CN117488408A - Single crystal aluminum nitride material and preparation method thereof - Google Patents
Single crystal aluminum nitride material and preparation method thereof Download PDFInfo
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- CN117488408A CN117488408A CN202210922436.0A CN202210922436A CN117488408A CN 117488408 A CN117488408 A CN 117488408A CN 202210922436 A CN202210922436 A CN 202210922436A CN 117488408 A CN117488408 A CN 117488408A
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 204
- 239000000463 material Substances 0.000 title claims abstract description 117
- 239000013078 crystal Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 152
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 75
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 67
- 239000002243 precursor Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims description 38
- 238000005530 etching Methods 0.000 claims description 14
- 229910052594 sapphire Inorganic materials 0.000 claims description 14
- 239000010980 sapphire Substances 0.000 claims description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 14
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- 238000005240 physical vapour deposition Methods 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 11
- 238000000137 annealing Methods 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 13
- 238000005299 abrasion Methods 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 238000001953 recrystallisation Methods 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 17
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
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- 229910001873 dinitrogen Inorganic materials 0.000 description 2
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- 238000001451 molecular beam epitaxy Methods 0.000 description 1
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- 238000005546 reactive sputtering 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
- C30B29/10—Inorganic compounds or compositions
- C30B29/38—Nitrides
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
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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
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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
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- 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
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
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Abstract
The application relates to the technical field of semiconductor materials, in particular to a monocrystalline aluminum nitride material and a preparation method thereof. The preparation method of the single crystal aluminum nitride material comprises the following steps: carrying out nitrogen plasma irradiation treatment on the precursor; the precursor comprises aluminum nitride layers and simple substance aluminum layers which are alternately stacked; the temperature of the nitrogen plasma irradiation treatment is not lower than 1300 ℃. Under the irradiation treatment of nitrogen plasma, the alternately stacked aluminum nitride layers and simple substance aluminum layers can be recrystallized at 1300 ℃ to form single crystal aluminum nitride materials, the single crystal has higher quality, and the dislocation density is less than 10 9 /cm 2 On the order of magnitude. Without being higher than 1The high-quality monocrystalline aluminum nitride material can be prepared by face-to-face annealing at the high temperature of 700 ℃, the preparation process is simple and easy to implement, the method is suitable for large-scale industrial production, mechanical abrasion such as surface scratches and the like caused by the face-to-face annealing process is avoided, the product yield is high, and the application range of the monocrystalline aluminum nitride material is greatly expanded.
Description
Technical Field
The application relates to the technical field of semiconductor materials, in particular to a monocrystalline aluminum nitride material and a preparation method thereof.
Background
Aluminum nitride is used as a new generation ultra-wide band gap semiconductor material, has excellent semiconductor characteristics such as high temperature resistance, high breakdown voltage resistance, wide optical window and the like, and also has high-frequency piezoelectric performance, so that the aluminum nitride material has advantages in the field of acoustic characteristics, particularly in the field of high-frequency communication filtering, and the demand of the industry for high-quality single crystal aluminum nitride materials is continuously increased.
At present, the preparation of high-quality monocrystalline aluminum nitride materials is difficult; although face-to-face annealing processes proposed in the current industry can achieve the preparation of high quality single crystal aluminum nitride materials, face-to-face annealing processes require high temperature environments above 1700 ℃ which increase equipment costs and batch preparation difficulties; in addition, the face-to-face annealing process requires mechanical contact, so that the surface of the single crystal aluminum nitride material prepared by face-to-face annealing has mechanical scratches and the like, and further the yield of the single crystal aluminum nitride material is low, and further application of the single crystal aluminum nitride material is greatly limited.
Disclosure of Invention
The invention aims to provide a single crystal aluminum nitride material and a preparation method thereof, which aim to solve the technical problems that the existing preparation of the single crystal aluminum nitride material requires extremely high temperature conditions and the preparation yield of the single crystal aluminum nitride material is not high.
In a first aspect, the present application provides a method for preparing a single crystal aluminum nitride material, comprising: carrying out nitrogen plasma irradiation treatment on the precursor; wherein the precursor comprises aluminum nitride layers and simple substance aluminum layers which are alternately stacked; the temperature of the nitrogen plasma irradiation treatment is not lower than 1300 ℃.
