CN114775043A - Preparation method for improving film thickness uniformity - Google Patents
Preparation method for improving film thickness uniformity Download PDFInfo
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- CN114775043A CN114775043A CN202210420002.0A CN202210420002A CN114775043A CN 114775043 A CN114775043 A CN 114775043A CN 202210420002 A CN202210420002 A CN 202210420002A CN 114775043 A CN114775043 A CN 114775043A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 100
- 238000000034 method Methods 0.000 claims abstract description 98
- 239000010408 film Substances 0.000 claims abstract description 96
- 239000010409 thin film Substances 0.000 claims abstract description 59
- 239000013078 crystal Substances 0.000 claims abstract description 45
- 238000000151 deposition Methods 0.000 claims abstract description 25
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 15
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 8
- 238000005566 electron beam evaporation Methods 0.000 claims abstract description 5
- 230000008020 evaporation Effects 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 5
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- 238000000137 annealing Methods 0.000 claims description 28
- 238000004549 pulsed laser deposition Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 19
- 238000011065 in-situ storage Methods 0.000 claims description 19
- 229910052710 silicon Inorganic materials 0.000 claims description 19
- 239000010703 silicon Substances 0.000 claims description 19
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003570 air Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910002601 GaN Inorganic materials 0.000 claims description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 3
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 3
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 claims description 3
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 3
- 229910001195 gallium oxide Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 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 3
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- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
-
- 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
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
-
- 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
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
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- Chemical & Material Sciences (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present disclosure provides a preparation method for improving film thickness uniformity and a film thereof, wherein one aspect of the present disclosure provides a preparation method for improving film thickness uniformity, comprising: growing a thin film seed crystal layer on the substrate by using a pulse laser deposition method to obtain the substrate with the thin film seed crystal layer; and continuing the homoepitaxial growth on the substrate with the thin film seed crystal layer by other growth methods different from the pulse laser deposition method until the thickness of the thin film reaches a preset threshold value, wherein the other growth methods comprise one of the following methods: electron beam evaporation, direct current magnetron sputtering, radio frequency magnetron sputtering, ion beam evaporation, metal organic chemical vapor deposition, molecular beam epitaxy, atomic layer deposition, plasma chemical vapor deposition.
Description
Technical Field
The invention relates to the technical field of film preparation, in particular to a preparation method for improving the thickness uniformity of a film.
Background
The thin film is a film which is prepared on a substrate capable of providing a supporting effect for growth by adopting a physical or chemical method, wherein the size of one dimension is far smaller than that of other two dimensions. Because of the special properties of the film, the film material is widely applied to a plurality of fields such as semiconductor functional devices, optical coating, security coatings and the like, and correspondingly, the preparation methods of the film are also infinite.
The pulse laser deposition technology is an advanced vacuum physical deposition technology, and uses an excimer laser to generate high-energy pulse laser to irradiate the surface of a target material and ablate the target material, so that the surface of the target material is rapidly heated to generate a highly-oriented plasma plume, and ions, molecules, clusters and other substances in the plume collide with the surface of the substrate and are cooled, and then nucleation growth is carried out on the surface of the substrate, and finally a continuous film is formed. The pulse laser deposition technology can accurately control the element stoichiometric ratio between the target material and the deposited film, flexibly select reaction gas, independently adjust a plurality of growth parameters in the growth process, and the high-energy pulse laser ablates the materials such as ions, molecules, clusters and the like in the plume generated by the target material, so that the particles still have high energy when reaching the surface of the substrate, thereby facilitating the full surface diffusion and being very beneficial to the epitaxial growth of the film from the aspect of growth dynamics. Therefore, the pulse laser deposition technology is widely applied to the modern epitaxial film preparation process, but the plume generated after the target material is ablated by the laser has a high orientation type, so that the epitaxial film with large area and good thickness uniformity is difficult to grow.
Although the literature reports the results of growing large-size epitaxial films by pulsed laser deposition techniques, the process often requires complicated mechanical structure of the apparatus or optical path moving devices, such as raster scanning the incident laser beam, rotating the substrate and target, bi-directionally ablating the target, and so on. These additional operations undoubtedly increase the production cost, increase the complexity and difficulty of the equipment, and limit the use of large-area production, and even so, when growing some thin film materials (such as refractory oxide films), it is still difficult to obtain large-sized, uniform-thickness thin film materials.
