WO2019240113A1 - GaN積層基板の製造方法 - Google Patents
GaN積層基板の製造方法 Download PDFInfo
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- WO2019240113A1 WO2019240113A1 PCT/JP2019/023032 JP2019023032W WO2019240113A1 WO 2019240113 A1 WO2019240113 A1 WO 2019240113A1 JP 2019023032 W JP2019023032 W JP 2019023032W WO 2019240113 A1 WO2019240113 A1 WO 2019240113A1
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L27/00—Devices consisting of a plurality of semiconductor or other solid-state components formed in or on a common substrate
- H01L27/02—Devices consisting of a plurality of semiconductor or other solid-state components formed in or on a common substrate including semiconductor components specially adapted for rectifying, oscillating, amplifying or switching and having at least one potential-jump barrier or surface barrier; including integrated passive circuit elements with at least one potential-jump barrier or surface barrier
- H01L27/12—Devices consisting of a plurality of semiconductor or other solid-state components formed in or on a common substrate including semiconductor components specially adapted for rectifying, oscillating, amplifying or switching and having at least one potential-jump barrier or surface barrier; including integrated passive circuit elements with at least one potential-jump barrier or surface barrier the substrate being other than a semiconductor body, e.g. an insulating body
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2310/00—Treatment by energy or chemical effects
- B32B2310/08—Treatment by energy or chemical effects by wave energy or particle radiation
- B32B2310/0875—Treatment by energy or chemical effects by wave energy or particle radiation using particle radiation
- B32B2310/0881—Treatment by energy or chemical effects by wave energy or particle radiation using particle radiation using ion-radiation, e.g. alpha-rays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B43/00—Operations specially adapted for layered products and not otherwise provided for, e.g. repairing; Apparatus therefor
- B32B43/006—Delaminating
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
- Y10T156/11—Methods of delaminating, per se; i.e., separating at bonding face
- Y10T156/1168—Gripping and pulling work apart during delaminating
- Y10T156/1179—Gripping and pulling work apart during delaminating with poking during delaminating [e.g., jabbing, etc.]
- Y10T156/1184—Piercing layer during delaminating [e.g., cutting, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
- Y10T156/19—Delaminating means
- Y10T156/1961—Severing delaminating means [e.g., chisel, etc.]
- Y10T156/1967—Cutting delaminating means
Definitions
- the present invention relates to a method for manufacturing a GaN laminated substrate whose surface is made of a Ga polar face (Ga face).
- Crystalline GaN has a wider band gap than Si and GaAs and is promising for high-speed and high-power device applications.
- a bulk GaN substrate having good crystallinity is a factor that hinders its spread because it has a small diameter and is very expensive.
- GaN is heteroepitaxially grown on an AlN substrate or Al 2 O 3 (sapphire) substrate by hydride vapor phase epitaxy (HVPE), metal organic vapor phase epitaxy (MOCVD), or the like.
- HVPE hydride vapor phase epitaxy
- MOCVD metal organic vapor phase epitaxy
- a laminated substrate in which a GaN thin film is formed on a Si substrate which is widely spread as a semiconductor material, can obtain excellent basic characteristics of GaN and apply advanced process technology for Si semiconductor devices. Therefore, it is highly expected as a substrate for high-performance devices.
- a thick buffer layer is indispensable between the Si substrate and the GaN thin film in order to obtain good crystalline GaN.
- warpage occurs as a laminated substrate due to a large difference in thermal expansion coefficient between the GaN film and the Si substrate, and the warpage increases as the GaN film thickness increases, causing various defects. That is, when the warpage of the multilayer substrate increases, there is a problem that the multilayer substrate eventually breaks.
- various problems occur in the semiconductor device process. In particular, it becomes a serious problem in the fine processing exposure process. Therefore, it was necessary to insert a thick buffer layer having a linear expansion coefficient between these two materials between the Si substrate and the GaN thin film in order to alleviate this warpage. Further, with this method, it is difficult to increase the thickness of the GaN layer having good characteristics on the multilayer substrate.
- a method of manufacturing a GaN laminated substrate by transfer according to the following procedure is conceivable. That is, first, a first substrate is prepared, and a GaN film having a certain thickness or more is epitaxially grown on the surface. Next, ion implantation is performed on the substrate to form an embrittlement layer (ion implantation region) at a certain depth from the surface. After this substrate is bonded to the second substrate, the embrittled layer is peeled off, and the GaN thin film is transferred to the second substrate to obtain a GaN laminated substrate.
- embrittlement layer ion implantation region
- the growth surface (front surface) side is a Ga polar surface (hereinafter referred to as Ga surface). Therefore, the ion-implanted surface side is a Ga surface, and the surface after peeling and transferring onto the second substrate is an N-polar surface (N surface).
- the GaN thin film transferred to the second substrate needs to be bonded again to the third substrate and transferred to form a Ga surface. was there.
- Patent Document 1 Japanese Patent Application Publication No. 2016-511934 (Patent Document 1) is given as a prior art related to the present invention.
- the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a method of manufacturing a GaN laminated substrate that obtains a GaN laminated substrate with good crystallinity having a Ga surface as a surface by a single transfer process.
