# US 11,898,269 B2 · Oxygen-doped group III metal nitride and method of manufacture

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- Number: US 11,898,269 B2
- Document ID: US11898269B2
- Status: Granted
- Kind: B2
- Application number: 16/868,528
- Filed: 2020-05-06
- Published: 2020-08-20
- Granted: 2024-02-13
- Earliest claimed: 2017-01-09
- Assignees: SLT Technologies, Inc.
- Applicants: SLT Technologies, Inc
- Inventors: Wenkan Jiang; Dirk Ehrentraut; Mark P. D'Evelyn
- Web page: https://patentgrep.com/patent/US11898269B2

## CPC

- C30B 29/406: {Gallium nitride}
- C01B 21/0632: {with gallium, indium or thallium}
- C30B 7/105: {using ammonia as solvent, i.e. ammonothermal processes}
- H10D 62/50: Physical imperfections
- H10D 62/8503: {Nitride Group III-V materials, e.g. AlN or GaN}
- C01P 2002/30: Three-dimensional structures
- C01P 2002/74: by peak-intensities or a ratio thereof only
- C01P 2002/80: defined by measured data other than those specified in group C01P2002/70
- C01P 2006/80: Compositional purity
- 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
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- H10D: INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A gallium-containing nitride crystals are disclosed, comprising: a top surface having a crystallographic orientation within about 5 degrees of a plane selected from a (0001)+c-plane and a (000-1)−c-plane; a substantially wurtzite structure; n-type electronic properties; an impurity concentration of hydrogen greater than about 5×1017 cm−3, an impurity concentration of oxygen between about 2×1017 cm−3 and about 1×1020 cm−3, an [H]/[O] ratio of at least 0.3; an impurity concentration of at least one of Li, Na, K, Rb, Cs, Ca, F, and Cl greater than about 1×1016 cm−3, a compensation ratio between about 1.0 and about 4.0; an absorbance per unit thickness of at least 0.01 cm−1 at wavenumbers of approximately 3175 cm−1, 3164 cm−1, and 3150 cm−1, and wherein, at wavenumbers between about 3200 cm−1 and about 3400 cm−1 and between about 3075 cm−1 and about 3125 cm−1, said gallium-containing nitride crystal is essentially free of infrared absorption peaks having an absorbance per unit thickness greater than 10% of the absorbance per unit thickness at 3175 cm.

## Claims

### Claim 1

A gallium-containing nitride crystal comprising:
a gallium-containing nitride in a substantially wurtzite structure comprising an n-type dopant;
impurities of hydrogen [H] and oxygen [O], wherein a ratio of an impurity concentration of hydrogen [H] to an impurity concentration of oxygen [O] is at least 0.3; and
impurities of at least one of Li, Na, K, Rb, Cs, Ca, F, and Cl having an impurity concentration of greater than about 1×1016 cm−3, wherein
a ratio of the impurity concentration of oxygen to an n-type carrier concentration n is between 1.0 and 4.0, and
at wavenumbers between about 3200 cm−1 and about 3400 cm−1, said gallium-containing nitride crystal is essentially free of infrared absorption peaks having an absorbance per unit thickness greater than 0.01 cm−1, as measured by Fourier transform infrared spectrometry (FTIR).

### Claim 2 (depends on 1)

The gallium-containing nitride crystal of claim 1, wherein at wavenumbers between about 3075 cm−1 and about 3125 cm−1, said gallium-containing nitride crystal is essentially free of infrared absorption peaks having an absorbance per unit thickness greater than 0.01 cm−1, as measured by Fourier transform infrared spectrometry.

### Claim 3 (depends on 1)

The gallium-containing nitride crystal of claim 1, further comprising defects that are characterized by an absorbance per unit thickness of at least 0.01 cm−1 at wavenumbers of approximately 3175 cm−1, 3164 cm−1, and 3150 cm−1, as measured by Fourier transform infrared spectrometry.