Under the irradiation treatment of nitrogen plasma, the alternately stacked aluminum nitride layers and elemental aluminum layers can be recrystallized at a lower temperature (the critical temperature is 1300 ℃) to form a single crystal aluminum nitride material, the single crystal has higher quality, and the dislocation density is less than 10 9 /cm 2 On the order of magnitude. The preparation method can be used for preparing the high-quality monocrystalline aluminum nitride material without carrying out face-to-face annealing in a high-temperature environment higher than 1700 ℃, is simple and easy to operate, is suitable for large-scale industrial production, is favorable for avoiding mechanical abrasion such as surface scratches and the like caused by the face-to-face annealing process, has higher product yield, and greatly expands the application range of the monocrystalline aluminum nitride material.
In some embodiments of the first aspect of the present application, the ratio of the thickness of the aluminum nitride layer to the thickness of the elemental aluminum layer in the precursor is (5-10): 1.
under the above conditions, the alternately stacked aluminum nitride layers and elemental aluminum layers can be fully recrystallized to form a single crystal aluminum nitride material, and the temperature required by aluminum nitride recrystallization can be further effectively reduced; if the thickness of the aluminum nitride layer is high, the temperature required by recrystallization of the aluminum nitride layer is increased, and the recrystallization is not easy to carry out; if the thickness of the aluminum nitride layer is low, the aluminum layer is excessively remained, so that the crystal content of the aluminum nitride single crystal is reduced.
In some implementations of the first aspect of the present application, each aluminum nitride layer has a thickness of 50nm or less and each elemental aluminum layer has a thickness of 10nm or less.
The thickness of each aluminum nitride layer is less than or equal to 50nm, and the thickness of each elemental aluminum layer is less than or equal to 10nm, so that under the treatment of nitrogen plasma irradiation, the alternately stacked aluminum nitride layers and elemental aluminum layers can be fully recrystallized to form a single crystal aluminum nitride material, the temperature required by recrystallization is further reduced, and the phenomenon that the quality of the single crystal of the aluminum nitride material is not improved due to incomplete recrystallization is avoided.
Optionally, the sum of the total thickness of the aluminum nitride layer and the total thickness of the elemental aluminum layer in the precursor is 0.1-2.0 μm.
Under the above conditions, the prepared monocrystalline aluminum nitride material has stable structure, is not easy to crack, and is not easy to generate surface decomposition phenomenon of the monocrystalline aluminum nitride material in a high temperature state.
In some embodiments of the first aspect of the present application, the power of the nitrogen plasma irradiation treatment is 50W or less.
The nitrogen plasma irradiation treatment is carried out under the power of less than or equal to 50W, so that the alternately stacked aluminum nitride layers and simple substance aluminum layers can be recrystallized to form the monocrystalline aluminum nitride material, and the surface roughening phenomenon of the monocrystalline aluminum nitride material caused by the over-high power can be avoided.
In some embodiments of the first aspect of the present application, the temperature of the nitrogen plasma irradiation treatment is 1400-1500 ℃.
The temperature of the nitrogen plasma irradiation treatment is 1400-1500 ℃, so that the alternately stacked aluminum nitride layers and elemental aluminum layers can be fully recrystallized to form a single crystal aluminum nitride material, the higher temperature (for example 1700 ℃ and above) is not needed for recrystallization of the aluminum nitride layers, and the lower nitrogen plasma irradiation treatment temperature is beneficial to reducing the energy consumption of equipment and prolonging the service life of the equipment.
In some embodiments of the first aspect of the present application, the nitrogen plasma irradiation treatment has a nitrogen atmosphere pressure of 0.1-2.0MPa.
Under the conditions, the surface smoothness of the aluminum nitride material is further improved.
In some embodiments of the first aspect of the present application, the method for preparing a single crystal aluminum nitride material further comprises: and carrying out surface etching on the product after the nitrogen plasma irradiation treatment.
And the product after the nitrogen plasma irradiation treatment is subjected to surface etching, so that the surface smoothness and flatness of the monocrystalline aluminum nitride material are improved.