- the present invention provides the following method for manufacturing a GaN laminated substrate.
- the C-plane sapphire substrate is subjected to high-temperature nitridation treatment at 800 to 1000 ° C. and / or deposition of crystalline AlN on the C-plane sapphire substrate at an off angle of 0.5 to 5 degrees.
- Processing step; GaN is epitaxially grown on the surface of the surface-treated C-plane sapphire substrate to produce a GaN film carrier having an N-polar surface.
- the ion implantation uses hydrogen ions (H + ) and / or hydrogen molecular ions (H 2 + ), implantation energy of 100 to 160 keV, and dose of 1.0 ⁇ 10 17 to 3.0 ⁇ 10 17 atoms / cm 2.
- a predetermined surface treatment is performed on a C-plane sapphire substrate having a predetermined off-angle, and GaN is epitaxially grown on the substrate to form a GaN film with good crystallinity having an N-polar surface. Therefore, it is possible to obtain a GaN laminated substrate whose surface is a Ga polar surface by one transfer.
- the process cost can be reduced by reducing the number of times of transfer compared to the prior art. Furthermore, it is possible to reduce the GaN film that disappears due to the transfer, and it is possible to reduce the material cost.
- the number of times of transfer can be reduced as compared with the conventional case, and this can be suppressed.
- a substrate having an epitaxial film which is easily increased in diameter is used as a donor substrate for GaN thin film transfer, the cost and the large diameter are reduced compared with the case where an expensive and small-diameter bulk GaN substrate is used as a donor substrate.
- a GaN laminated substrate is obtained.
- a GaN laminated substrate having a Ga polar surface on the surface obtained by the present invention can be used as a GaN template substrate, and a GaN substrate having a high withstand voltage and high characteristics can be obtained by epitaxially forming GaN.
- FIG. 1 It is a figure which shows the manufacturing process in one Embodiment of the manufacturing method of the GaN laminated substrate which concerns on this invention, (a) is preparation of a C surface sapphire substrate and a support substrate, (b) is the surface treatment of a C surface sapphire substrate, ( c) is GaN epitaxial growth, (d) is ion implantation treatment, (e) is bonded bonding, and (f) is peeling transfer of a GaN thin film.
- the method for producing a GaN laminated substrate according to the present invention includes a high-temperature nitridation treatment at 800 to 1000 ° C. of a C-plane sapphire substrate with an off angle of 0.5 to 5 degrees and / or crystalline AlN on the C-plane sapphire substrate.
- a GaN laminated substrate having a GaN thin film having a Ga polar surface on the support substrate is obtained by peeling the film at the ion implantation region and transferring the GaN thin film onto the support substrate. It is characterized in that it has a degree, the.
- the method for manufacturing a GaN laminated substrate according to the present invention includes (a) a C-plane sapphire substrate and supporting substrate preparation step (step 1), and (b) a C-plane sapphire substrate surface treatment step (step). 2), (c) GaN epitaxial growth process (process 3), (d) ion implantation process (process 4), (e) bonding and bonding process (process 5), (f) GaN thin film peeling and transfer process (process) The processing is performed in the order of 6).
- Step 1 Preparation of C-plane sapphire substrate and support substrate
- a C-plane sapphire substrate 11 and a support substrate 12 are prepared (FIG. 1A).
- the C-plane sapphire substrate 11 is a substrate made of sapphire ( ⁇ -Al 2 O 3 ) with the C-plane ((0001) plane) as the substrate plane.
- the c-axis sapphire substrate 11 has a c-axis off angle (hereinafter referred to as an off angle) of 0.5 to 5 degrees, preferably 2 to 3 degrees.
- the surface of the GaN film 13 subsequently formed on the C-plane sapphire substrate 11 becomes an N-polar plane (hereinafter referred to as an N-plane) and has good smoothness and crystallinity.
- N-plane N-polar plane
- the GaN thin film 13a as the transfer thin film has excellent smoothness.
- the off-angle is the angle when the substrate surface (surface to be crystal-grown) is slightly tilted from the closest surface in a specific direction
- the c-axis off-angle is the c-plane sapphire substrate 11 c.
- arithmetic mean roughness Ra JIS B0601: 2013, the same below
- arithmetic mean roughness Ra JIS B0601: 2013, the same below
- the support substrate 12 is a substrate that finally supports the GaN thin film 13a, and is preferably made of Si, Al 2 O 3 , SiC, AlN, or SiO 2 .
- the constituent material may be appropriately selected according to the use of a semiconductor device manufactured using the obtained GaN laminated substrate.
- the arithmetic average roughness Ra of the surface of the support substrate 12 is preferably 0.5 nm or less. As a result, stronger bonding is possible when the C-plane sapphire substrate 11 and the GaN layer carrier having the GaN layer 13 are bonded.
