WO2015019539A1 - Procédé de fabrication d'un substrat recyclé - Google Patents

Procédé de fabrication d'un substrat recyclé Download PDF

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Publication number
WO2015019539A1
WO2015019539A1 PCT/JP2014/003425 JP2014003425W WO2015019539A1 WO 2015019539 A1 WO2015019539 A1 WO 2015019539A1 JP 2014003425 W JP2014003425 W JP 2014003425W WO 2015019539 A1 WO2015019539 A1 WO 2015019539A1
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Prior art keywords
substrate
layer
gas
dry etching
nitride semiconductor
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PCT/JP2014/003425
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English (en)
Japanese (ja)
Inventor
基 永森
孝徳 園田
貴信 西田
坂本　健次
芳英 鈴木
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シャープ株式会社
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0093—Wafer bonding; Removal of the growth substrate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32082—Radio frequency generated discharge
    • H01J37/321—Radio frequency generated discharge the radio frequency energy being inductively coupled to the plasma
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30604—Chemical etching
    • H01L21/30612—Etching of AIIIBV compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30604—Chemical etching
    • H01L21/30612—Etching of AIIIBV compounds
    • H01L21/30621—Vapour phase etching

Definitions

  • the present invention manufactures a regenerated substrate by removing an unusable semiconductor layer from a semiconductor wafer in order to reuse the substrate for a semiconductor wafer formed by sequentially depositing semiconductor layers.
  • the present invention relates to a method for manufacturing a recycled substrate.
  • Patent Document 1 This type of conventional method of manufacturing a regenerated substrate is disclosed in Patent Document 1 in which a semiconductor layer is sublimated and removed from a semiconductor wafer by heat treatment, and a patent in which a semiconductor layer is mechanically removed from a semiconductor wafer by jetting a blast material. It is proposed in Document 2.
  • FIG. 13 (a) to 13 (c) are schematic views showing an example of a conventional method for manufacturing a recycled substrate disclosed in Patent Document 1.
  • FIG. 13 (a) to 13 (c) are schematic views showing an example of a conventional method for manufacturing a recycled substrate disclosed in Patent Document 1.
  • a semiconductor wafer 100 to be subjected to a regeneration process includes a substrate 101 and a semiconductor layer 102 formed on the substrate 101.
  • a sapphire substrate is used as the substrate 101 constituting the semiconductor wafer 100.
  • the semiconductor layer 102 is preferably a group III-V compound semiconductor layer, particularly a group III nitride compound semiconductor layer.
  • a buffer layer made of InGaN, AlGaN, or GaN is provided on the substrate 101.
  • the semiconductor wafer 100 is a starting material for manufacturing, for example, a blue light emitting chip that outputs blue light and a light emitting device using the blue light emitting chip.
  • the semiconductor layer 102 is removed by subjecting the semiconductor wafer 100 to a heat treatment.
  • the semiconductor wafer 100 is heated to a temperature higher than the sublimation point of the semiconductor layer 102 and lower than the melting point of the substrate 101.
  • This removal process includes a wafer installation process for installing the semiconductor wafer 100 in the chamber of the heating apparatus, a decompression process for reducing the pressure in the chamber of the heating apparatus, a temperature raising process for increasing the temperature of the semiconductor wafer 100, and the semiconductor wafer 100. Are held at a predetermined temperature for a certain period of time, and a temperature lowering step for lowering the temperature of the substrate 101 remaining after the semiconductor layer 102 is removed from the semiconductor wafer 100 by heat.
  • the substrate 101 from which the semiconductor layer 102 has been removed by the removal step is cleaned using a cleaning agent.
  • the above-described conventional method for manufacturing a recycled substrate includes a heating step as a removing step for removing the semiconductor layer 102 and a cleaning step for cleaning the surface of the substrate 101 from which the semiconductor layer 102 has been removed.
  • the semiconductor layer 102 that has become unusable can be removed from the semiconductor wafer 100, and the substrate 101 can be reclaimed to be usable again.
  • FIG. 14 (a) to 14 (d) are schematic diagrams showing an example of a conventional method for manufacturing a regenerated substrate disclosed in Patent Document 2.
  • FIG. 14 (a) to 14 (d) are schematic diagrams showing an example of a conventional method for manufacturing a regenerated substrate disclosed in Patent Document 2.
  • FIG. 14 (a) to 14 (d) are schematic diagrams showing an example of a conventional method for manufacturing a regenerated substrate disclosed in Patent Document 2.
  • a semiconductor wafer 200 to be subjected to substrate regeneration processing includes a substrate 201 such as a sapphire substrate, and a semiconductor layer 202 formed on the substrate 201.
  • the semiconductor layer 202 is a group III nitride compound semiconductor layer including a buffer layer made of, for example, InGaN, AlGaN, or GaN.
  • the blast material is sprayed onto the semiconductor wafer 200 to be processed to remove the semiconductor layer 202 from the semiconductor wafer 200.
  • the blasting apparatus includes a transport unit that transports the semiconductor wafer 200, a blast processing unit that sprays a slurry in which a blast material is mixed with water, from a nozzle toward the semiconductor layer 202 side of the semiconductor wafer 200, and a slurry after spraying.
  • a recovery unit for recovery and a control unit for comprehensively controlling the entire blasting apparatus are provided.
  • a material harder than a group III nitride compound for example, GaN
  • a group III nitride compound for example, GaN
  • aluminum oxide grains alumina grains
  • the blast material remaining on the regenerated substrate 101 affects the subsequent processes because the sapphire substrate and the alumina particles are of the same type. This is to make the influence extremely small.
  • the substrate 201 from which the semiconductor layer 202 has been removed is heated to a predetermined temperature (for example, 1400 degrees Celsius).
