hvpe-gan growth on the bumpy road to bulk gan and high ... · 13 calculated miscut deviation over...
TRANSCRIPT
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HVPE-GaN growth On the bumpy road to bulk GaN
and high quality wafers
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Indoor lighting
Decorative lighting
Sapphire
Silicon
Do we need GaN substrates?
T. Uesugi, T. Kachi, CS MANTECH Conference, May 16th-19th, 2011, Palm Spring, CA, USA
Silicon Carbide
Silicon
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3 http://jalopnik.com/how-bmws-new-laser-headlights-will-work-and-not-kill-y-1521586271
Do we need GaN substrates?
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T. Kachi, Japanese Journal of Applied Physics 53, 100210 (2014)
T. Uesugi, T. Kachi, CS MANTECH Conference, May 16th-19th, 2011, Palm Spring, CA, USA
Do we need GaN substrates?
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GaN growth methods
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Hydride Vapor Phase Epitaxy (HVPE growth method)
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HVPE method
Seed holder
Substrates zone T= 850oC Growth zone T= 1045oC
2HCl(g) + 2Ga(l) = 2GaCl(g) +H2(g)
GaCl(g) + 2HCl(g) = GaCl3(g) + H2(g)
GaCl(g) + NH3(g) = GaN(s) + HCl(g) + H2(g)
N2/H2 + NH3
Ga
N2/H2 + HCl
N2/H2 + GaCl
N2/H2 + GaCl + NH3
Carrier gas: N2/H2
∆PGa= [P˚GaCl – (PGaCl3
+ PGaCl)] at ammonia rich conditions
A. Koukitu, Y. Kumagai in Technology of Gallium Nitride Crystal Growth, Springer-Verlag, 2010, p. 31.
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High growth rate (>100 μm/h)
c-plane
Advantages of HVPE method
T. Sochacki et al. Journal of Crystal Growth 407 (2014) 52–57
High purity (impurities concentration < 1016 cm-3)
c-plane
Doping with Si or Ge
n = 5 x 1018 cm-3
µ = 170 [cm2/Vs]
Doping with C or Fe
semi-insulating
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Commercially available HVPE-GaN
K. Motoki, SEI Technical Review, Number 70, April 2010; 28
K. Motoki, et.al, J. Cryst Growth 237 (2002) 912; J. Cryst Growth 305 (2007) 377
Growth on GaAs (111)A/LT GaN by Dislocation Elimination by the Epitaxial growth with inverse pyramidal Pits (DEEP) and Advanced-DEEP (A-DEEP)
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http://www.aetech.jp/
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HVPE-GaN substrates suppliers
10
http://www.hitachi-metals.co.jp
MOCVD-GaN/sapphire
http://www.sinonitride.com
http://www.nanowin.com.cn
http://www.kymatech.com
http://www.m-kagaku.co.jp
http://www.furukawakk.co.jp
http://www.lumilog.com
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HVPE-GaN substrates suppliers
Y. Oshima et al. Jpn. J. Appl. Phys. V. 42 (2003)
Growth on sapphire/MOVPE-GaN/Ti by Void-Assisted Separation
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Bending of crystallographic planes
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13 13
Calculated miscut deviation over the wafer for different bow radii
Wafer Dia Lattice Bow Radius
5 m 10 m 20 m 30 m
1” 0.3° 0.15° 0.07° 0.05°
2” 0.6° 0.3° 0.15° 0.1°
3” 0.9° 0.5° 0.2° 0.15°
4” 1.6° 0.6° 0.3° 0.2°
The wafer’s surface needs to be offcut uniformly for 0.1 degree in a specific direction:
-to promote bilayer step flow, -to control the composition of ternary alloys in device layers, -to control the incorporation of dopants and unwanted impurities.
M. Boćkowski and Z. Sitar, CS Vol. 20 Issue 4 (2014) 48-51
Bending of crystallographic planes
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Free-standing HVPE-GaN substrate Uniform offcut required!
