INDO GERMAN WINTER

ACADEMY 2005
EPITAXIAL GROWTH
OF SILICON CARBIDE
THIN FILMS
G. SREECHAKRA
Indian Institute of Technology, Kharagpur
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 2
SYNOPSI S
Introduction to Epitaxy
What?... Why?... Types
Homoepitaxy
Vapour Phase Epitaxy
Hot-Wall Concept Youll see
Where does CVD take place?
How exactly does Epitaxial Growth take place?
Polytype control in Epitaxy
Unintentional Doping
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 3
SYNOPSI S Cont i nued
Intentional Doping
C:Si ratio
Dealing with the defects - I
Heteroepitaxy
Dealing with the defects II
Selective Epitaxial Growth
Summary
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 4
EPI TAXY
The stage is set courtesy Tairov and
Tsvetkov
Problems with Bulk Growth
The unique SiC properties, superior in comparison to
standard semiconductors, can be utilized only when the
material is of high quality.
Epitaxy here we come
Greek: epi = upon AND taxis = ordered
Why epitaxy?
Homoepitaxy and Heteroepitaxy
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 5
Types of Epi t ax y
Sublimation epitaxy Vodakov et al.
Vapour Phase Epitaxy
Growth more controllable
Liquid Phase Epitaxy
Molecular Beam Epitaxy
Very thin epitaxial layers nm/h growth rate!
Growth temperature quite low
Extremely precise control
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 6
VAPOUR PHASE EPI TAXY
Feed precursor gases : SiH
4
, C
3
H
8
Diluted in a carrier gas : H
2
Into a reaction chamber different types
Growing on a heated seed crystal
CHEMICAL VAPOUR DEPOSITION
PRINCIPLE
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 7
C.V.D.
Why CVD?
Redesign of III-V semiconductors reactor
Variety of SiC-CVD processes Your call!
Typical SiC-CVD
Deposition temperature: 1500 - 1650C
Pressure: 1 to 960 mbar
Temperature vs growth rate
Atmospheric or low pressure
Substrate rotation
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 8
The Hot -Wal l Conc ept
Cold-wall reactor graphite block, RF
heated from below
Hot-wall reactor graphite chamber
Horizontal hot-wall reactor first introduced
in 1993.
Hot hot hot crack crack crack!
The low thermal gradient takes care of it
allof what?
Thermal insulation
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 9
Hot Wal l Reac t or s
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 10
Sc hemat i c di agr am of an
at mospher i c -pr essur e CVD gr ow t h
syst em
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 11
Reac t or Desi gn Aspec t s
Demands layer uniformity, process control
Boundary layer problem higher gas-flow rate
Buoyancy-caused convection problems:
Reduction of layer uniformity
Memory effects
Remedies:
Low-reactor pressure
High carrier-gas flow-velocity
Low reactor-cell height
Choice of material:
Growth temperature: 1450 1650C
Radiation effective shielding
Thermal insulation
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 12
Schematic
Of Some
Horizontal
Reactions
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 13
Hor i zont al Reac t or s
Hot-wall reactor rotating substrate holder
Bigger reactor gas-insert / graphite liner
Drawback
limited possibility of multiple substrate growth
Rotational symmetry needed
Solutions
Planetary multi-wafer reactor (Aixtron, Epigress)
can handle seven 50-mm diameter substrates
Vertical reactor (Emcore) high gas-flow velocity,
high susceptor rotation-speed
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 14
Sc hemat i c s of t he Mul t i -Bat c h
Reac t or s
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 15
Epi t ax i al Gr ow t h Pr oc ess
Growth temperature 1450 - 1650C
Carrier gas Hydrogen
H
2
also acting as an etchantso?
Flow rates between 3 and 80 slm
Growth rate vs silane flow
Is reactor pressure a growth parameter?
Effect of growth parameters on C:Si ratio
Supersaturation
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 16
Typi c al Gr ow t h Sequenc e
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 17
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 18
You bet t er be of f t he ax i s!
