JP5881280B2 - Manufacturing method of LED light emitting element holding substrate and manufacturing method of LED light emitting element - Google Patents

Description

The present invention relates to a process for producing a preparation and LED devices of the holding substrate for LED devices.

  An LED (light emitting diode) is an element that emits light when a forward current flows through a pn junction of a semiconductor, and is manufactured using a III-V group semiconductor crystal such as GaAs or GaN. For example, a method has been proposed in which a buffer layer such as GaN is formed on a single crystal growth substrate such as a sapphire substrate, and GaN is epitaxially grown thereon (Patent Document 1). However, in this method, due to the difference in coefficient of linear expansion between the sapphire substrate and GaN, the sapphire substrate after epitaxial growth may be warped and the substrate may be cracked. Furthermore, since the single crystal sapphire constituting the sapphire substrate has a thermal conductivity of about 40 W / mK, the heat generated in the III-V group semiconductor element such as GaN cannot be sufficiently dissipated. For this reason, in the high-power LED in which a large current flows, the temperature of the element rises, resulting in a decrease in luminous efficiency and element life.

  In order to improve heat dissipation, there is a method in which a III-V group semiconductor crystal is epitaxially grown on a single crystal growth substrate, then a high thermal conductivity substrate is joined through a metal layer, and then the single crystal growth substrate is removed. Although it has been proposed (Patent Document 2), the difference in linear expansion coefficient from the III-V group semiconductor crystal is large, which is not satisfactory for high-power LEDs.

Japanese Patent Publication No. 5-73252 JP 2006-128710 A

  An object of the present invention is to provide an LED light-emitting element holding substrate having a small difference in linear expansion coefficient from an LED made of a III-V group semiconductor crystal (hereinafter also simply referred to as an LED) and excellent in thermal conductivity. An LED light emitting device is provided.

  Furthermore, the problem to be solved by the present invention is to provide a holding substrate for an LED light-emitting element that is excellent in chemical resistance against an acid and an alkali solution used at the time of manufacturing the LED light-emitting element and that is suitable for high-power LEDs. It is.

In the present invention, a metal matrix composite material substrate having a thickness of 0.05 to 1.0 mm, which is obtained by impregnating a silicon carbide porous body with an aluminum alloy, is manufactured through the following steps in sequence, and 5N HCl at a temperature of 25 ° C. This is a method for producing a holding substrate for an LED light emitting element, in which the weight loss amount of at least one main surface when immersed in a solution and a 10N NaOH solution at 75 ° C. for 1 minute is 0.2 mg / cm ² or less.
(1) A step of forming an aluminum layer having a thickness of 0.05 to 2 μm on the surface of the metal matrix composite substrate by a vapor deposition method or a sputtering method.
(2) A step of heat treatment at a temperature of 460 ° C. to 650 ° C. for 1 minute or more in nitrogen, argon, hydrogen, helium or a vacuum atmosphere.
(3) A step of forming a metal layer on the surface of the aluminum layer according to 1) or 2).
1) A step of forming a metal layer by sequentially forming a Ni plating layer having a thickness of 0.5 to 5 μm and a gold plating layer having a thickness of 0.05 to 2 μm on the surface of the aluminum layer by an electroless plating method or an electroplating method. .
2) A step of forming a metal layer having a thickness of 0.1 to 2 μm on the surface of the aluminum layer by vapor deposition or sputtering.

Furthermore, the metal matrix composite material substrate of the present invention is impregnated with a silicon carbide porous body having a porosity of 10 to 50% by volume and a three-point bending strength of 50 MPa or more with an aluminum alloy at an impregnation pressure of 30 MPa or more by a molten metal forging method. The thermal conductivity at a temperature of 25 ° C. is 150 to 300 W / mK, the linear thermal expansion coefficient at a temperature of 40 ° C. to 150 ° C. is 4 × 10 ⁻⁶ to 8 × 10 ⁻⁶ / K, and the three-point bending strength is 50 MPa. As described above, the volume resistivity is 10 ⁻⁹ to 10 ⁻⁵ Ω · m. Furthermore, the metal matrix composite material substrate of the present invention is formed by cutting and / or grinding to a plate thickness of 0.05 to 1.0 mm and a surface roughness (Ra) of 0.01 to 0.5 μm.

Furthermore, the present invention is a method for manufacturing an LED light emitting element in successively passed through Rukoto the following steps.
(1) A step of epitaxially growing a group III-V semiconductor crystal on one main surface of a disk-like or flat plate-like single crystal growth substrate.
(2) The above-mentioned LED light emitting element holding substrate is bonded to the III-V group semiconductor crystal surface through a metal layer, and the single crystal growth substrate is removed by laser irradiation, etching, or grinding on the back surface. Process.
(3) A step of cutting after performing surface processing of the III-V semiconductor crystal surface and electrode formation.

In addition, the present invention provides the LED light emitting device or the single crystal growth, wherein the single crystal growth substrate is selected from the group of single crystal sapphire, single crystal silicon carbide, single crystal GaAs, and single crystal Si. An LED light emitting device manufacturing method , wherein a substrate is surface-coated with a material selected from the group consisting of AlN, SiC, GaN, and GaAs.

In addition, the present invention is a method for manufacturing an LED light-emitting element , wherein the group III-V semiconductor crystal is any one of GaN, GaAs, and GaP.

  According to the present invention, there can be obtained a highly heat conductive holding substrate for an LED light-emitting element having a small difference in linear thermal expansion coefficient from the group III-V semiconductor crystal constituting the LED. By using this LED light-emitting element holding substrate, it is possible to provide a high-output LED light-emitting element having excellent heat dissipation and reliability. Furthermore, the LED light-emitting element holding substrate of the present invention is excellent in chemical resistance against acid and alkali solutions used in the manufacture of LED light-emitting elements, is conductive, and has both sides of the III-V group semiconductor crystal constituting the LED. An electrode can be formed on the substrate. Therefore, it is possible to reduce the manufacturing process of the LED light emitting element and increase the light emission amount per unit area.