Optionally, the step of surface etching includes: and soaking the product after the nitrogen plasma irradiation treatment in a strong alkali solution.
Optionally, the soaking time is 1-60min, and the soaking temperature is 10-50deg.C.
Optionally, the mass fraction of the strong base is 1-50%.
In some embodiments of the first aspect of the present application, the method for preparing the precursor includes: alternating depositing aluminum nitride layers and elemental aluminum layers on the substrate by adopting a chemical vapor deposition or physical vapor deposition mode.
The aluminum nitride layers and the elemental aluminum layers are alternately deposited on the substrate by adopting a chemical vapor deposition or physical vapor deposition mode, so that the combination between the aluminum nitride layers and the elemental aluminum layers is tighter, the subsequent recrystallization process under nitrogen plasma irradiation treatment is easier to carry out, and the recrystallization is more sufficient.
Optionally, the substrate is made of sapphire or silicon carbide.
Optionally, the preparation method of the precursor further comprises: the substrate is rinsed in a solution of acetone and/or ethanol before alternating layers of aluminum nitride and elemental aluminum are deposited on the substrate.
In some embodiments of the first aspect of the present application, the tray used in the nitrogen plasma irradiation treatment is a graphite tray.
The tray used in the nitrogen plasma irradiation treatment is a graphite tray, so that high-efficiency heat conduction can be realized, the heating uniformity of the precursor is improved, and the recrystallization process is fully performed.
Alternatively, the tray used in the nitrogen plasma irradiation treatment is a graphite tray having a silicon carbide coating on the surface.
In a second aspect, the present application provides a single crystal aluminum nitride material prepared by the method for preparing a single crystal aluminum nitride material as provided in the first aspect above.
The monocrystalline aluminum nitride material provided by the application has higher monocrystalline quality, and the dislocation density is less than 10 9 /cm 2 The order of magnitude is that the surface of the single crystal aluminum nitride has no mechanical abrasion such as scratch, and the application range of the single crystal aluminum nitride material is greatly expanded.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered limiting the scope, and that other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows a process flow diagram of the preparation of the single crystal aluminum nitride material provided by the present application.
Fig. 2 shows an X-ray rocking graph of the aluminum nitride material prepared in example 1 of the present application.
Fig. 3 shows an X-ray rocking graph of the aluminum nitride material prepared in comparative example 1 of the present application.
Fig. 4 shows an X-ray rocking graph of the aluminum nitride material prepared in comparative example 2 of the present application.
Fig. 5 shows a comparison of the surface flatness of the aluminum nitride materials produced in examples 1-2 and example 4 of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The present application provides a method for preparing a single crystal aluminum nitride material, fig. 1 shows a process flow chart for preparing a single crystal aluminum nitride material provided in the present application, referring to fig. 1, the method for preparing a single crystal aluminum nitride material includes:
s10, preparing a precursor with alternately stacked aluminum nitride layers and elemental aluminum layers.
In the present application, "precursor including aluminum nitride layers and elemental aluminum layers alternately stacked" means: the alternately stacked layer structure at least comprises an aluminum nitride layer positioned on the bottom layer, an elemental aluminum layer positioned on the bottom layer and an aluminum nitride layer positioned on the elemental aluminum layer.
It is understood that the precursor may have a plurality of aluminum nitride layers and a plurality of elemental aluminum layers, with one elemental aluminum layer between two adjacent elemental aluminum layers and one aluminum nitride layer between two adjacent elemental aluminum layers to form an "alternating stack" structure.
The precursor comprises alternately stacked aluminum nitride layers and simple substance aluminum layers, the alternately stacked aluminum nitride layers and simple substance aluminum layers are favorable for recrystallization under the subsequent nitrogen plasma irradiation treatment to form a single crystal aluminum nitride material, and the formed single crystal has higher quality and dislocation density of less than 10 9 /cm 2 On the order of magnitude. And the alternately stacked aluminum nitride layers and elemental aluminum layers can effectively reduce the temperature required by the recrystallization process, so that single crystal aluminum nitride can be recrystallized at 1300 ℃ without the temperature required by face-to-face annealing recrystallization above 1700 ℃.