Disclosure of Invention
In view of the above, the present disclosure provides a method for improving the thickness uniformity of a thin film and a thin film prepared by the method, which are used to solve the problem that it is difficult to prepare a large-area thin film with good thickness uniformity by using a pulsed laser deposition method.
In order to achieve the above object, one aspect of the present disclosure provides a method for improving film thickness uniformity, including: growing a thin film seed crystal layer on the substrate by using a pulse laser deposition method to obtain the substrate with the thin film seed crystal layer; and continuing the homoepitaxial growth on the substrate with the film seed crystal layer by other growth methods different from the pulse laser deposition method until the thickness of the film reaches a preset threshold value, wherein the other growth methods comprise one of the following methods: electron beam evaporation, direct current magnetron sputtering, radio frequency magnetron sputtering, ion beam evaporation, metal organic chemical vapor deposition, molecular beam epitaxy, atomic layer deposition, plasma chemical vapor deposition.
According to an embodiment of the present disclosure, the substrate includes at least one of: sapphire, silicon, magnesia, zirconia, gallium oxide, boron nitride, gallium nitride, silicon carbide, strontium titanate, gallium arsenide, indium phosphide, diamond.
According to the embodiment of the present disclosure, before growing the thin film seed layer on the substrate by using the pulsed laser deposition method, the method further comprises: cleaning the substrate, wherein the method for cleaning the substrate comprises at least one of the following steps: wet cleaning, in-situ argon plasma cleaning and in-situ hydrogen plasma cleaning.
According to the embodiment of the present disclosure, before the preparing the thin film seed crystal layer on the substrate by using the pulsed laser deposition method, the method further comprises: and carrying out in-situ annealing on the substrate for 0-24 h at the temperature of 200-1200 ℃.
According to the embodiment of the present disclosure, after obtaining the substrate with the thin film seed layer, the method further includes: and annealing the substrate with the seed crystal layer.
According to an embodiment of the present disclosure, the annealing process includes: and raising the temperature of the substrate with the thin film seed crystal layer to 200-1800 ℃ at a heating rate of 1-20 ℃/min, annealing for 0.1-72 hours, and cooling to room temperature at a cooling rate of 1-50 ℃/min.
According to an embodiment of the present disclosure, the annealing atmosphere used in the in-situ annealing and the annealing process includes at least one of: vacuum, oxygen, hydrogen, argon, nitrogen, air.
According to the embodiment of the present disclosure, before and after the annealing treatment, the method further includes: the method for cleaning the substrate with the thin film seed crystal layer comprises at least one of the following steps: wet cleaning, in-situ argon plasma cleaning and in-situ hydrogen plasma cleaning.
According to the embodiment of the disclosure, the form of the growth source adopted in the process of continuing the homoepitaxial growth on the substrate with the thin film seed layer by other growth methods comprises at least one of the following: a multi-component mixed growth source, a single-component multiple growth source, a single-component single growth source; the growth atmosphere comprises at least one of: vacuum, oxygen, hydrogen, argon, nitrogen, air.
A second aspect of the present disclosure provides a thin film prepared according to the above-described method for improving the uniformity of the thickness of a thin film.
According to the embodiment of the disclosure, the seed crystal layer of the film is grown by using the pulse laser deposition method, and then the homoepitaxial growth is continuously carried out on the substrate with the seed crystal layer of the film by using other growth methods, so that the problem of poor film thickness uniformity caused by high-orientation type plume generated by laser ablation of a target in the process of continuously growing the film by using the pulse laser deposition method can be avoided, and the problem that the preparation of the film with large area and good thickness uniformity by using the pulse laser deposition method in the related technology is at least partially solved.
