Processes for Micro and

Nano technologies
Yosi Shacham-Diamand

Fall 2017

Lecture 4: Then filmes - metals

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 Thin films (I) – metals

• Physical vapor deposition (PVD)

– Vacuum systems,
– principles of sputtering,
– various methods,
– modeling of sputtering,
– step coverage,

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Introduction to Vacuum Sciences

• Kinetic theory of gases

• Introduction to vacuum systems
– gas flow and conductance
– vacuum pump technology
– vacuum seals
– pressure measurement
• Rough vacuum pumps

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 Motivation

• A large number of semiconductor materials processing

techniques operate at pressures other than atmospheric
– chemical vapor deposition < 1 atm (760 Torr)
– plasma etching mTorr
– physical vapor deposition high vacuum
– molecular beam epitaxy ultra high vacuum (UHV)
• The vacuum environment will in many cases have a very
important influence on the structure, property and performance
of the fabricated materials
• An understanding the basics of vacuum (and plasmas) is a
necessity in the semiconductor industry
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 The kinetic theory of gases (1)
• All particles have various modes (or degrees of freedom) of energy
storage: gases at room
temperature
electronic vibrational rotational translational
highest energy lowest energy

• There are three translational

degrees of freedom: vx, vy, vz v
vz
• The total velocity of a molecule vy
vx
is the vector sum of these three
components:
v 2  vx2  v y2  vz2 sphere of
radius
5 c
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 The kinetic theory of gases (2)
• The absolute magnitude of v is the molecular speed c (note: c is
a scalar quantity
• The molecular translational energy of one degree of freedom is:
1 2 this is for the x-direction; similar
Etx  mvx expressions for the y- and z-directions
2
• At thermal equilibrium, we know from Boltzmann statistics that
for each degree of freedom, the probability of finding a molecule
at energy E is exponentially distributed in energy according to
the Boltzmann factor: exp(-E/kT)
• This provides the maximum number of ways of arranging a
group of molecules among the available energy states to
yield the same total energy for the group

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 The kinetic theory of gases (3)
• From before: v 2  c 2  vx2  v y2  vz2
• The probability of finding a molecule at speed c and energy ½mc2
will be proportional to the number of ways of distributing the
energy among the x,y,z components (the degeneracy of this
energy level)
• The degeneracy is proportional to the surface area of the sphere
of radius c in velocity space: 4c2
• The probability that a molecule will have a certain velocity will
depend on the product of the c2 and the exponential terms
– leads to a peak in the velocity distribution
– when evaluated over all space, the integral of the distribution
must equal unity
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 The kinetic theory of gases (4)

• Gas molecules are continually

colliding with each other and with
containing surfaces
• The energy exchange leads to an
equilibrium distribution of the
molecular speeds (the Maxwell -
Boltzmann distribution) given by:
32
 m 
P  v   4v 2   exp  mv 2 2kT 
 2 kT 
molecular mass (kg) Boltzmann’s constant temperature in K
1.3810-23 J/K (not ºC!!!)

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 Kinetic theory of gases (5)
4.5

4
• Average speed:

v  c   v Pv  dv 
3.5 8kT
3 0 m
P (v )*104

2.5

2
• Average component in any direction:
2kT
1.5
vx  v y  vz 
1 m
• Root-mean square velocity:
0.5

0
0 2000 4000 6000
Velocity (m/s) 3kT 3RT
vrms  
Maxwell-Boltzmann distribution m M
for hydrogen at room temperature per mole
per atom
 v =2404 m/s vrms=2609 m/s
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 Some results from the kinetic theory
• The mean free path is the average distance that a molecule will
travel before it strikes another molecule:
1

2d 2 n
• We can write the ideal gas law using n = molecules/unit volume as
n  P kT (R = Nok)
• The mean free path thus becomes
kT directly affects vacuum

2d 2 P system design

• The impingement rate (molecules cm-2 sec-1) is given by

P shows up in a large
Jn 
2mkT number of calculations
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 Useful quantities in describing gas flow

• There are two ways to describe the flow of gas through a

pumping port in a vacuum system:
 pumping speed (SP) -- volume of gas passing per second
 throughput (Q) -- pressure times the pumping speed

gas mass: G  V
dG
mass flow rate: qm  dt
P,V
Q
P
throughput: Q  qm

Pumping speed = SP Q dVP
pumping speed: S P  
PP dt
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 A note on units