- a bond film made of silicon oxide (SiOx thin film, where 0 ⁇ x ⁇ 2) may be provided on the outermost layer of the support substrate 12 (except when the support substrate 12 is made of SiO 2 ). Furthermore, when the surface roughness of the support substrate 12 itself is not sufficiently small (for example, when the arithmetic average roughness Ra of the surface of the support substrate 12 is more than 0.5 nm), this bond film is removed by chemical mechanical polishing (CMP) or the like. The surface may be smoothed by treatment. Thereby, the joint strength between the C-plane sapphire substrate 11 and the GaN layer carrier having the GaN layer 13 can be further increased.
- the film thickness of this bond film is preferably about 300 to 1000 nm.
- FIG. 1B the surface treatment of the C-plane sapphire substrate 11 is performed. That is, a high-temperature nitriding process is performed on the C-plane sapphire substrate 11 at 800 to 1000 ° C. and / or crystalline AlN is deposited on the C-plane sapphire substrate 11.
- the high-temperature nitriding treatment of the C-plane sapphire substrate 11 is performed at a temperature slightly lower than the film formation temperature of the GaN epitaxial growth performed thereafter in the nitrogen-containing atmosphere, specifically, 800 to 1000 ° C.
- an AlN film is formed on the surface of the C-plane sapphire substrate 11 as the surface treatment layer 11a.
- This process is preferably performed in situ in the same processing chamber of the MOCVD apparatus for epitaxially growing the GaN film, and is slightly lower than the deposition temperature (1050 to 1100 ° C.) for GaN epitaxial growth (800 to 100 ° C.). 1000 ° C.).
- the processing temperature is less than 800 ° C.
- the N-pole growth of the GaN film does not occur, and if it exceeds 1000 ° C., the smoothness deteriorates due to the epitaxial growth of GaN performed thereafter.
- ammonia gas can also be used. By using ammonia gas, more active N atoms are generated, and the surface morphology (crystal structure) of the GaN film can be improved.
- the high temperature nitriding treatment time is preferably about 30 seconds to 30 minutes. By extending the processing time, the surface morphology (crystal structure) of the GaN film can be improved.
- the deposition process of crystalline AlN on the C-plane sapphire substrate 11 is performed as a surface treatment layer 11a on the C-plane sapphire substrate 11 by chemical vapor deposition (CVD) or physical vapor deposition (PVD). A crystalline AlN film is formed. This deposition process may be performed under conditions that allow the surface of the C-plane sapphire substrate 11 to be covered with a crystalline AlN film (surface treatment layer 11a).
- CVD chemical vapor deposition
- PVD physical vapor deposition
- GaN is epitaxially grown on the surface of the surface-treated C-plane sapphire substrate 11 to form a GaN film 13 having an N-polar surface, thereby producing a GaN film carrier.
- Known epitaxial growth methods for GaN films include molecular beam epitaxy (MBE), hydride vapor phase epitaxy (HVPE), and metal organic vapor phase epitaxy (MOCVD).
- MBE molecular beam epitaxy
- HVPE hydride vapor phase epitaxy
- MOCVD metal organic vapor phase epitaxy
- the epitaxial growth of the GaN film 13 by the MOCVD method is preferably performed at a higher temperature (that is, higher than 1000 ° C.) than the high temperature nitridation process in the above step 2, and the film quality of the GaN film 13 and the film formation speed can be balanced. More than 1 ° C. and 1100 ° C. or less is suitable.
- the process gas may be trimethylgallium (TMG) and ammonia (NH 3 ), and hydrogen may be used as the carrier gas.
- TMG trimethylgallium
- NH 3 ammonia
- the thickness of the GaN film 13 depends on the thickness of the GaN thin film 13a to be finally obtained, and is, for example, 0.5 to 10 ⁇ m.
- a GaN buffer layer is formed at a low temperature, for example, 700 ° C. or lower, and then GaN epitaxial growth is performed on the GaN buffer layer by the MOCVD method, thereby forming a GaN film 13. It is preferable to form.
- the GaN film 13 on the buffer layer does not grow N pole well if the film formation temperature is higher than 700 ° C., and the film formation itself does not proceed below 400 ° C. It is preferable to form the film at 700 ° C., more preferably at 400 to 600 ° C. Further, if the thickness of the GaN buffer layer is too thin, the buffer effect may not be obtained, and if it is too thick, the film quality may be deteriorated. Therefore, the thickness is preferably 15 to 30 nm, more preferably 20 to 25 nm.
- the GaN film 13 whose surface is an N plane and has a very good crystallinity is formed on the C-plane sapphire substrate 11 (up to this point, FIG. 1C).
- the surface of a compound semiconductor crystal such as GaN has polarity.
- a single-crystal GaN film composed of the constituent elements Ga and N is inevitably composed (terminated) of Ga atoms.
- Polar face with exposed bonds (Ga polar face (also referred to as Ga face)) and polar face consisting of N atoms (terminated) with exposed unbonded hands of N atoms (N polar face (also referred to as N face)) ).
- the crystal structure of GaN is a hexagonal system, and its polar face appears on the closest surface of the crystal lattice.
- the close-packed surface of the hexagonal compound semiconductor crystal is the ⁇ 0001 ⁇ plane, but the (0001) plane and the (000-1) plane are not equivalent, the former is the plane where the cation atoms are exposed, and the latter is the anion atoms.