  • a predetermined temperature for example, 1400 degrees Celsius.
  • the surface of the substrate 201 is polished with respect to the substrate 201 that has been subjected to the heat treatment.
  • a polishing apparatus having a surface plate on which the substrate 201 is placed and a polishing pad for polishing the surface of the substrate 201 is used.
  • the method for manufacturing a recycled substrate includes a blasting process, a heat treatment process, and a polishing process.
  • the semiconductor layer 102 is sublimated and thermally removed from the substrate 101 of the semiconductor wafer 100 by heat treatment, which is disclosed in Patent Document 2.
  • the semiconductor layer 202 is mechanically removed from the substrate 201 of the semiconductor wafer 200 by spraying a blast material.
  • Patent Documents 1 and 2 if the nitride semiconductor layer is thermally and mechanically peeled off as a semiconductor layer, the crystallinity of the substrate may be adversely affected, or the uneven shape of the substrate surface may be adversely affected. There is. In particular, it is necessary to regenerate the substrate while accurately maintaining the triangular cross-sectional PSS shape of the concavo-convex structure on the surface of the sapphire substrate.
  • the present invention solves the above-mentioned conventional problems, and regenerates a substrate with a nitride semiconductor layer that has become unusable with a simple method without adversely affecting the crystallinity of the substrate and the surface roughness.
  • An object of the present invention is to provide a method of manufacturing a regenerated substrate that can be used.
  • the method for manufacturing a regenerated substrate of the present invention includes a first dry etching step of removing at least the nitride semiconductor layer by dry etching on a semiconductor substrate having one or more nitride semiconductor layers formed on the substrate.
  • a buffer layer is provided between the substrate and the nitride semiconductor layer, and the dry etching for removing the nitride semiconductor layer and the buffer layer is performed.
  • a wet etching step for removing the remaining residue is further included.
  • a mixed solution of hydrogen peroxide and sulfuric acid is used in the wet etching step in the method for producing a recycled substrate of the present invention
  • the buffer layer is an AlN layer
  • the Al compound and the residue of the AlN layer are used as the residue.
  • the chemical residue used in the ultrasonic residue removal step is a mixed solution of hydrogen peroxide water and ammonia water, or hydrogen peroxide water, ammonia water and pure water. It is a mixed solution.
  • a buffer layer is provided between the substrate and the nitride semiconductor layer, and the first dry etching step is performed by performing dry etching on the surface of the buffer layer or the buffer layer.
  • the third dry etching step is performed.
  • the gas flow rate is adjusted so as to increase the flow rate ratio of the SiCl 4 gas to the Cl 2 gas.
  • the substrate surface of the semiconductor substrate in the method for manufacturing a recycled substrate according to the present invention is subjected to uneven processing.
  • At least one of chlorine gas and chlorine-based gas is used for dry etching in the method for producing a recycled substrate of the present invention.
  • an AlN buffer layer is provided between the substrate and the nitride semiconductor layer in the method for manufacturing a regenerated substrate of the present invention, and the dry etching is performed by wet etching using a mixed solution of hydrogen peroxide and sulfuric acid.
  • the chemical liquid to be used is a mixed liquid of hydrogen peroxide water and ammonia water, or a mixed liquid of hydrogen peroxide water, ammonia water and pure water.
  • the mixing ratio of the mixed solution of hydrogen peroxide, ammonia and pure water in the method for producing a regenerated substrate of the present invention is in the range of 1: 1: 1 to 1: 1: 25.
  • the ultrasonic output in the ultrasonic residue removing step in the method for producing a regenerated substrate of the present invention is in the range of 100 W to 500 W.
  • the chemical temperature in the method for producing a regenerated substrate of the present invention is 20 degrees Celsius to 45 degrees Celsius.
  • the method for producing a recycled substrate according to the present invention includes removing a nitride semiconductor layer to a position near the buffer layer by dry etching on a semiconductor substrate having a buffer layer on the substrate and a nitride semiconductor layer formed thereon. And a third dry etching for removing the nitride semiconductor layer by dry etching using the buffer layer as an etch stop layer, thereby achieving the above object.
  • the substrate surface of the semiconductor substrate in the method for manufacturing a recycled substrate according to the present invention is subjected to uneven processing.
  • the second dry etching step in the method for manufacturing a regenerated substrate of the present invention uses a mixed gas of Cl 2 gas and SiCl 4 gas to perform etching to the uneven surface of the buffer layer or a position in the vicinity thereof, and then the second dry etching step.
  • the gas flow rate is adjusted so as to increase the flow rate ratio of the SiCl 4 gas to the Cl 2 gas.
  • it has a buffer layer removing step of removing the buffer layer with a chemical solution after removing the nitride semiconductor layer by the third dry etching step in the method for producing a recycled substrate of the present invention.
  • the buffer layer in the method for manufacturing a regenerated substrate of the present invention is an AlN layer.
  • the chemical solution in the method for producing a recycled substrate of the present invention is a mixed solution of sulfuric acid and hydrogen peroxide solution.
  • the present invention includes a first dry etching step of removing at least the nitride semiconductor layer by dry etching on a semiconductor substrate having one or more nitride semiconductor layers formed on the substrate.
  • the PSS substrate with a GaN layer that has become unusable without adversely affecting the crystallinity and surface roughness of the substrate as in the prior art by a simple chemical method using dry etching.
  • a substrate with a nitride semiconductor layer such as can be reproduced with good quality.
  • (A) And (b) is board
  • FIG. 5 is a block diagram for explaining the relationship between the methods for manufacturing each recycled substrate of the first to fourth embodiments.
  • FIG. 5 is a longitudinal sectional view showing an example of a main configuration of a nitride semiconductor light emitting device using a reproduction substrate manufactured by the method for manufacturing each reproduction substrate of Embodiments 1 to 4 of the present invention.