• The torr is the most commonly used unit of pressure

– 1 torr: raises a column of Hg 1 mm (1 atmosphere = 760 torr)
– 1 mtorr (mT) = 110-3 mm Hg = 1 mm Hg = 1 mm
• Other units of pressure:
– CGS: 1 dyne/cm2  760 torr (1 atm) = 1.0 106 dynes/cm2
– S.I.: 1 Pascal (Pa) = 1 N/m2 = 10 dynes/cm2 = 7.5 mtorr
• Units of throughput (Q) are torr-liter/second or Pa-liter/second
– “standard cc per minute” (sccm) refers to standard pressure
and temperature (760 torr and 0ºC) (molar volume 22,400 cm3)
– also used: “sccs”, “slm”
• Units of pumping speed (SP) are liters/second
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 Conductance
vacuum chamber at P1 tube with conductance C

gas in vacuum pump at P2

• The conductance C of an orifice or a length of tubing is a measure

of its ability to transmit a gas flow:
Q
C
P1  P2
• Conductances in parallel add; conductances in series add as inverses:

1 1 1
C  C1  C2     
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C C1 C2 15
 Types of gas flow
• High pressure (short mean free path)  the behavior of an
individual molecule is dominated by collisions with others, and
molecules will move in a stream: viscous flow
– laminar flow -- gas streams all move parallel
– turbulent flow -- gas streams are not parallel
• Low pressure (long mean free path)  collisions with other
molecules become rare, and most collisions are with chamber
walls: molecular flow
• If L is a characteristic length of the chamber, then:
 << L  viscous flow
 >> L  molecular flow

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 Types of gas flow (2)
• Intermediate between viscous and molecular flow, there is a
transition region: transition or Knudsen flow
• Characterized by 0.01L <  < L

Pressure  (cm) /L Gas Flow 10-4 Molecular

(torr)
10-3 5 0.1 transition
10-2 0.5 0.01 transition 10-3

P (torr)
10-1 0.05 0.001 viscous
1 0.005 0.0001 viscous Transition
10-2
Typical regimes of gas flow for a
chamber at room temperature with
a characteristic dimension of about 10-1
Viscous
50 cm
100
1 10 100
L (cm)
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 Vacuum ranges and appropriate pumps
Vacuum type Pressure range Typical pump
venturi,
mechanical RV,
Rough vacuum 0.1 torr - 760 torr Roots, sorption
mechanical RV,
Medium vacuum 10-4 torr - 10-1 torr turbomolecular,
diffusion
turbomolecular,
High vacuum 10-8 torr - 10-4 torr diffusion,
cryogenic

Ultrahigh vacuum < 10-8 torr Ti sublimation,

ion, cryogenic
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 Vacuum pumps (1) --
the Venturi pump

The simplest pump of all -- no moving parts!

high pressure low pressure region

N2 gas in pumps on system

gas compression
in a Venturi tube

gas to be pumped

The Venturi pump has a slow pumping speed and limited compression
ratio, but it is oil-free and a good way to (very) rough pump clean systems
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 Vacuum pumps (2) --
the liquid nitrogen sorption pump
gas to be pumped

high surface area

“molecular sieve”

liquid N2 (77K)

The liquid N2 sorption pump uses a high surface area molecular sieve
cooled to 77K to provide a surface for the pumped gases to condense
upon; clean but must be regenerated after each use
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Mechanical vacuum pumps

• Rotary vane pump

• Rotary piston pumps
• Roots pump (“Roots blower”)

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Operation of rotary vane (RV) pumps

suction exhaust exhaust suction

discharge
outlet valve

rotor

vanes

rough vacuum “high vacuum”

stage stage

single stage two stage

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 Operation of rotary vane (RV) pumps

• RV pumps have moveable vanes (usually 2 or 3) positioned in an

eccentrically mounted, slotted rotor within a cylindrical stator
• Rotation of the rotor causes a cycle of suction, compression,
and discharge to be achieved as the vanes slide along the
stator wall
• Oil is used to seal any gaps and to provide cooling of the pump
• Two-stage pumps achieve lower pressures because the oil on
the high-vacuum side is not exposed to atmosphere and hence
does not adsorb gas
• Special non-hydrocarbon oils are available if the pump is going
to be used with corrosive gases
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 “Gas ballast” to improve
pump operation
• When condensible vapors are pumped,
they can only be compressed to their
saturation vapor pressures
gas Example: H2O at 70ºC will condense when
ballast compressed to 312 mbar; further compression
will create no increase in pressure, so an
overpressure of the outlet valve will not be
achieved
• Water (in this case) would condense into
the oil; solvents could do worse!
• A “gas ballast” (air or N2 metered into
the pump) will reduce the partial
pressure of the condensing gas so that it
can
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 Rotary piston pump