- the (0001) plane is the Ga plane and the (000-1) plane is the N plane.
- a silicon oxide (SiOx, where 0 ⁇ x ⁇ 2) film is further formed on the GaN film 13 as a bond layer for bonding to the support substrate 12.
- a GaN film carrier may be used.
- the thickness of the silicon oxide film is preferably 200 to 1000 nm.
- the implantation energy defines the ion implantation depth (that is, the film thickness of the release film (GaN thin film 13a)), and is preferably 110 to 160 keV.
- the film thickness of the GaN thin film 13a can be 500 nm or more.
- the implantation damage becomes large, and the crystallinity of the peeled thin film may be deteriorated.
- the dose is preferably 1.0 ⁇ 10 17 to 3.0 ⁇ 10 17 atoms / cm 2 .
- an ion implantation region 13 ion that becomes a release layer (brittle layer) can be formed in the GaN film 13, and the temperature rise of the GaN film carrier can be suppressed.
- the ion implantation temperature is room temperature, and the GaN film carrier may be broken at a high temperature. Therefore, the GaN film carrier may be cooled.
- the ion implantation treatment may be performed on the GaN film carrier with the GaN film 13 formed in Step 3, but if the surface of the GaN film 13 as formed is rough, Correspondingly, the ion implantation depth becomes non-uniform, and the unevenness of the peeling surface (surface) of the GaN thin film 13a after peeling becomes large.
- the ion implantation surface of the GaN film carrier may be smoothed so that the arithmetic average roughness is preferably 0.3 nm or less, more preferably 0.2 nm or less.
- the surface of the GaN film 13 formed in step 3 may be polished and / or etched by CMP or the like so that the arithmetic average roughness Ra is preferably 0.3 nm or less, more preferably 0.2 nm or less. .
- the surface of the silicon oxide film is formed. Smoothing is performed by polishing and / or etching by CMP or the like so that the arithmetic average roughness Ra is preferably 0.3 nm or less, more preferably 0.2 nm or less. This is particularly effective when the GaN film 13 is thin and flattening by polishing or the like is difficult.
- the ion implantation depth in the next ion implantation process is performed.
- a peeling transfer layer (GaN thin film 13a) having a smooth surface (small surface roughness) can be obtained when it is peeled after being bonded to the support substrate 12.
- the surface of the GaN film 13 (N surface) of the GaN film carrier and the surface of the support substrate 12 are bonded.
- a laminated structure of C-plane sapphire substrate 11 / surface treatment layer 11a / (GaN buffer layer) / GaN film 13 (N-plane) / support substrate 12 is formed.
- the GaN film 13 surface (N surface) of the GaN film carrier and the support substrate 12 surfaces are bonded with a bond layer (silicon oxide film) interposed therebetween. That is, a laminated structure of C-plane sapphire substrate 11 / surface treatment layer 11a / (GaN buffer layer) / GaN film 13 (N-plane) / bond layer (silicon oxide film) / support substrate 12 is formed.
- a GaN film carrier to be surface-activated and / or a support substrate 12 is set in a general parallel plate plasma chamber, a high frequency of about 13.56 MHz and 100 W is applied, and Ar, N 2 are used as process gases. , O 2 and the like may be introduced for processing.
- the processing time is 5 to 30 seconds. Thereby, the target substrate surface is activated and the bonding strength after bonding is increased. Further, after bonding, annealing at about 200 to 300 ° C. is performed to form a stronger bond.
- Step 6 GaN thin film peeling and transfer step
- the GaN thin film 13a is transferred onto the support substrate 12 by peeling off at the ion implantation region 13 ion in the GaN film 13 (FIG. 1 (f)).
- the peeling process may be a process generally performed by an ion implantation peeling method, for example, mechanical peeling such as inserting a blade, light peeling such as laser light irradiation, and other physical processes such as jet water flow and ultrasonic waves. Impact stripping is applicable.
- the GaN laminated substrate 10 having the GaN thin film 13a on the support substrate 12 having a Ga polar face and a good crystallinity and a smooth surface is obtained.
- the surface of the transferred GaN thin film 13a after the peeling is sufficiently smooth, it may be smoothed by polishing or the like depending on the required characteristics of the device using the GaN laminated substrate 10. It is also possible to produce a thick GaN substrate with low defects by further epitaxially growing a GaN film on the GaN laminated substrate 10.
- the method for confirming the polar surface of the surface of the GaN thin film 13a of the GaN laminated substrate 10 may be determined by, for example, looking at the difference in the etching rate due to the KOH aqueous solution. That is, the N surface has a higher etching rate than the Ga surface. For example, when immersed in an aqueous solution of KOH at 40 ° C. and 2 mol / L for 45 minutes, the Ga surface is not etched, but the N surface is etched.
- Example 1 A GaN laminated substrate was produced under the following conditions.