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340 360 380 400 420 440 4600
500
1000
1500
2000
2500
3000
3500
Inte
nsity (
arb
. u
nits)
Emission wavelength (nm)
1 deg
0.2 deg
T. Suski et al., Applied Physics Letters Vol. 93 Issue: 17, 172117, 2008
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Na-flux growth method
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Discovered by Prof. Yamane at Tohoku Univ. 1997 Developed by Prof. Mori at Osaka Univ. N2 pressure < 100 MPa and temperature < 900⁰C Growth rate - 50 μm/h Growth run proceeds at constant temperature The mass transport is governed by convection caused by mechanical stirring of the flux
Na-flux growth method
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Growth by the Na-flux Point Seed Technique (SPST)
Y. Mori et al., CS MANTECH Conference, May 19th - 22nd, 2014, Denver, Colorado, USA
as-grown (4 inch)
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300m 300m
Na-flux GaN seed
HVPE-1st HVPE-2nd 212μm
41μm
430μm
GaN crystal by HVPE on coalesced GaN seed
SEM image of surface
Growth rate: ~80μm
18 Y. Mori et al., IWN 2014 Conference, August 24th – 29th, 2014, Poland
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Ammonothermal growth method
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Ammonothermal method
- analogous to hydrothermal crystallization of quartz or oxide crystals such as ZnO
- ammonia used instead of water; ammonia in a supercritical state (enhanced reactivity)
- applied pressure and temperature: 1000-6000 atm. and 300–750oC
- mineralizers are added to the solution in order to increase the solubility of GaN feedstok
20 basic acidic
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Ammonothermal method SCAATTM
Y. Mikawa et al., Proc. of SPIE Vol. 9363, 936302 (2015)
SuperCritical Acidic Ammonia Technology
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Ammonothermal method SCoRA
Scalable compact Rapid Ammonothermal technique from SORAA
D. Ehrentraut and M. Bockowski, in Handbook of Crystal Growth Second Edition (2015)
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R. Doradziński et al. in Technology of Gallium Nitride Crystal Growth, Springer-Verlag, Heidelberg, 2010, pp. 137-158
Ammonothermal GaN from Ammono S.A.
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n-type (2x1017 to 2x1019 cm-3) semi-insulating (106 -1010 Ωcm) p-type (1016 cm-3)
<c>=5.18573±0.00003 Å
<a>=3.18930±0.00005 Å
J. Domagała, IP PAS
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Ammonothermal GaN substrates
(0001) surface preparation
A. Sidor, G. Nowak, G. Kamler, A. Pawłowska, A. Nowakowska-Siwińska
CMP + cleaning
RMS < 0.1 nm
Visible atomic steps
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HVPE growth on Ammono-GaN
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Japanese Journal of Applied Physics 55, 05FC01 (2016)
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Our HVPE reactor configuration
GaCl nozzles
NH3 nozzle
susceptor
gallium
2HCl(g) + 2Ga(g) = 2GaCl(g) +H2(g)
GaCl(g) + NH3(g) = GaN(s) + HCl(g) + H2(g)
27 T. Sochacki et al. Journal of Crystal Growth 407 (2014) 52–57
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28 B. Łucznik, T. Sochacki, M. Amilusik, M. Fijałkowski, M. Iwińska, P. Kempisty, I. Grzegory
1-inch
2-inch 1.5- inch
1-inch
HVPE-GaN layers on Ammono-GaN seeds
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Average growth rate: 60-80 µm/h
After 1-2 h. of growth
HVPE growth modes: macrosteps
[11-20]
[10-10]
T. Sochacki et al. Journal of Crystal Growth 403 (2014) 32–37
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HVPE growth modes: hillocks and steps
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HVPE growth modes: hillocks
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HVPE growth modes: hillocks
Average growth rate: 150-380 µm/h in 10 – 2 hrs.
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Growth rate
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2Ga(l) + 2HCl(g) = 2GaCl(g) +H2(g) GaCl(g) + NH3(g) = GaN(s) + HCl(g) + H2(g)
Growth rate
HCl flow
NH
3 f
low
Constant NH3 flow
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Growth rate
0
50
100
150
200
250
300
350
400
0 20 40 60 80 100 120
NH3=480 NH3=960 NH3=1440 Σstream = 1600 ml/min
HCl flow [ml/min]
Gro
wth
ra
te [
µm
/h]
Growth time 8 h. 35
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Growth rate
HCl flow
NH
3 f
low
2Ga(l) + 2HCl(g) = 2GaCl(g) +H2(g) GaCl(g) + NH3(g) = GaN(s) + HCl(g) + H2(g)
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Growth rate
0
100
200
300
400
500
600
0 20 40 60 80 100 120
Gro
wth
Ra
te [
µm
/h]
HCl flow [ml/min]
V/III = 10 R2 V/III = 20 R2
Growth time 8 h. 37
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Wafering
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HVPE-GaN/Am-GaN HVPE-GaN/Am-GaN
Slicing
F-S HVPE-GaN
Slicing of HVPE-GaN/Am-GaN
1-inch
1.5-inch
Slicing
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WSD-K2 Single Wire Saw
Slicing of HVPE-GaN/Am-GaN
N-side as cut
Ga-side as cut
1-inch Slicing time: 2.5 h.
