WO2021210393A1 - 窒化アルミニウム基板の製造方法、窒化アルミニウム基板、及び、窒化アルミニウム層を形成する方法 - Google Patents
窒化アルミニウム基板の製造方法、窒化アルミニウム基板、及び、窒化アルミニウム層を形成する方法 Download PDFInfo
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- WO2021210393A1 WO2021210393A1 PCT/JP2021/013746 JP2021013746W WO2021210393A1 WO 2021210393 A1 WO2021210393 A1 WO 2021210393A1 JP 2021013746 W JP2021013746 W JP 2021013746W WO 2021210393 A1 WO2021210393 A1 WO 2021210393A1
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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
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
- C30B23/063—Heating of 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
-
- 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
- H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
- H10P14/29—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials characterised by the substrates
- H10P14/2901—Materials
- H10P14/2902—Materials being Group IVA materials
- H10P14/2904—Silicon carbide
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
- H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
- H10P14/29—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials characterised by the substrates
- H10P14/2924—Structures
- H10P14/2925—Surface structures
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
- H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
- H10P14/34—Deposited materials, e.g. layers
- H10P14/3402—Deposited materials, e.g. layers characterised by the chemical composition
- H10P14/3414—Deposited materials, e.g. layers characterised by the chemical composition being group IIIA-VIA materials
- H10P14/3416—Nitrides
Definitions
- the present invention relates to a method for manufacturing an aluminum nitride substrate, an aluminum nitride substrate, and a method for forming an aluminum nitride layer.
- a semiconductor substrate is manufactured by crystal-growth a growth layer on a base substrate.
- AlN crystals are grown by a sublimation method on a base substrate such as an aluminum nitride (AlN) substrate or a silicon carbide (SiC) substrate.
- AlN aluminum nitride
- SiC silicon carbide
- Patent Document 1 states, “By the vapor phase growth method, an AlN crystal is grown on a seed crystal substrate arranged in a crystal growth chamber in a crystal growth vessel provided in a reaction vessel. Therefore, a technique of "a method for growing an AlN crystal, which is characterized by supplying a carbon-containing gas into the crystal growth chamber during crystal growth” is described.
- An object to be solved by the present invention is to provide a novel technique capable of manufacturing a large-diameter AlN substrate. Another object of the present invention to be solved is to provide a new technique capable of producing an AlN substrate having a large diameter and good crystallinity.
- the present invention that solves the above-mentioned problems is a method for manufacturing an aluminum nitride substrate, which comprises a crystal growth step of forming an aluminum nitride layer on a silicon carbide base substrate having through holes.
- the aluminum nitride layer on the silicon carbide base substrate having through holes By forming the aluminum nitride layer on the silicon carbide base substrate having through holes in this way, it is possible to manufacture an aluminum nitride substrate having a large diameter and good crystallinity. By forming the aluminum nitride layer on the silicon carbide base substrate having through holes in this way, it is possible to manufacture an aluminum nitride substrate having a diameter equivalent to that of the silicon carbide base substrate. Therefore, by adopting a silicon carbide base substrate having a large diameter, an aluminum nitride substrate having a large diameter can be obtained.
- large diameter in the present specification means that a large area aluminum nitride layer can be obtained as compared with the case where the aluminum nitride layer is formed on the silicon carbide base substrate having no through holes. ..
- the crystal growth step is a step of heating so that a temperature gradient is formed along the vertical direction of the silicon carbide base substrate.
- the silicon carbide base substrate and the raw material of the aluminum nitride layer are arranged so as to face each other, and a temperature gradient is formed between the silicon carbide base substrate and the raw material. It is a process of heating so as to.
- the crystal growth step includes a lateral growth step in which the aluminum nitride layer grows in the horizontal direction of the silicon carbide base substrate and the aluminum nitride layer grows in the vertical direction of the silicon carbide base substrate. It has a vertical growth step to be carried out.
- a preferred embodiment of the present invention further includes a through hole forming step of forming a through hole in the silicon carbide base substrate and a strain layer removing step of removing the strain layer introduced by the through hole forming step.
