BITS Pilani

Sindhu S
BITS Pilani Dept of Physics, BITS Pilani, Pilani Campus
Dept of EEE, WILP Division, Bangalore
Pilani Campus
MELZG 611
IC Fabrication Technology
Lecture No.9
Date . 02/09/2023
• Epitaxy is the type of silicon
deposition that results in single
crystal growth due to contact with a
suitable crystalline lattice.

• Epitaxy usually performed using the

wafer, for economic reasons.
• Mechanism of epitaxial growth
• Methods of epitaxial deposition
• Properties of epitaxial layers
• Applications of epitaxial layers
 What is Epitaxy?
• Epitaxy: Deposition and growth of
monocrystalline structures/layers.

• Epitaxial growth results in

monocrystalline layers differing from MBE growth mechanism *
deposition which gives rise to
polycrystalline and bulk structures.

• Epitaxy types:
– Homoepitaxy: Substrate & material are
of same kind.
(Si-Si)
– Heteroepitaxy: Substrate & material
are of different kinds. (Ga-As)

MBE growth mechanism

5
 Epitaxial Growth

• Deposition of a layer on a Ordered,

substrate which matches the crystalline
crystalline order of the growth;
substrate NOT
epitaxial
• Homoepitaxy
– Growth of a layer of the same
material as the substrate
– Si on Si
• Heteroepitaxy Epitaxial
growth:
– Growth of a layer of a different
material than the substrate
– GaAs on Si
 Why Epitaxy?
• Epitaxial growth is useful for applications that place
stringent demands on a deposited layer:
– High purity
– Low defect density
– Abrupt interfaces
– Controlled doping profiles
– High repeatability and uniformity
– Safe, efficient operation
• Can create clean, fresh surface for device fabrication
General Epitaxial Deposition Requirements

• Surface preparation
• Clean surface needed
• Defects of surface duplicated in epitaxial layer
• Hydrogen passivation of surface with water/HF
• Surface mobility
• High temperature required heated substrate
• Epitaxial temperature exists, above which
deposition is ordered
• Species need to be able to move into correct
crystallographic location
– Relatively slow growth rates result
• Ex. ~0.4 to 4 nm/min., SiGe on Si
Thin film
 Epitaxy Techniques
• Vapor-Phase Epitaxy (VPE)
– Modified method of chemical
vapor deposition (CVD).
– Undesired polycrystalline layers
– Growth rate: ~2 µm/min.
• Liquid-Phase Epitaxy (LPE)
– Crystal layers are from the melt
existent on the substrate.
– Hard to make thin films
– Growth rate: 0.1-1 µm/min.
• Molecular Beam Epitaxy
(MBE)
– Relies on the sublimation of
ultrapure elements, then
condensation of them on wafer
– In a vacuum chamber (pressure:
~10-11 Torr).
– “Beam”: molecules do not collide
to either chamber walls or existent
gas atoms.
– Growth rate: 1µm/hr.
9
• Epitaxy is the type of silicon deposition
that results in single crystal growth due to
contact with a suitable crystalline lattice.

• Epitaxy usually performed using the

wafer, for economic reasons.
• Mechanism of epitaxial growth
• Methods of epitaxial deposition
• Properties of epitaxial layers
• Applications of epitaxial layers
 Epitaxial Growth

• Deposition of a layer on a Ordered,

substrate which matches the crystalline
crystalline order of the growth;
substrate NOT
epitaxial
• Homoepitaxy
– Growth of a layer of the same
material as the substrate
– Si on Si
• Heteroepitaxy Epitaxial
growth:
– Growth of a layer of a different
material than the substrate
– GaAs on Si
 Why Epitaxy?
• Epitaxial growth is useful for applications that place
stringent demands on a deposited layer:
– High purity
– Low defect density
– Abrupt interfaces
– Controlled doping profiles
– High repeatability and uniformity
– Safe, efficient operation
• Can create clean, fresh surface for device fabrication
General Epitaxial Deposition Requirements
• Surface preparation
– Clean surface needed
– Defects of surface duplicated in epitaxial layer
– Hydrogen passivation of surface with water/HF
• Surface mobility
– High temperature required heated substrate
– Epitaxial temperature exists, above which deposition is ordered
– Species need to be able to move into correct crystallographic
location
– Relatively slow growth rates result
• Ex. ~0.4 to 4 nm/min., SiGe on Si
 Vapor Phase Epitaxy
• Specific form of chemical vapor deposition (CVD)
• Reactants introduced as gases
• Material to be deposited bound to ligands
• Ligands dissociate, allowing desired chemistry to reach
surface
• Some desorption, but most adsorbed atoms find proper
crystallographic position
• Example: Deposition of silicon
– SiCl4 introduced with hydrogen
– Forms silicon and HCl gas
– Alternatively, SiHCl3, SiH2Cl2
– SiH4 breaks via thermal decomposition
 Precursors* for VPE