Drawings
Fig. 1 schematically illustrates a flow chart of a fabrication method for improving film thickness uniformity according to an embodiment of the present disclosure;
fig. 2 schematically shows an XRD scan of a YSZ film prepared on a silicon substrate according to an embodiment of the present disclosure;
fig. 3 schematically shows an Omega scan of the (200) direction diffraction peak of a YSZ film prepared on a silicon substrate according to an embodiment of the present disclosure;
fig. 4 schematically shows a phi scan of a YSZ film prepared on a silicon substrate according to an embodiment of the disclosure;
fig. 5 schematically shows a distribution diagram of test points characterizing thickness of a YSZ film prepared on a silicon substrate according to an embodiment of the present disclosure.
Detailed Description
Hereinafter, embodiments of the present disclosure will be described with reference to the accompanying drawings. It should be understood that the description is illustrative only and is not intended to limit the scope of the present disclosure. In the following detailed description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the embodiments of the disclosure. It may be evident, however, that one or more embodiments may be practiced without these specific details. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present disclosure.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. The terms "comprises," "comprising," and the like, as used herein, specify the presence of stated features, steps, operations, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, or components.
All terms (including 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, unless otherwise defined. It is noted that the terms used herein should be interpreted as having a meaning that is consistent with the context of this specification and should not be interpreted in an idealized or overly formal sense.
Where a convention analogous to "at least one of A, B and C, etc." is used, in general such a construction is intended in the sense one having skill in the art would understand the convention (e.g., "a system having at least one of A, B and C" would include but not be limited to systems that have a alone, B alone, C alone, a and B together, a and C together, B and C together, and/or A, B, C together, etc.). Where a convention analogous to "A, B or at least one of C, etc." is used, in general such a construction is intended in the sense one having skill in the art would understand the convention (e.g., "a system having at least one of A, B or C" would include but not be limited to systems that have a alone, B alone, C alone, a and B together, a and C together, B and C together, and/or A, B, C together, etc.).
Although the pulse laser deposition method can generate ions, molecules, clusters and other substances with very high energy, the ions with the high energy still have very high energy when reaching the surface, are convenient for full diffusion and are beneficial to nucleation growth on the surface of the substrate, the plume generated after the target is ablated by the laser has high directionality, so that the epitaxial film with large area and good thickness uniformity is difficult to grow. In the process of growing the epitaxial film by physical vapor deposition methods such as electron beam evaporation, direct current magnetron sputtering, radio frequency magnetron sputtering, ion beam evaporation and the like, highly directional plasma plume does not exist, and the transverse expansion distribution area of a deposited substance is large, so that the method has the advantages of increasing the transverse size and the thickness uniformity of the film. However, compared with the pulsed laser deposition technology, in the film preparation process of the magnetron sputtering method and other methods, the energy of ions and molecules in the excited plasma is smaller, so that the residual energy when the excited plasma reaches the surface of the substrate after deceleration in the background gas is smaller, and diffusion on the surface of the substrate is not facilitated, so that nucleation growth on the surface of the substrate is not facilitated, and if nucleation growth on the surface of the substrate is required, strict regulation and control on equipment and growth conditions are usually required to obtain an epitaxial film with higher crystal quality.
In view of the above, in order to improve the uniformity of the film thickness, after the thin film seed layer is prepared by the pulsed laser deposition method, the homoepitaxial growth is continued by other methods. The method combines the pulse laser deposition technology with other film growth methods which are beneficial to expanding the transverse size of the film and increasing the thickness uniformity of the film, is used for preparing the film, has important significance for realizing the stable preparation of the epitaxial film with large size, good thickness uniformity and high crystal quality, and is more beneficial to large-scale production.
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
Fig. 1 schematically shows a flow chart of a manufacturing method for improving the thickness uniformity of a thin film.
As shown in fig. 1, the method for improving the uniformity of the film thickness includes operations S101 to S102.
In operation S101, a thin film seed layer is grown on a substrate using a pulsed laser deposition method, resulting in a substrate having the thin film seed layer.
In operation S102, homoepitaxial growth is continued on the substrate having the thin film seed layer by a growth method other than the above-described pulsed laser deposition method until the thickness of the thin film reaches a preset threshold.
According to an embodiment of the present disclosure, the other growth method in operation S102 includes one of the following: electron beam evaporation, direct current magnetron sputtering, radio frequency magnetron sputtering, ion beam evaporation, metal organic chemical vapor deposition, molecular beam epitaxy, atomic layer deposition, plasma chemical vapor deposition.
