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Dabing Li State Key Laboratory of Luminescence, Changchun Institute of Optics, Fine Mechanics and Physics (CIOMP), Chinese Academy of Sciences, China *E-mail: [email protected] High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring

High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

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Page 1: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Dabing Li

State Key Laboratory of Luminescence, Changchun Institute

of Optics, Fine Mechanics and Physics (CIOMP), Chinese

Academy of Sciences, China*E-mail: [email protected]

High-temperature MOCVD growth of AlN

on sapphire by controlling initial stage

with in-situ monitoring

Page 2: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

High-temperature MOCVD growth of AlN on sapphire by controlling initial

stage with in-situ monitoring

1.Motivation

2.Experiments

3.Results and Discussion

(1) Growth of AlN by HT-MOCVD under different initial growth conditions

(2) Mechanism of “two-step” HT-MOCVD growth of AlN

4.Summary

Outline

Page 3: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Crack Free &

smooth surface

Optical

Microscopy

AlxGa1-xN on AlN (x=0.57)

AlxGa1-xN

Sapphire

AlN

AlxGa1-xN on GaN (x=0.49)

Sapphire

LT-GaN buffer

GaN

AlxGa1-xN

Crack & rough

surface

Motivation

1. High-efficiency UV devices (e.g LEDs, LDs and detectors) need

high-quality AlN

Page 4: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Motivation

2. To explore the growth mechanism of AlN by two-step HT-

MOCVD.

In-situ monitoring curves of “two-step” growth of GaN

(a): GaN nucleation & annealing

(b): Coalescence (3D)

(c): 2D growth

950nm

Page 5: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Motivation

I: AlN nucleation & annealing

II: Coalescence finished (?)

III: 2D growth (?)

In-situ monitoring curves of “two-step” growth of AlN

AFM image of AlN at the stage II

Light beam of 950nm wavelength is not good for in-situ monitoring of AlN.

After stage II, it is still 3D growth

950nm

Page 6: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Motivation

In-situ monitoring curves of “two-step” growth of AlN

Light beam of 405nm wavelength is powerful to

Monitor the initial stage of AlN.

405nm

Page 7: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

High-temperature MOCVD growth of AlN on sapphire by controlling initial

stage with in-situ monitoring

1.Motivation

2.Experiments

3.Results and Discussion

(1) Growth of AlN by HT-MOCVD under different initial growth conditions

(2) Mechanism of “two-step” HT-MOCVD growth of AlN

4.Summary

Outline

Page 8: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Experiments

Sapphire

HT-AlNLT-AlNAlN was grown by HT-MOCVD.

The in-situ monitoring system with

two light beams was used to monitor

the growth rates and surface

morphology.

AFM and XRD were employed to

characterize the surface state and

crystalline quality.

Time sequence for growth of AlN

Temp. for LT-AlN: 950oC

Temp. for HT-AlN: 1300oC

Reactor Pressure: 40Pa

V/III ratio for HT-AlN: 250

V/III ratio for LT-AlN: 7500

Growth conditions

Page 9: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

High-temperature MOCVD growth of AlN on sapphire by controlling initial

stage with in-situ monitoring

1.Motivation

2.Experiments

3.Results and Discussion

(1) Growth of AlN by HT-MOCVD under different initial growth conditions

(2) Mechanism of “two-step” HT-MOCVD growth of AlN

4.Summary

Outline

Page 10: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Growth of AlN by HT-MOCVD under different initial conditions

Sample No. Initial conditions

C109 Without nucl. layer, No treatment

C120 With nucl. layer

C121 Nitridation (@950oC for 5min)+ nucl. layer

C126 TMAl preflow treatment (2sec)+ nucl. Layer

Results and Discussion:

The smallest FWHM

value was achieved

when growth of HT-AlN

with only nucleation

layer

Page 11: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Results and Discussion:

C109 C120 C121 C126

C109: 3D

C120: 3D 2D

C121: 3D 3D+2D

C126: 2D

Page 12: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

AFM images of sample C109 and C121 before and after etching

Before

For Sample C109, the etching happened from the sidewall of the island;

for sample C121, the etching happened on the surface

C109 C121

After

RMS: 42.229nm

RMS: 73.484nm

RMS: 15.269nm

RMS:60.089nm

Mainly

N-polar

Mainly

Al-

polar

Page 13: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

High-temperature MOCVD growth of AlN on sapphire by controlling initial

stage with in-situ monitoring

1.Motivation

2.Experiments

3.Results and Discussion

(1) Growth of AlN by HT-MOCVD under different initial growth conditions

(2) Mechanism of “two-step” HT-MOCVD growth of AlN

4.Summary

Outline

Page 14: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

(a) nucl. layer (b) nucl. layer after annealing

(c) 2min growth for HT-AlN

(d) The lowest point of reflectance intensity (8min)

(e) Coalescence(22min) (f) 47min growth

Mechanism of “two-step” HT-MOCVD growth of AlN

Page 15: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

Mechanism of “two-step” HT-MOCVD growth of AlN

Island density: high

Island size: small

Island density: low

Island size: large2D growth

(a) (b) (c)

(d) (e) (f)

The two-step growth of AlN experienced a transition from

nuclei (3D island), nuclei decomposed and coalescence ,

and layer-by-layer (2D) growth.

Page 16: High-temperature MOCVD growth of AlN on sapphire by ......High-temperature MOCVD growth of AlN on sapphire by controlling initial stage with in-situ monitoring 1.Motivation 2.Experiments

The crystalline quality of HT-AlN was strongly affected by the

Initial growth conditions. The main reason is that different

initial growth conditions caused different growth mode of HT-

AlN.

Summary

The two-step growth of AlN experienced a transition from 3D

island growth to 2D growth.

The high crystalline quality AlN was grown by “two-step” HT-

MOCVD with in-situ monitoring system. The Laytec in-situ

monitoring system is very useful for growth high-quality AlN.