In the present application, the ratio of the thickness of the aluminum nitride layer to the thickness of the elemental aluminum layer in the precursor is (5-10): 1. under the above conditions, the alternately stacked aluminum nitride layers and elemental aluminum layers can be fully recrystallized to form a single crystal aluminum nitride material, and the temperature required by aluminum nitride recrystallization can be further effectively reduced; if the thickness of the aluminum nitride layer is high, the temperature required by recrystallization of the aluminum nitride layer is increased, and the recrystallization is not easy to carry out; if the thickness of the aluminum nitride layer is low, the aluminum layer is excessively remained, so that the crystal content of single crystals in the aluminum nitride material is reduced.
As an example, the ratio of the thickness of the aluminum nitride layer to the thickness of the elemental aluminum layer in the precursor may be 5: 1. 6: 1. 8: 1. 8.5: 1. 9:1 or 10:1, etc.
Further, the thickness of each aluminum nitride layer is less than or equal to 50nm, and the thickness of each elemental aluminum layer is less than or equal to 10nm; under the nitrogen plasma irradiation treatment, the alternately stacked aluminum nitride layers and simple substance aluminum layers can be fully recrystallized to form the single crystal aluminum nitride material, the temperature required by recrystallization is further reduced, and the phenomenon that the quality of the single crystal of the aluminum nitride material is not improved due to incomplete recrystallization is avoided.
As an example, the thickness of each aluminum nitride layer may be 20nm, 25nm, 30nm, 35nm, 40nm, 50nm, or the like, independently of each other; the thickness of each elemental aluminum layer may be, independently, 3nm, 3.5nm, 5nm, 7nm, 10nm, or the like.
Still further, the sum of the total thickness of the aluminum nitride layer and the total thickness of the simple substance aluminum layer in the precursor is 0.1-2.0 mu m, and the prepared single crystal aluminum nitride material has stable structure, is not easy to crack, and is not easy to generate the surface decomposition phenomenon of the single crystal aluminum nitride material in a high temperature state. If the sum of the total thickness of the aluminum nitride layer and the total thickness of the simple substance aluminum layer in the precursor is too large, the prepared single crystal aluminum nitride material is easy to crack; if the sum of the total thickness of the aluminum nitride layer and the total thickness of the elemental aluminum layer in the precursor is too small, the aluminum nitride layer is easy to decompose under the subsequent nitrogen plasma radiation treatment, so that the material is roughened.
As an example, the sum of the total thickness of the aluminum nitride layer and the total thickness of the elemental aluminum layer in the precursor may be 0.1 μm, 0.2 μm, 0.5 μm, 1.0 μm, 1.5 μm, or 2.0 μm, etc.
In the present application, the preparation method of the precursor includes: alternating deposition of aluminum nitride layers and elemental aluminum layers on a substrate by Chemical Vapor Deposition (CVD) or Physical Vapor Deposition (PVD). The aluminum nitride layers and the elemental aluminum layers are alternately deposited on the substrate by adopting a chemical vapor deposition or physical vapor deposition mode, so that the combination between the aluminum nitride layers and the elemental aluminum layers is tighter, the subsequent recrystallization process under nitrogen plasma irradiation treatment is easier to carry out, and the recrystallization is more sufficient.
As an example, in the present application, an aluminum nitride layer and an elemental aluminum layer are formed on a substrate by physical vapor deposition; the equipment used for physical vapor deposition may be a reactive sputtering deposition equipment or a molecular beam epitaxy equipment, etc.
In the present application, the substrate may be made of sapphire or silicon carbide. As an example, sapphire Al 2 O 3 The substrate is an alpha phase single crystal sapphire substrate, and the crystal orientation range includes but is not limited to (0001) Al 2 O 3 Substrate, (1102) Al 2 O 3 Substrate and (1010) Al 2 O 3 A substrate, etc.; the SiC substrate of the silicon carbide is 4H, 6H and 3The C-phase silicon carbide substrate comprises various crystal phases and bevel angles.
Further, in the present application, when the substrate is made of sapphire or silicon carbide, the method for preparing the precursor includes: an aluminum nitride layer is first deposited on the substrate and the last layer deposited is also an aluminum nitride layer.