- the through hole forming step is a step of forming a through hole by irradiating the silicon carbide base substrate with a laser.
- the strain layer removing step is a step of removing the strain layer of the silicon carbide base substrate by heat treatment.
- the strain layer removing step is a step of etching the silicon carbide base substrate in a silicon atmosphere.
- the present invention also relates to a method for forming an aluminum nitride layer. That is, the present invention that solves the above-mentioned problems forms an aluminum nitride layer including a through hole forming step of forming a through hole in the silicon carbide base substrate before forming the aluminum nitride layer on the silicon carbide base substrate. How to do it.
- a preferred embodiment of the present invention includes a strain layer removing step of removing the strain layer introduced by the through hole forming step.
- the strain layer removing step is a step of etching the silicon carbide base substrate by heat treatment.
- the disclosed technology it is possible to provide a new technology capable of manufacturing a large-diameter AlN substrate. Further, according to the disclosed technology, it is possible to provide a new technology capable of manufacturing an AlN substrate having a large diameter and good crystallinity.
- the method for manufacturing an AlN substrate according to the embodiment is a through hole forming step S10 for forming a through hole 11 in the SiC base substrate 10 and a strain layer removing step S20 for removing the strain layer 12 introduced by the through hole forming step S10. And the crystal growth step S30 for forming the AlN layer 20 on the SiC base substrate 10 having the through hole 11.
- the AlN layer has a large area including a through hole forming step S10 for forming a through hole 11 in the SiC base substrate 10 before forming the AlN layer 20 on the surface of the SiC base substrate 10. It can be grasped as a method of forming. Hereinafter, each step of the embodiment will be described in detail.
- the through hole forming step S10 is a step of forming the through hole 11 in the SiC base substrate 10. This through hole forming step S10 can be naturally adopted as long as it is a method capable of forming the through hole 11 in the SiC base substrate 10.
- a method for forming the through hole 11 for example, plasma etching such as laser processing, focused ion beam (FIB), and reactive ion etching (RIE) can be adopted.
- plasma etching such as laser processing, focused ion beam (FIB), and reactive ion etching (RIE) can be adopted.
- FIB focused ion beam
- RIE reactive ion etching
- SiC base substrate 10 As the SiC base substrate 10, a wafer or substrate processed from bulk crystals may be used, or a substrate having a buffer layer made of the above-mentioned semiconductor material may be used separately.
- the through hole 11 may be formed in a shape that reduces the strength of the SiC base substrate 10, and may be formed in a single number or a plurality of through holes 11. Further, a through-hole group (pattern) in which a plurality of through-holes 11 are arranged may be adopted.
- FIG. 3 is an explanatory diagram illustrating the pattern 100 according to the embodiment.
- the line segment indicated by the pattern 100 is the SiC base substrate 10.
- the pattern 100 preferably exhibits a regular hexagonal displacement shape that is three-fold symmetric.
- the "regular hexagonal displacement type" in the description in the present specification will be described in detail below with reference to FIG.
- the regular hexagonal displacement type is a dodecagon.
- the regular hexagonal displacement type is composed of 12 line segments having the same length and being linear.
- the pattern 100 exhibiting a regular hexagonal displacement shape is a regular triangle and includes a reference figure 101 having an area of 101a and including three vertices 104. Each of the three vertices 104 is included in the vertices of the pattern 100.
- the three vertices 104 may be located on the line segment constituting the pattern 100.
- the pattern 100 includes a line segment 102 (corresponding to the first line segment) extending from the apex 104 and including the apex 104, and a line segment 103 (second line segment) not extending from the apex 104 and not including the apex 104 and adjacent to the line segment 102. Corresponds to a line segment.) And.
- the angle ⁇ formed by the two adjacent line segments 102 in the pattern 100 is constant, and is equal to the angle ⁇ formed by the two adjacent line segments 103 in the pattern 100.
- regular hexagonal displacement type in the description of the present specification means that the regular hexagon is displaced (deformed) while maintaining the area of the regular hexagon based on the angle ⁇ indicating the degree of unevenness. It can be grasped that it is a dodecagon.