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 19
St ep-c ont r ol l ed Epi t ax y
Terraces and steps on SiC {0001} surface
According to a classical growth theory, adsorbed species migrate on the
surface and are incorporated into the crystal at steps and kinks where the
surface potential is low. [ B.R.Pamplin, Crystal Growth, Pergamon press,
Oxford, 1975 ]
Doesnt nucleation occur on terraces?
On-axis {0001} faces Twinning 3C-SiC!!
Off-axis the steps shall guide thee!
Off-orientation towards <11.0> direction
preferred.
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 20
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 21
But Si r , I w as not dopi ng i t !
Unintentional doping
Site-competition epitaxy
C:Si ratio the Ruler of Dopingham!
Nitrogen is there in Si epitaxy too, isnt it?
What about C-faces?
Decreasing system pressure stops N
incorporation too!
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 22
I n Situ I nt ent i onal Dopi ng
(CH
3
)
3
Al, B
2
H
6
, N
2
, PH
3
Precursors
Why Aluminium? Abrupt doping profiles!
Phosphine or Nitrogen? You decide!
The house of a dopant atom Si or C.
Si: 1.17, C: 0.77, P: 1.10, N: 0.74, Al:
1.26, B: 0.82 (non-polar covalent radii)
Equivalent size of B-H compound: 1.10
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 23
I mpur i t y-I nc or por at i on
Mec hani sm C:Si r at i o
C:Si ratio measurements
High C:Si ratio N dopant hampered
Low C:Si ratio N dopant enhanced
Passivation of B acceptor Anneal it!
1 < C/Si ratio < 2 is Si-rich condition
3 < C/Si ratio < 6 is C-rich condition
Through systematic growth experiments under various
C/Si ratio and TMA flow rate conditions, heavily doped
p+ layers (p > 1019 cm-3) can be obtained on Si-faces
only.
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 24
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 25
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 26
Look at t he C-f ac e!
Unlike on the Si-face, dopant incorporation on C-faces
is independent of the C/Si ratio and almost constant.
Why?
How do adsorbed dopants reach the steps?
C-rich surface not so rich after all
Si-rich surface not justifying its name
either
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 27
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 28
To er r i s c r yst al !
High supersaturation
Low temperatures
Unstable step flow
Propagation of defects from substrate
Substrate surface preparation
CVD process
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 29
Cr yst al l i ne Def ec t s
Classification 0-, 1-, 2- and 3-D defects
Intrinsic Point Defects
Extrinsic Point Defects
Not always defects, you know!
Line Defects further classified
Edge and Screw Dislocations
Area defects
Volume defects
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 30
An edge dislocation; note the insertion of
atoms in the upper part of the lattice
A screw dislocation;
note the screw-like 'slip' of
atoms in the upper part of the
lattice
Photo of a Stacking Fault; Image
Source: http://lmass.uah.edu
- J. A. Gavira-Gallardo, J. D. Ng and
M.A. George
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 31
Basal Pl ane Ter r ac e
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 32
A 20 m t hi c k 4H-Si C epi l ayer w i t h var i ous def ec t s:
(a) mi c r opi pe; (b) t r i angl e def ec t ; (c ) gr ow t h
pi t s; (d) c ar r ot l i k e def ec t (Nomar sk i phot ogr aph)
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 33
Mi c r opi pes
What is a micropipe?
Recently it has been shown that the deposition of
epitaxial layers on the seeds can lead to a reduction in
the micropipe density.
Ignition of microplasma
Micropipe conversion vs C:Si ratio
Substrates with epitaxially closed micropipes could be
used as seeds for bulk sublimation growth in order to
decrease the micropipe density!
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 34
Sur f ac e i mages of an epi t ax i al l ayer i n Nomar sk i c ont r ast (a,
c ) and mi c r opi pes i n t he (000-1) 4H-Si C
subst r at e at t he same posi t i ons i n t r ansmi ssi on l i ght (b, d)
(C/Si = 0.9 (a, b); C/Si = 1.5 (c , d)).