The schematic sectional drawing of the LED light emitting element which shows one embodiment of this invention The schematic sectional drawing of the LED light emitting element which shows one embodiment of this invention The schematic sectional drawing of the LED light emitting element which shows one embodiment of this invention

  The single crystal growth substrate used in the present invention requires a material having a small difference in lattice constant from a group III-V semiconductor crystal to be epitaxially grown in a later step and having few defects. From the standpoints of crystallinity and uniformity, it is common to process and use a single crystal material. These single crystal growth substrates need to withstand the temperature and atmosphere in the process of epitaxially growing a III-V semiconductor crystal. Therefore, the material for the single crystal growth substrate used in the present invention is preferably selected from the group of single crystal sapphire, single crystal silicon carbide, single crystal GaAs, and single crystal Si. Furthermore, the single crystal growth substrate used in the present invention is preferably surface-coated with a material selected from the group consisting of AlN, SiC, GaN, and GaAs.

  The group III-V semiconductor crystal constituting the LED is preferably GaN, GaAs, or GaP from the viewpoint of conversion efficiency as the LED light emitting element. These III-V semiconductor crystals have high luminous efficiency and can be used properly according to the application. The III-V semiconductor crystal is selected according to the optimum emission wavelength for each application.

In the present invention, first, a III-V semiconductor crystal is grown on one main surface of these single crystal growth substrates by epitaxial growth. The epitaxial growth of the group III-V semiconductor crystal is preferably performed by metal organic vapor phase epitaxy (MOCVD method) or halide vapor phase epitaxy (HVPE method). The MOCVD method is suitable for growing a group III-V semiconductor crystal with good crystallinity, and the HVPE method has a high crystal growth rate and can grow a group III-V semiconductor crystal efficiently. These methods are publicly known, and implementation conditions can be set as appropriate. The epitaxial growth method is not limited to the above method as long as it can grow a group III-V semiconductor crystal.

  The epitaxially grown III-V group semiconductor crystal can be subjected to a surface treatment in order to further improve the light emission characteristics. In addition, in order to improve the uniformity of the crystal surface and the like, the surface may be etched or polished. In order to bond to the metal matrix composite material substrate, a metal layer is formed on the surface of the group III-V semiconductor crystal by a technique such as vapor deposition or sputtering. The metal layer is preferably indium, aluminum, gold, silver and alloys thereof. The thickness of the metal layer is not preferable because the linear thermal expansion coefficient of the metal is different from that of the group III-V semiconductor crystal, and if it is extremely thick, the adhesiveness is lowered. When the thermal conductivity of the metal layer is low, it is not preferable from the viewpoint of heat dissipation. For this reason, it is preferable that the thickness of a metal layer is 0.5-10 micrometers, More preferably, it is 0.5-2 micrometers.

  In order to bond to the group III-V semiconductor crystal, a metal layer is similarly formed on the surface of the metal matrix composite material substrate by vapor deposition or sputtering. The metal layer is preferably indium, aluminum, gold, silver and alloys thereof. The characteristics required of the metal matrix composite material substrate are (1) strength sufficient to withstand bonding, and (2) that there are no inclusions such as voids and foreign matters on the bonding surface and the bonding surface is flat. In order to satisfy the condition (1), the three-point bending strength of the metal matrix composite material substrate is 50 MPa or more, preferably 200 MPa or more. In order to satisfy the condition (2), the surface roughness (Ra) of the metal matrix composite material substrate is 0.01 to 0.5 μm, preferably 0.01 to 0.2 μm.

  The joining of the III-V semiconductor crystal and the metal matrix composite material substrate is performed by heating in a state where the joining surfaces are combined while applying pressure as necessary. Although heating temperature changes with kinds of metal layer, generally it is 250 to 550 degreeC. The pressure for pressurization is generally 2 to 20 MPa.

Since the metal matrix composite material substrate is used while being joined to a III-V group semiconductor crystal, it is important that the difference in linear thermal expansion coefficient between the two materials is small. Therefore, it is preferable linear thermal expansion coefficient of the temperature 40 ° C. to 150 DEG ° C. of metal matrix composite material substrate is ^{4 × 10 -6 / K~9 × 10} -6 / K. More preferably ^{4 × 10 -6 / K~7 × 10} -6 / K. If the linear thermal expansion coefficient at a temperature 40 ° C. to 150 DEG ° C. of metal matrix composite material substrate is out of the range of ^{4 × 10 -6 / K~9 × 10} -6 / K, III-V group bonded semiconductor crystal or Due to the difference in linear thermal expansion coefficient with the growth substrate, warpage may occur after bonding, peeling of the bonding layer may occur when used as an LED light emitting element, or the III-V group semiconductor crystal may be broken. Absent.

  The metal matrix composite material substrate of the present invention serves as a holding substrate for the LED light emitting element. Most of the heat generated in the III-V semiconductor device is radiated through the substrate, and the substrate is required to have high heat dissipation characteristics. For this reason, it is preferable that the heat conductivity in the temperature of 25 degreeC of a metal-matrix composite material board | substrate is 100-300 W / mK, More preferably, it is 150-300 W / mK. If the thermal conductivity is less than 100 W / mK, the heat generated in the III-V group semiconductor device cannot be sufficiently dissipated, and particularly in a high-power LED that needs to pass a large current, the temperature of the device increases and the luminous efficiency And the accompanying decrease in device life are undesirable. On the other hand, the upper limit value of the thermal conductivity is not limited in terms of characteristics, but the substrate material becomes extremely expensive.

From the viewpoint of heat dissipation, it is preferable that the thickness of the metal matrix composite substrate is thin. On the other hand, a certain plate thickness is required because strength that can withstand the holding of the III-V group semiconductor element and the handling at the time of manufacturing the LED light emitting element is necessary. The plate thickness of the metal matrix composite material substrate is preferably 0.05 to 1.0 mm, more preferably 0.05 mm to 0.3 mm. If the thickness of the metal matrix composite substrate exceeds 1 mm, the heat dissipation characteristics of the LED light-emitting element deteriorate, which is not preferable. If it is less than 0.05 mm, the strength is weak and handling properties cannot be obtained, which is not preferable. The metal matrix composite material substrate of the present invention can be thinned by polishing or the like, if necessary, after bonding with a III-V semiconductor crystal.

In the present invention, the single crystal growth substrate is removed after the III-V group semiconductor crystal and the metal matrix composite substrate are bonded via the metal layer. In general, the single crystal growth substrate is removed by irradiating a laser from the substrate side. In addition, the single crystal growth substrate can be removed by polishing or etching. The III-V semiconductor crystal surface from which the single crystal growth substrate has been removed is subjected to surface polishing and etching as necessary to finish the surface shape as desired, and then electrodes are formed by a technique such as vapor deposition or sputtering. . Further, it is cut into a predetermined shape by laser cutting or dicing to manufacture an LED light emitting element.

