a study of pretreatment process on selective area growth

1
Annealing treatment in Nambient (before RIE and acid treatment) A problem in the beginning of study A study of pretreatment process on selective area growth of GaN using SiN masks S. Man 1 , R. Kayanuma 1 , Y. Takei 1 , T. Takahashi 3 , T. Ide 3 , M. Shimizu 3 , K. Tsutsui 1 ,K. Kakushima 1 , H. Wakabayashi 1 , Y. Kataoka 2 and H. Iwai 2 Tokyo Tech. 1 , Tokyo Tech. FRC 2 , AIST Advanced Power Electronics Research Center 3 Email: [email protected] BackgroudPurpose of this work Improving quality of epitaxial layersELO technologyFabrication technique of nano devices Promising for forming a three dimensional structure with a high quality a variety of applications mask GaN GaN MOCVD Reasons for using SiN maskSubject Selective area growth of GaN It was reported that GaN is not grown on SiN. Oxygen contamination to GaN by SiO2 mask will be suppressed. Acid treatment Experimental Procedures: SiN GaN 2μm Growth of GaN was not observed. Sapphire GaN SiN Sapphire GaN SiN Sapphire GaN SiN Some pretreatment processes are required to solve the problem that GaN was not grown. GaN was grown with island shapes 5μm GaN SiN Acid treament to clean GaN surface had some effects for GaN growth. However, GaN was not grown appropriately. RIE(reactive ion etching) treatment Sapphire GaN SiN Sapphire GaN SiN Sapphire GaN SiN depth20nm GaN SiN 5μm GaN was grown as a continuous film. The surface of grown GaN was rough. RIE treatment was effective for growth of GaN. However, surface roughness and inhibition of growth near SiN mask were problems. Annealing treatment in MOCVD reactor (between RIE and acid treatment) Sapphire GaN SiN Sapphire GaN SiN Sapphire GaN SiN Sapphire GaN SiN Sapphire GaN SiN Sapphire GaN SiN Sapphire GaN SiN Sapphire GaN SiN We expect to establish the process of the selective area growth of GaN using SiN mask so that GaN is grown appropriately as in the right figure. Purpose of this work GaN SiN mask SiN GaN 5μm SiN GaN 5μm Annealing treatment in MOCVD reacto rwas remarkable to solve the problem that GaN was not grown near the SiN mask edges. However, surface roughness of grown GaN was remained. (something on the GaN surface inhibited GaN growth ?) SiN GaN 5μm SiN GaN 5μm Process of selective area growth of GaN using SiN mask has not been established yet. Conclusion For growth of GaN, RIE treatment is more effective than acid treatment. SiN GaN Sapphire 1. Deposition of SiN films on GaN epi-layer (by sputtering method) Resist SiN GaN Sapphire 3. SiN etching by BHF for 5min. Resist SiN GaN Sapphire 2. Resists patterning to form stripe windows (by photolithography) 4. Resists were removed 5. GaN was grown by MOCVD with conditions for 300nm growth at 1040Grown GaN Sapphire GaN SiN Resultsby SEM: (a) plane veiew (b) cross section Fig 1. SEM micrographs after GaN selective growths Experimental Procedures (partially omitted): Treated by H 2 SO 4 /H 3 PO 4 (3:1) 20030min Resists were removed The growth of GaN Resultsby SEM: Fig 2. SEM micrographs after GaN selective growths with acid treatment (a) plane view (b) cross section (Some of inhibitors were removed) Experimental Procedures (partially omitted): Treated by RIE with BCl3 and Cl2 gas Resultsby SEM: Fig 3. SEM micrographs after GaN selective growths with RIE treatment (a) surface (b) cross section GaN was not grown near the SiN mask edge. Experimental Procedures (partially omitted): Treated by RIE with BCl3 and Cl2 gas Treated by annealing with NH+H, 1040, 10min in MOCVD reactorTreated by H 2 SO 4 /H 3 PO 4 (3:1) 1501h Resists were removed The growth of GaN The growth of GaN Resultsby SEM: Fig 3. SEM images after GaN growths without and with annealing treatment in MOCVD reactor. (a) without annealing (b) with annealing GaN was grown as a continuous film. The surface of grown GaN was rough. GaN was grown appropriately near SiN mask edges. Experimental Procedures (partially omitted): Treated by annealing in N, 1040, 10min by RTA: rapid thermal processTreated by H 2 SO 4 /H 3 PO 4 (3:1) 1501h The growth of GaN Treated by RIE with BCl3 and Cl2 gas Resultsby SEM: Fig 3. SEM micrographs after GaN growths with annealing treatment by RTA in N 2 ambient. (a) ) plane view (b) cross section GaN was grown appropriately near SiN mask edges. The surface of grown GaN was flattened. Annealing treatment in N2 before RIE and acid treatment is remarkable to solve the problem of surface roughness of grown GaN. By annealing treatment, GaN was grown appropriately near SiN edges. Surface roughness of grown GaN was suppressed by changing the order and conditions of annealing treatment. Further optimization is expected.