• Gas is expelled every cycle (versus every two cycles in a RV

pump) so the rotary piston pump can achieve lower operating
pressures
• Especially useful for backing large systems in conjunction with a
Roots blower TAU 2017/2018 25
Roots blower

• A Roots blower has counter-rotating

rotors that are separated by a small
distance (0.1 mm)
• No contact between rotors allows a
high rotational speed (~3600 rpm)
with no mechanical wear
• Absence of oil seal results in a low
compression ratio (needs a backing
pump such as an RV pump)
• Roots blowers are a useful “first line
of defense” in high gas throughput
systems
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 Roots blowers
• Roots blowers achieve higher pumping speeds at pressures near
1 torr than can be achieved by rotary vane pumps
• Operation at 1 atmosphere requires a lot of power and makes
the rotors very hot!!
• Typical semiconductor systems are first rough-pumped with a
mechanical pump before the blower is turned on

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Accessories used with mechanical pumps

• Foreline sorption traps -- help control oil backstreaming

(transport of pump oil through the inlet line into the system
being pumped
– usually filled with molecular seive materials
– may be cooled or heated
• Anti-suckback valves -- prevent oil backstreaming in the
event of a power failure

A fast-acting normally closed valve is placed at the pump

inlet; if power is lost, the valve automatically closes
vacuum systems hate
power failures!!
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Vacuum and Plasma Sciences

• High- and ultra-high vacuum pumps

– diffusion pump
– turbomolecular pump
– cryogenic pump
– titanium sublimation pump
– ion pump
• Review of pumping speed, conductance
and throughput
• Sample calculations
• Vacuum seals and connections
• Pressure measurement
• Vacuum leaks (ugh!)
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Diffusion pumps

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 Diffusion pumps
• A diffusion pump is one form of a fluid entrapment pump
– a fluid (usually oil) is heated and vaporized
– the vapor is sent through a nozzle with supersonic speed
– the pump fluid vapor is condensed on a cooled surface
• Gas molecules are transported to the bottom of the pump by the pump
fluid, where it is evacuated by a backing pump (usually a rotary vane
pump) through the pump exhaust (the foreline)
• In order to work, the pump cannot be started until the foreline pressure
is sufficiently low (~millitorr)

a typical plot of pump speed versus

inlet pressure for an oil diffusion pump

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Diffusion pumps -- additional information
• “The only justification for calling them diffusion pumps is due to
the observation that the molecules of the pumped gas penetrate
some distance into the vapor jet in a manner resembling diffusion
of one gas into another.” (Hablanian, High Vacuum Technology)
• Original pumping fluid (before 1928) was mercury, since it did not
break down and early oils did -- over 99% today use oil
• The boiler pressure inside a nozzle is 1 to 2 torr, while at the
center of the vapor stream it is about 0.1 torr
• A cold trap is often used in the high vacuum side to reduce oil
backstreaming

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Turbomolecular pump
• A turbomolecular pump (“turbo
pump) is like a small jet engine
attached to a vacuum chamber
• Momentum transfer between the
rotating rotor blades, the fixed stator
blades, and the gas molecules
transfers gas to the back of pump
(requires a backing pump)
• Very high rotation speeds (from 24K
to 60K RPM) are needed, with
serious problems associated with
materials and control
– blade material (fracture, fatigue)
– bearing material & lubrication
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high vacuum
moving rotors impart
downward momentum
to gas molecules
low pressure
stages moving rotors only:
a “molecular drag
pump”

med. pressure fixed stators

stages decelerate the
molecule for the
next rotor “hit”

without the stators,

high pressure the next rotor could
stages not impart additional
velocity to the gas
fore vacuum TAU 2017/2018 molecule 34
Cryogenic pump

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 Cryogenic pump (“cryopump”)
• A cryopump uses a closed-loop helium refrigerator to produce
very low temperatures within the pump body
– He is compressed by a mechanical compressor to >20 atm
– Compressed gas is cooled to room temperature
– Gas expands in the pump head and cools
• First stage (outer surfaces -- baffle and radiation shield) cools to
50K to 100K
• Second stage (inner surface covered with high surface area
carbon) cools to 10K to 20K
• Cryopumps can maintain very low pressures (to 10-10 torr) with
very high pumping speeds (>10,000 l/sec for H2O)
• Pumps will saturate and require periodic regeneration (warm to
room temperature under flowing N2)
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Titanium sublimation pump

