Thin Film Deposition using Vacuum

Techniques

• Thermal evaporation

• Sputtering

• Pulsed LASER deposition (PLD)

Ch i vapour
• Chemical l deposition (CVD)

• Molecular beam epitaxy (MBE)

 Thin Film
Substrate: Thick supporting solid base

Commonly used Substrates: Glass, Silicon, Al2O3,

Quartz, Stainless steel, SiC
SiC, GaAs, Metal foils,
foils Plastic
Plastic, Thin film
Polymer sheets etc.

Substrate thickness: Several

S micrometer-millimeter
l i t
(µm-mm)

Thin film: Thin (two dimensional due to very small

thickness) layer of material that is deposited onto a Substrate
metal, ceramic, semiconductor or plastic base
(substrate)

Thickness: Few angstrom (Å) to 1 micrometer (µm)

Relation between the units of length/height:

1 mm = 103 µm, 1 µm = 103 nm, 1 nm = 10 Å
 Substrate Cleaning
Methods
• Chemical method
• Sputtering
Chemical cleaning of Si

•RCA cleaning
•Piranha cleaning

Cleaning process varies with the type of substrates

• Si Substrate: HF is required
Glass HF
• Glass: HFattacks
attacks
SiOSiO
2
 Thin Film Based Microelectronics
Silicon (Si) wafer SiO2 on Si Gold film on Si

Intel motherboard ICs Patterned wafer

 Low Dimensional Materials and Devices

Figure 1. (a) Single ZnO nanowire based UV/gas sensor, (b) ZnO thin film-nanowires hybrid
p-n junction, (c) patterning of ZnO nanowires, (d) ZnO microtubes, (e) c-axis growth of ZnO
nanowires, (f) ZnO single-nanowire based air-gap transistor, (g) AlN film based MEMS, (h)
ZnO nanowires-based transparent flexible transistor arrays, (i) Si nanowires, (j) ZnO
nanowires in Si microcavity, (k) ZnO nanoplatelets, and (l) AlN film based SAW devices.
 Properties of the Substrate and Thin Film
• Crystal orientation
• Thermal conductivity
• Thermal expansion
• Electrical resistivity
•Transparency
Thin Film
• Thermal stability
• Chemical stability
• Hardness Substrate
• Flexibility
• Smoothness
• Thickness
Thickness
• Resistance to radiation
• Transmittance
• Composition
 Applications of Thin Fims
• Microelectronics
• Thin film transistors
• Flat panel display
• Sensors and detectors
• Protective coat
Thin Film
• Decoration
• Antireflection coating
• Thin-film battery Substrate
• Seed layer for nanostructures
• Optoelectronics
• Data storage
• Microelectromechanical Systems (MEMS)
• Biotechnology
Bi t h l
• Photographic plate/mask
Microelectronics
Sensors Shape memory
Alloy & GMR

MEMS Energy
Applications
harvesting

Drug Surface Optoelectronics

delivery modification
 Characterization Techniques of Thin Films
* scanning electron microscopy (SEM)
transmission ec ron microscopy (TEM)
* scanning probe microscopies (STM, AFM ...)
* X-ray diffraction (XRD)
* Low energy electron diffraction (LEED)
* Reflection high energy electron diffraction (RHEED)
* Auger Electron Spectroscopy (AES)
* Energy Dispersive Analysis of X-rays (EDAX)
* X-ray Photoelectron Spectroscopy (XPS)
* Secondary Ion Mass Spectrometry (SIMS)
* Rutherford Backscattering (RBS)
* UV-Vis Spectroscopy
* FTIR Spectroscopy
* Raman Spectroscopy
* Luminescence Measurements (PL, EL, CL)
Ellipsometry
* Hall Measurements
* Current-Voltage Measurements (I-V)
* Capacitance-Voltage Measurements (C-V)
*Stress Measurement
* Hardness measurements
 Advantages of Thin Fims
• Large surface area
• Better quality
• Better efficiency
• Low power consumption
• Less consumption of materials
• Light weight and portable in size
• Material properties can be varied in a wide range
• Easy to pattern in micrometer range
• Easy to dope Thin Film
• Ease of Stacking layer fabrication
• Low cost
Substrate
 Disdvantages of Thin Fims
• Needs a substrate
• Requires high cost equipments for its growth
• Sensitive to chemical and moisture
• Needs a storage chamber at a cool, dry and dark place
• Chance of mismatching with the substrate