• Must be sufficiently volatile to allow acceptable

growth rates
• Heating to desired T must result in pyrolysis
• Less hazardous chemicals preferable
– Arsine highly toxic; use t-butyl arsine instead
• VPE techniques distinguished by precursors used

( precursor is a compound that participates in the chemical reaction that produces another
compound)
(pyrolisis decomposition brought about by high temperatures)
 Varieties of VPE
• Chloride VPE
– Chlorides of group III and V elements
• Hydride VPE
– Chlorides of group III element
• Group III hydrides desirable, but too unstable
– Hydrides of group V element
• Organometallic VPE
– Organometallic group III compound
– Hydride or organometallic of group V element
• Not quite that simple
– Combinations of ligands in order to optimize
deposition or improve compound stability
– Ex. trimethylaminealane gives less carbon
contamination than trimethylalluminum
 Other Methods
• Liquid Phase Epitaxy
– Reactants are dissolved in a
molten solvent at high
temperature
– Substrate dipped into solution
while the temperature is held
constant
– Example: SiGe on Si
• Bismuth used as solvent
• Temperature held at 800°C
– High quality layer
– Fast, inexpensive
– Not ideal for large area layers
or abrupt interfaces
– Thermodynamic driving force
relatively very low
• Molecular Beam Epitaxy
– Very promising technique
– Elemental vapor phase
method
– Beams created by
evaporating solid source in
UHV
 Properties of Epitaxial Layer
• Crystallographic structure of film reproduces that of
substrate
• Substrate defects reproduced in epi layer
• Electrical parameters of epi layer independent of
substrate
– Dopant concentration of substrate cannot be reduced
– Epitaxial layer with less dopant can be deposited
• Epitaxial layer can be chemically purer than substrate
• Abrupt interfaces with appropriate methods
 Applications
• Engineered wafers
– Clean, flat layer on top of less
ideal Si substrate
– On top of SOI structures
– Ex.: Silicon on sapphire
– Higher purity layer on lower
quality substrate (SiC)
• In CMOS structures
– Layers of different doping
– Ex. p- layer on top of p+
substrate to avoid latch-up
 More applications
• Bipolar Transistor
– Needed to produce buried
layer
http://www.search.com/reference/Bipolar_junction_transistor
• III-V Devices
– Interface quality key
– Heterojunction Bipolar
Transistor
– LED
– Laser
http://www.veeco.com/library/elements/images/hbt.jpg
 Summary
• Deposition continues crystal structure
• Creates clean, abrupt interfaces and high
quality surfaces
• High temperature, clean surface required
• Vapor phase epitaxy a major method of
deposition
• Epitaxial layers used in highest quality wafers
• Very important in III-V semiconductor
production
 Liquid-Phase Epitaxy
• Molten semiconductor material is poured
directly onto wafer
• After allowing material to cool for a specified
time the non-bonded material is wiped away
• Wafer must then be reground and polished for
further processing
Drawbacks to Liquid-Phase Epitaxy
• Considered as economically undesirable due
to the costs incurred to repolish the wafer
after each step