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 Titanium sublimation pump

• The Ti-sublimation pump works on the principle that atomically-

clean titanium is extremely reactive
• Pump operation is simple:
– A high electric current (~50 amps) is passed through a high
purity Ti filament
– Titanium is evaporated onto a cold (l-N2 cooled) surface
– Reactive gas molecules (N2, O2, H2) will be attracted to the
clean surface with a very high pumping speed
• Unreactive gases will not be pumped
• While not suitable for continuous pumping operations, a titanium
sublimator is widely used in UHV systems for periodically
lowering the overall system pressure
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Sputter-ion pump
• A sputter-ion pump (“ion pump”)
works by the ionization of the gas
molecules
– the gas ions strike a titanium
cathode and cause sputtering
– the sputtered Ti is reactive and
will getter reactive gases (N2, O2)
– the gas ions can be buried by
self-ion implantation
• A strong magnetic field is applied to
cause the electrons to move in
helical paths and increase the
ionization efficiency
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 Sputter ion pumps
• Ion pumps have several serious disadvantages
– low pumping speeds (inert gases are pumped especially poorly)
– can only be started at low pressures (~ 10-4 torr)
– can “arc-over” if pressure increases suddenly
• However, ion pumps are very clean and can produce very high
vacuums (<10-12 torr)

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 Pumping speed versus conductance

Conductance – gives the

Pumping speed – gives the capacity of a tube to allow a
volume of gas that is removed from volume of gas pass from one
a system by a pump in unit time end to another in unit time
Throughput or gas load – the quantity of gas in pressure-volume units
flowing in unit time past some location in the system

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gas in equals gas out 41
 Some information on “throughput”
• “Gas load” means gases entering the chamber from all sources
– gas leaks (intentional and unintentional)
– wall outgassing
– permeation through gaskets
– evaporation of volatile material
– backstreaming of gases from pumps
• After several hours at high vacuum, the pressure drops, and when
throughput = gas load the system is at its base pressure
• A note on throughput units (remember 1 Pascal = 1 Newton/m2
and 1 Newton/m = 1 Joule):

torr-liter Pa  m3 Nm J
throughput  or    watts
second s s s
energy per unit time that is required to
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Sample vacuum situations and calculations

low conductance
connection
high conductance
connection

conductances in series lower the pumping speed and add as reciprocals:

1 1 1
  43
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 Pumping speed versus conductance

Conductance – gives the

Pumping speed – gives the capacity of a tube to allow a
volume of gas that is removed from volume of gas pass from one
a system by a pump in unit time end to another in unit time
Throughput or gas load – the quantity of gas in pressure-volume units
flowing in unit time past some location in the system

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gas in equals gas out 44
 Sample vacuum situations and calculations

500 l/sec pump two 500 l/sec pumps

+ “infinite” conductance 500 l/sec pump + 500 l/sec conductance connected in parallel

1/EPS = 1/500 + 1/500 = 2/500 l/sec EPS = 500 + 500

EPS = 500 l/sec 45
or EPS = 250 l/sec
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 Sample vacuum situations and calculations
gas flow
3 torr-liter/sec volume volume
pumping speed  and throughput  pressure 
time time

so throughput  pressure  pumping speed

Problem:
maximum pressure If the effective pumping speed from a chamber
0.03 torr is 100 l/sec and the chamber pressure must not
exceed 0.03 torr, what must the gas flow into
EPS = 100 l/sec (or the throughput out of) the chamber be ?
Solution:
maximum throughput = (100 l/sec)(0.03 torr),
or 3 torr-liter/second
throughput 3 torr-liter/second
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 Sample vacuum situations and calculations
gas flow
0.1 torr-liter/sec
Remember, throughput  pressure  pumping speed

