the transition metal oxide powder 5 (e.g., high-purity tungsten oxide powder or high-purity molybdenum oxide powder) is placed in a second quartz boat 9 in the quartz tube 1, and the inner diameter of the quartz tube 1 is 50 mm.
For example, by controlling the heating assembly to make the reaction temperature of the sulfur source and the transition metal source be 700-850 ℃ or other suitable temperature to form the transition metal chalcogenide film on the surface of the deposition surface, an inert gas, such as argon, may be introduced in addition to the sulfur source and the transition metal source during the reaction.
As an example, the target substrate 6 is held by a holding device so as to be at the predetermined angle with respect to the horizontal plane. In this embodiment, a quartz boat loaded with the transition metal oxide powder 5 is used as the holding device, the quartz boat includes a containing groove with an upward opening, a slot 7 for holding the target substrate 6 is disposed on a wall of the containing groove, and the slot is preferably wide enough to hold the target substrate.
As an example, the wall of the receiving groove may be provided with a plurality of pairs of slots with different inclination angles to facilitate selection of a desired inclination angle as required. Referring to fig. 3, the target substrate 6 is shown disposed horizontally on the second quartz boat 9 with the deposition surface facing downward. Referring to fig. 4 to 6, schematic views of the target substrates 6 being held in the clamping slots 7 of the second quartz boat 9 are shown, wherein fig. 4 shows a case where the predetermined angle is 30 °, fig. 5 shows a case where the predetermined angle is 60 °, and fig. 6 shows a case where the predetermined angle is 90 °.
It should be noted that, in other embodiments, other chucking devices disposed separately from the second quartz boat 9 may be used to make the deposition surface of the target substrate 6 have a predetermined angle with the horizontal plane, and the separately disposed chucking devices are disposed downstream of the transition metal oxide powder 5. The specific structure of the chucking device may be designed as required as long as it is sufficient to stably chuck the target substrate 1 and to adjust the chucking angle, and the scope of the present invention should not be unduly limited herein.
As an example, the preset angle ranges from 10 ° to 90 °. For comparison, referring to fig. 7, an optical microscope image of the tungsten disulfide thin film obtained when the target substrate 6 is horizontally placed on the second quartz boat 9 is shown, it can be seen that the triangular tungsten disulfide single crystal is unevenly distributed and rare in quantity, because the precursor concentration distribution near the target substrate is uneven, and the growth of the triangular tungsten disulfide single crystal is stopped incompletely because of lack of continuous sulfur source supply during the growth process.
As an example, the predetermined angle is set to 15 ° to 40 ° so that the area ratio of a single layer film in the transition metal chalcogenide film is greater than 50%. Referring to fig. 8, which shows an optical microscope image of the tungsten disulfide film obtained when the preset angle is 30 °, it can be seen that, since the precursor concentration near the target substrate is uniformly distributed, the triangle shape is complete, the film is uniformly distributed on the surface of the target substrate, the coverage rate of the film is about 50%, most of the film is few layers, and the inclination angle is preferred for preparing a single-layer film.
As an example, the predetermined angle is set to 45 ° to 75 ° so that a coverage of the transition metal chalcogenide film with respect to the deposition surface is greater than 70% and/or an area occupying ratio of a multi-layer film in the transition metal chalcogenide film is greater than 80%. Referring to fig. 9, which is an optical microscope image of the obtained tungsten disulfide film at the predetermined angle of 60 °, it can be seen that the concentration of the precursor near the target substrate is effectively modulated due to the increase of the tilt angle, the nucleation point is increased, the film coverage is about 70%, and during the continuous growth process, the film is grown longitudinally due to the continuous and sufficient supply of the sulfur source, and most of the film is multi-layered, which is the preferred tilt angle for preparing the high coverage film.
As an example, the predetermined angle is set to 80 ° to 90 ° so that the area ratio of the multi-layered thin film in the transition metal chalcogenide thin film is greater than 90%. Referring to fig. 10, an optical microscope image of the obtained tungsten disulfide film at the predetermined angle of 90 ° is shown, and it can be seen that when the predetermined angle is increased to be perpendicular to the target substrate, the sulfur source near the target substrate is excessive, resulting in a longitudinal growth behavior of the film, and the number of layers of the film is multiple.