• Also it is difficult to accurately control the

thickness of the epi layer in this process
 Low Pressure Chemical Vapor Deposition
(LPCVD Method)
• Wafers are mounted on an inductively heated
block and a mixture of Dichlorosilane and
hydrogen gas is passed over the wafers. These
gases react at the wafer surface to create a
slow growing layer monocrystalline silicon.
LPCVD Systems
 Advantages of LPCVD Method
• The rate of silicon growth can be regulated by varying
the temperature, pressure, and gas mixture.
• No polishing is required as the vapor deposited
silicon will faithfully reproduce the structure of the
underlying lattice.
• The epitaxial film can also be doped by adding small
amounts of gaseous dopants such as phosphine or
diborane.
 Advantages / Disadvantages of Epitaxy
• ADVANTAGES • DISADVANTAGES
• Create stacks of • Time required to grow
differently doped layers silicon layers
useful in the creation of • High cost of equipment
bipolar transistors used in process
• Create buried layers
 Vapor-phase epitaxy
• Layer formation by chemical reaction between
gaseous compounds.
• Also known as CVD.
• Can be performed at atmospheric pressure
(APCVD) or low pressure(LPCVD).
• Susceptors are made from graphite blocks.
Steps involved:
• Reactants transported to
substrate region.
• Transferring the reactants to
the substrate surface where
they are adsorbed.
• Chemical reaction followed
by growth.
• Gaseous products are
desorbed into the main gas
stream.
• Reaction products are
transported out of the
reaction chamber.
 Optimizing different process parameters

• Parameters:
– Temperature
– Pressure
• Temperature:
– High temperature => higher mobility
– But increases thermal stress
• Pressure:
– At low pressure, increase in velocity of gas stream can be
attained for the same amount of gas at normal pressure.
• LPCVD process
 Silicon CVD
• Main sources:
• Silicon tetrachloride
• Dichlorosilane
• Trichlorosilane
• Silane
• Commonly uses SiCl4high temp. process.
• Others used because of lower temperature.
SiCl4 + 2H2  Si (solid) + 4HCl (gas)
Accompanying reaction:
SiCl4 + Si (solid)  2SiCl2 (gas)
 Chemical Vapor Deposition
• Gases dissociate on surfaces at high temperature
• Typically done at low pressure (LPCVD) rather than
atmospheric (APCVD)
• LPCVD pressures around 300mT (0.05% atmosphere)
• Moderate Temperatures
– 450 SiO2
– 580-650 polysilicon
– 800 SixNy
• Very dangerous gases
– Silane: SiH4
– Arsine, phosphine, diborane: AsH3, PH3, B2H6
 Benefits and Drawbacks of MBE
Advantages Disadvantages
 Clean surfaces, free of an oxide layer  Expensive (106 $ per MBE chamber)

 In-situ deposition of metal seeds,  ATG instability

semiconductor materials, and dopants

 Low growth rate (1μm/h)  Very complicated system

 Precisely controllable thermal evaporation  Epitaxial growth under ultra-high vacuum

conditions

 Seperate evaporation of each component

 Substrate temperature is not high

 Ultrasharp profiles

34
 Applications
• Novel structures as quantum devices
• Silicon/Insulator/Metal Sandwiches
• Superlattices
• Microelectronic Devices

TEM image of MBE Growth of Ultra-Thin InGaAs/AlAsSb Quantum Wells*

35
 Conclusions
• Typically in ultra-high vacuum
• Deposition rates are very low (1monolayer/second)
• Very well controlled (Shuttering: 0.1s)
• Grow films with good crystal structure
• Often use multiple sources to grow alloy films
• Deposition rate is so low that substrate temperature
doesn’t need to be as high
• Expensive
• Sophisticated system

36
• Advantages
– Low deposition temp
– Precise control of layer thickness and doping profile
(excellent uniformity)
– Versatile (used for fabricating heterostructures, quantum
wells, etc)
– In-situ cleaning and characterization
• High temp. baking to decompose native oxygen.
• Low energy ion beam of inert gas to sputter impurity.
• Disadvantage:
– Expensive (UHV), very slow deposition
 Defects in epitaxial layers
• Defects from substrates
• Defects from interface.
• Precipitates or dislocation loops.
• Misoriented areas of an epitaxial film (low
angle grain boundary)
• Edge dislocation
• In heteroepitaxy of two lattice-mismatched
semiconductor.
 LPCVD
• Advantages: : • Disadvantages
• • Excellent uniformity of • Slows down deposition
thickness & purity rate
• • Simple • • Requires high
• •Reliable/reproducible temperatures, <600°C
• Homogenous layer
 Molecular Beam Epitaxy

• Evaporation at very low deposition rates

• Typically in ultra-high vacuum
• Very well controlled
• Grow films with good crystal structure
• Expensive
• Often use multiple sources to grow alloy films
• Deposition rate is so low that substrate temperature
does not need to be as high
 MBE ( Molecullar Beam Epitaxy)
• Evaporation of Si (or any other
semiconductor) and desired dopants
under very high vacuum (10-8 Torr)
and low Temp (4000 - 8000C) higher
temp gives better properties
– Predominantly used for III-V
semiconductors
• Atoms or molecules are directed to
heated substrate in ultra high vacuum
(UHV)
• By utilizing very low growth rates (≈
1μm/hour) can tailor doping profiles
and composition on a monolayer
scale.
 MBE: Working Principle
 Epitaxial growth: Due to the interaction of
molecular or atomic beams on a surface of a
heated crystalline substrate.