- Example 1-1 A C-plane sapphire substrate having a diameter of 100 mm, a thickness of 525 ⁇ m, an arithmetic average roughness Ra of 0.3 nm, and a C-axis off angle of 3 degrees was prepared. After this substrate is cleaned by RCA cleaning, high-temperature nitriding treatment (process gas: pure nitrogen) at a substrate temperature of 900 ° C. is performed for 30 minutes in an MOCVD apparatus, and then the GaN buffer layer is formed to a thickness of 20 nm at a substrate temperature of 400 ° C.
- process gas pure nitrogen
- a GaN film having a thickness of 2 ⁇ m was formed by epitaxial growth using a process gas: TMG and NH 3 at a substrate temperature of 1050 ° C.
- the arithmetic average roughness Ra of the GaN film was 8 nm.
- the silicon oxide film was polished to 200 nm by a CMP apparatus.
- the arithmetic average roughness Ra of the obtained GaN film carrier was 0.3 nm.
- H 2 + hydrogen molecular ions H 2 + were ion-implanted from the surface of the silicon oxide film of the GaN film carrier with an implantation energy of 160 keV and a dose of 3.0 ⁇ 10 +17 atoms / cm 2 .
- a Si substrate having a diameter of 100 mm and a thickness of 525 ⁇ m was prepared, and a thermal oxide film having a thickness of 300 nm was formed on the Si substrate.
- Ar plasma treatment was performed on the Si substrate, the thermal oxide film of each of the GaN film carriers, and the surface of the silicon oxide film (ion implantation surface).
- annealing was performed at 200 ° C. for 12 hours in a nitrogen atmosphere.
- a metal blade was inserted into the ion-implanted region of the GaN film for peeling, and the GaN thin film was transferred onto the Si substrate to obtain a GaN laminated substrate.
- the arithmetic average roughness Ra of the GaN thin film surface of the obtained GaN laminated substrate was 8 nm. Further, the crystallinity of the GaN thin film of the obtained GaN laminated substrate was evaluated by an X-ray rocking curve method.
- Example 1-2 In Example 1-1, after a GaN film having a thickness of 2 ⁇ m was epitaxially grown, the surface of the GaN film was subjected to CMP to make the arithmetic average roughness Ra of the surface 0.2 nm, and transferred as it was. Otherwise, a GaN laminated substrate was obtained in the same manner as in Example 1-1. The arithmetic average roughness Ra of the GaN thin film surface of the obtained GaN laminated substrate was 0.3 nm. Further, when the crystallinity of the GaN thin film of the obtained GaN laminated substrate was evaluated by the X-ray rocking curve method in the same manner as in Example 1-1, the result was FWHM250 arcsec, which showed the same crystallinity as in Example 1. Further, when the polar face of the surface of the GaN thin film was confirmed in the same manner as in Example 1-1, it was a Ga face.
- Example 1-1 a C-plane sapphire substrate with a c-axis off-angle of 0.05 degrees (arithmetic average roughness Ra 0.3 nm) was used, and other than that, GaN lamination was performed in the same manner as in Example 1-1. A substrate was obtained.
- the GaN film arithmetic average roughness Ra after the GaN film formation was 60 nm
- the arithmetic average roughness Ra of the GaN film carrier after the silicon oxide film CMP polishing was 0.2 nm.
- the arithmetic average roughness Ra of the GaN thin film surface of the obtained GaN laminated substrate was 60 nm.
- Example 1-1 a C-plane sapphire substrate having a c-axis off-angle of 6 degrees (arithmetic average roughness Ra 0.3 nm) was used, and other than that, a GaN laminated substrate was formed in the same manner as in Example 1-1. Obtained.
- the GaN film arithmetic average roughness Ra after the GaN film was formed was 80 nm, and the arithmetic average roughness Ra of the GaN film carrier after the silicon oxide film CMP polishing was 0.3 nm.
- the arithmetic average roughness Ra of the GaN thin film surface of the obtained GaN laminated substrate was 80 nm.
- Example 1-1 when the crystallinity of the GaN thin film of the obtained GaN laminated substrate was evaluated by the X-ray rocking curve method in the same manner as in Example 1-1, FWHM800 arcsec was obtained, and the crystallinity deteriorated. Further, when the polar face of the surface of the GaN thin film was confirmed in the same manner as in Example 1-1, it was a Ga face.
- GaN composite substrate 11 C-plane sapphire substrate 11a Surface treatment layer 12 Support substrate 13 GaN film 13a GaN thin film 13 ion ion implantation region
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Abstract
Description
即ち、まず第1の基板を準備し、表面に一定膜厚以上のGaN膜をエピタキシャル成長させる。次に、この基板にイオン注入を行い、表面から一定深さのところに脆化層(イオン注入領域)を形成する。この基板を第2の基板に接合させた後、脆化層から剥離を行い、GaN薄膜を第2の基板に転写させてGaN積層基板を得る。
なお、本発明に関連する先行技術として特表2016-511934号公報(特許文献1)が挙げられる。
1.
