Bulk Crystal Growth and Liquid Phase Epitaxy Techniques

Sebastian Lourdudoss 1
BULK CRYSTAL GROWTH and LIQUID PHASE EPITAXY BULK CRYSTAL GROWTH and LIQUID PHASE EPITAXY
Lecture-3, 2B 1700, 2B1823 - Advanced Semiconductor Materials
Bulk crystal growth techniques
Need for bulk crytals
Horizontal/Vertical Bridgman technique
Liquid Encapsulated Czochralski technique
Dopant distribution
Wafer specification
Liquid Phase Epitaxy
Various epitaxial techniques
Liquid phase epitaxy
Growth procedure and reactors
LPE phase diagrams
NEED
Device structure:
Several epitaxial layers often with different compositions and/or
doping on a substrate
Epitaxy (from Greek: epi = upon; taxis= ordered):
Growth of a crystal on a substrate with the same crystallographic structure as
the substrate
=> Monocrystalline substrate needed to grow epitaxial layers
Homoepitaxy: e.g., InP/InP
Heteroepitaxy: e.g., InGaAs/InP
Layer 3 Layer 3
Layer 2 Layer 2
Layer 1 Layer 1
Substrate Substrate
Epitaxial
growth
Bulk
growth
Requirements:
1) Wafers with least defects and dislocations
(if present can propagate into the
epitaxial layers)
2) Wafers of ultimate purity
(electrically active impurity atoms < 10
parts per billion atomic)
3) Wafers with controlled electrically active
dopant atoms
Practical Difficulties with certain
III-V semiconductors
1) In general, high melting points
=> Crucibles normally silica
(silica becomes soft at 1100 -
1200
o
C) graphite or
pyrolytic boron nitride (PBN)
2) Vapour pressures high at m.pt.
for InP, GaP and GaAs ( low for
InSb, GaSb and InAs)
3) Decomposition near the
melting point
=> loss of one of the elements
=> defects
(Remedy = Evacuated and
closed systems)
Compound M.Pt.
(
o
C)
Vap. Pr.
at M.pt.
(atm)
InSb 525 4x10
-8
GaSb 712 1x10
-6
InAs 943 0.33
GaAs 1238 1.0
InP 1062 27.5
GaP 1465 32
HgSe 799
HgTe 670 12.5
CdSe 1239 0.3
CdTe 1092 0.65
ZnSe 1526 0.5
ZnTe 1300 0.6
Ge 960
Si 1420
From Compound Semiconductor Devices,
Structures and Processing, Ed. K.A.J ackson,
Willey-VCH, Weinheim, 1998.
Phase diagram for the Ga-As
system
BRIDGMAN TECHNIQUE
Growth on the seed from a
melt ( T
seed
< T
melt
)
Hot wall
Growth in evacuated and
sealed containers
=> purity higher
Easy to control the
vapour pressure
Low vapour pressure
system only
LIQUID ENCAPSULATED CZOCHRALSKI (LEC)
METHOD
Cold wall system
High pressure with inert gas / active gas
Encapsulant (B
2
O
3
) hinders vapour escape from
the melt + wets the growing surface
Normally higher dislocation density than in
Bridgman technique (because of thermal
non-uniformity)
Contamination from the surrounding material
(e.g. carbon from graphite parts)
Low pressure LEC ( Dissociation pressure < 2 atm)
High pressure LEC (Dissociation pressure > 2 atm)
=> inert gas or active gas used
Czochralski Czochralski Growth Method Growth Method
Dopants
k
0
, eqm. Distribution coefficient = C
s
/C
l
i
C
l
i
= concentration in the melt at the interface (weight/g melt)
C
s
= concentration in the solid (weight/g solid)
k
e
, Effective distribution
coefficient = C
s
/C
l
where
C
l
= concentration in the
melt far from the interface
(weight/1g melt)
v = crystal growth rate
= diffusion barrier width
D = diff. coeff. of dopant in
the melt
D
v
l
s
e
e k k
k
C
C
k