 The solid source materials sublimate

 They provide an angular distribution of
atoms or molecules in a beam.
 The substrate is heated to the necessary
temperature.
A typical MBE system*  The gaseous elements then condense on the
wafer where they may react with each other.

 Atoms on a clean surface are free to

move until finding correct position
in the crystal lattice to bond.
 Growth occurs at the step edges
formed: More binding forces at an
Molecular Beam Epitaxy**
edge.
42
 MBE: Working Conditions
 The mean free path (l) of the
particles > geometrical size of the
chamber (10-5 Torr is sufficient)

Mean free path for Nitrogen molecules at 300 K *

Ultra-high vacuum (UHV= 10-11Torr) to obtain sufficiently clear epilayer.

Gas evalution from materials has to be as low as possible. Pyrolytic boron
nitride (PBN) is chosen for crucibles (Chemically stable up to 1400°C)
Molybdenum and tantalum are widely used for shutters.
Ultrapure materials are used as source.

The mean free path is the average distance traveled by a moving particle (such as an atom, a molecule, a
photon) between successive impacts (collisions), which modify its direction or energy or other particle
properties
43
 MBE: Results and Control Mechanisms
 Control of composition and doping of the growing structure at monolayer via computer
controlled shutters
 Growth rates are typically on the order of a few A°/s and the beams can be shuttered
in a fraction of a second allowing nearly atomically abrupt transition from one material
to another.)
 Independent heating of material sources
 RHEED (Reflection High Energy Electron Diffraction) for monitoring the growth of the
crystal layers.

RHEED oscillations *

 Mass spectrometer for monitoring the residual gases and checking source beams for leaking
 A cryogenic screening around the substrate as a pump for residual gases.

Reflection high-energy electron diffraction (RHEED) is a technique used to characterize the surface
of crystalline materials. RHEED systems gather information only from the surface layer of the sample,
which distinguishes RHEED from other materials characterization methods that also rely on
44
diffraction of high-energy electrons
MBE System at Max Planck Institute –Halle,
Germany

1. Manipulator

2. Rheed System

3. Electron Beam Evapor

on Source

4. Pyrometer

5. Thermal Evaporation S
rce

6. Ion Guage

7. Quadropole Mass
Spectrometer
 Manipulator
 The manipulator holds the wafer on four feet with special carbon plates, which
position it in the centre.
 The standard wafer size for MBE chamber is 5inch. Smaller ones can only be
used by adapter rings.
 The sample can be heated up to a temperature of 900°C. The heater is a
carbon meander which is thicker in the middle an thinner at the outside. By
this shape one achieves a better homogeneity of the temperature across the
wafer. The rotation of the wafer improves the homogeneity of the deposited
layers.
 The determination of the temperature of the wafer is not that simple since we
can't measure it directly. In our chamber we have a thermocouple available
which is situated around 1cm above the wafer. The thermocouple can be
calibrated by a modified Si wafer containing a thermocouple inside.
 RHEED system

The RHEED system in our MBE chamber is used

for in situ investigations of the surface of the
wafer and the layer growth.
The maximum voltage is 35kV and the RHEED
pictures from the screen can be taken by a
camera and saved to a file on the computer.
The software also allows us to take movies from
RHEED patterns.
 The electron beam evaporation sources
 The silicon source is a 10KW electron beam evaporation source.
 The other two electron beam evaporation sources work with a maximum
power of 4KW. All these sources are supplied with computer controlled
shutters and water cooled shields.
 In order to reduce the necessary energy for the evaporation we use liners
in the shape of the crucible in the copper crucibles.
Principle of electron beam evaporation

