# US 2014/0151716 A1 · Process for the manufacture of a doped iii-n bulk crystal and a free-standing iii-n substrate, and doped iii-n bulk crystal and free-standing iii-n substrate as such

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- Number: US 2014/0151716 A1
- Document ID: US20140151716A1
- Status: Published application
- Kind: A1
- Application number: 14/173,336
- Filed: 2014-02-05
- Published: 2014-06-05
- Earliest claimed: 2006-08-09
- Assignees: Freiberger Compound Materials GmbH
- Applicants: FREIBERGER COMPOUND MATERIALS GmbH
- Inventors: Ferdinand SCHOLZ; Peter Brückner; Frank Habel; Gunnar Leibiger
- Web page: https://patentgrep.com/patent/US20140151716A1

## CPC

- H10D 62/8503: {Nitride Group III-V materials, e.g. AlN or GaN}
- C30B 25/00: Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B 25/02: Epitaxial-layer growth
- C30B 25/165: {the flow of the reactive gases}
- C30B 29/403: {AIII-nitrides}
- C30B 29/406: {Gallium nitride}
- H10P 14/3416: {Nitrides}
- H10D: INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
- 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
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10

## Abstract

A process for producing a doped III-N bulk crystal, wherein III denotes at least one element of the main group III of the periodic system, selected from Al, Ga and In, wherein the doped crystalline III-N layer or the doped III-N bulk crystal is deposited on a substrate or template in a reactor, and wherein the feeding of at least one dopant into the reactor is carried out in admixture with at least one group III material. In this manner, III-N bulk crystals and III-N single crystal substrates separated therefrom can be obtained with a very homogeneous distribution of dopants in the growth direction as well as in the growth plane perpendicular thereto, a very homogeneous distribution of charge carriers and/or of the specific electric resistivity in the growth direction as well as in the growth plane perpendicular thereto, and a very good crystal quality.

## Claims

### Claim 1

A doped, epitaxially grown III-N bulk crystal, wherein III denotes at least one element of the main group III of the periodic system selected from Al, Ga and In, wherein the doped III-N bulk crystal satisfies at least one of the following conditions (a) to (c):
(a) in a micro-Raman mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the measured frequency positions of the LPP+-mode
in case of (i) is 5% or lower, and
in case of (ii) is 10% or lower:
(b) in an MDP mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the photoconductivity signals
in case of (i) is 5% or lower, and
in case of (ii) is 10% or lower;
(c) in a micro photoluminescence mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the line width of the D0X transition
in case of (i) is 5% or lower, and
in case of (ii) is 10% or lower.

### Claim 2 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein in a micro-Raman mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the measured half-widths of the E2-phonon
in case of (i) is 5% or lower, and
in case of (ii) is 5% or lower.

### Claim 3 (depends on 1)

The doped, epitaxially grown III-N hulk crystal according to claim 1, wherein the doped III-N hulk crystal has a circular or almost circular cross-section, and the diameter of the III-N bulk crystal is ≧5 cm.

### Claim 4 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein the length of the doped, epitaxially grown III-N bulk crystal is ≧0.1 mm.

### Claim 5 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein the length of the doped, epitaxially grown III-N bulk crystal is ≧1 mm.

### Claim 6 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein the length of the doped, epitaxially grown III-N bulk crystal is ≧1 cm.

### Claim 7 (depends on 1)

The doped III-N bulk crystal according to claim 1, wherein the length of the doped, epitaxially grown III-N bulk crystal is ≧3 cm.

### Claim 8 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein the doped III-N bulk crystal is grown by epitaxy above a foreign substrate selected from the group consisting of sapphire, silicon carbide, gallium arsenide, lithium aluminate and silicon.

### Claim 9 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein the doped III-N bulk crystal is grown by epitaxy on a doped or undoped GaN substrate as a substrate, or on a foreign substrate having GaN deposited on a foreign substrate.

### Claim 10 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein the doped III-N bulk crystal is grown by epitaxy comprising a mixed feeding from a common source material in which at least one dopant has been added to the at least one group III starting material.

### Claim 11 (depends on 10)

The doped, epitaxially grown III-N hulk crystal according to claim 10, wherein the common source material comprises at least one dopant in elemental form and the at least one group III starting material in elemental form.

### Claim 12 (depends on 10)

The doped, epitaxially grown III-N bulk crystal according to claim 10, wherein the common source material is in the form of a solid solution, an alloy or a mixed melt of the at least one dopant and the at least one group III starting material.

### Claim 13 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein the doped III-N bulk crystal is grown by hydride vapor phase epitaxy.

### Claim 14 (depends on 1)

The doped, epitaxially grown III-N bulk crystal according to claim 1, wherein the dopant is selected from the group consisting of silicon, tellurium, magnesium, iron, germanium, tin, selenium, beryllium, vanadium, manganese, zinc, chronic, nickel, copper and a mixture thereof.

### Claim 15

A free-standing doped III-N substrate, wherein III denotes at least one element of the main group III of the periodic system selected from Al, Ga and In, wherein the free-standing doped III-N substrate satisfies at least one of the following conditions (a) to (c):
(a) in a micro-Raman mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the measured frequency positions of the LPP+-mode
in case of (i) is 5% or lower, and
in case of (ii) is 5% or lower;
(b) in an MDP mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the photoconductivity signals
in case of (i) is 5% or lower, and
in case of (ii) is 5% or lower;
(c) in a micro photoluminescence mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the line width of the D0X transition
in case of (i) is 5% or lower, and
in case of (ii) is 5% or lower.

### Claim 16 (depends on 15)

The free-standing doped III-N substrate according to claim 15, wherein in a micro-Raman mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the measured half-widths of the E2-phonon
in case of (i) is 5% or lower, and
in case of (ii) is 5% or lower.

### Claim 17 (depends on 15)

The free-standing doped III-N substrate according to claim 15, which has a circular or almost circular cross-section, and the diameter of the substrate is ≧5 cm.

### Claim 18 (depends on 15)

The free-standing doped III-N substrate according to claim 15, which has been separated from a doped, epitaxially grown III-N bulk crystal, wherein the doped III-N bulk crystal satisfies at least one of the following conditions (d) to (f):
(d) in a micro-Raman mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the measured frequency positions of the LPP+-mode
in case of (i) is 5% or lower, and
in case of (ii) is 10% or lower;
(e) in an MDP mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the photoconductivity signals
in case of (i) is 5% or lower, and
in case of (ii) is 10% or lower;
(f) in a micro photoluminescence mapping on a plane
(i) parallel to a growth plane and/or
(ii) in a growth direction
a standard deviation of the line width of the D0X transition
in case of (i) is 5% or lower, and
in case of (ii) is 10% or lower.