  • (A)-(c) is a schematic diagram which shows an example of the manufacturing method of the conventional reproduction
  • FIG. (A)-(d) is a schematic diagram which shows an example of the manufacturing method of the conventional reproduction
  • each thickness, length, etc. of the structural member in each figure are not limited to the structure to illustrate from a viewpoint on drawing preparation.
  • the number of concave and convex shapes having a repeated cross-sectional triangle may not coincide with an actual device, and is set in consideration of the convenience of illustration and description, and is not limited to the configuration illustrated.
  • 1 (a) and 1 (b) are substrate cross-sectional views for explaining a method for manufacturing a regenerated substrate in Embodiment 1 of the present invention.
  • the manufacturing method of the reproduction substrate according to the first embodiment is a semiconductor in which a thin buffer layer 2 is formed on the unevenness of the sapphire substrate 1, and a nitride semiconductor layer 3 is formed thereon.
  • There is a first dry etching step in which the nitride semiconductor layer 3 or the buffer layer 2 and the nitride semiconductor layer 3 are removed from the semiconductor substrate 10 by dry etching the substrate 10 to obtain a reproduction substrate.
  • a sapphire substrate 1 for example, a sapphire substrate 1 as a substrate having a concavo-convex structure with a triangular cross section formed repeatedly on the surface, for example, about 1300 ⁇ m, is thin, for example, about 50 nm.
  • a buffer layer 2 is formed.
  • the surface of the buffer layer 2 has an uneven shape reflecting the uneven shape on the sapphire substrate 1.
  • a non-doped GaN layer made of non-doped GaN and having a thickness of, for example, about 10 ⁇ m is formed thereon as the nitride semiconductor layer 3.
  • the surface of the nitride semiconductor layer 3 (GaN layer) is flat.
  • the sapphire substrate 1, the AlN layer buffer layer 2 thereon, and the nitride semiconductor layer 3 such as the non-doped GaN layer thereon constitute a single crystal substrate (PSS substrate with a GaN layer).
  • a single crystalline substrate PSS substrate with a GaN layer
  • a light emitting layer is sandwiched between upper and lower cladding layers to form a semiconductor light emitting device.
  • FIG. 2 is a process diagram showing the flow of a method for manufacturing a recycled substrate in Embodiment 1 of the present invention.
  • a thin film of the buffer layer 2 (AlN layer) is formed on the sapphire substrate 1 having a concavo-convex shape (PSS shape 1a) having a triangular surface section.
  • the semiconductor substrate 10 on which a thick nitride semiconductor layer 3 (GaN layer) having a flat surface is formed is introduced into a predetermined stage position in a chamber of a substrate processing apparatus for performing dry etching.
  • step S12 dry etching is performed by supplying chlorine gas (Cl 2 ) into the chamber of the substrate processing apparatus.
  • Cl 2 chlorine gas
  • the thin films of the nitride semiconductor layer 3 (GaN layer) and the buffer layer 2 (AlN layer) on the irregular shape of the substrate surface are removed.
  • the chlorine gas supplied to the nitride semiconductor layer 3 of the semiconductor substrate 10 is fixed on a stage in a chamber of the substrate processing apparatus with the nitride semiconductor layer 3 facing upward.
  • the surface has a triangular cross section as shown in FIG.
  • a sapphire substrate 1 having an uneven shape (PSS shape 1a) can be obtained.
  • step S13 the nitride semiconductor layer 3 (GaN layer) and the buffer layer 2 (AlN layer) are removed to obtain a sapphire substrate 1 (PSS substrate) having an uneven PSS shape 1a.
  • the sapphire substrate 1 (PSS substrate) can be manufactured as a recycled substrate.
  • ICP inductively coupled plasma
  • FIG. 3 is a main part configuration diagram schematically showing a cross-sectional structure of a substrate processing apparatus used for dry etching in the manufacturing method of the recycled substrate of FIG.
  • this substrate processing apparatus 11 is an ICP (inductively coupled plasma) apparatus
  • an upper electrode 13 and a lower electrode 14 provided in the processing chamber 12 can be controlled independently.
  • a semiconductor substrate 10 that is an insulating substrate can be directly mounted thereon.
  • the substrate processing apparatus 11 includes a semiconductor substrate 10 disposed on a stage in a lower electrode 14 in a processing chamber 12 as a processing chamber, and supplies power to the upper electrode 13 and the lower electrode 14 independently, thereby processing chambers.
  • a substrate processing apparatus 11 that performs substrate processing (dry etching) by converting chlorine gas (Cl 2 ) or chlorine-based gas (for example, SiCl 4 ) as a processing gas in the plasma into 12 plasma, power is supplied only to the upper electrode 13.
  • Substrate processing dry etching
  • the substrate processing apparatus 11 controls only the upper electrode 13 while ensuring the back surface He for cooling at a pressure necessary for achieving the process, and the surface area of the insulating substrate on the semiconductor substrate 10 is reduced without using a mechanical chuck.
  • a processing gas pressure adjustment process (stability process) in which a processing gas is introduced into the processing chamber 12 instead of an inert gas and the processing gas pressure is adjusted to a predetermined pressure as in the prior art in a state where it is utilized to the maximum by electrostatic adsorption. ),
  • the negative charge of the plasma 15 is charged on the semiconductor substrate 10 by the plasma 15 obtained by converting the processing gas into plasma, and the semiconductor substrate 10 is electrostatically adsorbed on the stage of the lower electrode 14 to hold and fix it.
  • An adsorption holding process is provided.
  • the upper electrode 13 and the lower electrode 14 are both controlled to perform plasma etching.
  • the GaN layer as the nitride semiconductor layer 3 and the AlN layer as the buffer layer 2 are removed.
