# US 2018/0026159 A1 · Method for manufacturing light emitting diode device

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- Number: US 2018/0026159 A1
- Document ID: US20180026159A1
- Status: Published application
- Kind: A1
- Application number: 15/650,276
- Filed: 2017-07-14
- Published: 2018-01-25
- Earliest claimed: 2016-07-19
- Assignees: Kabushiki Kaisha Toshiba
- Applicants: Kabushiki Kaisha Toshiba
- Inventors: Ikuo UEMATSU; Makoto Saito; Shinya Ito; Kengo Furutani; Shinichi Sasaki
- Web page: https://patentgrep.com/patent/US20180026159A1

## CPC

- H10H 20/825: containing nitrogen, e.g. GaN
- C01G 15/00: Compounds of gallium, indium or thallium
- H10H 20/01335: {the light-emitting regions comprising nitride materials}
- H10P 90/126: {by chemical etching}
- H10H 20/819: characterised by their shape, e.g. curved or truncated substrates
- H10H: INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

According to one embodiment, a method for manufacturing an LED device includes forming a laminated semiconductor layer including a GaN layer of a first conductivity type, a GaN-based luminous layer, and a GaN layer of a second conductivity type stacked in this order on a surface of a substrate, forming a resist pattern on the laminated semiconductor layer, subjecting the laminated semiconductor layer to reactive ion etching using the resist pattern as a mask to selectively remove the laminated semiconductor layer to form an LED element structure part and an electrode connection region, removing the resist pattern, and treating the substrate including the LED element structure part and the electrode connection region with a first etching residue removing aqueous solution.

## Claims

### Claim 1

A method for manufacturing an LED device comprising:
forming a laminated semiconductor layer including a GaN layer of a first conductivity type, a GaN-based luminous layer, and a GaN layer of a second conductivity type stacked in this order on a surface of a substrate;
forming a resist pattern with a predetermined shape on the laminated semiconductor layer;
subjecting the laminated semiconductor layer to reactive ion etching using the resist pattern as a mask to selectively remove the laminated semiconductor layer so that the GaN layer of the first conductivity type remains to have a predetermined thickness on a surface of the substrate, thereby forming an LED element structure part and an electrode connection region integrated with the GaN layer of the first conductivity type of the structure part on the substrate;
removing the resist pattern; and
treating the substrate including the LED element structure part and the electrode connection region with a first etching residue removing aqueous solution containing a peroxosulfate, a fluorine-containing compound, and an acid for pH adjustment, and possessing a pH value of 0 to 3.

### Claim 2 (depends on 1)

The method of claim 1, wherein the substrate is a sapphire substrate.

### Claim 3 (depends on 1)

The method of claim 1, wherein a reactive gas to be used when the laminated semiconductor layer is subjected to reactive ion etching is a chlorine-based gas.

### Claim 4 (depends on 1)

The method of claim 1, wherein the peroxosulfate in the first etching residue removing aqueous solution is ammonium peroxodisulfate.

### Claim 5 (depends on 4)

The method of claim 4, wherein the ammonium peroxodisulfate is contained in the first etching residue removing aqueous solution at a concentration of 0.01 mol/L to 20 mol/L.

### Claim 6 (depends on 1)

The method of claim 1, wherein the fluorine-containing compound is contained in the first etching residue removing aqueous solution at a concentration of 1×10−4 mol/L to 1×10−2 mol/L.

### Claim 7 (depends on 1)

The method of claim 1, wherein the acid for pH adjustment is sulfuric acid.

### Claim 8 (depends on 1)

The method of claim 1, wherein the liquid temperature of the first etching residue removing aqueous solution is 20 to 35° C.

### Claim 9 (depends on 1)

The method of claim 1, further comprising, after the treatment using the first etching residue removing aqueous solution, carrying out rinsing treatment using a water-soluble organic solvent or pure water.

### Claim 10

A method for manufacturing an LED device comprising:
forming a laminated semiconductor layer including a GaN layer of a first conductivity type, a GaN-based luminous layer, and a GaN layer of a second conductivity type stacked in this order on a surface of a substrate;
forming a resist pattern with a predetermined shape on the laminated semiconductor layer;
subjecting the laminated semiconductor layer to reactive ion etching using the resist pattern as a mask to selectively remove the laminated semiconductor layer so that the GaN layer of the first conductivity type remains to have a predetermined thickness on a surface of the substrate, thereby forming an LED element structure part and an electrode connection region integrated with the GaN layer of the first conductivity type of the structure part on the substrate;
removing the resist pattern;
treating the substrate including the LED element structure part and the electrode connection region with a first etching residue removing aqueous solution containing a peroxosulfate, a fluorine-containing compound, and an acid for pH adjustment, and possessing a pH value of 0 to 3;
forming a protection film on the entire surface of the LED element structure part including the electrode connection region;
forming a resist pattern in which a part corresponding to part of the GaN layer of the second conductivity type of the LED element structure part, and a part corresponding to part of the electrode connection region are opened on the surface of the protection film, on the LED element structure part including the electrode connection region;
subjecting the protection film to reactive ion etching using the resist pattern as a mask to selectively remove the protection film, thereby forming a first extraction hole for a second conductivity type electrode in the protection film on the GaN layer of the second conductivity type of the LED element structure part, and forming a second extraction hole for a first conductivity type electrode in the protection film on the electrode connection region;
removing the resist pattern;
treating the protection film including the first and the second extraction holes with a second etching residue removing aqueous solution containing a peroxosulfate, a fluorine-containing compound, and an acid for pH adjustment, and possessing a pH value of 0 to 3; and
forming a second conductivity type electrode to be connected to the GaN layer of the second conductivity type of the LED element structure part through the first extraction hole and a first conductivity type electrode to be connected to the electrode connection region through the second extraction hole.

### Claim 11 (depends on 10)

The method of claim 10, wherein the substrate is a sapphire substrate.

### Claim 12 (depends on 10)

The method of claim 10, wherein a reactive gas to be used when the laminated semiconductor layer is subjected to reactive ion etching is a chlorine-based gas.

### Claim 13 (depends on 10)

The method of claim 10, wherein each of the peroxosulfates in the first and second etching residue removing aqueous solutions is ammonium peroxodisulfate.

### Claim 14 (depends on 13)

The method of claim 13, wherein the ammonium peroxodisulfate is contained in each of the first and second etching residue removing aqueous solutions at a concentration of 0.01 mol/L to 20 mol/L.

### Claim 15 (depends on 10)

The method of claim 10, wherein the fluorine-containing compound in each of the first and second etching residue removing aqueous solutions is contained in each of the first and second etching residue removing aqueous solutions at a concentration of 1×10−4 mol/L to 1×10−2 mol/L.

### Claim 16 (depends on 10)

The method of claim 10, wherein each of the acids for pH adjustment in the first and second etching residue removing aqueous solutions is sulfuric acid.

### Claim 17 (depends on 10)

The method of claim 10, wherein the liquid temperature of each of the first and second etching residue removing aqueous solutions is 20 to 35° C.

### Claim 18 (depends on 10)

The method of claim 10, further comprising, after each of the treatment processes using the first and second etching residue removing aqueous solutions, further carrying out rinsing treatment using a water-soluble organic solvent or pure water.

### Claim 19 (depends on 10)

The method of claim 10, further comprising, after the treatment using the second etching residue removing aqueous solution, and before forming the protection film, further forming a transparent electrode layer of the second conductivity type on the surface of the GaN layer of the second conductivity type of the LED element structure part.