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 35
St ep bunc hi ng
Poly-
type/
Face
Step
height >=
70% of
bilayers
Step
height ~
20% of
bilayers
6H/Si
3 -
6H/C
1 3
4H/Si
4 2
4H/C
1 2
Step height on off-cut substrates, in
number of Si-C bilayers at highest and
next highest probability
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 36
HETEROEPI TAXY
Growth of 3C SiC on Si substrates
Conventional reactor
Carbonization
Growth
Horizontal hot-wall low-pressure furnace
Efficiency measure
Buffer-layer optimizing parameters
Void formation a problem
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 37
The al t er nat i ve
het er oepi t ax y c hamber
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 38
Illustration of crystal
defects in 3C SiC: (right)
twin boundaries; (below)
anti-phase boundaries
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 39
An upc omi ng al t er nat i ve
Selective Epitaxial Growth (SEG) why
do we need it?
SEG and ELO go hand-in-hand!
Attractive features:
May reduce need for SiC etching
May reduce film tensile stress due to defects
ELO makes film forget the substrate!
Patterned SiC
Way to prevent leakage current
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 40
Sel ec t i ve Epi t ax y
Key factors
Growth temperature 1100 to 1400 C
Choice of mask material
Limiting factors
Oxide stability
Deposition time
The biggest challenge in SEG of SiC is based on the two
conflicting requirements: high growth temperatures and low
growth temperatures!
Masks
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 41
Sc hemat i c di agr am of SEG f ol l ow ed by ELO
pr oc ess; (a-c ) di f f er ent st ages of t he
over gr ow t h
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 42
Convent i onal SEG f ol l ow ed
by ELOG
First reported by Ohshita et al.
SEG of 3C-SiC/Si (100) using HCDS,
propane, H
2
and HCl gas by CVD at
1350C by Jacob et al.
Lower growth temperature use of
HMDS
Pyramidal Growth Okui et al.
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 43
Hi gh magni f i c at i on TEM i mage of Si C i n t he
w i ndow r egi on show i ng t he bendi ng of t he
def ec t s.
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 44
Schematic of the procedure for
pyramidal growth in mode A:
(a) CVD of thin SiC layer at
windows,
(b) Wet etching of SiO
2
mask,
(c) Dry etching of Si, and
(d) Regrowth of SiC.
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 45
Schematic of the procedure
for pyramidal growth in
another mode B:
(a) CVD of thin SiC layer at
windows after etching,
(b) Wet etching of SiO
2
mask, and
(c) Regrowth of 3C-SiC.
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 46
Out l ook
Lower off-axis angle substrates
development of a 3 inch epitaxial growth process at Infineon
Technologies AG for 4 off-cut substrates
Deleting the past glory?
CVD made more effective and moving ahead50 m
crossed!
CVD useful for investigation of defects in SiC and
improving bulk crystal substrates by micropipe healing
Hot-wall CVD fundamental now and great potential
SEG technique is a promising approach for
heteroepitaxial growth of 3C-SiC films, which are
useful for devices and MEMS applications.
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 47
Summar y
Epitaxy its origin, types and ways
Homoepitaxy Chemical Vapour
Deposition
The concept of hot-wall reactors
Site-competition and Step-controlled
epitaxy
Playing with defects
Heteroepitaxy Selective Epitaxial
Growth
3/5/2006 7:21 PM Epitaxial Growth of SiC thin films 48
REFERENCES
Akira Itoh and Hiroyuki Matsunami Single Crystal
Growth of SiC and Electronic Devices [Critical
Reviews in Solid State and Materials Sciences]
G. Wagner, D. Schulz, D. Siche Vapour phase growth
of epitaxial silicon carbide layers [Progress in Crystal
Growth and Characterization of Materials 47 (2003)
pages139-165]
Aparna Gupta, Chacko Jacob Selective epitaxy and
lateral overgrowth of 3C-SiC on Si: A review [Progress
in Crystal Growth and Characterization of Materials 51
(2005) pages 43-69]
Book: Process Technology for Silicon Carbide Devices
edited by Carl-Mikael Zetterling
Book: VLSI Technology S. M. Sze