  • a plasma 15 of a gas species having a high electron emission rate is generated, and supply of electric charges sufficient to secure adsorption force to the surface of the semiconductor substrate 10 is ensured.
  • the ESC voltage to the ESC electrode 16 it is possible to obtain sufficient adsorption force on the surface of the lower electrode 14 of the semiconductor substrate 10 together with the electric charge charged on the surface of the semiconductor substrate 10.
  • the application timing of the ESC voltage to the ESC electrode 16 in the adsorption holding process starts at the start of the stability process.
  • the semiconductor substrate 10 as an insulating substrate is electrostatically adsorbed by an electrostatic chuck (ESC).
  • ESC electrostatic chuck
  • the individual RF control of the upper electrode 13 and the lower electrode 14, the adoption of the ESC method, and the selection of conditions (gas type, RFPOWER, application timing, etc.) that make the electron emission rate to the insulator surface of the semiconductor substrate 10 effective are performed.
  • a gas species having a high electron emission rate that is easily plasmatized is selected as the processing gas.
  • chlorine gas (Cl 2 ) or chlorine-based gas (eg, SiCl 4 ) is used as a gas species having a high electron emission rate.
  • the buffer layer 2 (AlN layer) is formed on the sapphire substrate 1, and the nitride semiconductor layer 3 (GaN layer) is formed thereon (or a plurality of layers).
  • the semiconductor substrate 10 has a first dry etching step of removing the nitride semiconductor layer 3 (GaN layer) and the buffer layer 2 (AlN layer) therebelow by dry etching.
  • the Ga-based nitride semiconductor layer (GaN layer), which has become unusable without obtaining the desired characteristics without adversely affecting the crystallinity and surface irregularity shape, thermally or mechanically as in the past, by the removal method
  • the substrate can be regenerated by removing the GaN layer and the AlN layer from the semiconductor substrate 10 as a substrate with a nitride semiconductor layer such as a PSS substrate.
  • ICP dry etching is performed by converting chlorine gas (Cl 2 ) under a high flow rate into plasma, and thin films of the nitride semiconductor layer 3 (GaN layer) and the uneven buffer layer 2 (AlN layer) are formed.
  • the first dry etching step is not limited to this, and the ICP dry etching is performed by converting chlorine gas (Cl 2 ) under a high flow rate condition into a plasma, and the upper portion of the uneven shape is formed.
  • the second dry etching step described in the third embodiment may be performed in which only the nitride semiconductor layer 3 (GaN layer) before or up to the surface of the buffer layer 2 (AlN layer) is removed.
  • chlorine gas (Cl 2 ) or a mixed gas of chlorine gas (Cl 2 ) and chlorine-based gas (SiCl 4 ) is used, and in the case of a mixed gas, chlorine gas (Cl 2 )
  • a mixed gas chlorine gas (Cl 2 )
  • the first dry etching process of the first embodiment includes a second dry etching process in which the nitride semiconductor layer 3 (GaN layer) is removed to the surface of the buffer layer 2 (AlN layer) or a position in the vicinity thereof by dry etching.
  • the third dry etching step of removing the remaining nitride semiconductor layer 3 (GaN layer) by dry etching using the buffer layer 2 (AlN layer) as an etch stop layer may be employed. This will be described in detail in the next embodiment liquid 3.
  • nitride semiconductor layer 3 or the buffer layer 2 and the nitride semiconductor layer 3 are removed from the semiconductor substrate 10 has been described.
  • a plurality of nitride semiconductor layers may be removed by dry etching on a semiconductor substrate having a plurality of nitride semiconductor layers formed on the substrate instead of the semiconductor substrate 10.
  • the upper and lower cladding layers and the light emitting layers therebetween are removed from the semiconductor light emitting device formed by sandwiching the light emitting layers between the upper and lower cladding layers as a plurality of nitride semiconductor layers on the semiconductor substrate 10. Thereafter, the buffer layer 2 and the nitride semiconductor layer 3 are further removed from the semiconductor substrate 10.
  • Embodiment 2 In the first embodiment, the case where the substrate is regenerated by removing the GaN layer and the AlN layer by performing dry etching has been described. However, in the second embodiment, dry etching and wet etching (AlN residue removal) are performed to further increase the thickness. A case will be described in which the GaN layer and the AlN layer are removed by sonic cleaning (AlN residue removal) and the substrate is regenerated without residue.
  • FIG. 4 (a) to 4 (c) are substrate cross-sectional views for explaining a method for manufacturing a recycled substrate according to Embodiment 2 of the present invention.
  • FIG. 5 is a process diagram showing a flow of a method for manufacturing a recycled substrate according to Embodiment 2 of the present invention.
  • a buffer layer 2 (on the sapphire substrate 1 having a concavo-convex shape (PSS shape 1a) having a triangular surface cross section.
  • a predetermined stage position in a chamber of a substrate processing apparatus for performing ICP dry etching on a semiconductor substrate 10 on which a thin nitride semiconductor layer 3 (GaN layer) having a flat surface is formed.
  • FIG. 4 (b) and FIG. 5 as shown in, in the first dry etching process at Step S22, chlorine gas (Cl 2 was supplied chlorine gas (Cl 2) into the chamber 12 of the substrate processing apparatus 11 ICP dry etching is performed using plasma.
  • the thin films of the nitride semiconductor layer 3 (GaN layer) and the uneven buffer layer 2 (AlN layer) are removed.
  • a part of the buffer layer 2 (AlN layer) (residue 2a) remains between the irregular shapes on the surface of the sapphire substrate 1.
  • the Al compound generated by dry etching and the buffer layer 2 (AlN layer) partially remained as a residue 2a in the hydrogen peroxide treatment process of Step S23.