The electrons emitted by the filament are deflected by electric and magnetic fields
towards the the evaporation material. In this way one avoids atoms and ions from the
cathode hitting the ingot.
 Pyrometer
 The pyrometer applied to our MBE chamber is used for
additional control of the wafer temperature.
 As long as the emission coefficient of the wafer doesn't change,
we can compare the temperatures measured by pyrometer and
by thermocouple respectively.
 The pyroelectric detector of our pyrometer is sensitive for a wave
length range from 12 to 14 µm.
 In this range the transmission of silicon is lower than 50% so that
it measures the temperature of the wafer as well as the
temperature of the heater above.
 For such measurements in the mentioned IR region, a special
window material has to be used. In our cse we have chosen ZnSe.
 Thermal evaporation source

For the evaporation of the doping materials we apply

thermal evaporation sources.
They are installed in water cooled flanges at the side
of the chamber.
They are inclined to the wafer normal by about 30°.
The crucibles of our doping sources are heated by
thermal radiation.
The temperatures of the crucibles are measured by a
thermocouples and regulated by EurothermTM
controllers.
 Ion gauge

The pressure in MBE machine is measured by

several not screened hot filament ion gauges.
In the range of 10-11mbars one normally should
use an ion gauge with a screened cathode to
reduce the error by x-rays.
But during growth processes we have a working
pressure of 10-9mbars so that the unscreened
cathode is totally sufficient for our purposes.
 The quadrupole mass spectrometer

Our growth chamber is supplied with two quadrupole

mass spectrometers which are mainly used to control
the flux of the electron beam evaporation sources.
They are connected to EurothermTM controllers which
regulate the heating current of the filaments of the
electron beam evaporation sources.
Our mass spectrometers work in a mass range from 1
to 300 amu
 MBE System consists of-
• Three vacuum chambers:
• the loading chamber,
• the buffer chamber and
• the growth chamber.
– The loading chamber and the buffer chamber are pumped by turbomolecular pumps.
– The growth chamber is equipped with an ion pump, a turbo-molecular pump and a
titanium sublimation pump.
– Additionally the chamber contains cooling shields (liquid nitrogen). The typical
working pressure in the growth chamber is in the range of 2 x 10 -9mbars.
– The growth chamber is equipped with three electron beam evaporation sources
which we use for the evaporation of silicon, germanium and other materials and with
up to four thermal evaporation cells which are mainly used as doping sources-use
materials like aluminium, antimony and boron.
– The growth chamber contains a manipulator for 5 inch wafers, a RHEED system,
2 quadrupole mass spectrometers and 2 quartz monitors.
– The buffer chamber is equipped with a transport system which can hold a cassette. In
this cassette we can store up to eight wafers under ultra high vacuum conditions. Via
a transfer rod the wafers can be moved into the growth chamber.
 Benefits and Drawbacks of MBE
Advantages Disadvantages
 Clean surfaces, free of an oxide Expensive (106 $ per MBE
layer chamber)
 In-situ deposition of metal seeds, Very complicated system
semiconductor materials, and
dopants
 Low growth rate (1μm/h) Epitaxial growth under ultra-high
vacuum conditions
 Precisely controllable thermal
evaporation
 Seperate evaporation of each
component
 Substrate temperature is not high

 Ultrasharp profiles
54
 Applications
• Novel structures as quantum devices
• Silicon/Insulator/Metal Sandwiches
• Superlattices
• Microelectronic Devices

TEM image of MBE Growth of Ultra-Thin InGaAs/AlAsSb Quantum Wells* 55

 What does the sample look like ?

•optical microscopy
•on a macroscopic scale
•scanning electron
•on a microscopic scale
microscopy (SEM)
•on an atomic scale
•transmission electron

microscopy (TEM)
•scanning probe

microscopies (STM, AFM..)

 What is the sample made of ?
• Auger Electron Spectroscopy
• elemental (AES)
• Energy Dispersive Analysis of
composition
X-rays (EDAX)
• impurities
• X-ray Photoelectron
• chemical states
Spectroscopy (XPS)
• Secondary Ion Mass
Spectrometry (SIMS)
• Rutherford Backscattering
(RBS)
What are the electrical properties of the sample?

• device properties
• resistance - four
• material properties
point probe
• resistance / conductance
• capacitance
• capacitance • ……
What are the optical properties of the sample ?

• refractive index, absorption

• dielectric properties
• ellipsometry
• as a function of wavelength
• ……
What are the magnetic properties of the sample ?

• magneto-optical Kerr effect

• hysteresis loops (MOKE)
• magnetization • ferromagnetic resonance
(FMR)
• vibrating sample magnometry
• SQUID magnetometry
• ……..