According to an embodiment of the present disclosure, the preset threshold may be a thickness value determined according to actual conditions. Can be adjusted adaptively according to actual needs.
According to the embodiments of the present disclosure, the target material used in the preparation of the thin film by the pulsed laser deposition method or other methods may be a multi-component single target material, or may be a plurality of single-component target materials. The material used for growing the thin film twice in operations S101 and S102 may be the same material.
According to the embodiment of the disclosure, the problem of poor film thickness uniformity caused by high-orientation type plume generated by laser ablation of a target in the process of continuing epitaxial growth of the film by the pulse laser deposition method can be avoided by combining the pulse laser deposition technology with other growth methods which are beneficial to expanding the transverse size of the film and improving the film thickness uniformity.
According to an embodiment of the present disclosure, the material of the substrate may be a material capable of providing a supporting effect for the growth of the thin film, for example: sapphire, silicon, magnesia, zirconia, gallium oxide, boron nitride, gallium nitride, silicon carbide, strontium titanate, gallium arsenide, indium phosphide and diamond, and the selection of the substrate can be adaptively adjusted according to actual needs.
According to the embodiment of the present disclosure, before growing the thin film seed layer on the substrate by using the pulsed laser deposition method, the method further comprises: cleaning the substrate, wherein the method for cleaning the substrate comprises at least one of the following steps: wet cleaning, in-situ argon plasma cleaning, and in-situ hydrogen plasma cleaning. The substrate is cleaned to remove impurities on the surface of the substrate, so that the influence of the impurities on the thickness uniformity of the thin film can be avoided while the purity of the thin film is improved.
According to the embodiment of the present disclosure, before the preparing the thin film seed layer on the substrate by using the pulsed laser deposition method, the method further comprises: and carrying out in-situ annealing on the substrate for 0-24 h at the temperature of 200-1200 ℃.
According to the embodiment of the present disclosure, after the substrate with the thin film seed layer is obtained, the method further includes: and annealing the substrate with the seed crystal layer.
According to an embodiment of the present disclosure, annealing a substrate having a seed layer includes: and raising the temperature of the substrate with the film seed crystal layer to 200-1800 ℃ at a heating rate of 1-20 ℃/min, annealing for 0.1-72 h, and cooling to room temperature at a cooling rate of 1-50 ℃/min.
According to an embodiment of the present disclosure, the annealing atmosphere used in the in-situ annealing and the annealing process includes at least one of: vacuum, oxygen, hydrogen, argon, nitrogen, air.
According to the embodiment of the disclosure, the in-situ annealing of the substrate or the annealing of the substrate with the seed crystal layer can eliminate the internal stress generated by the substrate in the processing process, refine the crystal grains, homogenize the structure and improve the performance of the prepared film.
According to the embodiment of the present disclosure, before and after the annealing treatment, the method further includes: the method for cleaning the substrate with the thin film seed crystal layer comprises at least one of the following steps: wet cleaning, in-situ argon plasma cleaning, and in-situ hydrogen plasma cleaning. The substrate with the thin film seed crystal layer is cleaned to remove impurities on the surface of the substrate, so that the influence of the impurities on the thickness uniformity of the thin film can be avoided while the purity of the thin film is improved.
According to the embodiment of the present disclosure, the form of the growth source adopted in the process of continuing the homoepitaxial growth on the substrate with the thin film seed layer by other growth methods includes at least one of the following: a multi-component mixed growth source, a single-component multiple growth source and a single-component single growth source; the growth atmosphere comprises at least one of: vacuum, oxygen, hydrogen, argon, nitrogen, air.
According to the embodiment of the present disclosure, the growth source may also be understood as a target used in the process of performing epitaxial growth, specifically, the target and the growth mode used in the process of continuing homoepitaxial growth on the substrate with the thin film seed crystal layer by using other growth methods may be the target and the growth mode that are used by using a single-component target for epitaxial growth, or may be the target and the growth mode that are used by using a plurality of single-component targets for common epitaxial growth, or may be the target and the growth mode that are used by using a single-component target for epitaxial growth, or may be the target and the growth mode that are used by adaptively adjusted according to actual needs.