  • a chemical solution is applied to the sapphire substrate 1 in which the Al compound and the buffer layer 2 (AlN layer) remain as the residue 2a in the sulfuric acid treatment process in step S24.
  • the Al compound and the residue 2a of the buffer layer 2 (AlN layer) are removed using a mixed solution of hydrogen peroxide water (H 2 O 2 ) and sulfuric acid (H 2 SO 4 ).
  • step S25 the Al compound attached to the sapphire substrate 1 (PSS substrate) and the residue 2a of the buffer layer 2 (AlN layer) are removed by washing with pure water.
  • the wet etching process in step S20A is constituted by the hydrogen peroxide solution treatment process in step S23, the sulfuric acid treatment process in step S24, and the water washing process in step S25.
  • the sapphire substrate 1 in which the Al compound and the extremely small residue 2a of the buffer layer 2 (AlN layer) remain in the ultrasonic cleaning process in step S26 is used as a chemical solution.
  • an ultrasonic cleaning process is performed at an ultrasonic output of 100 W to 500 W used in the ultrasonic vibration device.
  • a mixed solution of 2.6 liters of hydrogen peroxide water, 2.6 liters of ammonia water, and 25.8 liters of pure water was used.
  • the ratio (volume ratio or weight ratio) of the mixed solution of hydrogen peroxide water, ammonia water and pure water is 1: 1: 1 to 1: 1: 25 (in this case, 1: 1: 10). Used).
  • the temperature of the chemical solution used in the ultrasonic cleaning at this time is a temperature range from room temperature RT (for example, 20 degrees Celsius or 25 degrees Celsius) to 45 degrees Celsius.
  • step S24 since the sulfuric acid treatment process of step S24 has an adverse effect on the uneven shape of the surface (PSS shape 1a), the next ultrasonic cleaning treatment process is performed even in a state where the treatment time is set as short as possible and a part of the residue 2a is left. Performed to completely remove residue.
  • step S27 the sapphire substrate 1 in which the Al compound residue attached to the sapphire substrate 1 (PSS substrate) or the extremely small residue 2a of the buffer layer 2 (AlN layer) remains is washed with pure water to obtain the residue 2a. Remove. In step S28, this is dried.
  • the ultrasonic cleaning process of step S26, the water washing process of step S27, and the drying process of step S28 constitute the ultrasonic residue removing process of step S20B.
  • the sapphire substrate 1 (PSS substrate with Al residue) in which the Al compound and a partial residue 2 a of the buffer layer 2 (AlN layer) remain between the PSS shapes 1 a.
  • the Al compound and the buffer layer 2 (AlN layer) are partially removed (residue 2a) by the wet etching process, and the ultrasonic residue removal process in step S20B completely removes the extremely small residue 2a.
  • the sapphire substrate 1 (PSS substrate) having the PSS shape 1a having an uneven surface can be obtained with high quality. In this way, the sapphire substrate 1 (PSS substrate) can be satisfactorily manufactured as a recycled substrate.
  • the GaN layer / AlN layer can be completely peeled off with high quality.
  • the PSS substrate can be reproduced easily and with high quality without adversely affecting the crystallinity of the sapphire substrate 1 and the uneven shape of the surface.
  • FIG. 6 is a main part configuration diagram schematically showing a cross-sectional structure of a substrate processing apparatus used for dry etching with chlorine gas in a high temperature atmosphere without using plasma.
  • the substrate processing apparatus 31 includes a processing chamber 32 in which one or a plurality of semiconductor substrates 10 are accommodated, an electric furnace 33 that is disposed above and below the processing chamber 32, and heats the processing chamber 32.
  • a stage 34 and a boat 35 for placing one or a plurality of semiconductor substrates 10 in the processing chamber 32 are provided.
  • the processing chamber 32 is provided with a gas introduction part 36 for introducing an etching gas such as a chlorine-based gas therein and a gas exhaust part 37 for exhausting an etching gas such as a chlorine-based gas from the inside thereof.
  • one or a plurality of semiconductor substrates 10 are disposed in a processing chamber 32, and a dry etching process is performed by introducing a chlorine-based gas into the interior while heating.
  • a typical condition is that the heating temperature is 800 degrees Celsius under atmospheric pressure.
  • FIG. 7 (a) to 7 (c) are substrate cross-sectional views for explaining a method for manufacturing a recycled substrate according to Embodiment 3 of the present invention.
  • FIG. 8 is a process diagram showing the flow of a method for manufacturing a recycled substrate in Embodiment 3 of the present invention.
  • a buffer layer 2 (on the sapphire substrate 1 having a surface-repetitive uneven shape (PSS shape 1a) having a triangular cross section).
  • a predetermined stage position in a chamber of a substrate processing apparatus for performing ICP dry etching on a semiconductor substrate 10 on which a thin nitride semiconductor layer 3 (GaN layer) having a flat surface is formed.
  • the depth of the uneven shape is 0.5 ⁇ m.
  • ICP dry etching is performed under a low flow rate condition of SiCl 4 gas with respect to Cl 2 gas. That is, the SiCl 4 gas mixing ratio (volume ratio) to Cl 2 gas is 0.4, and the low selectivity ratio condition (rate ratio is GaN ⁇ AlN ⁇ Al 2 O 3 ), the SiCl gas with respect to the Cl 2 gas flow rate.
  • the ICP dry etching is performed by rapidly etching at a high rate with respect to GaN by setting the 4 gas flow rate to a low gas flow rate and increasing the Cl 2 gas flow rate. This ICP dry etching is performed to the surface of the concavo-convex buffer layer 2 (here, the AlN layer), to the front (near the tip), or to the tip.
  • the nitride semiconductor layer 3 (GaN layer) on the surface of the concave-convex buffer layer 2 (AlN layer) or in front (near the tip) or up to the tip is removed earlier.