Bow < 10 µm TTV = 20 µm
T. Sochacki
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2-inch F-S HVPE-GaN
R = 100 μm/h Thickness = 500 μm
EPD = 5x104 cm-2 n = ~1017 cm-3
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Regrowth by HVPE and ammonothermal methods
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Three crystals after third re-growth procedure
Crystal no. 1
Crystal no. 3
Crystal no. 2
Regrowth by HVPE method
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X-ray rocking curve for as-grown HVPE-GaN crystals after three
re-growth procedures
Crystal no. 2 FWHM (002) 38.2 arcsec
Crystal no. 1 FWHM (002) 28.4 arcsec
Crystal no. 3 FWHM (002) 32.4 arcsec
Regrowth by HVPE method
beam size 1x10 mm2
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Regrowth by HVPE method
F-S HVPE-GaN
HVPE-GaN
FWHM=66 arc sec beam size 1x10 mm2
1.5-inch
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F-S HVPE-GaN
Am-GaN
Regrowth by ammonothermal method
Conductivity: n-type (n~ 5x1017 cm-3) Oxygen concentration (SIMS) – 1x1018 cm-3 Absorption coefficient ~ 3 cm-1 at 450 nm
-c
16,70 16,75 16,80 16,85
0
200
400
FWHM = 20 arcsec
Rcurve
=100m
Inte
nsity (
a.u
.)
(deg)
Ammono-GaN/Ammono-HVPE
beam size 0.1 mm x 0.1 mm
Am-GaN/F-S HVPE-GaN
R. Kucharski et al. Journal of Crystal Growth 427 (2015) 1–6
1-inch
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Properties of F-S HVPE-GaN
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Structural quality of F-S HVPE-GaN
L. Kirste et al., ECS Transactions, 66 (1) 93-106 (2015) 48
sample size thickness
H-1 2 inch 260 µm
H-2 10 mm 10 mm 261 µm
A-H half of 1 inch 310 µm
H-1 commercially available HVPE-GaN H-2 A-H F-S HVPE-GaN from Am-GaN
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49
Structural quality of F-S HVPE-GaN Synchrotron white-beam X-ray topography (SWXRT)
L. Kirste ECS Journal of Solid State Science and Technology, 4 (8) P324-P330 (2015)
Uniform gray contrast indicates a high degree of crystalline perfection
A-H
cellular dislocation network
H-1 H-2
The dislocation rearrangement into cell networks takes place under external or internal stress
in the course of plastic relaxation.
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50
J. Weyher, T. Sochacki
Edge dislocation Screw
dislocation Mixed
dislocation
J. L. Weyher et al., Journal of Crystal Growth 305 (2007) 384–392
Structural uniformity - etch pit distribution
EPD = 5x104 cm-2
molten KOH/NaOH 450oC
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51
Room temperature transmission
-Hg(Xe) arc lamp source -Princeton Instruments Acton SP2750 0.75 m high-resolution monochromator with 3600 grooves/mm grating
No structure was observed in the absorption spectrum close to the band edge.
T. Sochacki et al., Appl. Phys. Expri 6, 075504 (2013)
The absorption coefficient below the bandgap was
measured to be less than 1 cm-1
M. Bobea, Z. Bryan, I. Bryan R. Collazo, Z. Sitar
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52
3.468 3.472 3.476 3.480
XA
SioX
B
OoX
BISiX
2a
IOX
2a
D+X
A
Do
?X
AA
oX
A
SioX
A
OoX
A
Lo
g I
nte
nsity (
a.
u.)