Because the bonding constants of the aluminum nitride and the sapphire substrate or the silicon carbide substrate are relatively similar, the aluminum nitride layer is deposited and grown on the sapphire substrate or the silicon carbide substrate, so that the generated aluminum nitride layer is more tightly bonded with the sapphire substrate or the silicon carbide substrate, and the precursor structure is more stable. The last layer deposited is an aluminum nitride layer, so that the aluminum nitride layer can be directly subjected to a recrystallization process under the irradiation treatment of nitrogen plasma; if the last layer is an elemental aluminum layer, the elemental aluminum of the outermost layer is directly volatilized at the temperature of the nitrogen plasma irradiation treatment; thus, from a process cost perspective, in this application the last layer deposited on the substrate is an aluminum nitride layer.
In this application, the preparation method of the precursor further includes: the substrate is rinsed in a solution of acetone and/or ethanol before alternating layers of aluminum nitride and elemental aluminum are deposited on the substrate.
Further, the substrate can be cleaned by ultrasonic cleaning. Still further, the deposition is blown dry with nitrogen after the substrate is cleaned to perform the deposition reaction.
S20, performing nitrogen plasma irradiation treatment on the precursor.
Under the irradiation treatment of nitrogen plasma, the alternately stacked aluminum nitride layers and simple substance aluminum layers in the precursor can be recrystallized to form a single crystal aluminum nitride material, the single crystal has higher quality, and the dislocation density is less than 10 9 /cm 2 On the order of magnitude. The high-quality monocrystalline aluminum nitride material can be prepared by nitrogen plasma irradiation treatment at the critical temperature of 1300 ℃ without carrying out face-to-face annealing at the high temperature of 1700 ℃, and the preparation process is simple and easy to implement and is suitable for large-scale industrial production.
When the nitrogen plasma irradiation treatment is adopted, the surface of the precursor to be treated does not contact any object, so that the mechanical abrasion such as surface scratch and the like caused by the face-to-face annealing process is avoided, the product yield is high, and the application range of the single crystal aluminum nitride material is greatly expanded.
In the present application, the temperature at which the precursor is subjected to nitrogen plasma irradiation treatment is 1300-1500 ℃.
Further, the temperature of the nitrogen plasma irradiation treatment of the precursor is 1400-1500 ℃, the temperature of the nitrogen plasma irradiation treatment is 1400-1500 ℃, the alternately stacked aluminum nitride layers and simple substance aluminum layers can be fully recrystallized to form a single crystal aluminum nitride material, the surface of the obtained single crystal aluminum nitride material is not easy to decompose, the higher temperature (for example 1700 ℃ and above) is not needed to be used for recrystallization of the aluminum nitride layer, and the lower nitrogen plasma irradiation treatment temperature is also beneficial to reducing the energy consumption of equipment and prolonging the service life of the equipment.
As an example, the temperature at which the precursor is subjected to the nitrogen plasma irradiation treatment may be 1300 ℃, 1320 ℃, 1350 ℃, 1370 ℃, 1400 ℃, 1450 ℃, 1500 ℃, or the like.
In the application, the power of the nitrogen plasma irradiation treatment is less than or equal to 50W. The nitrogen plasma irradiation treatment is carried out under the power of less than or equal to 50W, so that the alternately stacked aluminum nitride layers and simple substance aluminum layers can be recrystallized to form the monocrystalline aluminum nitride material, and the surface roughening phenomenon of the monocrystalline aluminum nitride material caused by the over-high power can be avoided.
As an example, the power of the nitrogen plasma irradiation treatment may be 15W, 20W, 25W, 30W, 40W, 50W, or the like.
In the present application, the nitrogen atmosphere pressure of the nitrogen plasma irradiation treatment is 0.1 to 2.0MPa. Under the conditions, the surface smoothness of the aluminum nitride material is further improved.
As an example, the pressure of the nitrogen plasma irradiation treatment may be 0.1MPa, 0.5MPa, 1.0MPa, 1.2MPa, 1.5MPa, 2.0MPa, or the like.
In the present application, the flow rate of nitrogen gas used in the nitrogen plasma irradiation treatment is 0.1 to 2.0sccm.
