INTEGRATED CIRCUIT

FABRICATION TECHNOLOGY

LECTURE -04

EPITAXY
VINOD G

Epitaxy
 Nomenclature

Epitaxy
Epi – upon
Taxis –
i ordered
d d

Chemically same material & 
Ch i ll t i l& ‐ Homoepitaxy  / 
H it /
substrate  Autoepitaxy

Chemically different  ‐ Heteroepitaxy
material & substrate
material & substrate
Epitaxy
 Epitaxy
p y
• Deposition of a thin film (0.5 to 20 µm) of a 
single crystalline layer over a single crystalline
single crystalline layer over a single crystalline 
substrate

E i
Epitaxial
i l Layer
L over Bulk
B lk Layer
L
• Often
Often grown under tightly controlled conditions & at 
grown under tightly controlled conditions & at
temperatures below melting point ‐ Better electrical 
quality 

Epitaxy
 Epitaxial Layer over Bulk Layer

• O
Often grown under tightly controlled conditions & at 
e g o u de g y co o ed co d o s a
temperatures below melting point ‐ Better electrical 
quality 

Epitaxy
 Need for Epitaxial Layer
• Minimise contamination levels
• Minimise pin holes / other structural defects 
h l / h ld f
– Defects often results in contamination during deposition
• Minimise stress in films
• Film should be mechanically stable
• Good adhesion to underlying layer
• Uniform thickness across the layer
Uniform thickness across the layer
– Conformal step coverage in horizontal and vertical
directions

Epitaxy
 Factors
• Deposition of film & technique
– Determined by the quality of film needed

• Quality of deposition means
– Composition
p
– Contamination levels
– Defect densityy
– Mechanical properties
– Electrical properties
Electrical properties
Epitaxy
 Problems with Heteroepitaxy
p y
• Substrate must be physically and chemically inert to 
growth environment
growth environment
• Should provide a damage free surface
• Chemical compatibility between material to avoid 
p y
compound formation
• Massive dissolution of one layer by another
• Layer & substrate should have closely matched thermal 
characteristics
– Prevents stress upon cooling to ambient
• Stress can lead to dislocation & can break the surface
• Layers should have closely matched lattice parameters

Epitaxy
 Ways to Grow Epi Layer
• MBE – Physical transport of material to a heated 
substrate – done by vacuum evaporation 
y p
– Delivery rate to substrate is very low
– High degree of control over the quality & thickness of the film
• VPE
VPE – Transport of constituents in the form of one or 
Transport of constit ents in the form of one or
more volatile compounds to substrate where they react 
to form epilayer 
– Excellent control of impurity concentration & crystalline
perfection
• LPE 
LPE – Growth by direct precipitation from liquid phase 
Growth by direct precipitation from liquid phase
– Slow growth rate – good to grow thin layers
– Used to grow III – V compounds

Epitaxy
 Vapour Phase Epitaxy
• Involves Chemical Vapour Deposition (CVD)
• Simplest & the most cost effective method SIC 
p
process 
• 5 fundamental steps
5 fundamental steps
– Reactants are transported to the substrate surface
• Reactants will be one of the chlorosilanes
– Reactants are adsorbed on the substrate surface
– Chemical reaction takes place leading to film 
formation & reaction products
– Reaction by‐products are desorbed from the surface
– By‐products are transported away from the surface
Epitaxy
 Grove Epitaxial Film Growth Model
• Considers only
– Reactants are transported to the substrate 
R d h b
surface
– Reactants are adsorbed on the substrate surface
R t t d b d th bt t f
– Chemical reaction takes place leading to film 
formation & reaction products
formation & reaction products
– Reaction by‐products are desorbed from the 
surface
– By‐products are transported away from the 
surface
Epitaxy
 Grove Model (1)

• F1 – Flux of the gas from the bulk 
Flux of the gas from the bulk
to the surface of the growing film
• F2 – Flux corresponding to the 
Flux corresponding to the
consumption of the reactant gas
• Cg – Concentration of the 
C i f h
reactant gas in the bulk
• Cs – Concentration of the gas at 
the surface of the substrate

Epitaxy
 Grove Model (2)

• Approximated that
Approximated that
F1  α (Cg – Cs)
F1 
1 = h
= hg (Cg – Cs)
;hg = gas phase mass transfer coefficient

F 2 α Cs
F2 = kks Cs
;ks = chemical surface reaction rate constant 

Epitaxy
 Grove Model (3)

• At steady state 
At steady state – no build up or depletion of material
F1 = F2 = F
⇒