Energy (eV)
Low temperature photoluminescence
T. Sochacki et. al, Journal of Crystal Growth 394 (2014) 55–60
two sharp donor bound exciton emission lines
acceptor bound exciton emission
free exciton emissions
M. Bobea, Z. Bryan, I. Bryan R. Collazo, Z. Sitar
3 K
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Thermal conductivity by 3ω and hyper flash methods
Z. Sitar
k = 250 50 W/(m.K) @ room T
-100 0 100 200 300 400 500
0
50
100
150
200
250
300
350
400
450
Th
erm
al
Co
nd
ucti
vit
y [
W/(
m. K
)]
Temperature [oC]
k > 200 W/(m.K) @ room T
M. Seiss
53 T. Sochacki et al., Appl. Phys. Expri 6, 075504 (2013)
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54
Thermal conductivity
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55
Doping in HVPE growth method
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56
FWHM (002) 32.4 arcsec
Thickness: 600 μm Growth rate: 120 μm/h
Doping: HVPE-GaN:Si
B. Łucznik, T. Sochacki, M. Amilusik, M. Fijałkowski, M. Iwińska, P. Kempisty, I. Grzegory
beam size 1x10 mm
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57
E2
A1(LO)
z(xx)z
LPP- A1(LO)+LPP+
In doped semiconductors polar
longitudinal modes are coupled with plasmons
resulting in new LPP modes which positions
are very sensitive to the free carrier
concentration.
Typical Raman spectrum for GaN crystal with: n < 2 x 1017 cm-3 n > 2 x 1017 cm-3
Free carrier concentration Raman spectroscopy
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58
Typical Raman spectrum for GaN crystal with: n < 2 x 1017 cm-3 n > 2 x 1017 cm-3
E2
LPP-
z(xx)z A1(LO)
LPP+
Raman:
n = 6 x 1018 cm-3
Hall:
n = 5.7 x 1018 cm-3
µ = 170 [cm2/Vs]
Raman spectroscopy versus Hall effect
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59
Free carrier concentration by Raman spectroscopy
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60
Limiting factors of HVPE method
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61
150-250 μm/h 10 - 6 h 250-380 μm/h 6 - 2 h
Parasitic deposition
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62 62
susceptor
GaN substrate
GaCl
NH3
Different HVPE reactor configuration
Efficiency of GaN synthesis is lower !
Parasitic deposition
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63
GaCl NH3
susceptor
separation inert gas
reactor tube
Parasitic deposition
Different HVPE reactor configuration
reactor tube susceptor
GaCl NH3
separation inert gas
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64 K. Fujito et al., Journal of Crystal Growth 311 (2009) 3011–3014
In general, a parasitic growth of polycrystalline GaN in a growth reactor is one of the major problems for bulk GaN crystals growth by HVPE. An optimization of gas nozzles configurations and flow rates can solve this problem, so the parasitic nucleation was not a severe problem.
Parasitic deposition
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65 65 65
c
(000-1) Ammono-GaN
(000-1) Ammono-GaN
HVPE-GaN wing
Anisotropy of the growth
+ C
a-plane
m-plane m-plane
[11-20]
[10-10] [10-10]
dodecagon shape*
* K. Fujito et al., Journal of Crystal Growth 311 (2009) 3011–3014
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66
Anisotropy of the growth
Same thicknesses of deposited layers – 1.5 mm
thinner seed – 300 μm thicker seed – 600 μm
dodecagon shape
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67
Anisotropy of the growth
T. Sochacki et al., Phys. Status Solidi B 252, No. 5 (2015) 1172
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300 µm
interface wings
c
a
X2
X1
Anisotropy of the growth
68 J. Domagała, IP PAS
Increase of "a" lattice parameter is accompanied with decrease of "c" parameter. It is typical for elastic strain of a system.
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69 J. Domagała, IP PAS
600 µm
interface wings
c
a
X2
X1
Anisotropy of the growth
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70
Cross-section after photo-etching m-plane
Anisotropy of the growth
HVPE-GaN
AM-GaN
HVPE-GaN
Wing
+ c
0 5 10 15 20 25 3010
16
1017
1018
1019
1020
1021
O
Si
Co
nce
ntr
atio
n [
at/cm
3 ]
Depth [ m ]
0 2 4
1017
1018
1019
1020
1021
O
Si
Depth [ m ]
Co
nce
ntr
atio
n [ a
t/cm
3 ]
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substrate
a > aHVPE a > aHVPE deposited layer
Δε = 0
- the HVPE-GaN seed&layer are under tensile stress derived from wings; plastic deformation can occur in the HVPE-GaN seed&layer.