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Page 1: A study of pretreatment process on selective area growth

Annealing treatment in N₂ ambient (before RIE and acid treatment)

A problem in the beginning of study

A study of pretreatment process on selective area growth of GaN

using SiN masks S. Man1, R. Kayanuma1, Y. Takei1, T. Takahashi3, T. Ide3, M. Shimizu3,

K. Tsutsui1,K. Kakushima1, H. Wakabayashi1, Y. Kataoka2 and H. Iwai2

Tokyo Tech. 1, Tokyo Tech. FRC2, AIST Advanced Power Electronics Research Center3

Email: [email protected]

Backgroud・ Purpose of this work

Improving quality of epitaxial layers(ELO technology)

Fabrication technique of nano devices

Promising for forming a three dimensional structure with

a high quality

a variety of

applications

mask

GaN GaN

MOCVD

Reasons for using SiN mask・Subject

Selective area growth of GaN

It was reported that GaN is not grown on SiN.

Oxygen contamination to GaN by SiO2 mask will be suppressed.

Acid treatment

Experimental Procedures:

SiN GaN

2µm

・Growth of GaN was not

observed.

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Some pretreatment processes are required to solve the problem

that GaN was not grown.

・GaN was grown with island

shapes

5µm

GaN SiN

Acid treament to clean GaN surface had some effects for GaN

growth. However, GaN was not grown appropriately.

RIE(reactive ion etching) treatment

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Sapphire

GaN

SiN

depth:20nm

GaN SiN

5µm

・GaN was grown as a continuous

film.

・The surface of grown GaN was

rough.

RIE treatment was effective for growth of GaN. However, surface

roughness and inhibition of growth near SiN mask were problems.

Annealing treatment in MOCVD reactor (between RIE and acid treatment)

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Sapphire

GaN

SiN

Sapphire

GaN

SiN

We expect to establish the process of the

selective area growth of GaN using SiN mask

so that GaN is grown appropriately as in the

right figure.

Purpose of this work

GaN

SiN mask

SiN GaN

5µm

SiN GaN

5µm

Annealing treatment in MOCVD reacto rwas remarkable to solve the

problem that GaN was not grown near the SiN mask edges.

However, surface roughness of grown GaN was remained.

(something on the GaN

surface inhibited GaN

growth ?)

SiN GaN

5µm

SiN GaN

5µm

Process of selective area growth of GaN using SiN mask has not been

established yet.

Conclusion

・For growth of GaN, RIE treatment is more effective than acid treatment.

SiN

GaN

Sapphire

1. Deposition of

SiN films on

GaN epi-layer

(by sputtering method)

Resist SiN

GaN

Sapphire

3. SiN etching by BHF

for 5min.

Resist

SiN

GaN

Sapphire

2. Resists patterning

to form

stripe windows

(by photolithography)

4. Resists were removed

5. GaN was grown

by MOCVD with

conditions for 300nm

growth at 1040℃

Grown GaN

Sapphire

GaN

SiN

Results(by SEM):

(a) plane veiew (b) cross section

Fig 1. SEM micrographs after GaN selective growths

Experimental Procedures (partially omitted):

Treated by

H2SO4/H3PO4(3:1) 200℃ 30min

Resists were removed The growth of GaN

Results(by SEM):

Fig 2. SEM micrographs after GaN selective growths with acid treatment

(a) plane view (b) cross section

(Some of inhibitors were

removed?)

Experimental Procedures (partially omitted):

Treated by

RIE with BCl3 and Cl2 gas Results(by SEM):

Fig 3. SEM micrographs after GaN selective growths with RIE treatment

(a) surface (b) cross section

・GaN was not grown near the SiN

mask edge.

Experimental Procedures (partially omitted):

Treated by RIE

with BCl3 and Cl2 gas

Treated by annealing with

NH₃+H₂, 1040℃, 10min

(in MOCVD reactor)

Treated by

H2SO4/H3PO4(3:1)

150℃ 1h

Resists were removed The growth of GaN

The growth of GaN

Results(by SEM):

Fig 3. SEM images after GaN growths without and with annealing treatment in MOCVD reactor. (a) without annealing (b) with annealing

・GaN was grown as a continuous

film.

・The surface of grown GaN was

rough.

・GaN was grown appropriately

near SiN mask edges.

Experimental Procedures (partially omitted):

Treated by annealing in

N₂, 1040℃, 10min

(by RTA: rapid thermal process)

Treated by

H2SO4/H3PO4(3:1)

150℃ 1h

The growth of GaN Treated by RIE

with BCl3 and Cl2 gas

Results(by SEM):

Fig 3. SEM micrographs after GaN growths with annealing treatment by RTA in N2 ambient. (a) ) plane view (b) cross section

・GaN was grown appropriately

near SiN mask edges.

・The surface of grown GaN was

flattened.

Annealing treatment in N2 before RIE and acid treatment is

remarkable to solve the problem of surface roughness of grown GaN.

・By annealing treatment, GaN was grown appropriately near SiN edges.

・Surface roughness of grown GaN was suppressed by changing the order

and conditions of annealing treatment. Further optimization is expected.