A second aspect of the present disclosure provides a thin film prepared according to the above-described method for improving the uniformity of the thickness of a thin film.
The present invention is further described with reference to the following embodiments, which are only some preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily made by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. The reaction or detection apparatus or device used in the present invention is not particularly limited as long as the object can be achieved, and any conventional apparatus or device known to those skilled in the art can be used.
Example 1
Take the example of preparing a Yttrium Stabilized Zirconia (YSZ) film on a 2 inch silicon substrate with the crystal orientation (100) direction.
And (2) performing ultrasonic treatment on a 2-inch (100) -oriented silicon substrate by using acetone and ethanol in sequence, cleaning by using deionized water, and blow-drying the surface of the substrate by using nitrogen to finish cleaning of the substrate.
Placing the cleaned substrate in a sample holder in a cavity of a pulsed laser deposition device, placing a ternary oxide target of YSZ in the target holder in the cavity of the pulsed laser deposition device, adjusting the target base distance of the pulsed laser deposition device, and vacuumizing until the background vacuum is less than 5 multiplied by 10-4mtorr, making the chamber a vacuum environment.
In a pulse laser deposition equipment cavity, heating the substrate to the temperature of 600-800 ℃, starting a KrF excimer laser, adjusting the wavelength to 248nm and the pulse width to 25ns, and generating pulse laser; after cleaning the target material by using pulse laser, removing the baffle above the substrate, and depositing a thin film seed crystal layer; and after the growth of the film is finished, cooling to room temperature, breaking vacuum to standard atmospheric pressure by using nitrogen, and taking out the substrate to finish the growth of the YSZ film seed crystal layer.
Placing the substrate with the YSZ film seed crystal layer on a magnetron sputtering sample holder, placing the YSZ ternary oxide target on the magnetron sputtering target holder, and adjusting the target base distance of magnetron sputtering equipment; vacuumizing until the background vacuum degree is less than 5 multiplied by 10-4mtorr, making the inside of the chamber a vacuum environment.
Heating the substrate to over 900 ℃ in a magnetron sputtering cavity; introducing oxygen into the cavity, and annealing for 0.1-24 hours in an oxygen atmosphere, so that the temperature in the cavity is conveniently reduced to the growth temperature; introducing argon, adjusting the flow ratio of oxygen to argon, and continuing to grow the YSZ film on the YSZ seed crystal layer;
and after the film growth is finished, closing argon, reducing the temperature of the substrate to room temperature, and breaking vacuum by using nitrogen to obtain the 2-inch YSZ film material with the average thickness of 100nm and the thickness nonuniformity of 6.62%.
Fig. 2 schematically shows an XRD scan of a YSZ film prepared on a silicon substrate according to an embodiment of the present disclosure; fig. 3 schematically shows an Omega scan of the (200) direction diffraction peak of a YSZ film prepared on a silicon substrate according to an embodiment of the present disclosure; fig. 4 schematically shows a phi scan of a YSZ film prepared on a silicon substrate according to an embodiment of the disclosure.
FIGS. 2-4 are representations of the properties of the YSZ films prepared in example 1. As shown in fig. 2, XRD diffraction peak positions of the YSZ film indicate that the YSZ film is a cubic structure. The silicon in fig. 2 is (400) -oriented, and since for silicon having a diamond structure, the (100) -oriented crystal plane generates extinction by virtue of crystal plane diffraction, and the (400) -oriented crystal plane and the (100) -oriented crystal plane are a set of parallel crystal planes, the (100) -oriented crystal plane can be described by the (400) -oriented crystal plane, so that it can be shown from the XRD result in fig. 2 that the YSZ film prepared on the silicon substrate by the method of embodiment 1 of the present application can be a single crystal epitaxial film having only (100) -oriented. Furthermore, the result of scanning the YSZ (200) diffraction peak with an X-ray rocking curve is shown in fig. 3, where the full width at half maximum of the YSZ (200) X-ray rocking curve is 0.75 °, which indicates that the epitaxial single crystallinity of the thin film is good; further, as shown in fig. 4, the azimuthal scans for YSZ (111) and Si (111) both showed four-fold symmetry, indicating that they are both cubic structures, and the location of the characteristic peak indicates that the YSZ film has a cubic-cubic epitaxial relationship with the silicon substrate, further demonstrating that the YSZ film is a high crystal quality single crystal epitaxial film.