Thin Film

Substrate
 Thin Film Growth Techniques
•Physical vapor deposition *
Evaporation (thermal, e-beam)
Sputtering
Pulsed LASER deposition (PLD)
•Molecular beam epitaxy (MBE)

•Chemical vapor deposition (CVD)

Atmospheric pressure chemical vapor deposition (APCVD)
Low pressure chemical vapor deposition (APCVD)
Plasma enhanced chemical vapor deposition (PECVD)
Metal-organic chemical vapor deposition (MOCVD)
Photo chemical vapor deposition (PhotoCVD)

•Chemical method (non-vacuum technique)

Spin coating, Dip coating, Spray pyrolysis, Electroplating,
Electroless
 Physical Vapor Deposition (PVD)

PVD methods use mainly physical processes to deposit the films.

Types of PVD process

(a) Evaporation: Thin

Thifilms
filare producedd by either
d b evaporation
ith of ti f
solid or molten source

(b) Sputtering: Thin films are deposited by using energetic gaseous

ions in a plasma to knock off or sputter the atoms from a source
(target). These atoms /molecules then travel through the vacuum
and condense on the substrate surface to form the film.

(c) Pulsed LASER deposition (PLD): A high power pulsed laser beam
is focused inside a vacuum chamber to strike a target of source
material to grow its thin films.
 Thermal Evaporation

•High vacuum required (Al, Au, Cu, Al2O3, ZnO,…..)

• Low cost
•Wastage of materials in comparison to other vacuum methods
• Low temperature deposition and nontoxic method
•Parameters: Sub.-Source distance, Sub. Temp., Rate of heating,
flow rate of reactive gas, working pressure
Thin Film Deposition Process by Evaporation
• Vent and open the vacuum chamber
• Load the source (solid) material on the
• Load the filament substrate or samples
• Close the chamber
• Rough (low) vacuum by rotary pump
• High vacuum (10-6 torr) by diffusion or turbo pump
• Heat the filament by a specially designed electric power
• supply
• Increase the power slowly untill the evaporation starts
• Open the shutter
• Close the shutter after getting a film of desired thickness
• Slowly decrease the filament power
• Switch off the power supply of the filament
• Wait for the cooling of filament/chamber/substrate etc.
• Switch off vacuum gauges
• Close high vacuum valve
• Vent the vacuum chamber
• Collect thechamber
Close the thin film coated samples
• Create vacuum inside the
chamber.
 Filaments for Thermal Evaporation
Heating Materials (filaments): Tungsten, Molybdenum,
Tantalum
Shape: helical wire, basket, boat
• Conical baskets are better adopted to hold poorly wetting materials
i comparison
in i to helical
h li coils
l il
• Boats are good for evaporation of powder sources

Helical wire Conical Basket Boat

 Properties of Filaments/Boats
• High melting point (for W ≈ 3700 K)
• High corrosion resistance
• High temperature resistance (for W ≈ 3300 K)

• Lowest thermal expansion

I i to react with iother
• Inactive h hgases
• low vapor pressure at elevated temperatures
• Good electrical and thermal conductivity

• Non-toxic and bio-friendly

Types of Tungsten (W) Filament
•Pure W

•Doped W: doped with trace amounts of potassium (K), causing the

wire to exhibit an elongated interlocking grain structure with non-sag

properties after recrystallization.