  • the mixing ratio of the SiCl 4 gas and the Cl 2 gas is 12:28, and the flow rate of the SiCl 4 gas is not more than half of the Cl 2 gas flow rate (volume ratio).
  • ICP dry etching is performed under a high flow rate condition of SiCl 4 gas with respect to Cl 2 gas. That is, ICP dry etching is performed with the SiCl 4 gas flow rate set to a high gas flow rate with respect to the Cl 2 gas flow rate so that the high selection ratio condition (rate ratio is GaN> Al 2 O 3 > AlN).
  • SiCl 4 gas since a very low etching rate with respect to the buffer layer 2 (AlN layer) using the same, left the AlN buffer layer 2 as an etch stop layer by increasing the gas flow rate of SiCl 4 gas Only the nitride semiconductor layer 3A (GaN layer) can be removed by etching.
  • the semiconductor substrate 10A remaining on the surface of the buffer layer 2 (in this case, the AlN layer) on the uneven shape or in front (near the tip) or up to the tip under a high selection ratio condition of SiCl 4 high flow rate condition,
  • the remaining nitride semiconductor layer 3A (GaN layer) is etched away using AlN of the buffer layer 2 as an etch stop layer.
  • the mixing ratio of SiCl 4 gas and Cl 2 gas is from 12:28 to 56:28 (“56” is twice that of Cl 2 gas “28”), and the flow rate of SiCl 4 gas is twice that of Cl 2 gas. (Volume ratio).
  • the SiCl 4 gas flow rate is increased from less than half (for example, 0.4) to twice the Cl 2 gas flow rate to adjust the high selection ratio condition (rate ratio is GaN> Al 2 O 3 > AlN).
  • rate ratio is GaN> Al 2 O 3 > AlN.
  • SiCl of more SiCl 4 low flow conditions of the gas was set to the gas flow rate of 0.2-1 times the SiCl 4 gas is Cl 2 gas (volume or weight) (volume), more SiCl 4 gas Four gases are set to a gas flow rate (volume) of 1 to 3 times (volume or weight), more preferably 1.5 to 3 times (easier to determine an etching stop) than Cl 2 gas.
  • the buffer layer 2 here, the AlN layer
  • etch stop layer etching stop layer
  • the depth of the irregularities on the relationship between (0.5 [mu] m), nitrides becomes thin the concentration of Cl 2 gas semiconductor layer 3A Since the etching rate for the (GaN layer) becomes too slow, there is no point in increasing the flow rate ratio of the SiCl 4 gas.
  • the flow rate ratio of the SiCl 4 gas to the Cl 2 gas needs to be larger than 3 times (volume mixing ratio).
  • the depth (level difference) of the uneven shape on the surface is about 0.3 ⁇ m to 1 ⁇ m.
  • the SiCl 4 gas is 1 to 3 times (volume or weight) of the Cl 2 gas, so when the unevenness depth is 1 ⁇ m, the SiCl 4 gas 1-6 times (volume or weight) of Cl 2 gas.
  • the SiCl 4 gas is about half of the Cl 2 gas, for example, about 0.4 here, but if the mixing ratio of the SiCl 4 gas to the Cl 2 gas is less than 0.2, the buffer layer 2 (AlN layer) It becomes difficult to control to stop the progress of etching once at the tip of the film.
  • the mixture ratio of the SiCl 4 gas may be 0 for dry etching the nitride semiconductor layer 3 (GaN layer).
  • the low-flow conditions SiCl 4 gas, SiCl 4 gas mixture ratio and Cl 2 gas are set to 12:28, high flow conditions SiCl 4 gas, SiCl 4 gas and Cl 2
  • the gas mixing ratio is set to 56:28.
  • the nitride semiconductor layer 3 (GaN layer) is sequentially removed by mixing Cl 2 gas and SiCl 4 gas, and the surface of the buffer layer 2 (AlN layer) near the uneven surface or in front thereof.
  • the ratio of the SiCl 4 gas flow rate to the Cl 2 gas flow rate is increased to remove only the nitride semiconductor layer 3A (GaN layer) using the buffer layer 2 as an etch stop layer.
  • the sapphire substrate 1 (PSN substrate with AlN) in which the thin film of the buffer layer 2 (AlN layer) remains on the PSS shape 1a without the residue of the GaN layer can be obtained.
  • the sapphire substrate 1 (PSN substrate with AlN) in which the thin film of the buffer layer 2 (AlN layer) remains can be manufactured as a reproduction substrate.
  • ICP dry etching is performed by mixing Cl 2 gas and SiCl 4 gas, and after the etching proceeds to the surface of the buffer layer 2 (AlN layer) on the uneven surface or the vicinity thereof, A chemical and simple removal method of adjusting the flow rate ratio of the SiCl 4 gas to remove the nitride semiconductor layer 3 (GaN film) using the buffer layer 2 (AlN layer) as an etch stop layer.
  • the PSS substrate with AlN can be reproduced with high quality without adversely affecting the crystallinity and uneven shape of the sapphire substrate 1.
  • the buffer layer 2 (AlN layer) on the uneven surface can be used as it is, the step of forming the buffer layer 2 (AlN layer) can be omitted. Further, in the third embodiment, since there is no wet etching processing step in step S20A and the ultrasonic residue removing step in step S20B in the second embodiment, a recycled substrate can be manufactured with a smaller number of steps.
  • FIG. 9 (a) to 9 (d) are substrate cross-sectional views for explaining a method for manufacturing a recycled substrate in Embodiment 4 of the present invention.
  • FIG. 10 is a process diagram showing a flow of a method for manufacturing a recycled substrate in Embodiment 4 of the present invention.
  • a buffer layer 2 on the sapphire substrate 1 having a concavo-convex shape (PSS shape 1a) having a triangular surface cross section.