If  hg >>ks, Cs → Cg  ⇒ Surface reaction rate control

If hg <<kks, C
If  h → 0 ⇒ mass transfer control
Cs → 0 f l

Epitaxy
 Grove Model (4)

Growth rate of epitaxial film, V (cm/sec)

So

Cg = CT Y
; CT = total no. of molecules /cm3 of the gas
;Y = mole fraction of the reaction species   
Epitaxy
 Grove Model (5)

So

2i
2 important effects predicted
ff di d
– Growth rate mole fraction of the mole fraction of 
the reacting species in gas phase
h h
– Growth rate at constant Y is controlled by smaller 
value of k
l f ks and h
d hg

Epitaxy
 Grove Model (6)

Limiting cases
V = CT Y ks // N1 – Surface reaction control
V = CT Y hg / N1 – Mass transfer control

hg is temperature independent and depends on the gas flow

ks describes the kinetics of the reaction at the surface
Chemical reactions are thermally activated →

k0 = temperature independent frequency factor
Ea = activation energy of the reaction

Epitaxy
 Grove Model (7)

At low temps. (hg>>ks)
– Growth rate controlled by ks 
– ks rises rapidly with temp. –
i idl ith t
reactant gas supply reaching 
the substrate cannot keep up 
with rate growth rate levels 
with rate – growth rate levels
off 
At high temps. (hg<<ks)
– Mass transfer rate dominates  
‐ growth rate becomes temp. 
insensitive
At intermediate temps. – both hg & 
ks contribute – reaction rate 
does not increase rapidly as
does not increase rapidly as 
at low temp.
Epitaxy
 Limitations of Grove Model

• Simplified model
Simplified model
– Neglects flux of reaction products
– Assumes that the reaction rate is dependent linearly 
Assumes that the reaction rate is dependent linearly
on the surface concentration – valid only for low Y
– Neglects the effect of gradient of temp. on the gas 
phase mass transfer

Predicts the growth rate in mass transfer and surface 
controlled regions ‐ Gives reasonable estimate of hg & 
ks  from growth rate data
from growth rate data

Epitaxy
 Si Growth rate as a Function of SiCl4
C
Concentration
t ti
• Growth rate rapidly 
departs from linearity
departs from linearity
– Growth rate of 1µm/min –
Crystalline
– Growth rate of 2 to 3
µm/min – Polycrystalline
• Even
Even at 0.1 mole fraction, 
at 0 1 mole fraction
growth rate begins to  Growth 
decay Etchingg
• For mole fraction > 0.27, 
etching occurs – due to the
presence of HCl on reduction of
SiCl4 in H2
Epitaxy
 Chemical Reactions in Silicon Epitaxy

Four major chemical sources
j
¾SiH4 – Silane
¾SiH2Cl2 – Dichlorosilane
¾SiHCl3 – Trichlorosilane
¾SiCl4 – Silicon tetra chloride

• Successive replacement of Cl atom with H atom makes 
the compound increasingly unstable
p gy
• Si epitaxy can be performed at temperatures successively 
lowered by 50°C as we go fromSiCl4 to SiH4

Epitaxy
Chemical Reactions in Silicon Epitaxy (1)

• Widely used method ‐ H2  reduction of SiCl4

• Not the only reaction taking place
• Presence of HCl and SiCl
P f HCl d SiCl2 also observed
l b d
– Leads a large no. of chemical reactions in the 
reaction atmosphere
ti t h
• Surface reactions
• Gas phase reactions
Gas phase reactions
Epitaxy
Chemical Reactions in Silicon Epitaxy -

Li t of
List f Reactions
R ti

Epitaxy
Chemical Reactions in Silicon Epitaxy (2)

Fig (1)
Fig (2)

Epitaxy
Chemical Reactions in Silicon Epitaxy
p y (2)

• Based
Based on the results from fig (2), the reactions 
on the results from fig (2) the reactions
can be summed up as 

Epitaxy
 Effect of Temperature
p

• Very
Very much a sensitive process
much a sensitive process
• Growth happens between 
1100°C & 1600°C
• Etching occurs outside this 
range
• Growth rate depends on
h
– Chemical source
– Deposition temperature
Deposition temperature
– Mole fraction of reactants

Epitaxy
 Alternate Growth

Pros
– Not reversible at normal processing temperatures
– No HCl as product –
l d no possibility of etching
bl f h

Cons
– No HCl – Cl could remove metallic impurities as 
chlorides
– Homogeneous gas phase reaction can occur –
p
powdery deposits on the reactor walls and wafers
y p