 Melting Point of Metals
Metals (°C) Metals (°C)
Admiralty Brass 900 - 940 Cupronickel 1170 - 1240
Aluminum 660 Gold 1063
Aluminum Hastelloy C 1320 - 1350
Bronze 600 - 655
Inconel 1390 - 1425
Antimony 630 Incoloy 1390 - 1425
Beryllium 1285
Iridium 2450
Beryllium Copper 865 - 955 Iron 1536
Bismuth 271.4 Lead 327.5
Brass 930
Magnesium 650
Cadmium 321 Manganese 1244
Cast Iron, gray 1175 - 1290 Manganese
865 - 890
890
Chromium 1860 bronze
Cobalt 1495 Mercury -38.86
Copper
Copper 1084 Molybdenum
Molybdenum 2620
 Melting Point of Metals
Metals (°C) Metals (°C)
Monel 1300 - 1350 Stainless Steel 1510
Nickel 1453 Tantalum 2980
Niobium Thorium 1750
(Columbium) 2470
Tin 232
Osmium 3025 Titanium 1670
Platinum 1770
Tungsten 3400
Plutonium 640 Uranium 1132
Potassium 63.3 Vanadium 1900
Red Brass 990 - 1025
Yellow Brass 905 - 932
932
Rhodium 1965 Zinc 419.5
Selenium 217 Zirconium 1854
Silicon 1411
Silver 961
Sodium 97.83
Carbon Steel 1425 - 1540
 Advantages of Thermal Evaporation
• Little damage caused to substrate, since the substrates are not
subjected to energetic radiations/particles/ions.
• Deposited films are pure in comparison to aqueous (non-vacuum)
method. Because in a high vacuum, there are no residual gases or
particles to get incorporated in
in the film
film.
• Simple and low cost vacuum system
• Several thin
thi films can be deposited
b by one
b system by changing
b the th
filaments
• Deposition rate is high in comparison to sputtering
• Easy to handle
 Disadvantages of Thermal Evaporation
• When evaporation of films from a source containing
multicomponents (alloys/compound) the difference in the evaporation
rates, the composition of source material and thin film varies during
the process of evaporation.

•The melting point of source materials should be less than the melting
point
i tof the
th filament

•Materials with low vapor pressure (such as W) is difficult to evaporate

•There is no in-situ precleaning method of substrate like sputtering

• Poor step coverage

• More chances of contamination in comparison to e-beam

evaporation

• Consumption of source materials are more in comparison to

sputtering and e-beam evaporation
 Step Coverage by Thin Films
• Due to high vacuum, the mean free path of the gaseous species are
very large and therefore the evaporated species travel essentially in
straight-lines from the source (filament) to the substrate surface
f
•In fact, the source is ismall (point
( source),
i hi h that the
which means h
atoms arrive at a limited range of angles leading to poor step
coverage.
• Substrate rotation helps to widen the range of the arrival angle

Good step Poor step

coverage
coverage
Step coverage also depends on the sticking coefficient. The sticking
coefficient is the ratio of the number of species that actually stay or
stick on the surface relative to the
the number of
of incident species
species

Sticking coefficient can be increased by increasing substrate

temperature. OnOthe otherthhand, substrate
b heating
t t promotes surface
t
diffusion and change the film composition and microstructure.
 Flash Evaporation

Powder source
material
substrate
Vibrator
Guide
Boat

Vacuum
* Flash evaporation is similar to the thermal evaporation except the
limited supply of the sources.
* Flash evaporation is suitable for deposition of thin films of alloys and
compounds (ability to produce films of uniform composition).
* Because of the high temperature of the boat as well as the limited
amount of the source material, there will be no time for constituents to
build up by differential vapour pressure as a result of decomposition.
 e-beam Evaporation

E-beam Evaporaton - Shortcut.lnk

Deflecting
magnet

Focusing
magnet

Filament
• High vacuum required (Al, Au, Cu, 3
Al2O3, ZnO, ….)
• Less contamination and less wastage of materials in
comparison to thermal evaporation
•Low temperature deposition and nontoxic method
• Parameters: Sub.-Source distance, Sub. Temp., Rate of
heating, flow rate of reactive gas, working pressure
 e-beam Evaporation System
E-beam power supply
Crucible for Source

e-gun in
i
operation

Vacuum
system
 e-beam Evaporation
e-beam heater: A high-energy electron beam is focused on to the
source material in a crucible using magnetic field

Advantages
* e-beam heater can achieve higher temperature so that a wider range
of materials can be evaporated
•This preocess is cleaner (less contamination) since no metal
filaments are used (Note: Na, K are used in the production of tungsten
filament)
• Since only top of the surface in the e beam system is usually melted
e-beam melted,
so no contamination from the crucible occurs.

Disadvantages
•Needs expensive crucible, e-gun and its power supply (KWatt)
•X-rays can be emitted when an e-beam strikes source (e.g. Al). These
X-rays can create trapped charges in the surface of other thin films
(e.g. gate oxide on Si wafer) . Annealing of the film is required to
remove this damage.
• Difficult to deposit several thin films by one system due to the lack
of crucibles with many e-gun arrangements
Evaporation Vs Sputtering (Part-A)
Evaporation Vs Sputtering (Part-B)
Evaporation Vs Sputtering (Part-C)