In summary, in the preparation method of the transition metal chalcogenide thin film, the target substrate is placed in the chemical vapor deposition chamber, the deposition surface of the target substrate faces the raw material conveying direction, a preset angle is formed between the deposition surface and the horizontal plane, and the preset angle is larger than 0 °; and conveying a sulfur source and a transition metal source to the deposition surface to form a transition metal chalcogenide film with preset layer number distribution and preset coverage rate on the surface of the deposition surface. The method can controllably modulate the concentration of the precursor near the target substrate by changing the inclination angle of the target substrate, can effectively control the coverage rate and the layer number of the transition metal chalcogenide film, and is favorable for expanding the application of the transition metal chalcogenide. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (11)
1. A method for preparing a transition metal chalcogenide thin film, comprising the steps of:
placing a target substrate in a chemical vapor deposition cavity, wherein a deposition surface of the target substrate faces to a raw material conveying direction, a preset angle is formed between the deposition surface and a horizontal plane, and the preset angle is larger than 0 degree;
and conveying a sulfur source and a transition metal source to the deposition surface to form a transition metal chalcogenide film with preset layer number distribution and preset coverage rate on the surface of the deposition surface.
2. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: the transition metal source comprises a tungsten source and the transition metal chalcogenide film comprises a tungsten disulfide film, or the transition metal source comprises a molybdenum source and the transition metal chalcogenide film comprises a molybdenum disulfide film.
3. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: the preset angle ranges from 10 degrees to 90 degrees.
4. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: setting the preset angle to be 15-40 degrees so that the area ratio of a single-layer film in the transition metal chalcogenide film is more than 50%.
5. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: the preset angle is set to 45-75 ° so that the coverage of the transition metal chalcogenide thin film with respect to the deposition plane is greater than 70%.
6. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: the preset angle is set to be 45-75 degrees so that the area ratio of the multilayer thin film in the transition metal chalcogenide is larger than 80%.
7. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: setting the preset angle to be 80-90 degrees so that the area ratio of the multilayer film in the transition metal chalcogenide film is more than 90%.
8. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: the chemical vapor deposition cavity comprises a first heating area and a second heating area, the first heating area and the second heating area are sequentially arranged along the raw material conveying direction, the sulfur source is obtained by placing sulfur powder in the first heating area and heating and gasifying the sulfur powder, and the transition metal source is obtained by placing transition metal oxide powder in the second heating area and heating and gasifying the transition metal oxide powder.
9. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: and clamping the target substrate by a clamping device so that the deposition surface and the horizontal plane form the preset angle.
10. The method for preparing a transition metal chalcogenide thin film according to claim 9, wherein: the clamping device comprises a quartz boat, the quartz boat comprises an accommodating groove with an upward opening, and a clamping groove for clamping the target substrate is formed in the wall of the accommodating groove.
11. The method for preparing a transition metal chalcogenide thin film according to claim 1, wherein: the target substrate comprises a silicon layer and a silicon dioxide layer which are stacked, and one surface of the target substrate with the silicon dioxide layer is used as the deposition surface.
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| CN202210959994.4A CN115125513A (en) | 2022-08-11 | 2022-08-11 | Preparation method of transition metal chalcogenide film |
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| CN202210959994.4A CN115125513A (en) | 2022-08-11 | 2022-08-11 | Preparation method of transition metal chalcogenide film |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110241400A (en) * | 2019-06-17 | 2019-09-17 | 西安交通大学 | The method that no glue transfer prepares single layer Transition-metal dichalcogenide longitudinal direction hetero-junctions |
| CN114574955A (en) * | 2022-03-04 | 2022-06-03 | 北京大学 | Preparation method of catalyst double-assisted two-dimensional transition metal chalcogenide film |
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- 2022-08-11 CN CN202210959994.4A patent/CN115125513A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110241400A (en) * | 2019-06-17 | 2019-09-17 | 西安交通大学 | The method that no glue transfer prepares single layer Transition-metal dichalcogenide longitudinal direction hetero-junctions |
| CN114574955A (en) * | 2022-03-04 | 2022-06-03 | 北京大学 | Preparation method of catalyst double-assisted two-dimensional transition metal chalcogenide film |
Non-Patent Citations (1)
| Title |
|---|
| 岳皎洁等: ""衬底位置与角度对CVD法制备单层MoS2形貌的影响"", 《西安工业大学学报》, vol. 39, no. 6, pages 669 - 675 * |
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