オフ角度0.5~5度のC面サファイア基板の800~1000℃での高温窒化処理及び/又は該C面サファイア基板上への結晶性AlNの堆積処理を行って上記C面サファイア基板を表面処理する工程と、
上記表面処理されたC面サファイア基板の表面上にGaNをエピタキシャル成長させて表面がN極性面からなるGaN膜担持体を作製する工程と、
上記GaN膜にイオン注入を行ってイオン注入領域を形成する工程と、
上記イオン注入したGaN膜担持体のGaN膜側表面と支持基板とを貼り合わせて接合する工程と、
上記GaN膜におけるイオン注入領域で剥離させてGaN薄膜を支持基板上に転写して、表面がGa極性面からなるGaN薄膜を支持基板上に有するGaN積層基板を得る工程と
を有するGaN積層基板の製造方法。
2.
上記GaNエピタキシャル成長が上記高温窒化処理よりも高温で行われる1記載のGaN積層基板の製造方法。
3.
MOCVD法により上記GaNのエピタキシャル成長を行う1又は2記載のGaN積層基板の製造方法。
4.
上記C面サファイア基板を表面処理した後、700℃以下でGaNバッファー層を形成し、次いで該GaNバッファー層上に上記GaNエピタキシャル成長を行う1~3のいずれかに記載のGaN積層基板の製造方法。
5.
上記GaNバッファー層の厚みが15~30nmである4記載のGaN積層基板の製造方法。
6.
上記エピタキシャル成長によりGaN膜を形成した後、更に該GaN膜上に酸化シリコン膜を形成して上記GaN膜担持体とする1~5のいずれかに記載のGaN積層基板の製造方法。
7.
更に、上記イオン注入前にGaN膜担持体のイオン注入面を算術平均粗さRa0.3nm以下に平滑化する1~6のいずれかに記載のGaN積層基板の製造方法。
8.
上記イオン注入が水素イオン(H+)及び/又は水素分子イオン(H2 +)を用いた、注入エネルギー100~160keV、ドーズ量1.0×1017~3.0×1017atom/cm2の処理である1~7のいずれかに記載のGaN積層基板の製造方法。
9.
上記支持基板が、Si、Al2O3、SiC、AlN又はSiO2からなる1~8のいずれかに記載のGaN積層基板の製造方法。
10.
上記支持基板は、GaN膜担持体との接合面に酸化シリコン膜を形成したものである(ただし、支持基板がSiO2からなる場合を除く)9記載のGaN積層基板の製造方法。
また本発明によれば、GaN薄膜転写のドナー基板として大口径化し易いエピタキシャル成膜した基板を使用するため、高価で小口径なバルクGaN基板をドナー基板として使用する場合に比べて低コストかつ大口径のGaN積層基板が得られる。本発明で得られた表面がGa極性面からなるGaN積層基板はGaNテンプレート基板として、更にGaNのエピタキシャル成膜をすることにより高耐圧、高特性のGaN基板を得ることができる。
本発明に係るGaN積層基板の製造方法は、オフ角度0.5~5度のC面サファイア基板の800~1000℃での高温窒化処理及び/又は該C面サファイア基板上への結晶性AlNの堆積処理を行って上記C面サファイア基板を表面処理する工程と、上記表面処理されたC面サファイア基板の表面上にGaNをエピタキシャル成長させて表面がN極性面からなるGaN膜担持体を作製する工程と、上記GaN膜にイオン注入を行ってイオン注入領域を形成する工程と、上記イオン注入したGaN膜担持体のGaN膜側表面と支持基板とを貼り合わせて接合する工程と、上記GaN膜におけるイオン注入領域で剥離させてGaN薄膜を支持基板上に転写して、表面がGa極性面からなるGaN薄膜を支持基板上に有するGaN積層基板を得る工程と、を有することを特徴とするものである。
本発明に係るGaN積層基板の製造方法は、図1に示すように、(a)C面サファイア基板及び支持基板の準備工程(工程1)、(b)C面サファイア基板の表面処理工程(工程2)、(c)GaNエピタキシャル成長工程(工程3)、(d)イオン注入処理工程(工程4)、(e)貼り合わせ接合工程(工程5)、(f)GaN薄膜の剥離、転写工程(工程6)の順に処理を行うものである。
まずC面サファイア基板11と支持基板12を準備する(図1(a))。
ここで、C面サファイア基板11は、C面((0001)面)を基板面とするサファイア(α-Al2O3)からなる基板である。また、C面サファイア基板11のc軸オフ角度(以下、オフ角度)は、0.5~5度であり、2~3度であることが好ましい。オフ角度をこの範囲内とすることにより、この後にC面サファイア基板11上に形成されるGaN膜13においてその表面がN極性面(以下、N面)となると共に平滑性が良好で結晶性がよいエピタキシャル成長膜となり、更にイオン注入剥離法によりこれの一部を剥離して支持基板12に転写した場合にその転写薄膜であるGaN薄膜13aが平滑性に優れたものとなる。なお、オフ角度とは基板表面(結晶成長させようとする面)を最密面から特定方向に微傾斜させた場合のその角度であり、c軸オフ角度とは、C面サファイア基板11のc軸(C面の法線軸)のa軸方向への傾きの大きさをいう。
なお、このボンド膜の膜厚は、概ね300~1000nmが好ましい。
次に、C面サファイア基板11の表面処理を行う(図1(b))。