- the angle ⁇ is preferably larger than 60 °, preferably 66 ° or more, preferably 80 ° or more, preferably 83 ° or more, and preferably 120 ° or more, and preferably 120 ° or more. It is 150 ° or more, and preferably 155 ° or more.
- the angle ⁇ is preferably 180 ° or less, preferably 155 ° or less, preferably 150 ° or less, preferably 120 ° or less, and preferably 83 ° or less. Further, it is preferably 80 ° or less, and preferably 66 ° or less.
- the pattern 100 may have a configuration of a regular dodecagonal displacement type having 6-fold symmetry instead of the regular hexagonal displacement type having 3-fold symmetry.
- the regular dodecagonal displacement type is a 24-sided type.
- the regular dodecagonal displacement type is composed of 24 line segments having the same length and being linear.
- the pattern 100 exhibiting a regular dodecagonal displacement shape is a regular hexagon, has an area of 101a, and includes a reference figure 101 including six vertices 104. Each of the six vertices 104 is included in the vertices of the pattern 100.
- the angle ⁇ formed by the two adjacent line segments 102 in the pattern 100 is constant, and is equal to the angle ⁇ formed by the two adjacent line segments 103 in the pattern 100. That is, in the "regular dodecagon displacement type" described in the present specification, the regular dodecagon is displaced (deformed) while maintaining the area of the regular dodecagon based on the angle ⁇ indicating the degree of unevenness. It can be grasped that it is a dodecagon.
- the pattern 100 is said to exhibit a 2n square displacement shape, which is a 4n square formed by the regular 2n square being displaced (deformed) while maintaining the area of the regular 2n square based on the angle ⁇ indicating the degree of unevenness. It may be a configuration.
- the 2n polygonal displacement type includes a regular n-sided polygon (corresponding to the reference figure 101).
- the pattern 100 may have a configuration including a regular 2n square displacement type (including a regular hexagonal displacement type and a regular dodecagonal displacement type). Further, the pattern 100 is a line segment connecting the intersection of two adjacent line segments 103 in the regular 2n square displacement type and the center of gravity of the reference figure 101 in addition to the line segment constituting the regular 2n square displacement type. It may be configured to further include at least one (corresponding to a third line segment). Further, the pattern 100 connects the intersections of two adjacent line segments 103 in the regular 2n square displacement type and the vertices 104 forming the reference figure 101 in addition to the line segments forming the regular 2n square displacement type. The configuration may further include at least one line segment. Further, the pattern 100 may further include at least one line segment constituting the reference figure 101 included in the regular 2n square displacement shape in addition to the line segment constituting the regular 2n square displacement shape.
- the through hole forming step S10 is preferably a step of removing 50% or more of the effective area of the SiC base substrate 10. Further, more preferably, it is a step of removing 60% or more of the effective area, more preferably 70% or more of the effective area, and further preferably 80% or more of the effective area. ..
- the effective area in the present specification refers to the surface of the SiC base substrate 10 to which the raw material adheres in the crystal growth step S30. In other words, it refers to a remaining region other than the region removed by the through hole 11 on the growth surface of the SiC base substrate 10.
- the strain layer removing step S20 is a step of removing the strain layer 12 formed on the SiC base substrate 10 by the through hole forming step S10.
- a means for etching the SiC base substrate 10 by heat-treating the SiC base substrate 10 can be exemplified. Further, any means capable of removing the strain layer 12 can be naturally adopted.
- Examples of the method for removing the strain layer 12 include a hydrogen etching method using hydrogen gas as an etching gas, a Si vapor pressure etching (Si-Vapor Etching: SiVE) method for heating in a Si atmosphere, and Example 1 described later.
- the described etching method can be adopted.
- the crystal growth step S30 is a step of forming the AlN layer 20 on the SiC base substrate 10 on which the through holes 11 are formed.