  • a predetermined stage position in a chamber of a substrate processing apparatus for performing ICP dry etching on a semiconductor substrate 10 on which a thin nitride semiconductor layer 3 (GaN layer) having a flat surface is formed.
  • step S42 the Cl 2 gas into the chamber of the substrate processing apparatus at a high flow rate conditions of Cl 2 gas (chlorine gas)
  • the Cl 2 gas (chlorine gas) is turned into plasma, and the semiconductor substrate 10 is ICP dry etched to further form the nitride semiconductor layer 3 (GaN layer) before the buffer layer 2 (AlN layer) above the uneven shape. Remove quickly.
  • the Cl 2 gas flow rate is set so that the high selection ratio condition (rate ratio is GaN> Al 2 O 3 > AlN).
  • ICP dry etching is performed with the SiCl 4 gas flow rate set to a high gas flow rate.
  • the semiconductor substrate 10A remaining on the surface of the buffer layer 2 (in this case, the AlN layer) above the uneven shape or in front (near the tip) or up to the tip under a high selection ratio condition of SiCl 4 high flow rate condition,
  • a high selection ratio condition of SiCl 4 high flow rate condition By ICP dry etching, AlN of the buffer layer 2 is used as an etch stop layer (etching stop layer), and the remaining GaN layer of the nitride semiconductor layer 3A is etched away.
  • the mixing ratio of SiCl 4 gas and Cl 2 gas is set to about 56:28.
  • the SiCl 4 gas flow rate is increased from 1.5 times to 3 times (here, 2 times) with respect to the Cl 2 gas flow rate so that a high selection ratio condition (rate ratio is GaN> Al 2 O 3 > AlN)
  • rate ratio is GaN> Al 2 O 3 > AlN
  • dry etching removes the nitride semiconductor layer 3 (GaN layer) halfway with chlorine gas (Cl 2 gas) and chlorine-based gas (SiCl 4 gas), and the buffer layer 2 (AlN layer) near the uneven surface.
  • the mixing ratio of the SiCl 4 gas to the Cl 2 gas is increased, and the nitride semiconductor layer 3A remaining with the buffer layer 2 as an etch stop layer Just get rid of.
  • the sapphire substrate 1 PSN substrate with AlN
  • the thin film of the buffer layer 2 (AlN layer) remains on the PSS shape 1a can be obtained.
  • step S44 a mixed solution of hydrogen peroxide (H 2 O 2 ) and sulfuric acid (H 2 SO 4 ) is used as the chemical.
  • the buffer layer 2 AlN layer is removed by wet etching.
  • step S45 the residue of the buffer layer 2 (AlN layer) attached to the sapphire substrate 1 (PSS substrate) is removed by washing with pure water.
  • step S46 this is dried.
  • the wet etching process in step S40 is constituted by the chemical solution process in step S44, the water washing process in step S45, and the drying process in step S46.
  • the sapphire substrate 1 (PSN substrate with AlN) in which the thin film of the buffer layer 2 (AlN layer) remains on the PSS shape 1a is formed.
  • the buffer layer 2 (AlN layer) is removed by the wet etching process in step S40, and the sapphire substrate 1 (PSS substrate) having the PSS shape 1a having an uneven surface can be obtained in step S47. In this way, the sapphire substrate 1 (PSS substrate) can be manufactured as a recycled substrate.
  • the PSS substrate can be reproduced with high quality without adversely affecting the crystallinity and uneven shape of the sapphire substrate by a simple chemical removal method.
  • FIG. 11 is a block diagram for explaining the relationship between the manufacturing methods of the respective reproduction substrates of the first to fourth embodiments.
  • step S51 ICP dry etching is performed with chlorine gas (Cl 2 ) under a high flow rate condition, so that the nitride semiconductor layer 3 (GaN layer) and the uneven buffer layer 2 (AlN Layer) is removed together.
  • Cl 2 chlorine gas
  • step S51 chlorine gas (Cl 2 ) under a high flow rate condition is converted into plasma and ICP dry etching is performed, so that the nitride semiconductor layer 3 (GaN) before the buffer layer 2 (AlN layer) above the uneven shape is formed. Only the layer) is removed.
  • This is the second dry etching step of the third embodiment.
  • step S52 ICP dry etching is performed by converting chlorine gas (Cl 2 ) under a low flow rate into plasma, and the GaN layer of the nitride semiconductor layer 3 is etched using AlN of the buffer layer 2 as an etch stop layer. Remove.
  • This is the third dry etching step of the third embodiment.
  • the PSS shape 1a is better than that after the first dry etching process of the first embodiment.
  • step S53 a wet etching process including sulfuric acid treatment is performed, and in step S54, an ultrasonic residue removing process including ultrasonic cleaning is performed to remove the GaN layer and the AlN layer, and to remove the AlN layer residue. Perform substrate regeneration.
  • This is the wet etching process and the ultrasonic residue removing process of the second embodiment. Therefore, in the second embodiment, the wet etching process and the ultrasonic residue removing process are sequentially performed after the first dry etching process of the first embodiment.
  • step S53 sulfuric acid treatment is further performed in step S53.
  • the PSS substrate is regenerated by removing the buffer layer 2 (AlN layer) by performing a wet etching process including Thereafter, an ultrasonic residue removing process including an ultrasonic cleaning process in step S54 may be performed to more reliably remove residues on the surface.
  • the PSS substrate with AlN regenerated by removing the nitride semiconductor layer 3 (GaN layer), or the PSS substrate from which the nitride semiconductor layer 3 (GaN layer) and the buffer layer 2 (AlN layer) are removed.
  • a semiconductor light emitting element is formed, in which a light emitting layer is sandwiched between upper and lower cladding layers. This will be described with reference to FIG.