The metal matrix composite material substrate of the present invention requires chemical resistance in the LED light emitting device manufacturing process. Specifically, a 5N HCl solution at a temperature of 25 ° C. and a 10N NaOH solution at a temperature of 75 ° C. The total weight reduction amount per unit area of at least one main surface when immersed in each of for 1 minute is preferably 0.2 mg / cm ² or less, more preferably 0.1 mg / cm ² or less. . If the weight loss per unit area when immersed in a 5N HCl solution at a temperature of 25 ° C and a 10N NaOH solution at a temperature of 75 ° C for 1 minute exceeds 0.2 mg / cm ² , This is not preferable because a decrease in characteristics such as thermal conductivity due to elution of the metal component occurs, and chipping occurs when cutting into a predetermined shape by laser cutting or dicing, thereby reducing the yield of the LED light emitting elements. In actual use of the metal matrix composite material substrate of the present invention, one principal surface of the metal matrix composite material substrate is bonded to the III-V group semiconductor crystal via the metal layer, so that the non-bonded surface has the above-described resistance. Any material that satisfies the chemical characteristics may be used.

In the metal matrix composite material of the present invention, the substrate itself has conductivity. For this reason, an electrode can be formed on both surfaces of the III-V semiconductor crystal which comprises LED. When an insulating material such as a sapphire substrate is used as the substrate, it is necessary to remove part of the upper p-type or n-type III-V group semiconductor crystal by etching or the like to form electrodes on the same surface side. In the present invention, the manufacturing process of the LED light emitting element can be reduced. Further, since it is not necessary to form an electrode by removing a part of the p-type or n-type III-V semiconductor crystal by etching or the like, the amount of light emission per unit area of the LED light-emitting element can be increased. . The volume resistivity of the metal matrix composite material of the present invention is preferably 10 ⁻⁹ to 10 ⁻⁵ Ω · m. When the volume resistivity exceeds 10 ⁻⁵ Ω · m, the luminous efficiency is lowered, which is not preferable. The lower limit of the volume resistivity is not limited in terms of characteristics, but is generally 10 ⁻⁹ Ω · m or more from the material composition.

The metal matrix composite manufacturing methods are roughly classified into two types: an impregnation method and a powder metallurgy method. Of these, what is actually commercialized in terms of characteristics such as thermal conductivity is the impregnation method. There are various impregnation methods, and there are a method performed at normal pressure and a method performed under high pressure (high pressure forging method). High pressure forging methods include a molten metal forging method and a die casting method. A method suitable for the present invention is a high-pressure forging method in which impregnation is performed under high pressure, and a molten forging method is preferable to obtain a dense composite having excellent characteristics such as thermal conductivity. The molten metal forging method is a method in which a ceramic material or a compact is loaded into a high-pressure vessel, and a molten material such as an aluminum alloy is impregnated at high temperature and high pressure to obtain a composite material.

Hereafter, the example of a manufacturing method by the molten metal forging method is demonstrated. It is necessary to use a material having a high thermal conductivity and a low linear thermal expansion coefficient as the raw material ceramics. In the present invention, silicon carbide is used. The metal matrix composite material of the present invention can adjust the thermal conductivity and the linear thermal expansion coefficient by compounding silicon carbide and an aluminum alloy. The metal matrix composite material of the present invention is a composite material containing 50 to 90% by volume of silicon carbide and the balance being made of an aluminum alloy. The silicon carbide content is preferably 70 to 85% by volume. If the content of silicon carbide is less than 50% by volume, the linear thermal expansion coefficient of the obtained metal matrix composite material becomes large, which is not preferable as a substrate material for an LED light emitting element. On the other hand, if the silicon carbide content exceeds 90% by volume, the aluminum alloy cannot be sufficiently impregnated at the time of compounding, and as a result, the thermal conductivity is lowered, which is not preferable.

Ceramics can be compounded as a powder, but a porous body (hereinafter referred to as a preform) having a porosity of 10 to 50% by volume by forming a molded body using an inorganic binder or by performing a sintering process. ) Is preferably combined. The porosity of the preform is adjusted by adjusting the particle size of the raw material powder, molding pressure, sintering conditions, and the like. The preform can be molded by a general ceramic powder molding method such as press molding or cast molding. Further, the preform is processed into a flat plate shape or a cylindrical shape as needed. Furthermore, in the present invention, it is preferable to use a preform having a three-point bending strength of 50 MPa or more in order to process into a plate shape having a plate thickness of 0.05 to 1.0 mm. When the strength of the preform is low, warping may occur when the plate thickness is processed to a plate shape of 0.05 to 1.0 mm by grinding or the like.

  The preform is fixed with a jig or the like coated with a release agent, and a plurality of layers are laminated and connected with bolts and nuts to form a laminated body. As a jig for fixing the preform, an iron or graphite jig can be used. Moreover, each jig | tool can also be laminated | stacked on both sides of the release plate which apply | coated the mold release agent, and it can also be set as a laminated body. As the release plate, a stainless plate or a ceramic plate can be used, and there is no particular limitation as long as it is a dense body that is not impregnated with an aluminum alloy by a molten metal forging method. Moreover, about the mold release agent apply | coated to a jig | tool or a mold release plate, mold release agents, such as graphite, boron nitride, an alumina, can be used. Furthermore, it is preferable to apply a release agent after coating the surface of a jig or a release plate with alumina sol or the like.

  The obtained laminate is heated at a temperature of 600 to 800 ° C., and one or two or more are placed in a high-pressure vessel, and the aluminum alloy is heated to the melting point or more as quickly as possible to prevent the temperature of the laminate from decreasing. A metal matrix composite material is obtained by supplying molten metal and pressurizing it with a pressure of 30 MPa or more, and impregnating the aluminum alloy in the voids of the preform. For the purpose of removing distortion during impregnation, the impregnated product may be annealed.

  When the heating temperature of the laminated body is less than 600 ° C., the aluminum alloy is not sufficiently combined, and the properties such as the thermal conductivity of the obtained metal matrix composite material are deteriorated. On the other hand, when the heating temperature exceeds 800 ° C., the surface of the ceramic powder is oxidized at the time of compounding with the aluminum alloy, and the properties such as thermal conductivity of the obtained metal matrix composite material are deteriorated. Furthermore, regarding the pressure at the time of impregnation, if it is less than 30 MPa, the composite of the aluminum alloy becomes insufficient, and the properties such as the thermal conductivity of the resulting metal matrix composite material are undesirably lowered. Preferably, the impregnation pressure is 50 MPa or more.