Epitaxy
 Doping of Epitaxial Layer
To control conductivity type & carrier concentration 
(electrical resistivity)
• Intentional Doping
– Epitaxial films with well controlled doping 
p p g
concentrations in the range of 1014 to 1020 atoms/cm3
can be achieved
• Autodoping & Outdiffusion
– To grow lightly doped layer (1014 to 1017 atoms/cm3) on a 
heavily doped substrate (1019 to 1021 atoms/cm3) 
– Substrate  ‐ uniformly doped (CMOS) or isolated regions 
of heavy doping buried layer ‐(bipolar applications)
of heavy doping – buried layer (bipolar applications)
Epitaxy
 Intentional Doping
• Intentional Doping
– Dopant gases are added to the reactant gases
Dopant gases are added to the reactant gases
• usually hydrides  ‐ toxic ‐ diluted to low concentration –
10 to 1000 ppm
pp
• Diborane (B2H6) – Boron
• Phosphine (PH3) – Phosphorous
• Arsine (AsH3) ‐ Arsenic
– Hydrides relatively unstable above room 
temperature but prevented from dissociating in gas 
phase by the H2 ambient in the reactor

Epitaxy
 Intentional Doping
p g (1)

• No simple rule yet to qualify the incorporation 
of dopant atoms from gas phase to Si film
of dopant atoms from gas phase to Si film
• Incorporation depends on
– Substrate temp.
Substrate temp
– Deposition rate
– Dopant mole volume relative to source gas mole 
D t l l l ti t l
volume
– Geometry of the reactor
Geometry of the reactor

Epitaxy
 Autodoping & Outdiffusion

• Dopants
Dopants from heavily doped substrate enter 
from heavily doped substrate enter
the epitaxial film by
– Outdiffusion (Solid state diffusion)
Outdiffusion (Solid state diffusion)
• Diffusion of impurity atoms into the growing film at 
elevated temp.
– Autodoping
• Evaporation of dopant atoms from the substrate, edges 
and backside of the wafer and their subsequent 
incorporation on the growing film 
• Necessary to contain evaporated dopants to reduce this
Necessary to contain evaporated dopants to reduce this

Epitaxy
 Autodoping & Outdiffusion (1)

• Manifests
Manifests themselves as 
themselves as
thicker transition layer 
between substrate &
between substrate & 
film
• Faster film growth can 
Faster film growth can
reduce this transition 
profile

Epitaxy
 Limitations to Technology

• Autodoping imposes limits on the minimum 
utodop g poses ts o t e u
thickness and doping of epilayer
• To reduce this
– Boron autodoping can be prevented by performing 
deposition process at lowest possible temp. and 
reasonable deposition rate
reasonable deposition rate
– Substrate and buried layer dopants with low vapor 
pressure and high diffusivity to be selected
• Sb (low vapor pressure) or P (high diffusivity) instead of As
– Operate epitaxial system at reduced pressures –
reduces lateral auto doping
reduces lateral auto doping
Epitaxy
 Limitations to Technology (1)

• Operate epitaxial system at reduced pressures
Operate epitaxial system at reduced pressures
• reduces lateral auto doping by increased diffusivity at 
reduced pressure
• dopant reaches main gas flow & is removed from the 
reactor –
• works well for As & P but not for B
works well for As & P but not for B
• Use ion implanted buried layer to reduce substrate 
surface contaminations
surface contaminations

Epitaxy
 Defects in Epitaxial Films

• Process induced crystalline defects due to
Process induced crystalline defects due to
– Reactor contamination
– Substrate Preparation
p
– Substrate imperfection
• Crystal
Crystal quality cannot surpass that of the 
quality cannot surpass that of the
substrate – take great care in substrate 
preparation
• Common defects are dislocations & stacking 
faults

Epitaxy
 Dislocations

• Mechanisms
– Propagation of a dislocation line in the substrate 
on to the grown film
on to the grown film
– Large lattice parameter difference between 
substrate and film – heavily doped substrate and 
substrate and film  heavily doped substrate and
lightly doped film resulting in misfit dislocations
– Thermal stress exceeding yield strength if silicon –
gy g
results in slip