As an example, the flow rate of nitrogen gas used in the nitrogen plasma irradiation treatment may be 0.1sccm, 0.2sccm, 0.5sccm, 1.0sccm, 1.5sccm, 2.0sccm, or the like.
Further, in the present application, the tray used in the nitrogen plasma irradiation treatment is a graphite tray or a graphite tray having a silicon carbide coating on the surface. The tray used in the nitrogen plasma irradiation treatment is a graphite tray or a graphite tray with a silicon carbide coating on the surface, so that high-efficiency heat conduction can be realized, the heating uniformity of the precursor is improved, and the recrystallization process is fully carried out.
And S30, carrying out surface etching on the product after the nitrogen plasma irradiation treatment.
And (3) carrying out surface etching on the product subjected to the nitrogen plasma irradiation treatment, which is beneficial to improving the smoothness and flatness of the surface of the single crystal aluminum nitride material so as to expose a flat aluminum nitride crystal face.
In the present application, the step of surface etching includes: and soaking the product after the nitrogen plasma irradiation treatment in a strong alkali solution. As an example, the alkali solution used in the surface etching treatment may be potassium hydroxide or sodium hydroxide solution or the like.
Further, the soaking time is 1-60min, the soaking temperature is 10-50 ℃, and the mass fraction of the strong alkali is 1-50%.
S40, cleaning the product after surface etching.
In the present application, the step of performing cleaning treatment on the product after the surface etching includes: and carrying out ultrasonic cleaning on the etched product, and then drying with nitrogen.
The application also provides a single crystal aluminum nitride material which is prepared by adopting the preparation method of the single crystal aluminum nitride material.
The monocrystalline aluminum nitride material provided by the application has higher monocrystalline quality, and the dislocation density is less than 10 9 /cm 2 The order of magnitude is that the surface of the single crystal aluminum nitride has no mechanical abrasion such as scratch, and the application range of the single crystal aluminum nitride material is greatly expanded.
The characteristics and properties of the single crystal aluminum nitride material and the method of producing the same of the present application are described in further detail below with reference to examples.
Example 1
The embodiment provides a single crystal aluminum nitride material, which is prepared by the following steps:
(1) And (2) mixing the sapphire substrate with a mass ratio of 1:1 in a mixed solution of acetone and ethanol for 10min, and then drying by nitrogen. Wherein the sapphire substrate has a dimension of 2 inches and a crystal plane orientation of (0001), and the cleaned sapphire substrate is obtained.
(2) And alternately growing aluminum nitride layers (10 layers in total) and elemental aluminum layers (9 layers in total) on the cleaned sapphire substrate by adopting a magnetron sputtering mode, wherein the bottommost layer and the topmost layer are aluminum nitride layers, so as to obtain a precursor.
The thickness of each aluminum nitride layer is 50nm, the target material for forming the aluminum nitride layers is an elemental aluminum target, the sputtering power is 3000W, the sputtering temperature is 600 ℃, the atmosphere in the cavity is a mixed gas of nitrogen and argon (the volumes of the nitrogen and the argon are 5:1), and the sputtering time is 3min.
The thickness of each elemental aluminum layer is 5nm, the target material for forming the elemental aluminum layers is an elemental aluminum target, the sputtering power is 3000W, the sputtering temperature is 200 ℃, the atmosphere in the cavity is pure argon, and the sputtering time is 10s.
(3) And (3) carrying out nitrogen plasma irradiation treatment on the precursor obtained in the step (2), and then naturally cooling. Wherein, the power of the plasma is 20W, the treatment temperature is 1400 ℃, the treatment time is 300min, the atmosphere condition is nitrogen normal pressure, and the flow of the nitrogen is 1.0sccm.
(4) Immersing the product treated in the step (3) into 30% potassium hydroxide solution for etching for 5min, wherein the etching temperature is room temperature; then, the mass ratio of the product after surface etching is 1:1, and then drying by nitrogen after ultrasonic cleaning in the mixed solution of acetone and ethanol.
Example 2
The present embodiment provides a single crystal aluminum nitride material, which is different from embodiment 1 in that the power of the plasma in step (3) is different, and in this embodiment, the power of the plasma is 60W.