Problem:
Suppose the effective pumping speed from a
steady-state pressure
chamber is 250 l/sec and we wish to inject a
410-4 torr gas flow of 0.1 torr-liter/second flow of gas into
the chamber. What will the steady-state
EPS = 250 l/sec pressure be?
Solution:
0.1 torr-liter/second
= 410-4 torr
250 liter/second
throughput 0.1 torr-liter/second
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 Sample vacuum situations and calculations
N2 flow standard cm3 per minute
Problem:
810-3 sccm
A calibrated N2 leak of 810-3 sccm is attached
to a chamber and the measured pressure is
1.5 10-6 torr. What is the effective pumping
speed of the chamber in liters/sec?
Solution: “standard” = “atmospheric pressure”
chamber pressure
1.510-6 torr 810-3 sccm = (8/60)10-3 standard cc/sec
= (8/60)10-6 standard liter/sec
EPS = 67 l/sec = 760(8/60)10-6 torr-liter/sec
= 1.01 10-4 torr-liter/sec
We divide by the indicated pressure to get:
1.01 10-4 torr-liter/sec
= 67 liters/sec
1.5 10-6 torr
throughput 810-3 sccm
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 Vacuum seals and connections
• Low and medium vacuum  elastomeric O-rings
– Quick-connect (“KF”) flanges simplify multiple and
complex connections
– High vacuum, low vapor pressure greases used
• High and ultra-high vacuum: no grease or elastomers!
– high purity (OFHC) copper gaskets
– knife-edge Conflat flanges

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 Pressure measurement -- low vacuum
mV
• Thermocouple gauge -- a current is passed
though a wire, and the wire temperature is i i
measured with an attached thermocouple
• As pressure increases, the wire temperature
goes down due to the thermal conduction of
the gas q

• Capacitance manometer (Baratron) -- a Pr

thin metal diaphragm separates a region
at pressure from a reference vacuum
C2 C1 C2
• The deflection of the diaphragm causes a
change in the capacitance; the difference
between center and edge gives a measure
of the deflection and measures allows the P
pressure to be determined 50
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Pressure measurement -- high vacuum
• Hot cathode (Bayard-Alpert) gauge -- a current is passed
though a filament, and the thermionically-emitted electrons
generate ion from the residual gas
• The ions are collected as a current, with the filament current
being proportional to the gas pressure
• Useable to about 10-11 torr (X-ray limit – electrons striking
the grid generate X-rays; the X-rays will strike the collector
and cause photoelectrons to be ejected)

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 Vacuum leaks

• Finding and fixing leaks in a complex vacuum system can drive

you nuts!!!
• Rough vacuum -- squirt acetone on a suspected leak and
observe the thermocouple gauge
• High vacuum and UHV -- connect a mass spectrometer to the
vacuum system and squirt helium gas on a suspected leak
• “Virtual leak” -- gas is entrapped in confined area (example: the
bottom of a threaded hole inside a vacuum chamber) and comes
out only very slowly under molecular flow conditions

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 Physical vapor deposition

• Physics of evaporation
– vapor pressures
– deposition rates
– step coverage
• Evaporation sources
– resistive heating
– effusion cells
– electron beam
• Sputtering
– review of sputtering physics
– DC, RF, and magnetron sputtering
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 Evaporation processes

• P-V-T behavior of a fixed

amount of a pure material liquid

pressure
shows a characteristic solid
behavior (right)
– evaporation (L  V) gas
– sublimation (S  V)
temperature

• The vapor pressure over a liquid is given by

1 2  H v 
Pe  C T 32
exp 
 NkT 
surface tension enthalpy of evaporation
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Vapor pressures of the elements

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 Deposition rates (1)
• The impingement rate (molecules cm-2sec-1) was given by
P developed from the kinetic theory of gases,
J but perfectly applicable to evaporation from
2MkT a solid or liquid source

• The mass evaporation rate (g cm-2sec-1) is

M this is the evaporation rate at the source

RM  Pe 
2kT what is the rate at the receiving surface?

• The mass loss rate of the source (g sec-1) is given by

M Pe M Pe
RML 
2k  T
dA 
2k T
A
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 Deposition rates (2)
• So much for the source -- how about the substrate?
• Conditions that enhance the deposition rate
– Wafers facing the source
– Wafers directly above the source
– Wafers close to the source
• The obvious solution  to obtain a high deposition
rate, put a wafer in close proximity to the source!

Problem -- we don’t want to deposit onto a single wafer

How can we uniformly deposit onto multiple wafers?