The aluminum alloy in the metal matrix composite of the present invention is an aluminum alloy containing 70% by mass or more of aluminum. If the aluminum content is less than 70% by mass, the thermal conductivity of the aluminum alloy is lowered, which is not preferable. The aluminum alloy preferably has a melting point as low as possible in order to sufficiently penetrate into the voids of the preform when impregnated. Examples of such an aluminum alloy include an aluminum alloy containing 5 to 25% by mass of silicon. Further, it is preferable to contain magnesium because the bond between the ceramic particles and the metal portion becomes stronger. The metal components other than aluminum, silicon, and magnesium in the aluminum alloy are not particularly limited as long as the characteristics do not change extremely. For example, copper or the like may be included.

Next, an example of a method for processing the obtained metal matrix composite material will be described. When the obtained metal matrix composite has a columnar shape, the outer shape is processed to a predetermined size using a diamond grindstone with a cylindrical grinder or the like, and then the final shape is reduced to 0. Cut to a thickness of about 1 to 0.5 mm. The cutting method is not particularly limited, but it is preferable to cut with a multi-wire saw having a small cutting margin and suitable for mass production. Cutting with a multi-wire saw can employ processing using a loose abrasive type and a wire to which an abrasive such as diamond is attached. The plate-like metal matrix composite after the cutting process is a processing machine such as a double-sided grinding machine, a rotary grinding machine, a surface grinding machine, a lapping machine, and has a plate thickness of 0.05 to 1.0 mm and a surface roughness ( Surface processing is performed so that Ra) becomes 0.01 to 1 μm. In the surface processing, in order to further reduce the surface roughness, the surface processing may be performed by a lapping machine after the surface processing is performed by a double-side grinding machine, a rotary grinding machine, a surface grinding machine, or the like. In addition, when the metal matrix composite material substrate of the present invention is polished after bonding to the III-V semiconductor crystal in the manufacturing process of the LED light emitting element, surface processing is performed only on one side (bonding surface) to a predetermined surface roughness. Sometimes.

When the obtained metal matrix composite is plate-like, the thickness is 0.05 to 1.0 mm and the surface roughness is a processing machine such as a double-side grinding machine, a rotary grinding machine, a surface grinding machine, or a lapping machine. Surface processing is performed so that (Ra) becomes 0.01 to 1 μm, and then outer periphery processing is performed in a predetermined shape by a water jet processing machine, an electric discharge processing machine, a laser processing machine, a dicing machine, a cylindrical grinding machine, or the like. When the obtained metal matrix composite is plate-shaped, the outer periphery is processed into a predetermined shape with a water jet machine, electric discharge machine, laser machine, dicing machine, cylindrical grinder, etc., and then a double-side grinder, Surface processing is performed with a processing machine such as a rotary grinder, a surface grinder, or a lapping machine so that the plate thickness is 0.05 to 1.0 mm and the surface roughness (Ra) is 0.01 to 1 μm. You can also.

Next, after washing the surface of the plate-like metal matrix composite material, an aluminum layer having a thickness of 0.05 to 2.0 μm is formed on the surface. If the thickness of the aluminum layer is less than 0.05 μm, an unattached part of the aluminum layer is generated, or the aluminum layer reacts during plating pretreatment, etc., and an unplated part is generated due to the generation of pinholes, resulting in reduced chemical resistance. It is not preferable. On the other hand, if the aluminum layer thickness exceeds 2.0 μm, the linear thermal expansion coefficients of the aluminum layer and the metal matrix composite material are different, so that stress and peeling occur due to the difference in thermal expansion between the two materials. The aluminum layer thickness is more preferably 0.3 to 0.6 μm.

As a formation method of an aluminum layer, it forms in 0.05-2.0 micrometers in thickness by a vapor deposition method or sputtering method.

In the vapor deposition method, it is difficult to form an aluminum layer on the outer peripheral portion, and chemical resistance can be further improved by performing a plating treatment or the like on the outer peripheral portion in advance.

The aluminum alloy constituting the aluminum layer is pure aluminum or an aluminum alloy containing 70% by mass or more of aluminum. If the aluminum content is less than 70% by mass, Ni plating with sufficient adhesion by the zincate treatment cannot be performed, which is not preferable. The metal components other than aluminum and silicon in the aluminum alloy are not particularly limited as long as the characteristics do not change extremely. For example, magnesium, copper, and the like may be included.

  Moreover, in this invention, in order to improve the adhesiveness of a metal matrix composite material substrate and an aluminum layer, heat processing are performed at a temperature of 460-650 degreeC for 1 minute or more in nitrogen, argon, hydrogen, helium, or a vacuum atmosphere. When the treatment is performed in an oxidizing atmosphere, an oxide film is formed on the surface and subsequent plating defects occur, which is not preferable. The temperature is preferably 480-570 ° C. When the temperature is 460 ° C. or lower, the adhesion between the metal matrix composite material substrate and the aluminum layer is deteriorated. When the temperature is 650 ° C. or higher, the aluminum layer is dissolved and the surface roughness is deteriorated.

  Next, the metal matrix composite material substrate on which the aluminum layer is formed has a Ni plating layer having a thickness of 0.5 to 5.0 μm and a thickness of 0.05 to 2.0 μm by electroless plating or electroplating on the surface. The gold plating layer is formed. When the Ni plating layer thickness is 0.5 μm or less, pinholes are generated and chemical resistance is lowered, which is not preferable. On the other hand, when the Ni plating layer thickness is 5.0 μm or more, the thermal conductivity characteristics are lowered and the electric resistance is increased. When the thickness of the gold plating layer is 0.05 μm or less, pinholes are generated and chemical resistance is lowered, which is not preferable. On the other hand, when the thickness of the gold plating layer is 2.0 μm or more, the cost increases, which is not preferable.

  Examples of the pretreatment for plating include zincate treatment, palladium treatment, and the like, but zincate treatment capable of plating with adhesion to aluminum is more preferable.

Alternatively, an aluminum layer is formed, and a metal layer of 0.1 to 2.0 μm of gold or the like is formed on the surface of the metal matrix composite material substrate that has been subjected to heat treatment by a vapor deposition method or a sputtering method. If a metal layer does not react with the chemical | medical solution used in a process, there will be no restriction | limiting.