Example 3
This example provides a single crystal aluminum nitride material, which differs from example 1 in that the treatment temperature in step (3) is different, and in this example, the temperature of the nitrogen plasma irradiation treatment is 1300 ℃.
Example 4
This example provides a single crystal aluminum nitride material, which differs from example 1 in that the process pressure in step (3) is different, and in this example, the pressure of the nitrogen plasma irradiation process is 0.08MPa.
Example 5
The present embodiment provides a single crystal aluminum nitride material, which is different from embodiment 1 in that the thickness of the aluminum nitride layer in step (2) is different, and in this embodiment, the thickness of the aluminum nitride layer is 80nm.
Example 6
This example provides a single crystal aluminum nitride material, which differs from example 1 in that the thickness of the aluminum nitride layer in step (2) is different and the processing temperature in step (3) is different, in this example, the thickness of the aluminum nitride layer is 60nm and the temperature of the nitrogen plasma irradiation treatment is 1500 ℃.
Example 7
The present embodiment provides a single crystal aluminum nitride material, which is different from embodiment 1 in that the thickness of the elemental aluminum layer in step (2) is different, and in this embodiment, the thickness of the elemental aluminum layer is 12nm.
Comparative example 1
This comparative example provides an aluminum nitride material, and the difference between this comparative example and example 1 is in the step (2). In this comparative example, step (2) is as follows:
and growing an aluminum nitride layer on the cleaned sapphire substrate by adopting a magnetron sputtering mode to obtain a precursor. Wherein the thickness of the aluminum nitride layer is 545nm.
Comparative example 2
This comparative example provides an aluminum nitride material, and this comparative example differs from example 1 in that: this comparative example does not have step (3) and step (4) in example 1.
Experimental example 1
The aluminum nitride materials prepared in example 1, comparative example 1 and comparative example 2 were subjected to X-ray rocking curve test, respectively, and the test results are shown in fig. 2 to 4, respectively.
As can be seen from FIG. 2, the aluminum nitride material (including 002 face and 102 face) obtained in example 1 has a higher single crystal quality.
As can be seen from fig. 3, the single crystal quality of the aluminum nitride material prepared in comparative example 1 is significantly lower than that of the aluminum nitride material prepared in example 1; it was shown that single crystal aluminum nitride materials with high quality can be formed after nitrogen plasma irradiation treatment of a precursor having alternating stacked aluminum nitride layers and elemental aluminum layers.
As can be seen from fig. 4, the aluminum nitride material prepared in comparative example 2 has no RC diffraction peak, i.e., the aluminum nitride material prepared in comparative example 2 does not form a single crystal structure. It is shown that the single crystal aluminum nitride material with high quality cannot be formed effectively only by alternately stacking aluminum nitride layers and simple substance aluminum layers or directly performing nitrogen plasma irradiation treatment on the aluminum nitride layers.
Experimental example 2
The aluminum nitride materials prepared in examples 1, 3, 5 to 7 and comparative example 1 were each characterized in terms of dislocation density, and experimental results are shown in table 1.
TABLE 1
As can be seen from table 1, the single crystal quality of the aluminum nitride materials prepared in example 1, example 3, and examples 5 to 7 is significantly better than that of the aluminum nitride material prepared in comparative example 1, indicating that the single crystal aluminum nitride material having high quality can be formed after the nitrogen plasma irradiation treatment of the precursor having the alternately stacked aluminum nitride layers and elemental aluminum layers.
Further, the single crystal quality of the aluminum nitride materials prepared in examples 3, 5 and 7 was slightly lower than that of the aluminum nitride material prepared in example 1, indicating that the temperature of nitrogen plasma irradiation, the thickness of the aluminum nitride layer and the thickness of the elemental aluminum layer all had a certain influence on the single crystal quality of the prepared aluminum nitride material.
As can be seen from a comparison of example 1 and example 6, the single crystal quality of the aluminum nitride material prepared in example 1 was slightly higher than that of the aluminum nitride material prepared in example 6, indicating that when the thickness of the aluminum nitride layer was relatively increased, the temperature at which the nitrogen plasma irradiation treatment was performed also required to be increased accordingly, so that sufficient recrystallization could be achieved to form an aluminum nitride material of high single crystal quality.