- a physical vapor transport method Physical Vapor Transport: PVT
- PVT Physical Vapor Transport
- CVT chemical vapor transport method
- CVT organic vapor deposition method
- Adopt a known vapor phase growth method corresponding to the vapor phase epitaxial method
- MOVPE metal-organic vapor phase epitaxy
- HVPE hydride vapor phase epitaxy
- PVD physical vapor deposition
- CVD chemical vapor deposition
- FIGS. 4 and 5 are explanatory views illustrating the crystal growth step S30 according to the embodiment.
- the SiC base substrate 10 and the semiconductor material 40 as the raw material of the AlN layer 20 are arranged and heated in a crucible 30 having a semi-closed space so as to face each other. It is a process.
- the term "quasi-closed space” as used herein refers to a space in which the inside of the container can be evacuated, but at least a part of the vapor generated in the container can be confined.
- the crystal growth step S30 is a step of heating so that a temperature gradient is formed along the vertical direction of the SiC base substrate 10.
- the raw material is transported from the semiconductor material 40 onto the SiC base substrate 10 via the raw material transport space 31.
- the above-mentioned temperature gradient and the difference in chemical potential between the SiC base substrate 10 and the semiconductor material 40 can be adopted.
- the SiC base substrate 10 is set lower than that of the semiconductor material 40. It becomes supersaturated and condenses on top. As a result, the AlN layer 20 is formed on the SiC base substrate 10.
- the crystal growth step S30 includes a horizontal growth step S31 in which the AlN layer 20 grows in the horizontal direction of the SiC base substrate 10, and a vertical growth step S32 in which the AlN layer 20 grows in the vertical direction of the SiC base substrate 10.
- the growth component in the horizontal direction may be larger than the growth component in the vertical direction, and the growth component in the vertical direction may be included (growth component: horizontal direction> vertical direction).
- the vertical growth step S32 the growth component in the vertical direction may be larger than the growth component in the horizontal direction, and the growth component in the horizontal direction may be included (growth component: vertical direction> horizontal direction).
- an inert gas or a doping gas may be introduced into the raw material transport space 31 to control the doping concentration and the growth environment of the AlN layer 20. Further, in the crystal growth step S30, it is desirable to grow the inside of the raw material transport space 31 as a nitrogen atmosphere by introducing nitrogen gas.
- a large-diameter AlN substrate can be manufactured by crystal-growth the AlN layer 20 on the SiC base substrate 10 having the through holes 11. That is, the growth driving force acts in the horizontal direction of the SiC base substrate 10 by escaping heat from the region where the through hole 11 is formed. As a result, the bonding of the AlN layer 20 is promoted on the region where the through hole 11 is formed, and the AlN layer 20 having a diameter equivalent to the diameter of the SiC base substrate 10 can be formed. Therefore, by adopting the SiC base substrate 10 having a large diameter, an AlN substrate having a large diameter can be obtained.
- the crystallinity of the AlN layer 20 can be improved by forming the AlN layer 20 on the region where the through hole 11 is formed. That is, the AlN layer 20 formed on the region where the through hole 11 is formed is not located directly above the SiC base substrate 10. Therefore, the dislocations of the penetrating system existing in the SiC base substrate 10 (for example, penetrating spiral dislocations, penetrating blade-shaped dislocations, micropipes, etc.) are not inherited, and the dislocations of the penetrating system in the AlN layer 20 can be reduced.
- the dislocations of the penetrating system existing in the SiC base substrate 10 for example, penetrating spiral dislocations, penetrating blade-shaped dislocations, micropipes, etc.
- Example 1 >> ⁇ Through hole forming process> Under the following conditions, the SiC substrate 10 was irradiated with a laser to form a through hole 11.
- FIG. 6 is an explanatory diagram for explaining the pattern of the through hole 11 formed in the through hole forming step S10 according to the first embodiment.
- FIG. 6A is an explanatory view showing how a plurality of through holes 11 are arranged.
- the region shown in black indicates the portion of the through hole 11, and the region shown in white is left as the SiC base substrate 10.
- FIG. 6B is an explanatory view showing an enlarged state of the through hole 11 of FIG. 6A.
- the region shown in white indicates the portion of the through hole 11, and the region shown in black is left as the SiC base substrate 10.