即ち、C面サファイア基板11の800~1000℃での高温窒化処理及び/又はC面サファイア基板11上への結晶性AlNの堆積処理を行う。
次に、上記表面処理されたC面サファイア基板11の表面上にGaNをエピタキシャル成長させて表面がN極性面からなるGaN膜13を形成し、GaN膜担持体を作製する。
また、GaN膜13の厚みは、最終的に得ようとするGaN薄膜13aの厚さに応じるものであり、例えば0.5~10μmである。
ここで、GaNなどの化合物半導体結晶表面は極性を有しており、例えば構成元素GaとNからなる単結晶のGaN膜は、必然的に、Ga原子からなり(終端され)該Ga原子の未結合手が露出した極性面(Ga極性面(Ga面ともいう))と、N原子からなり(終端され)該N原子の未結合手が露出した極性面(N極性面(N面ともいう))を有する。
また、GaNの結晶構造は六方晶系であり、その極性面は結晶格子の最密面に現れる。なお、六方晶系化合物半導体結晶の最密面は{0001}面であるが、(0001)面と(000-1)面は等価ではなく、前者はカチオン原子が露出する面、後者はアニオン原子が露出する面であり、窒化ガリウム(GaN)においては(0001)面がGa面、(000-1)面がN面となる。
次に、上記GaN膜担持体のGaN膜13の表面からイオン注入を行ってGaN膜13中に層状のイオン注入領域13ionを形成する(図1(d))。
例えば、工程3で形成したGaN膜13表面をCMP等による研磨及び/又はエッチングして算術平均粗さRaが好ましくは0.3nm以下、より好ましくは0.2nm以下となるように平滑化するとよい。
次に、上記イオン注入したGaN膜担持体のGaN膜13側表面と支持基板12とを貼り合わせて接合する(図1(e))。
例えば、一般的な平行平板型プラズマチャンバーに、表面活性化処理するGaN膜担持体及び/又は支持基板12をセットし、13.56MHz、100W程度の高周波を印加し、プロセスガスとしてAr、N2、O2等を導入して処理すればよい。処理時間は5~30秒とする。これにより、対象の基板表面が活性化され、貼り合わせ後の接合強度が増大する。
また、貼り合せ後は200~300℃程度のアニールを実施することで、より強固な接合が形成される。
次に、上記GaN膜13におけるイオン注入領域13ionで剥離させてGaN薄膜13aを支持基板12上に転写する(図1(f))。
なお、剥離後の転写したGaN薄膜13aの表面は十分に平滑であるが、このGaN積層基板10を使用するデバイスの要求特性の如何によっては研磨等でより平滑化してもよい。また、このGaN積層基板10に更にGaN膜をエピタキシャル成長させることで、低欠陥で厚膜のGaN基板を製造することも可能である。
以下の条件でGaN積層基板を作製した。
直径100mm、厚み525μm、算術平均粗さRa0.3nm、C軸オフ角3度のC面サファイア基板を準備した。この基板をRCA洗浄にて洗浄した後、MOCVD装置にて、基板温度900℃の高温窒化処理(プロセスガス:純窒素)を30分実施し、続いて基板温度400℃でGaNバッファー層を厚み20nm成膜した後に、更に基板温度1050℃にて、プロセスガス:TMG及びNH3を用いてエピタキシャル成長させてGaN膜を2μm成膜した。そのGaN膜の算術平均粗さRaは8nmであった。
次いで、このGaN膜上にプラズマCVD法により厚み1μmの酸化シリコン膜を成膜した後、CMP装置でこの酸化シリコン膜を200nmまで研磨した。得られたGaN膜担持体の算術平均粗さRaは0.3nmであった。
次に、このGaN膜担持体の酸化シリコン膜表面から水素分子イオンH2 +を、注入エネルギー160keV、ドーズ量3.0×10+17atom/cm2でイオン注入した。
得られたGaN積層基板のGaN薄膜表面の算術平均粗さRaは8nmであった。また、得られたGaN積層基板のGaN薄膜についてX線ロッキングカーブ法により結晶性を評価した。詳しくは、X線回折により上記GaN薄膜のGaN(0002)面反射のロッキングカーブ(ωスキャン)におけるチルト分布(半価幅)を求めたところ、300arcsecと良好な結晶性を示した。
また、GaN薄膜の表面の極性面の確認として、サンプルを40℃、2mol/LのKOH水溶液に45分浸した後、表面を観察したところ、GaN薄膜表面はエッチングされておらず、GaN薄膜表面がGa面となっていることが分かった。
実施例1-1において、厚み2μmのGaN膜をエピタキシャル成長させた後、このGaN膜表面をCMP研磨してその表面の算術平均粗さRaを0.2nmとし、そのまま転写した。それ以外は実施例1-1と同様にしてGaN積層基板を得た。
得られたGaN積層基板のGaN薄膜表面の算術平均粗さRaは0.3nmであった。また、得られたGaN積層基板のGaN薄膜について実施例1-1と同様にX線ロッキングカーブ法により結晶性を評価したところ、FWHM250arcsecとなり、実施例1と同等の結晶性を示した。
また、実施例1-1と同様にしてGaN薄膜の表面の極性面を確認したところ、Ga面となっていた。
