# US 10,119,200 B2 · Silicon carbide single crystal substrate and process for producing same

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- Number: US 10,119,200 B2
- Document ID: US10119200B2
- Status: Granted
- Kind: B2
- Application number: 14/441,001
- Filed: 2013-11-15
- Published: 2015-09-24
- Granted: 2018-11-06
- Earliest claimed: 2012-11-15
- Assignees: Showa Denko K.K.
- Applicants: Showa Denko K.K.
- Inventors: Shinya Sato; Tatsuo Fujimoto; Hiroshi Tsuge; Masakazu Katsuno
- Web page: https://patentgrep.com/patent/US10119200B2

## CPC

- C30B 23/02: Epitaxial-layer growth
- C30B 23/002: {Controlling or regulating}
- C30B 23/025: {characterised by the substrate}
- C30B 29/36: Carbides
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR

## Abstract

Provided are: a silicon carbide single crystal substrate which is cut out from a silicon carbide bulk single crystal grown by the Physical Vapor Transport method; and a process for producing the same. The number of screw dislocations in one of the semicircle areas of the substrate is smaller than that in the other thereof, namely, the number of screw dislocations in a given area of the substrate is reduced. The semicircle areas of the substrate correspond respectively to the halves of the substrate. The present invention pertains to: a silicon carbide single crystal substrate which is cut out from a silicon carbide bulk single crystal grown by the Physical Vapor Transport method and which is characterized in that the average value of the screw-dislocation densities observed at multiple measurement points in one of the semicircle areas, which correspond respectively to the halves of the substrate, is 80% or less of the average value of screw-dislocation densities observed at multiple measurement points in the other of the semicircle areas; and a process for producing the same.

## Claims

### Claim 1

A method for manufacturing a silicon carbide single crystal by a physical vapor transport method using a seed crystal, the method being characterized by including:
(i) a first growth step of growing a silicon carbide single crystal having a thickness of at least 1 mm at a first growth atmosphere pressure of not lower than 0.13 kPa and not higher than 2.6 kPa and a first growth temperature in which the temperature of the seed crystal is not lower than 2100° C. and not higher than 2400° C.;
(ii) a second growth step of growing the silicon carbide single crystal having a thickness of at least 0.5 mm at a second growth atmosphere pressure of higher than 2.6 kPa and not higher than 65 kPa and a second growth temperature in which the temperature of the seed crystal is not lower than 2100° C. and not higher than 2400° C.; and
(iii) a third growth step of growing the silicon carbide single crystal to a larger thickness than in the first growth step at a third growth atmosphere pressure of not lower than 0.13 kPa and not higher than 2.6 kPa and a third growth temperature in which the temperature of the seed crystal is not lower than 2100° C. and not higher than 2400° C.;
wherein the seed crystal is composed of SiC single crystal and has an off angle θs of more than 0° and not more than 16° relative to (0001) plane,
wherein a constant growth temperature is maintained throughout the steps (i) to (iii).

### Claim 2 (depends on 1)

The method for manufacturing a silicon carbide single crystal according to claim 1, wherein the first and the second growth atmosphere pressures are changed to the second and the third growth atmosphere pressures, respectively, at a pressure changing rate of 13.3 kPa or less per hour.

### Claim 3 (depends on 1)

The method for manufacturing a silicon carbide single crystal according to claim 1, wherein crystal growth rate in the second growth step is 100 μm/hr or less.

### Claim 4

A method for manufacturing a silicon carbide single crystal by a physical vapor transport method using a seed crystal, the method being characterized by including:
(i) a first growth step of growing a silicon carbide single crystal having a thickness of at least 1 mm at a first growth atmosphere pressure of not lower than 0.13 kPa and not higher than 2.6 kPa and a first growth temperature in which the temperature of the seed crystal is not lower than 2100° C. and not higher than 2400° C.;
(ii) a second growth step of growing the silicon carbide single crystal having a thickness of at least 0.5 mm at a second growth atmosphere pressure of higher than 2.6 kPa and not higher than 65 kPa and a second growth temperature in which the temperature of the seed crystal is not lower than 2100° C. and not higher than 2400° C.; and
(iii) a third growth step of growing the silicon carbide single crystal to a larger thickness than in the first growth step at a third growth atmosphere pressure of not lower than 0.13 kPa and not higher than 2.6 kPa and a third growth temperature in which the temperature of the seed crystal is not lower than 2100° C. and not higher than 2400° C.;
wherein the seed crystal is composed of SiC single crystal and has an off angle θs of more than 4° and not more than 16° relative to (0001) plane,
wherein a constant growth temperature is maintained throughout the steps (i) to (iii).