- 80% or more of the effective area of the SiC base substrate 10 is removed to reduce the strength of the SiC base substrate 10.
- FIG. 7 is an explanatory diagram illustrating the strain layer removing step S20 according to the first embodiment.
- the SiC base substrate 10 on which the through hole 11 was formed in the through hole forming step S10 was housed in the SiC container 50, and the SiC container 50 was further housed in the TaC container 60 and heated under the following conditions.
- Heating temperature 1800 ° C Heating time: 2h Etching amount: 8 ⁇ m
- SiC container 50 Material: Polycrystalline SiC Container size: diameter 60 mm x height 4 mm Distance between the SiC base substrate 10 and the bottom surface of the SiC container 50: 2 mm
- the SiC container 50 is a fitting container including an upper container 51 and a lower container 52 that can be fitted to each other.
- a minute gap 53 is formed in the fitting portion between the upper container 51 and the lower container 52, and is configured so that the inside of the SiC container 50 can be exhausted (evacuated) from the gap 53.
- the SiC container 50 is formed by facing a part of the SiC container 50 arranged on the low temperature side of the temperature gradient and the SiC base substrate 10 in a state where the SiC base substrate 10 is arranged on the high temperature side of the temperature gradient. It has an etching space 54 to be formed.
- the etching space 54 is a space for transporting and etching Si atoms and C atoms from the SiC base substrate 10 to the SiC container 50 by using a temperature difference provided between the SiC base substrate 10 and the bottom surface of the SiC container 50 as a driving force. be.
- the SiC container 50 has a substrate holder 55 that holds the SiC base substrate 10 in a hollow shape to form an etching space 54.
- the substrate holder 55 may not be provided depending on the direction of the temperature gradient of the heating furnace. For example, when the heating furnace forms a temperature gradient so that the temperature decreases from the lower container 52 toward the upper container 51, the SiC base substrate 10 is arranged on the bottom surface of the lower container 52 without providing the substrate holder 55. You may.
- TaC container 60 Material: TaC Container size: diameter 160 mm x height 60 mm Si steam source 64 (Si compound): TaSi 2
- the TaC container 60 is a fitting container including an upper container 61 and a lower container 62 that can be fitted to each other, and is configured to be able to accommodate the SiC container 50.
- a minute gap 63 is formed in the fitting portion between the upper container 61 and the lower container 62, and is configured so that the TaC container 60 can be exhausted (evacuated) from the gap 63.
- the TaC container 60 has a Si steam supply source 64 capable of supplying the vapor pressure of a vapor phase species containing a Si element in the TaC container 60.
- the Si steam supply source 64 may have a configuration in which the vapor pressure of the vapor phase species containing the Si element is generated in the TaC container 60 during the heat treatment.
- FIG. 8 is an explanatory diagram illustrating the crystal growth step S30 according to the first embodiment.
- the SiC base substrate 10 from which the strain layer 12 was removed by the strain layer removing step S20 was housed in the crucible 30 so as to face the semiconductor material 40, and heated under the following conditions.
- Heating temperature 2040 ° C Heating time: 70h Growth thickness: 500 ⁇ m N 2 gas pressure: 10 kPa
- the crucible 30 has a raw material transport space 31 between the SiC base substrate 10 and the semiconductor material 40. The raw material is transported from the semiconductor material 40 onto the SiC base substrate 10 through the raw material transport space 31.
- FIG. 8A is an example of the crucible 30 used in the crystal growth step S30.
- the crucible 30 is a fitting container including an upper container 32 and a lower container 33 that can be fitted to each other.
- a minute gap 34 is formed in the fitting portion between the upper container 32 and the lower container 33, and is configured to allow exhaust (evacuation) in the crucible 30 from the gap 34.
- the crucible 30 has a substrate holder 35 that forms a raw material transport space 31.
- the substrate holder 35 is provided between the SiC base substrate 10 and the semiconductor material 40, and the semiconductor material 40 is arranged on the high temperature side and the SiC base substrate 10 is arranged on the low temperature side to form a raw material transport space 31. ..
- FIGS. 8 (b) and 8 (c) are other examples of the crucible 30 used in the crystal growth step S30.