Experimental example 3
The aluminum nitride materials prepared in examples 1-2 and example 4 were subjected to surface flatness comparison, and the comparison results are shown in fig. 5.
As can be seen from fig. 5, the surface of the aluminum nitride material prepared in example 1 is smoother, while the surface of the aluminum nitride materials prepared in examples 2 and 4 is rougher (i.e., roughening phenomenon exists), which indicates that the power and pressure of the nitrogen plasma irradiation treatment can affect the surface smoothness of the prepared single crystal aluminum nitride material.
In summary, the precursor with alternately stacked aluminum nitride layers and elemental aluminum layers can be recrystallized to form a single crystal aluminum nitride material by nitrogen plasma irradiation treatment, the temperature required by recrystallization can be effectively reduced, the single crystal quality is higher, and the dislocation density is less than 10 9 /cm 2 On the order of magnitude. The preparation method can be used for preparing the high-quality monocrystalline aluminum nitride material without carrying out face-to-face annealing in a high-temperature environment higher than 1700 ℃, is simple and easy to operate, is suitable for large-scale industrial production, is favorable for avoiding mechanical abrasion such as surface scratches and the like caused by the face-to-face annealing process, has higher product yield, and greatly expands the application range of the monocrystalline aluminum nitride material.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (10)
1. A method for preparing a single crystal aluminum nitride material, comprising: carrying out nitrogen plasma irradiation treatment on the precursor;
wherein the precursor comprises aluminum nitride layers and elemental aluminum layers which are alternately stacked; the temperature of the nitrogen plasma irradiation treatment is not lower than 1300 ℃.
2. The method for producing a single crystal aluminum nitride material according to claim 1, wherein a ratio of a thickness of the aluminum nitride layer to a thickness of the elemental aluminum layer in the precursor is (5-10): 1.
3. the method for producing a single crystal aluminum nitride material according to claim 2, wherein the thickness of each of the aluminum nitride layers is 50nm or less and the thickness of each of the elemental aluminum layers is 10nm or less;
optionally, the sum of the total thickness of the aluminum nitride layer and the total thickness of the elemental aluminum layer in the precursor is 0.1-2.0 μm.
4. A method for producing a single crystal aluminum nitride material according to any one of claims 1 to 3, wherein the power of the nitrogen plasma irradiation treatment is 50W or less.
5. A method for producing a single crystal aluminum nitride material according to any one of claims 1 to 3, wherein the temperature of the nitrogen plasma irradiation treatment is 1400 to 1500 ℃.
6. A method for producing a single crystal aluminum nitride material according to any one of claims 1 to 3, wherein the nitrogen plasma irradiation treatment has a nitrogen atmosphere pressure of 0.1 to 2.0MPa.
7. The method for producing a single crystal aluminum nitride material according to claim 1, characterized in that the method for producing a single crystal aluminum nitride material further comprises: carrying out surface etching on the product subjected to the nitrogen plasma irradiation treatment;
optionally, the step of surface etching includes: soaking the product subjected to the nitrogen plasma irradiation treatment in a strong alkali solution;
optionally, the soaking time is 1-60min, and the soaking temperature is 10-50 ℃;
optionally, the mass fraction of the strong base is 1-50%.
8. The method for producing a single crystal aluminum nitride material according to claim 1, wherein the method for producing a precursor comprises: alternately depositing the aluminum nitride layers and the elemental aluminum layers on the substrate by adopting a chemical vapor deposition or physical vapor deposition mode;
optionally, the substrate is made of sapphire or silicon carbide;
optionally, the preparation method of the precursor further comprises: the substrate is washed in a solution containing acetone and/or ethanol before the alternating deposition of the aluminum nitride layers and the elemental aluminum layers on the substrate.
9. The method for producing a single crystal aluminum nitride material according to claim 1, wherein the tray used in the nitrogen plasma irradiation treatment is a graphite tray;
alternatively, the tray used in the nitrogen plasma irradiation treatment is a graphite tray having a silicon carbide coating on the surface.
10. A single crystal aluminum nitride material, characterized by being produced by the method for producing a single crystal aluminum nitride material according to any one of claims 1 to 9.
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