Example 1
<Preparation of LED light-emitting element holding substrate>
1800 g of silicon carbide (hereinafter referred to as SiC) powder A (manufactured by Taiyo Random Co., Ltd., NG-60, average particle diameter 200 μm), silicon carbide powder B (manufactured by Taiyo Random Co., Ltd., NG-600, average particle diameter 20 μm) 900 g, 300 g of silicon carbide powder C (manufactured by Taiyo Random Co., Ltd., NC-6000, average particle size 2 μm) and 150 g of a molded binder (methyl cellulose, manufactured by Shin-Etsu Chemical Co., Ltd., “Metroses”) are weighed and stirred for 30 minutes. After mixing, it was press-molded into a cylindrical shape with a size of Φ55 mm × 110 mm at a surface pressure of 10 MPa, and then CIP-molded at a molding pressure of 100 MPa to produce a compact.

  The obtained molded body was degreased in an air atmosphere at a temperature of 600 ° C. for 2 hours and then calcined in an argon atmosphere at a temperature of 2100 ° C. for 2 hours to produce a SiC preform having a porosity of 20% by volume. The obtained SiC preform was processed into a shape having an outer dimension of Φ52 mm × 100 mm using a diamond grindstone at a machining center. Further, a three-point bending strength measurement specimen (3 mm × 4 mm × 40 mm) was prepared by grinding, and the three-point bending strength was measured. The three-point bending strength was 120 MPa.

A boron nitride mold release agent was applied to the obtained SiC preform and inserted into a cylindrical graphite jig having an outer dimension of 70 mm × 70 mm × 100 mm (inner diameter: Φ52.5 mm × 100 mm) to obtain a structure. . Next, a release plate is prepared by applying a graphite release material to a 70 mm × 100 mm × 0.8 mmt stainless plate, and the four structures are released so as to have a shape of 140.8 mm × 140.8 mm × 100 mm. Laminated with the plates sandwiched, 12 mm thick iron plates were placed on both sides and connected with 8 M10 bolts to form one laminate. Next, the laminate is preheated to a temperature of 700 ° C. in an electric furnace and then placed in a pre-heated press mold having an inner diameter of Φ400 mm × 300 mmH, and contains 12% by mass of silicon and 1% by mass of magnesium. The molten metal (temperature: 800 ° C.) was poured and pressurized at 100 MPa for 25 minutes to impregnate the SiC preform with the aluminum alloy. After cooling to room temperature, it was cut along the shape of the release plate with a wet band saw, the release plate was peeled off, and the graphite jig part was removed with a lathe to obtain a metal matrix composite material having a shape of Φ52 mm × 100 mm. The obtained metal matrix composite material was annealed at a temperature of 530 ° C. for 3 hours in order to remove strain at the time of impregnation.

Next, from the obtained metal matrix composite material, a thermal expansion coefficient measurement specimen (diameter 3 mm length 10 mm), a thermal conductivity measurement specimen (25 mm × 25 mm × 1 mm), and three-point bending strength measurement by grinding. Test specimens (3 mm × 4 mm × 40 mm) and volume resistivity test specimens (50 mm × 50 mm × 5 mm) were produced. Using each test specimen, the thermal expansion coefficient at a temperature of 25 ° C. to 150 ° C. was measured with a thermal dilatometer (manufactured by Seiko Denshi Kogyo; TMA300), and the thermal conductivity at a temperature of 25 ° C. was measured with a laser flash method (manufactured by ULVAC; TC3000), a three-point bending strength was measured with a bending strength tester, and a volume resistivity was measured with a four-terminal method (based on JIS R1637). As a result, the thermal expansion coefficient at a temperature of 40 ° C. to 150 ° C. is 4.9 × 10 ⁻⁶ / K, the thermal conductivity at a temperature of 25 ° C. is 250 W / mK, the three-point bending strength is 350 MPa, and the volume resistivity is 8 ×. 10 ⁻⁷ Ω · m.

  The outer circumference of the metal matrix composite material was processed into a cylindrical shape of Φ50.8 mm × 100 mm using a diamond grindstone with a cylindrical grinder. The obtained columnar metal matrix composite material was cut into a disk shape having a plate thickness of 0.3 mm at a cutting cutting speed of 0.2 mm / min using diamond abrasive grains with a multi-wire saw. The disk-shaped metal matrix composite material is ground to a plate thickness of 0.22 mm using a # 600 diamond grindstone with a double-side grinding machine, and then the diamond abrasive grains are used with a lapping machine to obtain a plate thickness of 0.2 mm. Then, ultrasonic cleaning was performed in pure water and then in isopropyl alcohol, followed by drying to produce a metal matrix composite substrate. As a result of measuring the surface roughness (Ra) with a surface roughness meter, it was Ra 0.05 μm.

  Next, an aluminum layer having a thickness of 0.4 μm was formed on the surface of the metal matrix composite material by vapor deposition, and heat treatment was performed at 500 ° C. for 30 minutes in a nitrogen atmosphere. Next, electroless Ni—P and electrogold plating were performed on the metal matrix composite material substrate on which the aluminum layer was formed, to form a plating layer of 1.3 μm (Ni—P: 1 μm + Au: 0.3 μm) on the surface. The characteristic value of the obtained metal matrix composite material substrate was calculated from the thickness ratio of the physical property value of the plating layer metal and the physical property value of the metal matrix composite material substrate before plating. The results are shown in Table 1. Further, the metal matrix composite material after the plating film is formed is immersed in a 5N HCl solution at a temperature of 25 ° C. and a 10N NaOH solution at a temperature of 75 ° C. for 1 minute, and the amount of weight reduction per unit area by each treatment is determined. It was measured. Furthermore, the surface roughness (Ra) of the metal matrix composite material substrate after plating was measured with a surface roughness meter. The results are shown in Table 2.

<Production of LED light-emitting element>
On a single crystal sapphire substrate having a thickness of 0.5 mm, ammonia gas and trimethyl gallium are used, and a mixed gas of hydrogen and nitrogen is used as a carrier gas, and the temperature is 1100 ° C. by MOCVD (1) to (4 ) Single crystal GaN was grown to a thickness of 4 μm. FIG. 1 shows the structure.
(1) n-type GaN buffer layer 2
(2) n-type GaN semiconductor layer 3
(3) GaN active layer (light emitting layer) 4
(4) p-type GaN semiconductor layer 5

Next, a silver / tin alloy was deposited to a thickness of 2 μm on the surface of the p-type GaN semiconductor layer by vacuum deposition. On the other hand, a silver / tin alloy was deposited to a thickness of 2 μm on the surface of one side of the LED light emitting element holding substrate in the same manner. Both substrates were laminated as shown in FIG. 1 where the silver / tin alloy layer was in contact, and held at a temperature of 400 ° C. under a pressure of 5 MPa for 5 minutes for bonding. The obtained bonded body was irradiated with a nitrogen gas laser from the sapphire substrate side so that the output was 40 MW / cm ^2, and the sapphire substrate was peeled off. The n-type GaN buffer layer was decomposed into Ga and nitrogen by laser irradiation, and the sapphire substrate could be peeled off by the generated nitrogen gas.