実施例1-1において、C面サファイア基板のc軸オフ角度を0.05度(算術平均粗さRa0.3nm)としたものを用い、それ以外は実施例1-1と同様にしてGaN積層基板を得た。なお、GaN膜成膜後の該GaN膜算術平均粗さRaは60nmであり、酸化シリコン膜CMP研磨後のGaN膜担持体の算術平均粗さRaは0.2nmであった。
得られたGaN積層基板のGaN薄膜表面の算術平均粗さRaは60nmであった。また、得られたGaN積層基板のGaN薄膜について実施例1-1と同様にX線ロッキングカーブ法により結晶性を評価したところ、FWHM600arcsecとなり、結晶性が悪化した。
また、実施例1-1と同様にしてGaN薄膜の表面の極性面を確認したところ、Ga面となっていた。
実施例1-1において、C面サファイア基板のc軸オフ角度を6度(算術平均粗さRa0.3nm)としたものを用い、それ以外は実施例1-1と同様にしてGaN積層基板を得た。なお、GaN膜成膜後の該GaN膜算術平均粗さRaは80nmであり、酸化シリコン膜CMP研磨後のGaN膜担持体の算術平均粗さRaは0.3nmであった。
得られたGaN積層基板のGaN薄膜表面の算術平均粗さRaは80nmであった。また、得られたGaN積層基板のGaN薄膜について実施例1-1と同様にX線ロッキングカーブ法により結晶性を評価したところ、FWHM800arcsecとなり、結晶性が悪化した。
また、実施例1-1と同様にしてGaN薄膜の表面の極性面を確認したところ、Ga面となっていた。
11 C面サファイア基板
11a 表面処理層
12 支持基板
13 GaN膜
13a GaN薄膜
13ion イオン注入領域
Claims (10)
- オフ角度0.5~5度のC面サファイア基板の800~1000℃での高温窒化処理及び/又は該C面サファイア基板上への結晶性AlNの堆積処理を行って上記C面サファイア基板を表面処理する工程と、
上記表面処理されたC面サファイア基板の表面上にGaNをエピタキシャル成長させて表面がN極性面からなるGaN膜担持体を作製する工程と、
上記GaN膜にイオン注入を行ってイオン注入領域を形成する工程と、
上記イオン注入したGaN膜担持体のGaN膜側表面と支持基板とを貼り合わせて接合する工程と、
上記GaN膜におけるイオン注入領域で剥離させてGaN薄膜を支持基板上に転写して、表面がGa極性面からなるGaN薄膜を支持基板上に有するGaN積層基板を得る工程と
を有するGaN積層基板の製造方法。 - 上記GaNエピタキシャル成長が上記高温窒化処理よりも高温で行われる請求項1記載のGaN積層基板の製造方法。
- MOCVD法により上記GaNのエピタキシャル成長を行う請求項1又は2記載のGaN積層基板の製造方法。
- 上記C面サファイア基板を表面処理した後、700℃以下でGaNバッファー層を形成し、次いで該GaNバッファー層上に上記GaNエピタキシャル成長を行う請求項1~3のいずれか1項記載のGaN積層基板の製造方法。
- 上記GaNバッファー層の厚みが15~30nmである請求項4記載のGaN積層基板の製造方法。
- 上記エピタキシャル成長によりGaN膜を形成した後、更に該GaN膜上に酸化シリコン膜を形成して上記GaN膜担持体とする請求項1~5のいずれか1項記載のGaN積層基板の製造方法。
- 更に、上記イオン注入前にGaN膜担持体のイオン注入面を算術平均粗さRa0.3nm以下に平滑化する請求項1~6のいずれか1項記載のGaN積層基板の製造方法。
- 上記イオン注入が水素イオン(H+)及び/又は水素分子イオン(H2 +)を用いた、注入エネルギー100~160keV、ドーズ量1.0×1017~3.0×1017atom/cm2の処理である請求項1~7のいずれか1項記載のGaN積層基板の製造方法。
- 上記支持基板が、Si、Al2O3、SiC、AlN又はSiO2からなる請求項1~8のいずれか1項記載のGaN積層基板の製造方法。
- 上記支持基板は、GaN膜担持体との接合面に酸化シリコン膜を形成したものである(ただし、支持基板がSiO2からなる場合を除く)請求項9記載のGaN積層基板の製造方法。
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GB2589994B (en) | 2022-03-02 |
TW202006196A (zh) | 2020-02-01 |
KR20210019066A (ko) | 2021-02-19 |
GB2589994A (en) | 2021-06-16 |
US20210111076A1 (en) | 2021-04-15 |
US11967530B2 (en) | 2024-04-23 |
TWI829709B (zh) | 2024-01-21 |
JP6915591B2 (ja) | 2021-08-04 |
CN112262456A (zh) | 2021-01-22 |
KR102570935B1 (ko) | 2023-08-28 |
JP2019216180A (ja) | 2019-12-19 |
GB202100192D0 (en) | 2021-02-24 |
DE112019002977T5 (de) | 2021-03-04 |
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