- the temperature gradients of FIGS. 8 (b) and 8 (c) are set to be opposite to those of FIG. 8 (a), and the SiC base substrate 10 is arranged on the upper side. That is, similarly to FIG. 8A, the semiconductor material 40 is arranged on the high temperature side and the SiC base substrate 10 is arranged on the low temperature side to form the raw material transport space 31.
- FIG. 8B shows an example in which the raw material transport space 31 is formed between the SiC base substrate 10 and the semiconductor material 40 by fixing the SiC base substrate 10 to the upper container 32 side.
- FIG. 8C shows an example in which a raw material transport space 31 is formed between the upper container 32 and the semiconductor material 40 by forming a through window and arranging the SiC base substrate 10. Further, as shown in FIG. 8C, the raw material transport space 31 may be formed by providing the intermediate member 36 between the upper container 32 and the lower container 33.
- the AlN sintered body of the semiconductor material 40 was sintered by the following procedure.
- the AlN powder was placed in the frame of the TaC block and compacted with an appropriate force. Then, the AlN powder and the TaC block compacted in the pyrolytic carbon crucible were stored and heated under the following conditions.
- Heating temperature 1850 ° C N 2 gas pressure: 10 kPa Heating time: 3h
- FIG. 9 is a schematic view showing the crystal growth step S30 of Example 1.
- Comparative Example 1 >> The SiC substrate 10 according to Comparative Example 1 formed a groove 13 instead of the through hole 11 of Example 1.
- the SiC base substrate 10 was subjected to the crystal growth step S30 under the same conditions as in Example 1. That is, in Comparative Example 1, the through hole forming step S10 was not performed, but the crystal growth step S30 was performed.
- FIG. 10 is a schematic view showing the crystal growth step S30 of Comparative Example 1.
- a region in which the AlN layer 20 did not grow was formed on the groove 13.
- the temperature of the region of the groove 13 does not decrease and the temperature gradient is not formed in the horizontal direction of the SiC base substrate 10. As a result, it is considered that the growth driving force in the lateral direction is not generated and the AlN layer 20 is not formed in the region of the groove 13.