Thereafter, the n-type GaN buffer layer exposed on the surface was removed by etching, and then a transparent conductor layer of indium tin oxide was formed. Then, Au was vapor-deposited as an n-type electrode, and it was set as each LED light emitting element by dicing. It was confirmed that the obtained LED light emitting element was able to suppress a decrease in luminous efficiency due to an increase in element temperature due to heat radiation from the holding substrate.

(Examples 2-8, Comparative Examples 1-3)
An aluminum-forming metal obtained by forming 0.4 μm of an aluminum layer on the metal matrix composite material of Φ50.8 mm × 0.2 mmt produced in Example 1 by vapor deposition or sputtering, and performing heat treatment at 500 ° C. for 30 minutes in a nitrogen atmosphere. A plating film shown in Table 4 was formed on the surface of the base composite material. Table 3 shows the characteristic values of the obtained metal matrix composite material. Further, the metal matrix composite material after the plating film is formed is immersed in a 5N HCl solution at a temperature of 25 ° C. and a 10N NaOH solution at a temperature of 75 ° C. for 1 minute, and the amount of weight reduction per unit area by each treatment is determined. It was measured. Further, the surface roughness (Ra) of the metal matrix composite material after the plating film was formed was measured with a surface roughness meter. The results are shown in Table 4.

(Examples 9 to 12, Comparative Example 4)
An aluminum-forming metal matrix composite material obtained by forming 0.4 μm of an aluminum layer on the metal matrix composite material of Φ50.8 mm × 0.2 mmt produced in Example 1 by vapor deposition and performing heat treatment at 500 ° C. for 30 minutes in a nitrogen atmosphere. The metal layer shown in Table 6 was formed on the surface. Table 5 shows the characteristic values of the obtained metal matrix composite. Further, the metal matrix composite material after the plating film is formed is immersed in a 5N HCl solution at a temperature of 25 ° C. and a 10N NaOH solution at a temperature of 75 ° C. for 1 minute, and the amount of weight reduction per unit area by each treatment is determined. It was measured. Further, the surface roughness (Ra) of the metal matrix composite material after the plating film was formed was measured with a surface roughness meter. The results are shown in Table 6.

(Examples 13 to 19, Comparative Examples 5 to 7)
<Preparation of LED light-emitting element holding substrate>
1800 g of silicon carbide (hereinafter referred to as SiC) powder A (manufactured by Taiyo Random Co., Ltd., NG-60, average particle diameter 200 μm), silicon carbide powder B (manufactured by Taiyo Random Co., Ltd., NG-600, average particle diameter 20 μm) 900 g, 300 g of silicon carbide powder C (manufactured by Taiyo Random Co., Ltd., NC-6000, average particle size 2 μm) and 150 g of a molded binder (methyl cellulose, manufactured by Shin-Etsu Chemical Co., Ltd., “Metroses”) are weighed and stirred for 30 minutes. After mixing, it was press-molded at a surface pressure of 30 MPa into a cylindrical shape with a size of Φ55 mm × 110 mm to produce a molded body.

  The obtained molded body was degreased for 2 hours at a temperature of 600 ° C. in an air atmosphere, and then fired for 2 hours at a temperature of 1950 ° C. in an argon atmosphere to produce a SiC preform having a porosity of 30% by volume. The obtained SiC preform was processed into a shape having an outer dimension of Φ52 mm × 100 mm using a diamond grindstone at a machining center. Further, a three-point bending strength measurement specimen (3 mm × 4 mm × 40 mm) was prepared by grinding, and the three-point bending strength was measured. The three point bending strength was 80 MPa.

A boron nitride mold release agent was applied to the obtained SiC preform and inserted into a cylindrical iron jig having an outer dimension of 70 mm × 70 mm × 50 mm (inner diameter: Φ52.5 mm × 50 mm) to obtain a structure. Next, a release plate is produced by applying a graphite release material to a 70 mm × 70 mm × 0.8 mmt stainless plate, and the four structures are released so as to have a shape of 140.8 mm × 140.8 mm × 50 mm. They were stacked with a plate in between. A ceramic board having a ceramic fiber content of 10% by volume and a thickness of 10 mm is sandwiched between both sides, an iron plate having a thickness of 12 mm is disposed, and connected with eight M10 bolts to form a single laminate. Next, the laminate is preheated to a temperature of 700 ° C. in an electric furnace and then placed in a pre-heated press mold having an inner diameter of Φ400 mm × 300 mmH, and contains 12% by mass of silicon and 1% by mass of magnesium. The molten metal (temperature: 800 ° C.) was poured and pressurized at 100 MPa for 25 minutes to impregnate the SiC preform with the aluminum alloy. After cooling to room temperature, it was cut along the shape of the release plate with a wet band saw, the release plate was peeled off, and the graphite jig part was removed with a lathe to obtain a metal matrix composite material having a shape of Φ52 mm × 100 mm. The obtained metal matrix composite material was annealed at a temperature of 530 ° C. for 3 hours in order to remove strain at the time of impregnation.

Next, from the obtained metal matrix composite material, a thermal expansion coefficient measurement specimen (diameter 3 mm length 10 mm), thermal conductivity measurement specimen (25 mm × 25 mm × 1 mm), and three-point bending strength measurement by grinding. Test specimens (3 mm × 4 mm × 40 mm) and volume resistivity test specimens (50 mm × 50 mm × 5 mm) were produced. Measurement was performed in the same manner as in Example 1 using each specimen. As a result, the thermal expansion coefficient at a temperature of 40 ° C. to 150 ° C. is 6.9 × 10 ⁻⁶ / K, the thermal conductivity at a temperature of 25 ° C. is 220 W / mK, the three-point bending strength is 380 MPa, and the volume resistivity is 4 ×. 10 ⁻⁷ Ω · m.