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 The geometry of deposition

r
f
f
q
q
R r R

arbitrary orientation wafers placed on spherical surface

deposition rate depends on R, q and f cos q = cos f = R/2r
geometric effects cancel!
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 Deposition rates (3)
• The net deposition rate is given by

M Pe A
Rd 
2k2 T 4r 2

density of the film

materials properties temperature and geometry of the

of the film vapor pressure deposition chamber

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 Step coverage
• Evaporation is a line-of-sight process that can lead to
poor coverage of surface topographic features
incident flux
direction

perfect step coverage poor coverage (thin layer) poor coverage (thick layer)
• Shadowing due to surface topography leads to non-uniform
deposition in thin layers
• Thick layers may exhibit “self-shadowing” as excess
material builds up at edges
• Can be improved by rotating the substrate and heating it
during deposition (enhancing surface diffusion) 60
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 Deposition sources (1)

The simplest sources are resistive evaporator sources:

i i
i
i

• Tungsten wire coils and baskets are very simple -- liquid is

held in place by surface tension
• Useful for “flash evaporation”, but precise control is difficult
• A dimpled boat (usually W, Ta or Mo) offers somewhat more
control (cutouts provide high resistance regions)
• Both have the problem of metallic contamination
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 Crucible evaporation
(effusion cell or Knudsen cell)
• Crucibles made of high purity, high temperature ceramic (usually
pyrolytic boron nitride (pBN)) hold the evaporation charge
• Heating may be resistive or inductive
• Temperature control via thermocouple feedback

pBN crucible (may be quartz or graphite)

resistive or RF heating element

heat shield
source material

thermocouple
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 Temperature controllers
on

off heater power

setpoint
temperature

time

• A simple on-off temperature control is simple and inexpensive,

but the temperature will fluctuate about the set point

• Not suited for precision applications

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 Temperature controllers (2)
• Proportional-integral-derivative (PID) controllers are universally
used for critical applications
Proportional -- range of proportional power band
Integral -- integrates the deviation (offset) from set point and shifts
the proportional band
Derivative -- amount of shift of the proportional band depends on
the rate-of-change of the temperature

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Electron beam sources

• Electron beam (e-beam)

sources are widely used for
the deposition of refractory
materials
• No contamination from the
crucible
• Since a magnetic field “steers”
the e-beam, the substrate does
not have to “see” the filament,
thus reducing contamination

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 E-beam evaporators

• e-beam evaporators can deposit a wide range of materials

(example: refractory metals)
• multiple sources are possible within a single evaporator
• problems:
– particulate generation -- “spitting”
– X-ray generation (10 keV electrons  10 keV X-rays that
can damage MOS devices)
– deposition rates can be difficult to monitor -- the vapor
pressure over an effusion cell will vary predictably with
temperature, but not with e-beams

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 Quartz thickness monitors

quartz • A piezoelectric material like quartz

~ 5 MHz
crystal generates an oscillating voltage if
driven at its resonant frequency
• The mass loading of a deposited
film will reduce the resonant
frequency
film • By comparing the resonant
(tf, f)
incident flux frequency to that from a standard
crystal, the difference (and hence
The resonant frequency is given by: the deposited thickness) can be
1 1 ks determined with high accuracy
r  
Tv 2 m • Crystal must be replaced when the
and Tv  m f   f t f film thickness is about 10% of the
crystal thickness (~350 mm) 67
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 Physical vapor deposition

• Sputtering
– review of sputtering physics
– DC, RF, and magnetron sputtering
• Structure of sputter-deposited films
• Multicomponent (alloy) films

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 Sputter deposition
• More widely used than evaporative processes (high deposition
rates, large number of materials that can be deposited, better
step coverage)
• Uses the physical process of sputtering to propel the depositing
material into the gas phase
• Glow discharge plasmas (DC and RF) are universally used to
perform the sputtering process
• Subjects to be covered:
– review of the physics of sputtering
– sputtering methods (especially magnetron)
– film characteristics
– specific materials

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 Review -- the physics of sputtering
reflected atom
incident
ion secondary electron
sputtered
atom

implanted
atom

The sputter yield is defined as

mean number of emitted atoms M ion ln E 1
S= S
incident ion M sub E cos q
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 DC sputter deposition
• A DC sputtering system is similar
to a plasma etching system
cathode
– two electrodes (anode &
cathode)
– low pressure gas (usually Ar+ reduced
for sputtering) pressure gas
– power supply
• In an etching system the material anode
to be etched is placed at the
cathode
• In a sputter deposition system Schematic of a DC sputtering system
the sputter target is placed at the
cathode, and the wafers being
deposited are at the anode
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 RF sputter deposition
AC power source
“blocking capacitor”
to prevent current
flow (important!)
electrons
ions
• At radio frequencies (13.56 MHz) the
powered electrode will develop a net
negative charge (the “self-bias”) due to
the difference in the mobilities between
electrons and ions
• Positive ions will bombard the powered
electrode, thus leading to sputtering of
this target
• The substrates to be coated are then
placed at the grounded electrode (or
anywhere else in the chamber)
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 Magnetrons