- Example 1 From the results of Example 1 and Comparative Example 1, it can be understood that a large-diameter AlN substrate can be manufactured by forming the AlN layer 20 on the SiC base substrate 10 having the through hole 11.
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Abstract
Description
また、本発明の解決しようとする課題は、大口径で結晶性のよいAlN基板を製造可能な新規の技術を提供することにある。
このように、貫通孔を有する炭化ケイ素下地基板に窒化アルミニウム層を形成することで、炭化ケイ素下地基板の径と同等の径を有する窒化アルミニウム基板を製造することができる。そのため、大きな径の炭化ケイ素下地基板を採用することで、大口径な窒化アルミニウム基板を得ることができる。
また、開示した技術によれば、大口径で結晶性のよいAlN基板を製造可能な新規の技術を提供することができる。
図1ないし図4は、本発明の実施の形態にかかるAlN基板の製造方法の工程を説明する説明図である。
実施の形態にかかるAlN基板の製造方法は、SiC下地基板10に貫通孔11を形成する貫通孔形成工程S10と、貫通孔形成工程S10により導入された歪層12を除去する歪層除去工程S20と、この貫通孔11を有するSiC下地基板10にAlN層20を形成する結晶成長工程S30と、を含み得る。
以下、実施の形態の各工程について詳細に説明する。
貫通孔形成工程S10は、SiC下地基板10に貫通孔11を形成する工程である。この貫通孔形成工程S10は、SiC下地基板10に貫通孔11を形成可能な手法であれば当然に採用することができる。
歪層除去工程S20は、貫通孔形成工程S10によりSiC下地基板10に形成された歪層12を除去する工程である。この歪層除去工程S20として、SiC下地基板10を熱処理することにより、SiC下地基板10をエッチングする手段を例示することができる。
また、歪層12を除去可能な手段であれば、当然に採用することができる。
結晶成長工程S30は、貫通孔11が形成されたSiC下地基板10上に、AlN層20を形成する工程である。
実施の形態にかかる結晶成長工程S30は、SiC下地基板10と、AlN層20の原料となる半導体材料40とを、準閉鎖空間を有した坩堝30内に相対(対峙)させて配置し加熱する工程である。なお、本明細書における「準閉鎖空間」とは、容器内の真空引きは可能であるが、容器内に発生した蒸気の少なくとも一部を閉じ込め可能な空間のことをいう。
なお、横方向成長工程S31は、水平方向への成長成分が垂直方向への成長成分より大きければよく、垂直方向への成長成分を含んでいても良い(成長成分:水平方向>垂直方向)。
また、縦方向成長工程S32は、垂直方向への成長成分が水平方向への成長成分より大きければよく、水平方向への成長成分を含んでいても良い(成長成分:垂直方向>水平方向)。
〈貫通孔形成工程〉
以下の条件で、SiC下地基板10にレーザーを照射し貫通孔11を形成した。
半導体材料:4H-SiC
基板サイズ:横幅11mm×縦幅11mm×厚み524μm
成長面:Si-face
オフ角:on-axis
種類:グリーンレーザー
波長:532nm
スポット径:40μm
平均出力:4W(30kHzにて)
図6は、実施例1にかかる貫通孔形成工程S10で形成した貫通孔11のパターンを説明する説明図である。図6(a)は、複数の貫通孔11を配列した様子を示す説明図である。この図6(a)においては、黒く示した領域が貫通孔11の部分を示し、白く示した領域がSiC下地基板10として残されている。
なお、図6のパターンにおいては、SiC下地基板10の有効面積の80%以上を除去して、SiC下地基板10の強度を低下させている。
図7は、実施例1にかかる歪層除去工程S20を説明する説明図である。
貫通孔形成工程S10により貫通孔11を形成したSiC下地基板10をSiC容器50内に収容し、さらにSiC容器50をTaC容器60に収容し、以下の条件で加熱した。
加熱温度:1800℃
加熱時間:2h
エッチング量:8μm
材料:多結晶SiC
容器サイズ:直径60mm×高さ4mm
SiC下地基板10とSiC容器50の底面との距離:2mm
SiC容器50は、図5に示すように、互いに嵌合可能な上容器51と下容器52とを備える嵌合容器である。上容器51と下容器52の嵌合部には、微小な間隙53が形成されており、この間隙53からSiC容器50内の排気(真空引き)が可能なよう構成されている。
材料:TaC
容器サイズ:直径160mm×高さ60mm
Si蒸気供給源64(Si化合物):TaSi2
TaC容器60は、SiC容器50と同様に、互いに嵌合可能な上容器61と下容器62とを備える嵌合容器であり、SiC容器50を収容可能に構成されている。上容器61と下容器62の嵌合部には、微小な間隙63が形成されており、この間隙63からTaC容器60内の排気(真空引き)が可能なよう構成されている。
図8は、実施例1にかかる結晶成長工程S30を説明する説明図である。
歪層除去工程S20により歪層12を除去したSiC下地基板10を半導体材料40と相対させて坩堝30内に収容し、以下の条件で加熱した。