  The obtained metal matrix composite material was peripherally processed into a cylindrical shape of Φ50.8 mm × 50 mm using a diamond grindstone with a cylindrical grinder. Next, the cylindrical metal matrix composite material was cut into a disk shape with a plate thickness of 0.25 mm at a cutting cutting speed of 5 mm / min using a diamond blade with an inner peripheral cutting machine. The disk-shaped metal matrix composite material was ground to a plate thickness of 0.2 mm using a # 800 diamond grindstone with a double-side grinding machine to prepare a metal matrix composite material substrate.

Next, after cleaning the surface of this metal matrix composite material, an aluminum layer was formed by the vapor deposition method under the conditions shown in Table 7. Next, electroless Ni—P and electrogold plating were performed on the metal matrix composite material substrate on which the aluminum layer was formed, to form a plating layer of 1.3 μm (Ni—P: 1 μm + Au: 0.3 μm) on the surface. Table 7 shows the characteristic values of the obtained metal matrix composite. Further, the metal matrix composite material after the plating film is formed is immersed in a 5N HCl solution at a temperature of 25 ° C. and a 10N NaOH solution at a temperature of 75 ° C. for 1 minute, and the amount of weight reduction per unit area by each treatment is determined. It was measured. Further, the surface roughness (Ra) of the metal matrix composite material after the plating film was formed was measured with a surface roughness meter. The results are shown in Table 8.

<Production of LED light-emitting element>
Next, preparation examples of LED light emitting devices using the LED light emitting device holding substrates of Examples 13 to 19 will be described.
After forming a growth substrate by forming a SiC layer with a thickness of 2 μm on a single crystal Si substrate having a thickness of 0.5 mm by a CVD method, ammonia gas and gallium chloride are used, hydrogen gas is used as a carrier gas, and temperature is increased. The GaN single crystals (1) to (3) were grown to a thickness of 4 μm by HVPE at 1050 ° C. FIG. 3 shows the structure.
(1) n-type GaN semiconductor layer 3
(2) GaN active layer (light emitting layer) 4
(3) p-type GaN semiconductor layer 5

  Next, silver was deposited to a thickness of 0.5 μm on the surface of the p-type GaN semiconductor layer by a vacuum deposition method, and then an Au / tin alloy was deposited to a thickness of 1.5 μm. On the other hand, Au / tin alloy was vapor-deposited to a thickness of 1.5 μm on the surface of one side of the LED light emitting element holding substrates of Examples 13 to 19 in the same manner. The two substrates were laminated as shown in FIG. 3 where the Au / tin alloy layer was in contact, and held at a temperature of 500 ° C. under a pressure of 5 MPa for 5 minutes for bonding. In the obtained bonded body, the single crystal Si layer was removed by etching by acid treatment, and then the SiC layer was completely removed by grinding.

Thereafter, the surface of the exposed n-type GaN layer was roughened by etching, and then a transparent conductor layer of indium tin oxide was formed. Next, Au was vapor-deposited as an n-type electrode, and individual LED light-emitting elements were formed by laser processing. It was confirmed that the obtained LED light emitting element was able to suppress a decrease in luminous efficiency due to an increase in element temperature due to heat radiation from the holding substrate.

(Examples 20 to 24, Comparative Example 8)
<Preparation of LED light-emitting element holding substrate>
1300 g of silicon carbide powder D (manufactured by Taiyo Random Co., Ltd., NG-80, average particle size: 150 μm), 700 g of silicon carbide powder E (manufactured by Yakushima Electric Works, GC-1000F, average particle size: 10 μm), silica sol (Nissan Chemical Co., Ltd.) (Product: Snowtex) 300 g was weighed and mixed with a stirrer / mixer for 30 minutes, and then pressed into a cylindrical shape with a size of Φ60 mm × 55 mm at a surface pressure of 30 MPa to prepare a molded body. The obtained molded body was dried at a temperature of 120 ° C. for 1 hour and then calcined at a temperature of 1400 ° C. for 2 hours in a nitrogen atmosphere to obtain a SiC preform having a porosity of 35% by volume. The obtained SiC preform was processed into a shape having an outer dimension of Φ52 mm × 50 mm using a diamond grindstone at a machining center. From the obtained SiC preform, a three-point bending strength measurement specimen (3 mm × 4 mm × 40 mm) was prepared by grinding, and the three-point bending strength was measured. As a result, the three-point bending strength was 50 MPa.

A boron nitride mold release agent was applied to the obtained SiC preform and inserted into a cylindrical iron jig having an outer dimension of 70 mm × 70 mm × 50 mm (inner diameter: Φ52.5 mm × 50 mm) to obtain a structure. Next, a release plate is produced by applying a graphite release material to a 70 mm × 70 mm × 0.8 mmt stainless plate, and the four structures are released so as to have a shape of 140.8 mm × 140.8 mm × 50 mm. They were stacked with a plate in between. A ceramic board having a ceramic fiber content of 10% by volume and a thickness of 10 mm is sandwiched between both sides, an iron plate having a thickness of 12 mm is disposed, and connected with eight M10 bolts to form a single laminate. Next, the laminate is preheated to a temperature of 700 ° C. in an electric furnace and then placed in a pre-heated press mold having an inner diameter of Φ400 mm × 300 mmH, and contains 12% by mass of silicon and 1% by mass of magnesium. The molten metal (temperature: 800 ° C.) was poured and pressurized at 100 MPa for 25 minutes to impregnate the SiC preform with the aluminum alloy. After cooling to room temperature, it was cut along the shape of the release plate with a wet band saw, the release plate was peeled off, and the graphite jig part was removed with a lathe to obtain a metal matrix composite material having a shape of Φ52 mm × 100 mm. The obtained metal matrix composite material was annealed at a temperature of 530 ° C. for 3 hours in order to remove strain at the time of impregnation.

Next, from the obtained metal matrix composite material, a thermal expansion coefficient measurement specimen (diameter 3 mm length 10 mm), thermal conductivity measurement specimen (25 mm × 25 mm × 1 mm), and three-point bending strength measurement by grinding. Test specimens (3 mm × 4 mm × 40 mm) and volume resistivity test specimens (50 mm × 50 mm × 5 mm) were produced. Measurement was performed in the same manner as in Example 1 using each specimen. As a result, the thermal expansion coefficient at a temperature of 40 ° C. to 150 ° C. is 7.6 × 10 ⁻⁶ / K, the thermal conductivity at a temperature of 25 ° C. is 200 W / mK, the three-point bending strength is 400 MPa, and the volume resistivity is 3 ×. 10 ⁻⁷ Ω · m.