+
= =
) 1 (
0 0
0
From S.M.Sze,
Semiconductor
devices, Physics and
Technology, J ohn
Wiley, NY, 2nd ed.,
2001
Equilibrium segregation coefficients for dopants
in silicon and GaAs
From S.M.Sze,
Semiconductor
devices, Physics and
Technology, J ohn
Wiley, NY, 2nd ed.,
2001
Dopant concentration in the solid C
s
:
where k
0
, eqm. distribution coefficient
= C
s
/C
l
(C
l
is the concn. in the melt),
C
0
= Initial concentration in the melt and
M/M
0
= Fraction of the melt solidified
1
0
0
1
0 0
=
k
M
M
C k
s
C
As solidification progress, i.e. As solidification progress, i.e.
when M/M when M/M
0 0
increases, increases,
C C
s s
/C /C
0 0
increases if k increases if k
0 0
< 1 and < 1 and
C C
s s
/C /C
0 0
decreases if k decreases if k
0 0
> 1 > 1
(M/M
0
)
Seed end Seed end Tail end Tail end
From S.M.Sze, Semiconductor
devices, Physics and Technology,
J ohn Wiley, NY, 2nd ed., 2001
Orientation flat, index flat, G-type, J -type
Dovetail groove and V-groove
SEVERAL EPITAXIAL TECHNIQUES
Liquid Phase Epitaxy (LPE) Liquid Phase Epitaxy (LPE)
- - Semiconductor solid from a liquid solution Semiconductor solid from a liquid solution
- - An equilibrium process using An equilibrium process using liquidus liquidus - - solidus solidus
equilibrium equilibrium
Vapour Phase Epitaxy (VPE) Vapour Phase Epitaxy (VPE)
- - Semiconductor solid from gas sources Semiconductor solid from gas sources
- - A special case of Chemical Vapour Deposition (CVD) A special case of Chemical Vapour Deposition (CVD)
Molecular Beam Epitaxy (MBE) Molecular Beam Epitaxy (MBE)
- - Semiconductor solid from atomic or molecular beams Semiconductor solid from atomic or molecular beams
- - Beams arrive directly on the growth surface without Beams arrive directly on the growth surface without
any prior any prior interferance interferance or interaction (feasible in an or interaction (feasible in an
ultra high vacuum environment) ultra high vacuum environment)
Liquid Phase Epitaxy
Observations:
1) III-V comounds decompose before reaching their melting points (melting
points are very high)
This means normally H
fusion
/H
0
formation
> 1
AlSb 0.848 GaAs 1.26
GaSb 1.48 InAs 1.35
InSb 1.43
NaCl 0.07 KF 0.05
2) High vapour pressure of V species at the congruent melting point
Remedy:
Dissolve V species (solutes) in III species (solvents)
Use solidus liquidus equilibrium to carry out epitaxy
THIS IS LPE!
Implication:
Growth predicted by thermodynamics almost accurately
Liquid Phase Epitaxy reactors
LPE PHASE DIAGRAMS LPE PHASE DIAGRAMS
Doping of Doping of InGaAsP InGaAsP lattice lattice
matched to InP with LPE matched to InP with LPE
p-quaternary
contact layer
p-InP
cladding layer
n-InP
p-InP
n-InP
substrate
Regrowth by LPE Regrowth by LPE
Active layer
ADVANTAGES OF LPE
Simple
Inexpensive
Rather non-hazardous
Suitable for selective growth
Al and Sb compounds possible
=> Highly suitable for simple structures
DISADVATAGES OF LPE
Too simple to grow quantum structures
Thickness control and composition control difficult
Redissolution of the grown material
High growth temperatures for certain compounds
(e.g. GaAs at ~ 800-900
o
C but InP at ~ 600
o
C)
Fe doping (for semi-insulation) difficult because of low
distribution coefficient

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Sebastian Lourdudoss 1

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