加熱温度:2040℃
加熱時間:70h
成長厚み:500μm
N2ガス圧力:10kPa
材料:炭化タンタル(TaC)及び/又はタングステン(W)
容器サイズ:10mm×10mm×1.5mm
SiC下地基板10-半導体材料40間距離:1mm
坩堝30は、SiC下地基板10と半導体材料40との間に原料輸送空間31を有している。この原料輸送空間31を介して、半導体材料40からSiC下地基板10上に原料を輸送している。
図8(c)は、上容器32に貫通窓を形成しSiC下地基板10を配置することで、半導体材料40との間に原料輸送空間31を形成する例を示している。また、この図8(c)に示すように、上容器32と下容器33との間に中間部材36を設けることで、原料輸送空間31を形成しても良い。
材料:AlN焼結体
サイズ:横幅20mm×縦幅20mm×厚み5mm
半導体材料40のAlN焼結体は、以下の手順により焼結した。
AlN粉末をTaCブロックの枠内に入れ、適度な力で押し固めた。その後、熱分解炭素坩堝に押し固めたAlN粉末およびTaCブロックを収納し、以下の条件で加熱した。
N2ガス圧力:10kPa
加熱時間:3h
比較例1にかかるSiC下地基板10は、実施例1の貫通孔11に代わりに、溝13を形成した。このSiC下地基板10に対して、実施例1と同様の条件で結晶成長工程S30を施した。すなわち、比較例1は貫通孔形成工程S10を行わず、結晶成長工程S30を行った。
11 貫通孔
12 歪層
13 溝
20 AlN層
30 坩堝
31 原料輸送空間
40 半導体材料
50 SiC容器
60 TaC容器
S10 貫通孔形成工程
S20 歪層除去工程
S30 結晶成長工程
S31 横方向成長工程
S32 縦方向成長工程
Claims (12)
- 貫通孔を有する炭化ケイ素下地基板に窒化アルミニウム層を形成する結晶成長工程を含む、窒化アルミニウム基板の製造方法。
- 前記結晶成長工程は、前記炭化ケイ素下地基板の垂直方向に沿って温度勾配が形成されるよう加熱する工程である、請求項1に記載の窒化アルミニウム基板の製造方法。
- 前記結晶成長工程は、前記炭化ケイ素下地基板と前記窒化アルミニウム層の原料とを相対させて配置し、前記炭化ケイ素下地基板と前記原料との間に温度勾配が形成されるよう加熱する工程である、請求項1又は請求項2に記載の窒化アルミニウム基板の製造方法。
- 前記結晶成長工程は、前記炭化ケイ素下地基板の水平方向に前記窒化アルミニウム層が成長する横方向成長工程と、前記炭化ケイ素下地基板の垂直方向に前記窒化アルミニウム層が成長する縦方向成長工程と、を有する、請求項1~3の何れか一項に記載の窒化アルミニウム基板の製造方法。
- 前記炭化ケイ素下地基板に貫通孔を形成する貫通孔形成工程と、
前記貫通孔形成工程により導入された歪層を除去する歪層除去工程と、をさらに含む、請求項1~4の何れか一項に記載の窒化アルミニウム基板の製造方法。 - 前記貫通孔形成工程は、レーザーを前記炭化ケイ素下地基板に照射することにより貫通孔を形成する工程である、請求項5に記載の窒化アルミニウム基板の製造方法。
- 前記歪層除去工程は、熱処理することにより前記炭化ケイ素下地基板の歪層を除去する工程である、請求項5又は請求項6に記載の窒化アルミニウム基板の製造方法。
- 前記歪層除去工程は、前記炭化ケイ素下地基板をシリコン雰囲気下でエッチングする工程である、請求項5~7の何れか一項に記載の窒化アルミニウム基板の製造方法。
- 請求項1~8の何れか一項に記載の製造方法により製造された窒化アルミニウム基板。
- 炭化ケイ素下地基板の表面上に窒化アルミニウム層を形成する前に、前記炭化ケイ素下地基板に貫通孔を形成する貫通孔形成工程を含む、窒化アルミニウム層を形成する方法。
- 前記貫通孔形成工程により導入された歪層を除去する歪層除去工程を含む、請求項10に記載の方法。
- 前記歪層除去工程は、熱処理することにより前記炭化ケイ素下地基板をエッチングする工程である、請求項11に記載の方法。
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| EP21789219.9A EP4137623A4 (en) | 2020-04-14 | 2021-03-30 | METHOD FOR PRODUCING AN ALUMINUM NITRIDE SUBSTRATE, ALUMINUM NITRIDE SUBSTRATE AND METHOD FOR PRODUCING AN ALUMINUM NITRIDE LAYER |
| CN202180028128.7A CN115443352B (en) | 2020-04-14 | 2021-03-30 | Method for manufacturing aluminum nitride substrate, and method for forming aluminum nitride layer |
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| CN115443352A (zh) | 2022-12-06 |
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| JP7758909B2 (ja) | 2025-10-23 |
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