Example 2
Example 2 may be a control experiment of example 1, taking the example of using only a pulsed laser deposition apparatus to prepare YSZ thin films on a 2-inch silicon substrate.
And (3) ultrasonically treating the 2-inch (100) -oriented silicon substrate by using acetone and ethanol in sequence, cleaning the substrate by using deionized water, and blow-drying the surface of the substrate by using nitrogen to finish cleaning the substrate.
Carrying out sample support in a cavity of the cleaned substrate pulse laser deposition equipment; placing the YSZ ternary oxide target material in a target material support in a cavity of pulse laser deposition equipment; adjusting the target base distance of the pulse laser deposition equipment to be the same as that of the pulse laser deposition equipment in the embodiment 1; vacuumizing until the background vacuum is less than 5X 10-4mtorr, making the inside of the chamber a vacuum environment.
Heating the substrate temperature to the same substrate temperature as in example 1 in the chamber of the pulsed laser deposition apparatus; starting a KrF excimer laser, adjusting the wavelength to 248nm and the pulse width to 25ns, and generating pulse laser; after cleaning the target material by using pulse laser, removing a baffle plate above the substrate, and starting a growth process of a YSZ film with the thickness of 100 nm;
and after the growth of the YSZ film is finished, cooling the temperature in the cavity to room temperature, breaking the vacuum by using nitrogen to reach standard atmospheric pressure, and taking out the substrate to obtain the YSZ film.
Fig. 5 schematically shows a distribution diagram of test points characterizing thickness of a YSZ film prepared on a silicon substrate according to an embodiment of the present disclosure.
As shown in fig. 5, the abscissa may represent each test point, and the ordinate may represent the corresponding film thickness value for each test point. The YSZ thin film obtained in example 1 and the thin film obtained in example 2 were respectively tested by an ellipsometer, 9 test points were respectively selected on the surfaces of the two thin films, and the data of the 9 test points were calculated, so that the non-uniformity of the thin films obtained in example 1 and example 2 can be calculated, and the calculation process can be as shown in formulas (1) to (2).
Film unevenness (maximum-minimum)/(average × 2) × 100% (1)
Wherein the maximum value may be the maximum value of the film thickness; the minimum value may be a minimum value of the film thickness; the average value may be an average value of the film thickness, and the calculation process of the average value may be as shown in equation (2).
Average value of the sum of the thicknesses/number of test points (2)
The thickness sum may be obtained by adding thicknesses corresponding to each test point.
By calculating the data of the 9 test points, the thickness non-uniformity of the YSZ film prepared by the combination of the pulsed laser deposition method and other growth methods is 6.62%, while the thickness non-uniformity of the YSZ film prepared by the pulsed laser deposition method alone is 20.62%, which indicates that the thickness uniformity of the film prepared by the combination of the pulsed laser deposition method and other growth methods is improved.
According to the embodiment of the disclosure, by combining a pulse laser deposition technology and other film growth technologies which are beneficial to expanding the transverse size of a film and increasing the uniformity of the film, a seed crystal layer with high crystal quality of the required film is grown on a substrate material by using pulse laser deposition equipment, and then homoepitaxy is performed on the seed crystal layer of the film by using other material growth equipment, so that the subsequent film growth is completed, the high crystal quality is ensured, the traditional defect of the film prepared by using the pulse laser deposition equipment can be optimized, the uniformity of the prepared film is improved, and the growth rate is increased.
According to the embodiment of the disclosure, the pulsed laser deposition technology and other film growth technologies have high reliability and mature technology, the pulsed laser deposition technology beneficial to epitaxial growth is combined with other film growth technologies beneficial to expanding the transverse size of the film and increasing the uniformity of the film, and the film forming quality and the process stability are high. In addition, the pulse laser deposition equipment and other film growth equipment required by the embodiment of the disclosure do not need to be designed with special structures and additional functions, the cost is saved, the operation is simple and convenient, the method is simple and easy to implement, and the method has great application potential.