Epitaxy
 Thermal Stress
• Due to the difference in temp. between 
the front end and back end of the
the front end and back end of the 
wafer
• Front side radiates heat while back side 
cannot Front side
Front side
– Different thermal expansion rates 
between the sides
– Wafer bowing at the back side 
W f b i h b k id
Back side
– Results in heat confining to smaller area 
– side heated less & cooled to lower 
susceptor
t
temp. ‐ more bowing
b i
– Stress levels exceeds yield strength of Si 
at elevated temp. – results in crystal slip
• Severe for large dimension wafers
f l f
Epitaxy
 Thermal Stress - Solutions
• Design sample holders into pockets
– Wafer contacts susceptor only at the edges

• Pl
Placing heat reflectors above the wafer
i h t fl t b th f
• Use a radiant or IR heater focusing on the front 
side of the wafer – heat flux through the wafer 
side of the wafer  heat flux through the wafer
decreases
Epitaxy
Stacking Faults

Epitaxy
Silicon Source Deposition Characteristics

Epitaxy
 Considerations

• SiCl4
– High deposition temp. – autodoping & outdiffusion
– Very little deposition on the reactor walls – clean 
process
– Used for thick layer deposition

• SiHCl3
– Temp. somewhat low compared to above – faster 
growth rate Used for thick layer deposition
growth rate ‐ Used for thick layer deposition
– No significant advantage compared to films formed by 
using SiCl4

Epitaxy
 Considerations (1)

• Si H2Cl2
– Used for thin layer deposition
Used for thin layer deposition
– Operating temp. even lower
– High quality films ~ 1000°C
– Lowest defect densities
d f d
– Increased device yield

• SiH4
– Thinnest layer at a lower temperature of 1000°C
– Substantially less autodoping & outdiffusion
Substantially less autodoping & outdiffusion
– SiH4  can decompose at low temperatures leading to heavy 
deposition on the reactor walls
– Reduced effective throughput
R d d ff ti th h t
Epitaxy
Epitaxial
p Process Sequence
q

Epitaxy
 Chemical Vapour Deposition Equipment
High temperature , batch, CVD systems
• Demands
– Tight thickness & resistivity control
Ti h hi k & i i i l
– Low number of process induced defects
– Minimised pattern shift and washout
– Reduced autodoping
– Reduced operating temperature
– High productivity
High productivity
– Capability of handling the specified wafer

• 2 major commercially viable equipments
2 j i ll i bl i
– Barrel reactor
– Pancake reactor

Epitaxy
 Pancake reactor

Horizontal reactor

Vertical reactor

Epitaxy
Barrel Reactor

Epitaxy
 Molecular Beam Epitaxy

• Non
Non CVD process
CVD process
• Uses evaporation 
method
• Direct physical transport 
of the material to be 
f h i l b
grown or its 
components to the h
heated substrate 

Epitaxy
 Molecular Beam Epitaxy (1)

• Growth
Growth achieved by directing atomic / molecular 
achieved by directing atomic / molecular
beams in a well controlled , high vacuum system
• Uses elemental solid sources
Uses elemental solid sources
– Contamination minimum
– Need to open the vacuum chamber to replenish the 
Need to open the vacuum chamber to replenish the
reactants
• Materials
Materials transported from effusion cells I 
transported from effusion cells I
gaseous form
Done at ultra high vacuum (10‐8 to 10
• Done at ultra high vacuum (10 to 10‐10 torr)
Epitaxy
 MBE –Advantages
Advantages & Disadvantages
Advantages
• UHV ‐ Collision of atoms unimportant
• Growth of uniform surface
• Conventional MBE @400
Conventional MBE @400°C C to 800
to 800°C
C
• Higher growth than CVD
• Wider choice of dopants

Disadvantages
• Low throughput
Low throughput
• Expensive

Epitaxy
 MBE Growth Chamber

RHEED – Reflective High Electron Energy Diffraction

Epitaxy
 MBE Growth Chamber (1)

• Uses Mo block to mount wafer
– Rotated during growth at a few rpm for layer 
uniformity
• Growth chamber backed up by a sample 
introduction chamber – separately pumped and 
interconnected by high vacuum gate valves
• Cassette loading – many slices at a time
• Final wafer preparation is done in the chamber 
prior to growth
p y g
• Low pressure maintained by the cooling shrouds
Epitaxy
 MBE Growth Chamber (2)

• High
High energy electrons, 10 to 50 KeV range, 
energy electrons 10 to 50 KeV range
impinges on the substrate and reflects on to a 
fluorescent screen
fluorescent screen

Epitaxy
 MBE over CVD

• Low temp processing 
Low temp processing – used in VLSI
used in VLSI
– Reduces outdiffusion & autodoping
• Precise
Precise control of doping
control of doping
• Doping not affected by time constraints –
complex doping profiles can be easily 

Epitaxy