• A magnetron is a diode sputtering source in which magnetic

fields are used in concert with the cathode surface to form
electron traps
• These traps are configured so the EB electron drift currents
close on themselves
• Magnetrons offer numerous advantages as sputter sources
and are almost universally used in all phases of semiconductor
materials processing

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 Plasmas -- the DC Glow Discharge
• The interactions between electrons and ions, the fact that they
have much different masses, and various requirements based in
electrodynamics results in a series of both glowing and dark
spaces in the normal glow regime of a DC discharge
Faraday dark space -- a
cathode (Crooke) dark space --
nearly field-free region; positive column --
secondary electrons repelled by
electrically connects the most nearly like a
the cathode generate a “sheath”
negative glow to the simple plasma
of positive ions
positive column

cathode anode

cathode glow -- incoming
discharge ions and positive
ion produced at the cathode
are neutralized
negative glow -- electrons
repelled by the cathode and
ions recombine
TAU 2017/2018
anode dark space -- anode
is a sink for electrons, so
little emission occurs
74
 Magnetrons (2)
• Consider the operation of a simple DC planar diode sputter source:
• Electrons emitted by the cathode by
ion bombardment enter the negative cathode (target)
glow region and produce ions that e-
e-
sustain the discharge
• At low pressures, ions are produced e- e-
far from the cathode and are lost
• At high pressures, the transport of anode
sputtered ions is reduced by gas-
phase scattering
Schematic illustration of some
• Thus the maximum deposition rate of the most important processes
that can be achieved is limited by in planar diode sputtering
the physics of the glow discharge
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 Magnetic field effects
• If a magnetic field is applied to a plasma, the Lorentz force will
deflect the motion of the electrons
   the direction of the force is perpendicular to both
F  qv B
the velocity and the magnetic field

• This will induce a circular motion of radius

mv W1/ 2 W = the energy (eV) associated with the
r  3.37 cm electron motion perpendicular to the field
qB B and B is in Gauss

• The frequency of rotation (the cyclotron frequency) is

eB
o   1.76 10 7 B rad/ sec generates a helical path
m
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 Magnetrons (3)
• If there is an electric field component E perpendicular to B, an
electron drift develops in a direction perpendicular to both E
and B

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Planar magnetron sputtering source

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Cylindrical magnetron sputtering source

plasma environment -- top view side view

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S-gun magnetron sputtering source

schematic illustration of the

side view
magnetic plasma confinement

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 Random aspects of sputtering systems

• The typical input electrical power requirement for magnetron

sputtering systems is ~1000V and ~10A (high, constant current
power supplies that can shut off and restart when arcs occur)
• Argon gas pressure 1 to 10 mTorr
• Magnetic field strengths 100 to 1000 Gauss (0.01 to 0.1 Tesla);
achievable with conventional permanent magnets
• Water cooling of the cathode is needed
• Deposition rates up to several hundreds of Å/minute

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PVD - Thin film growth

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 The “idealized” thin film growth process

single atom migration & combination of

arrives re-evaporation single atoms

nucleation growth coalescence continuous film

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 Substrate bombardment in
sputter deposition

Argon:
- thermal neutrals electrons
- fast (target & charge exchange) complexes (fast & slow)
- metastables (Ar+, Ar++, Ar2+) (ArH+, H3O+)
sputtered contaminants negative ions
atoms photons

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 85
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 Properties of sputter-deposited films (1)
• The basic model for the structure of sputter-deposited metallic films
was developed by Movchan and Demchishin (modified by Thornton)

homologous temperature
T/Tm (in K, not ºC)
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 Properties of sputter-deposited films (2)
Zone 1

• At low homologous temperature

surface diffusion is negligible
(diffusion length < ao)
• The structure is columnar (~tens
of nanometers across) but is
highly defective and may even
be amorphous
• Voids and domes due to self-
shadowing effects; the resultant
surface morphology is rough

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 Properties of sputter-deposited films (3)
Zone T

• The transition zone also occurs

when the diffusion length is small
• Contains defected columns
similar to Zone 1, but void and
domes are absent
• Thought to be caused by energy
enhancement (radiation induced
diffusion)

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 Properties of sputter-deposited films (4)
Zone 2

• Zone 2 occurs when T/Tm > 0.3,

when surface diffusion becomes
significant
• Structure consists of columns
with tight grain boundaries; the
diameters increase with T/Tm
• The effect of increasing argon
pressure is to reduce surface
mobility, thus requiring increased
temperature to attain the same
structure found at lower values of
pressure and T/Tm