  The obtained metal matrix composite material was peripherally processed into a cylindrical shape of Φ50.8 mm × 50 mm using a diamond grindstone with a cylindrical grinder. Next, the cylindrical metal matrix composite material was cut into a disk shape with a plate thickness of 0.25 mm at a cutting cutting speed of 5 mm / min using a diamond blade with an inner peripheral cutting machine. The disk-shaped metal matrix composite material was ground to a plate thickness of 0.2 mm using a # 800 diamond grindstone with a double-side grinding machine to prepare a metal matrix composite material substrate.

Next, after cleaning the surface of this metal matrix composite material, an aluminum layer was formed by the vapor deposition method under the conditions shown in Table 9. Next, electroless Ni—P and electrogold plating were performed on the metal matrix composite material substrate on which the aluminum layer was formed, to form a plating layer of 1.3 μm (Ni—P: 1 μm + Au: 0.3 μm) on the surface. Table 9 shows the characteristic values of the obtained metal matrix composite. Further, the metal matrix composite material after the plating film is formed is immersed in a 5N HCl solution at a temperature of 25 ° C. and a 10N NaOH solution at a temperature of 75 ° C. for 1 minute, and the amount of weight reduction per unit area by each treatment is determined. It was measured. Further, the surface roughness (Ra) of the metal matrix composite material after the plating film was formed was measured with a surface roughness meter. The results are shown in Table 10.

  An LED light-emitting element was produced using the LED light-emitting element holding substrate obtained in Examples 20 to 24, and it was confirmed that a decrease in luminous efficiency due to an increase in element temperature was suppressed by heat dissipation from the holding substrate. An LED light emitting device was manufactured using Comparative Example 8, but the aluminum alloy in the holding substrate reacted to the acid and alkali solution used in the process, and the plating film was peeled off and the characteristics were deteriorated. The generated heat could not be sufficiently dissipated, resulting in a decrease in luminous efficiency.

The LED light-emitting element holding substrate of the present invention is a high thermal conductivity holding substrate having a low coefficient of linear thermal expansion with a group III-IV semiconductor crystal constituting the LED, and a high-power LED excellent in heat dissipation and reliability. A light-emitting element can be provided. Furthermore, the LED light-emitting element holding substrate of the present invention is excellent in chemical resistance against acid and alkali solutions used in the manufacture of LED light-emitting elements, is conductive, and has both sides of the group III-IV semiconductor crystal constituting the LED. An electrode can be formed on the substrate. Therefore, it is possible to reduce the manufacturing process of the LED light emitting element and increase the light emission amount per unit area, which is effective as a holding substrate for the LED light emitting element.

1) growth substrate 2) nitride buffer layer formed on the growth substrate 3) n-type III-V group semiconductor layer 4) light emitting layer 5) p-type group III-V semiconductor layer 6) metal layer (reflection) layer)
7) Metal layer 8) Metal matrix composite material 9) Transparent conductive layer 10) Surface coating layer 11) Base material

Claims (9)

A metal matrix composite material substrate having a thickness of 0.05 to 1.0 mm obtained by impregnating a silicon carbide porous body with an aluminum alloy is manufactured through the following steps in sequence, and a 5N HCl solution at a temperature of 25 ° C. and 75 ° C. The manufacturing method of the holding | maintenance board | substrate for LED light emitting elements whose weight reduction amount of at least 1 main surface when each immersed in 10 normal NaOH solution of 1 each is 0.2 mg / cm < ² > or less.
(1) A step of forming an aluminum layer having a thickness of 0.05 to 2 μm on the surface of the metal matrix composite substrate by a vapor deposition method or a sputtering method.
(2) A step of heat treatment at a temperature of 460 ° C. to 650 ° C. for 1 minute or more in nitrogen, argon, hydrogen, helium or a vacuum atmosphere.
(3) A step of forming a metal layer on the surface of the aluminum layer according to 1) or 2).
1) A step of forming a metal layer by sequentially forming a Ni plating layer having a thickness of 0.5 to 5 μm and a gold plating layer having a thickness of 0.05 to 2 μm on the surface of the aluminum layer by an electroless plating method or an electroplating method. .
2) A step of forming a metal layer having a thickness of 0.1 to 2 μm on the surface of the aluminum layer by vapor deposition or sputtering. The method for producing a holding substrate for an LED light-emitting element according to claim 1, wherein a porous silicon carbide having a porosity of 10 to 50% by volume and a three-point bending strength of 50 MPa or more is used. Thermal conductivity at a temperature of 25 ° C. is 150 to 300 W / mK, linear thermal expansion coefficient at a temperature of 40 ° C. to 150 ° C. is 4 × 10 ⁻⁶ to 8 × 10 ⁻⁶ / K, three-point bending strength is 50 MPa or more, volume specific 3. The method for producing a holding substrate for an LED light-emitting element according to claim 1, wherein the resistance is 10 ⁻⁹ to 10 ⁻⁵ Ω · m. 4. The method for manufacturing a holding substrate for an LED light-emitting element according to claim 1, wherein the surface roughness (Ra) is 0.01 to 0.5 [mu] m. A silicon carbide porous body is impregnated with an aluminum alloy at an impregnation pressure of 30 MPa or more by a molten metal forging method, and then cut into a plate thickness of 0.05 to 1.0 mm and a surface roughness (Ra) of 0.01 to 0.5 μm. The method for producing a holding substrate for an LED light-emitting element according to claim 1, wherein the method is performed by grinding. The manufacturing method of the LED light emitting element manufactured through the following process one by one.
(1) A step of epitaxially growing a group III-V semiconductor crystal on one main surface of a disk-like or flat plate-like single crystal growth substrate.
(2) The holding substrate for an LED light-emitting device according to any one of claims 1 to 5 is bonded to the III-V group semiconductor crystal surface via a metal layer, and the back surface is any one of laser irradiation, etching, and grinding. The step of removing the single crystal growth substrate by the method.
(3) A step of cutting after performing surface processing of the III-V semiconductor crystal surface and electrode formation. The method for manufacturing an LED light-emitting element according to claim 6, wherein the single crystal growth substrate is selected from the group consisting of single crystal sapphire, single crystal silicon carbide, single crystal GaAs, and single crystal Si. 8. The method for manufacturing an LED light emitting device according to claim 6, wherein the single crystal growth substrate is surface-coated with a material selected from the group consisting of AlN, SiC, GaN, and GaAs. The method for producing an LED light-emitting element according to any one of claims 6 to 8, wherein the III-V semiconductor crystal is any one of GaN, GaAs, and GaP.

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