  • FIG. 12 is a longitudinal sectional view showing an example of the configuration of the main part of a nitride semiconductor light emitting device using a reproduction substrate manufactured by the method for manufacturing each reproduction substrate according to Embodiments 1 to 4 of the present invention.
  • the nitride semiconductor light emitting device 20 using each reproduction substrate of Embodiments 1 to 4 is, for example, on the sapphire substrate 1 as a substrate having an uneven shape (PSS shape 1a) and a thickness of about 1300 ⁇ m. Further, a buffer layer 2 made of aluminum nitride (AlN) having a thickness of about 50 nm is formed, and a nitride semiconductor layer 3 which is a non-doped GaN layer having a thickness of about 10 ⁇ m made of non-doped GaN is formed thereon. Yes.
  • the sapphire substrate 1, the buffer layer 2, and the nitride semiconductor layer 3 (GaN layer) constitute a semiconductor substrate 10 that is a single crystal substrate.
  • the nitride semiconductor layer 3 (GaN layer) of the nitride semiconductor layer 3 (GaN layer) and the buffer layer 2 (AlN layer) is removed from the unusable semiconductor substrate 10 in the above embodiment.
  • the reproduction substrate (PSS substrate or PSS substrate with AlN) obtained in 1 to 4 is used, and the buffer layer 2 (AlN layer) and the nitride semiconductor layer 3 (GaN layer) or the nitride semiconductor layer 3 are again formed on the reproduction substrate. (GaN layer) is replaced and reproduced.
  • an n-type contact layer 41 (about 5 ⁇ m thick) made of GaN doped with silicon (Si) 1 ⁇ 10 18 / cm 3 on the semiconductor substrate 10 of the single crystal substrate.
  • a high carrier concentration n ⁇ + layer is formed.
  • a multi-layer 51 is formed on the n-type contact layer 41, and a light-emitting layer 52 having a multi-quantum well structure is formed on the multi-layer 51.
  • an electron block layer 6 which is a p-type layer made of 25 nm-thick p-type Al — 0.15 Ga — 0.85 N doped with 2 ⁇ 10 19 / cm 3 of Mg, is formed on the light emitting layer 52.
  • a p-type contact layer 42 made of 100-nm thick p-type GaN doped with 8 ⁇ 10 19 Mg is formed.
  • a light-transmitting thin film electrode 7 (ITO) is formed by metal deposition, and a p-electrode 81 is formed on a part of the light-transmitting thin film electrode 7, while the n-type contact layer
  • An n electrode 82 is formed on the end of 41.
  • a protective film 9 made of a SiO 2 film is formed on the top.
  • the case where the sapphire substrate 1 having a concavo-convex shape (PSS shape 1a) is used has been described.
  • the present invention is not limited thereto, and the concavo-convex processing is performed on the surface of the substrate such as the sapphire substrate 1.
  • the inventions of Embodiments 1 to 4 can also be applied when no is applied.
  • the present invention relates to a method of manufacturing a regenerated substrate in which a regenerated substrate is manufactured by removing the laminated semiconductor layer from the laminated semiconductor wafer in order to reuse the substrate for the laminated semiconductor wafer on which the laminated semiconductor layer is formed.
  • the PSS substrate with a GaN layer that has become unusable can be regenerated with high quality without adversely affecting the crystallinity of the substrate and the surface irregularities.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
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Abstract

La présente invention vise à recycler un PSS doté d'une couche de GaN inutilisable pour obtenir un PSS de grande qualité à l'aide d'un procédé simple et sans altérer les propriétés cristallines ni la topographie de surface du substrat. Ledit procédé comprend un premier processus de gravure sèche au cours duquel un substrat semi-conducteur (10) comportant une couche tampon (2) (couche d'AlN) ainsi qu'une ou plusieurs couches semi-conductrices de nitrure (3) (couches de GaN) formées sur un substrat de saphir (1) est gravé à sec de manière à éliminer de ce substrat (10) la ou les couches semi-conductrices de nitrure (3) (couches de GaN) et la couche tampon (2) (couche d'AlN).
PCT/JP2014/003425 2013-08-06 2014-06-26 Procédé de fabrication d'un substrat recyclé WO2015019539A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014045097A (ja) * 2012-08-27 2014-03-13 Sharp Corp 再生基板の製造方法
CN109509818A (zh) * 2018-09-25 2019-03-22 华灿光电(苏州）有限公司 一种发光二极管的外延片及其制备方法
CN111063615A (zh) * 2019-12-30 2020-04-24 徐州同鑫光电科技股份有限公司 一种用于干法蚀刻中去除PSS衬底AlN涂层的方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006518544A (ja) * 2003-01-07 2006-08-10 エス．オー．アイ．テック、シリコン、オン、インシュレター、テクノロジーズ 薄層を除去した後の多層構造を備えるウェハのリサイクル
JP2013012719A (ja) * 2011-05-31 2013-01-17 Hitachi Kokusai Electric Inc 基板処理装置および基板処理方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006518544A (ja) * 2003-01-07 2006-08-10 エス．オー．アイ．テック、シリコン、オン、インシュレター、テクノロジーズ 薄層を除去した後の多層構造を備えるウェハのリサイクル
JP2013012719A (ja) * 2011-05-31 2013-01-17 Hitachi Kokusai Electric Inc 基板処理装置および基板処理方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014045097A (ja) * 2012-08-27 2014-03-13 Sharp Corp 再生基板の製造方法
CN109509818A (zh) * 2018-09-25 2019-03-22 华灿光电(苏州）有限公司 一种发光二极管的外延片及其制备方法
CN111063615A (zh) * 2019-12-30 2020-04-24 徐州同鑫光电科技股份有限公司 一种用于干法蚀刻中去除PSS衬底AlN涂层的方法

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