It should also be noted that the directional terms mentioned in the embodiments, such as "upper", "lower", "front", "back", "left", "right", etc., are only directions referring to the drawings, and are not intended to limit the protection scope of the present invention. Throughout the drawings, like elements are represented by like or similar reference numerals. Conventional structures or constructions will be omitted when they may obscure the understanding of the present invention.
And the shapes and sizes of the respective components in the drawings do not reflect actual sizes and proportions, but merely illustrate contents of the embodiments of the present invention. In addition, the size of the substrate, the annealing temperature and other growth conditions adopted in the film preparation process can be adaptively adjusted according to actual needs. Furthermore, the word "comprising" does not exclude the presence of elements or steps not listed in a claim. The word "a" or "an" preceding an element does not exclude the presence of a plurality of such elements.
Similarly, it should be appreciated that in the foregoing description of exemplary embodiments of the invention, various features of the invention are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure and aiding in the understanding of one or more of the various inventive aspects. However, the method of the invention should not be construed to reflect the intent: that the invention as claimed requires more features than are expressly recited in each claim. Rather, as the following claims reflect, inventive aspects lie in less than all features of a single foregoing disclosed embodiment. Thus, the claims following the detailed description are hereby expressly incorporated into this detailed description, with each claim standing on its own as a separate embodiment of this invention.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and should not be construed as limiting the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method for improving the thickness uniformity of a film comprises the following steps:
growing a thin film seed crystal layer on the substrate by using a pulse laser deposition method to obtain the substrate with the thin film seed crystal layer;
and continuing to perform homoepitaxial growth on the substrate with the thin film seed crystal layer by other growth methods different from the pulsed laser deposition method until the thickness of the thin film reaches a preset threshold value, wherein the other growth methods comprise one of the following methods: electron beam evaporation, direct current magnetron sputtering, radio frequency magnetron sputtering, ion beam evaporation, metal organic chemical vapor deposition, molecular beam epitaxy, atomic layer deposition, plasma chemical vapor deposition.
2. The method of claim 1, wherein the substrate comprises at least one of: sapphire, silicon, magnesia, zirconia, gallium oxide, boron nitride, gallium nitride, silicon carbide, strontium titanate, gallium arsenide, indium phosphide, diamond.
3. The method of claim 1, wherein prior to said growing a thin film seed layer on a substrate using a pulsed laser deposition method, further comprising:
cleaning the substrate, wherein the method of cleaning the substrate comprises at least one of: wet cleaning, in-situ argon plasma cleaning, and in-situ hydrogen plasma cleaning.
4. The method of claim 1, wherein prior to said preparing a thin film seed layer on a substrate using a pulsed laser deposition method, further comprising:
and carrying out in-situ annealing on the substrate for 0-24 h at the temperature of 200-1200 ℃.
5. The method of claim 1, wherein after said obtaining a substrate having a thin film seed layer further comprises:
and annealing the substrate with the seed crystal layer.
6. The method of claim 5, wherein the annealing process comprises:
and raising the temperature of the substrate with the film seed crystal layer to 200-1800 ℃ at a heating rate of 1-20 ℃/min, annealing for 0.1-72 h, and cooling to room temperature at a cooling rate of 1-50 ℃/min.
7. The method of claim 5, wherein the in-situ annealing and the annealing atmosphere employed in the annealing process comprises at least one of: vacuum, oxygen, hydrogen, argon, nitrogen, air.
8. The method of claim 5, wherein before and after the annealing process comprises:
cleaning the substrate with the thin film seed layer, wherein the method for cleaning the substrate with the thin film seed layer comprises at least one of the following steps: wet cleaning, in-situ argon plasma cleaning, and in-situ hydrogen plasma cleaning.
9. The method of claim 1, wherein the form of the growth source employed in continuing homoepitaxial growth on the substrate with the thin film seed layer by other growth methods comprises at least one of: a multi-component mixed growth source, a single-component multiple growth source, a single-component single growth source; the growth atmosphere comprises at least one of: vacuum, oxygen, hydrogen, argon, nitrogen, air.
10. A film produced by the production method according to any one of claims 1 to 9.
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