# US 11,443,942 B2 · Plasma-assisted atomic layer epitaxy of cubic and hexagonal InN films and its alloys with AIN at low temperatures

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- Number: US 11,443,942 B2
- Document ID: US11443942B2
- Status: Granted
- Kind: B2
- Application number: 15/698,344
- Filed: 2017-09-07
- Published: 2018-02-08
- Granted: 2022-09-13
- Earliest claimed: 2012-06-18
- Assignees: The Government of the United States of America, as represented by the Secretary of the Navy
- Applicants: The Government of the United States of America, as represented by the Secretary of the Navy
- Inventors: Neeraj Nepal; Charles R. Eddy, Jr.; Nadeemullah A. Mahadik; Syed B. Qadri; Michael J. Mehl
- Web page: https://patentgrep.com/patent/US11443942B2

## CPC

- H10P 14/3416: {Nitrides}
- H10D 62/8503: {Nitride Group III-V materials, e.g. AlN or GaN}
- H10P 14/24: using chemical vapour deposition [CVD]
- H10P 14/2905: {Silicon, silicon germanium or germanium}
- H10P 14/2921: {being crystalline insulating materials}
- H10P 14/2926: {Crystal orientations}
- H10P 14/3216: {Nitrides}
- H10P 14/3602: {In-situ cleaning}
- C30B 25/02: Epitaxial-layer growth
- C30B 25/205: {the substrate being of insulating material}
- C30B 29/38: Nitrides
- C30B 29/40: AIIIBV compounds {wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi}
- C30B 29/403: {AIII-nitrides}
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- 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

## Abstract

Described herein is a method for growing indium nitride (InN) materials by growing hexagonal and/or cubic InN using a pulsed growth method at a temperature lower than 300° C. Also described is a material comprising InN in a face-centered cubic lattice crystalline structure having an NaCl type phase.

## Claims

### Claim 1

A method for growing crystalline, epitaxial indium nitride (InN) material, the method comprising:
providing an a-plane Al2O3 template and growing cubic InN thereon using pulsed growth plasma-assisted atomic layer epitaxy at a temperature lower than 300° C.,
wherein the obtained cubic InN has the same crystal structure throughout.

### Claim 2 (depends on 1)

The method of claim 1, using N2 plasma as a nitrogen precursor.

### Claim 3 (depends on 1)

The method of claim 1, using trimethylindium as an indium precursor.

### Claim 4 (depends on 1)

The method of claim 1, wherein said cubic InN consists of a homogenous phase of cubic InN.

### Claim 5 (depends on 1)

The method of claim 1, wherein said temperature is intentionally varied during said growing in order to control conductivity of said cubic InN.

### Claim 6 (depends on 1)

The method of claim 1, further comprising in situ surface treatment with atomic hydrogen, nitrogen, a mixture of hydrogen and nitrogen, and/or ammonia plasma.

### Claim 7 (depends on 1)

The method of claim 1, further comprising variation of purge time with pumping speed, thereby controlling formation of carbon impurities.

### Claim 8 (depends on 1)

The method of claim 1, wherein said temperature is lower than 200° C.

### Claim 9 (depends on 8)

The method of claim 8, using N2 plasma as a nitrogen precursor.

### Claim 10 (depends on 8)

The method of claim 8, wherein said cubic InN consists of a homogenous phase of cubic InN.

### Claim 11 (depends on 8)

The method of claim 8, wherein said temperature is intentionally varied during said growing in order to control conductivity of said cubic InN.

### Claim 12 (depends on 8)

The method of claim 8, further comprising in situ surface treatment with atomic hydrogen, nitrogen, a mixture of hydrogen and nitrogen, and/or ammonia plasma.

### Claim 13 (depends on 8)

The method of claim 8, further comprising variation of purge time with pumping speed, thereby controlling formation of carbon impurities.

### Claim 14 (depends on 1)

The method of claim 1, wherein said pulsed growth method comprises pulsed growth of an AlxIn1-xN film at a temperature lower than 300° C. by via alternate pulses of indium or aluminum precursor and nitrogen precursor, such that x is a number greater than 0 and less than 1.

### Claim 15 (depends on 14)

The method of claim 14, using N2 plasma and/or ammonia plasma as said nitrogen precursor.

### Claim 16 (depends on 14)

The method of claim 14, wherein said film has a homogenous phase.

### Claim 17 (depends on 14)

The method of claim 14, further comprising in situ surface treatment with atomic hydrogen, nitrogen, a mixture of hydrogen and nitrogen, and/or ammonia plasma.

### Claim 18 (depends on 14)

The method of claim 14, further comprising variation of purge time with pumping speed, thereby controlling formation of carbon impurities.

### Claim 19 (depends on 14)

The method of claim 14, further comprising the use of a trimethylaluminum as an aluminum precursor.