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 Properties of sputter-deposited films (5)
Zone 3

• Zone 3 occurs when T/Tm > 0.5,

when bulk diffusion becomes
significant
• Dynamic annealing operative
leading to defect reduction or
recrystallization
• Structure consists of equiaxed or
isotropic grains; high temperature
grooving at grain boundaries

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 Multicomponent deposition (1)

• Often multicomponent (or alloy) materials need to be deposited

by a PVD process (examples: AlCu, TiW)
• Problems arise if the source is a mixture of the components
– evaporation: different vapor pressures of the two
constituents (Ti: 1 torr at 2500°C; W: 310-8 torr at
2500°C)
– sputtering: different masses (Ti: 47.88 g/mole; W: 183.84
g/mole) will have different deposition rates due to solid-state
effects (sputter yield) and gas phase effects (power and
pressure)
– e-beam: least susceptible to alloy composition variation, but
requires e-beam evaporation (cost, X-ray production)!
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 Multicomponent deposition - (2)

• Single alloy source (left) -- simple, but the vapor pressures of the
constituents must be similar
• Multiple source (center) -- individual evaporation cells for each
source material make it possible to precisely control alloy content
• Shuttered multiple source (right) -- permits sequential deposition by
opening and closing of shutters; requires annealing to have the
layers interdiffuse
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 Multicomponent deposition (3)
• Multicomponent deposition by sputtering has to deal with two
major factors that can alter layer composition

before sputtering during sputtering

Sputter source effects:
In a two component source, one of the
components may have a higher sputter
yield -- the near-surface region of the
target will become depleted of that
component, so the deposited film will
have a lower concentration of the high
sputter-yield constituent
TAU 2017/2018
Gas phase effects:
The component with the lower mass
will be preferentially scattered on
the way to the substrate -- as either
the pressure or the power are
increased, the relative scattering of
the lighter species will increase
93
 Incorporation of sputtering gas atoms
• At 20 mTorr, the flux of the sputtering gas may be 104 greater than
the flux of the desired sputtered atoms!

• In Ar-sputtered Ni, the Ar/Ni ratio depends strongly on the substrate

temperature (left), Ar-pressure (center) and bias voltage (right) 94
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Equipment configuration in a sputter
deposition system

• Sputter target assembly – composition, heat dissipation,

electrical isolation, “ground shields”
• Power supply – DC or RF
• Instrumentation and control – voltage, current (DC),
power (RF), and sputtering gas pressure
• Substrate heating and/or cooling
• “Wall losses”
• Shields and shutters
• Scale-up can be a big problem!

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Equipment configuration in a sputter
deposition system

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Equipment configuration in an
evaporation deposition system

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 Stress in thin film deposition
• Most films, when deposited, are stressed with respect to the
substrate
• Thermal mismatch stress
– arises when the deposition is performed at a temperature
different from room temperature
– difference in thermal expansion coefficients of the film and the
substrate will lead to stress

    sub  dT
Efilm Tdep
 th 
1   film
film
To

– obviously as the deposition temperature increases, the

magnitude of the stress increases
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 Stress in thin film deposition (2)
• Intrinsic stress is the stress that arises during deposition process
due to the nature of the process itself
• There are at least three common sources of intrinsic stress:
– chemical reactions during the deposition process
• Ti deposition in poor vacuums can develop compressive stress due to
continued oxidation beneath the surface
– microstructure and defects
• densification of (microscopic) vacancies and (macroscopic) voids will
generate tensile stresses; these can be very large
– particle bombardment
• implantation of ions or energetic neutrals lead to compressive stress in
the layer due to interstitials
• The magnitude of the net intrinsic stress will be very sensitive to the
details of the deposition process
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 Stress in thin film deposition (3)
• High film stresses usually lead to problems
– tensile stress leads to cracking and peeling
– compressive stress leads to de-adherence and buckling

tensile compressive

• Stress is usually measured by monitoring the warpage it causes in

an underlying substrate (by profilometry, laser or X-ray)

 E Tsub2 

t film 1   3Rsub
2

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 Metallization

• Metallization is the process that connects individual devices together

by means of microscopic wires to form circuits
– typical interconnect current density ~105 A/cm2
– wires introduce parasitic resistance and capacitance
• As the dimensions of devices are scaled down, interconnect delay will
dominate
• Virtually all IC circuits are made with 2-6 levels of metal wiring
– substantial reduction in die size (hence chip cost)
– greater flexibility in circuit design

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Interconnect materials

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Architecture

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