HVPE-GaN growth model
aHVPE
aHVPE
71
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equivalent stress – 30MPa
Max equivalent stress – 398MPa
4-inch substrate
Numerical simulation
72
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Stress Distribution
0,00E+00
5,00E+01
1,00E+02
1,50E+02
2,00E+02
2,50E+02
3,00E+02
3,50E+02
4,00E+02
4,50E+02
32 34 36 38 40 42 44 46
Vo
n M
ises
Str
ess
(MP
a)
Radial Coordinate (mm)
Wings
Layer
73
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74
75MPa
27MPa
Negative role of wings
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75 75
HVPE: wafer to wafer technology
2.2 – 2.4-inch 3.2 – 3.4-inch 4.2 – 4.4-inch
2-inch 3-inch 4-inch
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Potential solutions Challenges
Concentration of impurities as well as the types of impurities are different
on c-plane and on non-polar and semi-polar facets.
This causes stress in the growing crystal.
Uniform doping on all GaN facets can be helpful (Fermi level control).
prof. Z. Sitar
Lattice constants engineering should be introduced.
prof. K. Kakimoto
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High Nitrogen Pressure Solution (HNPS)
Perfect crystallographic quality but…too small!
I. Grzegory et al. in Bulk Crystal Growth of Electronic, Optical and Optoelectronic Materials, ed. by P. Capper, Wiley&Sons, (2005), 173
Ga
Dissolution and transport to the crystallization zone Ga
crucible
T
T
N2 molecules under pressure
Spontaneous crystallization
GaN
Dissociative adsorption of N2 on liquid metal surface
10 000 atm 1500oC
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Compound a (Å) c (Å)
1. GaN undoped homoepitaxial layers (MOCVD) 3,18850.0003 5.1850 0.0001
2. Mg-doped bulk (low free electron concentration) 3,18850.0003 5.1850 0.0001
3. GaN bulk, free electron concentration 5x1019 3,18900.0003 5.1864 0.0001
High Nitrogen Pressure Solution (HNPS)
EF
GaN – „undoped” Ga : Mg
EF
VGa>1018 cm-3
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Potential solutions
substrate
aMg = aHVPE aMg = aHVPE deposited layer
Δε = 0
aHVPE
aHVPE
Mg Mg
Magnesium loves oxygen; oxygen loves magnesium!
79
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80
GaN
m-plane; cross section
wing
wing
N-side GaN
GaN:Mg
m-plane; cross section
wing
N-side GaN
wing
Potential solutions
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81
Potential solutions
SIMS
0 2 410
16
1017
1018
1019
1020
1021
1022
left axis
H
O
Mg
Si
Depth [ m ]
Concentr
ation
[ a
t/cm
3 ]
100
101
102
103
104
105
106
SIM
S S
ignal [ c
/s ]
0 2 410
17
1018
1019
1020
1021
1022
left axis
H
O
Mg
Si
Depth [ m ]
Concentr
ation
[ a
t/cm
3 ]
100
101
102
103
104
105
106
SIM
S S
ignal [ c
/s ]
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GaN vs GaN:Mg – lattice parameters
beam size: 0.04 mm x 0.1 mm
GaN
wing c-plane layer
GaN:Mg
wing c-plane layer
Potential solutions
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83
Summary
Concentration of impurities as well as the types of impurities are different on c-plane and on non-polar and semi-polar facets. This causes stress in the growing crystal.
Lattice constants engineering should be introduced.
There are three GaN growth methods; today only one of them is applied for „GaN substrates mass production”.
The main disadvantage of all GaN growth methods is anisotropy of the growth and growth in lateral direction.
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84
This research was supported by Polish National Centre for Research and Development through projects: PBS1/B5/7/2012 and
PBS3/B5/32/2015.
This research was also supported by Polish National Science Center through project No. 2012/05/B/ST3/02516.
Part of this research was also supported by ECSEL through project
AGATE (‘Development of Advanced GaN substrates & Technologies’).