### Claim 4 (depends on 1)

The gallium-containing nitride crystal of claim 1, wherein the n-type carrier concentration n is between about 3×1017 cm−3 and about 1×1020 cm−3 and a carrier mobility n, in units of centimeters squared per volt-second, is such that a logarithm to the base 10 of a quantity (1.2×η) is greater than about −0.4115[log10(n)]+10.028.

### Claim 5 (depends on 1)

The gallium-containing nitride crystal of claim 1, further comprising impurities of at least one of silicon and germanium having an impurity concentration of between about 1×1017 cm−3 and about 3×1019 cm−3.

### Claim 6 (depends on 1)

The gallium-containing nitride crystal of claim 1, wherein the n-type carrier concentration n is between about 3×1017 cm−3 and about 5×1019 cm−3.

### Claim 7 (depends on 1)

The gallium-containing nitride crystal of claim 1, wherein a first surface has a diameter greater than about 10 millimeters and the crystal has a thickness, measured in a direction orthogonal to the first surface, greater than about 100 micrometers.

### Claim 8 (depends on 1)

The gallium-containing nitride crystal of claim 1, wherein the ratio of the impurity concentration of oxygen to the n-type carrier concentration n is between about 1.5 and about 3.5.

### Claim 9 (depends on 8)

The gallium-containing nitride crystal of claim 8, wherein the ratio of the impurity concentration of oxygen to the n-type carrier concentration n is between about 1.75 and about 3.2.

### Claim 10 (depends on 1)

The gallium-containing nitride crystal of claim 1, wherein the ratio of the impurity concentration of hydrogen to the impurity concentration of oxygen is between about 0.5 and about 1.3.

### Claim 11 (depends on 1)

The gallium-containing nitride crystal of claim 1, wherein:
the impurity concentration of hydrogen [H] is greater than about 5×1017 cm−3,
the impurity concentration of oxygen [O] between about 2×1017 cm−3 and about 1×1020 cm−3, and
the impurity concentrations are measured using calibrated secondary ion mass spectrometry (SIMS).

### Claim 12 (depends on 1)

The gallium-containing nitride crystal of claim 1, characterized by a cathodoluminescence peak at about 423 nm.

### Claim 13 (depends on 12)

The gallium-containing nitride crystal of claim 12, further characterized by a cathodoluminescence peak at about 550 nm.

### Claim 14 (depends on 12)

The gallium-containing nitride crystal of claim 12, wherein the ratio of an intensity of the cathodoluminescence peak at about 423 nm to the integrated FTIR intensity is between 0.05 and 0.10, where the cathodoluminescence spectrum is measured at room temperature and the intensity is normalized by dividing each individual data point by a total integrated cathodoluminescence intensity between 350 to 900 nm for the spectra and then multiplying by 1000, and the absorbance per unit thickness of the FTIR spectrum is integrated between about 3000 cm−1 and about 3250 cm−1.

### Claim 15 (depends on 1)

The gallium-containing nitride crystal of claim 1, wherein a ratio of an optical absorption coefficient at a wavelength of about 423 nm to the integrated FTIR intensity is between 0.02 and about 0.05, where the absorbance per unit thickness of the FTIR spectrum is integrated between about 3000 cm−1 and about 3250 cm−1.

### Claim 16 (depends on 3)

The gallium-containing nitride crystal of claim 3, further comprising:
point defects having defect types and relative concentrations resulting in a compensation ratio between about 1.0 and about 4.0, wherein the point defects are further characterized by an absorbance per unit thickness of at least 0.01 cm−1 at a wavenumber of approximately 3188 cm−1, wherein the absorbance per unit thickness at 3188 cm−1 has a value between 5% and 25% of that of the absorbance per unit thickness at 3175 cm−1.

### Claim 17 (depends on 16)

The gallium-containing nitride crystal of claim 16, wherein
said point defects are further characterized by an absorbance per unit thickness at wavenumbers from about 3188 cm−1 to about 3400 cm−1 that is less than 25% of that of the absorbance per unit thickness at 3175 cm−1.