ThinFilmPhysicsandTechnology

Thin Film Physics and Technology

SCPY663(SpecialTopicsinPhysicsI)
( p p y )

Somsak Dangtip, Ph.D.

Department of Physics
Faculty of science, Mahidol University

Semester 2 Academic year 2009

O t b 2009 March
October M h 2010
1
 www sc mahidol ac th/scpy/
www.sc.mahidol.ac.th/scpy/

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 ThinFilmoverview
Solid
S lid
Liquid
Source Vapor
Gas
Supply Rate
Vacuum
T
Transport
t Fluid
Fl id
Plasma
Uniformity
SubstrateCondition
S b t t C diti
ReactivityofSource
Deposition material
EnergyInput
E I t
Annealing
Structure
Characterization
Composition
andAnalysis
Properties

Process Modification

5
 BasicVacuumTechnology

6
 DiagramofVacuum System
Thin Film & Sensor Laboratory (K406)
ThinFilm&SensorLaboratory(K406)

MFC
 Vacuum system

Materials:
Stainless Steel
The most widely used material is stainless steel, 304 and 316. Their melt point is
~1060 oC. They are chemically stable, not easily react with oxygen, bakeable, can
be applied at both low and high temperature.
The 316LN type stainless steel has exceptional properties compared to type 304:
316LN flanges are harder and their knife edge does not roll over as quickly,
making g them ideal for frequently
q y dismantled chamber ports
p or critical beam-line
flanges.
During manufacture, 316LN is fired at 950oC in N2 to purge H2 from the steel
matrix, producing a much lower H2 background.
A 316LN system with 316LN flanges reaches lower ultimate pressures, since it
can be baked to 550 oC.
For systems with heat-sensitive components, 316LN material reach the same
b
base pressure as 304 flanges
fl at lower
l bakeout
b k temperatures.
For applications susceptible to magnetic fields, 316LN offers lower magnetic
permeability (1.001, versus 1.03 for 304).
 Vacuum system
Materials:
Aluminum (melt point: 660 oC) can also be used for vacuum components,
although a fresh Al surface can quickly react with water and oxygen. The
drawbacks are their lower mechanical properties and difficulty in welding.

Brass (Copper-zinc alloy) has excellent mechanical properties and can

be easily welded. But they can be used in vacuum only at a room
temperature or below since at a high temperature the Zn will generate a
vapor as its melting point is low (419 oC).

Pure copper free of oxygen (OFC) OFC is used for the electric or
thermal conductors in vacuum.

Iron or usual steel should not be employed in vacuum as they can easily
react with water and oxygen.
 Flanges (i)

Flanges
CF (Knife-edge) flanges
Gasket
Standard copper gaskets
Fully annealed copper gaskets
Silver-plated copper gaskets Aluminum
gaskets
Viton gaskets
Special gaskets from materials such as
gold--plated
gold plated copper, silver
silver-diffused
diffused
copper, zirconium-copper alloy, nickel
and lead have been requested for
uncommon applications.
pp
 Flanges (ii)
KF (QF,
( NW)) fl
flanges
KF (Klein Flange) is a simple and flexible O-ring vacuum coupling. The system
(defined by the International Standards Organization) is also known as `QF' or
`NW
NW.'' Th
The system
t iincludes
l d KF10,
KF10 KF16,
KF16 KF25,
KF25 KF40,
KF40 and d KF50.
KF50 When
Wh ththe tube
t b
diameter exceeds 2 inches or 50 mm OD, the system name changes to `ISO' or
'Large ISO.' The sealing mechanism does not change but there are substantial
differences between KF and ISO flange designs and clamps
clamps.
KF fittings are used for rough or foreline vacuum plumbing and simple HV (10-6 Torr)
chambers. The elastomeric O-ring limits the connection's temperature range and
ultimate vacuum
vacuum.
 ISO flanges

ISO-K Flanges
g
A: Double claw clamp attaching two K-
style flanges
C:Clamp p to bolt fastener for K- style
y to F-
style connection
E: Claw clamp with screw fastener for
K-style to a blind tapped mating flange
ISO-F Flanges
B: Bolt and nut fastener for two F- style
flanges
D B l and
D:Bolt d nut fastener
f ffor K
K-style
l bolt
b l
ring to F-style
F: Stud and nut fastener for F-style
fl
flange to
t a bli
blind
d tapped
t d mating
ti flange
fl

E
F
Examples of flange connection
 Valves

Types of valves: Although there are a

vast number of valves, they can be
grouped into the following categories:
Gate valves
Rectangular
g valves
Right-angle and block valves
Straight-through valves
Ball valves
Inline valves
Butterfly valves
Variable conductance controllers
Leak valves
 Valves

Gate valves
Its purpose is to leave a wide,
wide
unobstructed bore between two
parts of a vacuum system and
provide a high conductance path.
path
The most frequent application is to
close the chamber from the HV/UHV
pumps so that the system can be
pumps,
vented. Secondary applications
include providing an unobstructed
portt for
po o sa
sample
p e ttransfer
a s e from
o o onee
section to another, transferring UV
radiation in synchrotron experiments,
or transferring
g a particle
p beam in
accelerator experiments.
 Valves

Rectangular Valve:
These simple gate valves are used on
systems that require valves with minimal
height while maximizing the width. These
are excellent valves for systems that
move discs from one level to another.
 Valves

Right-angle Valve: This popular valve

can have O-ring or metal-to-metal seals
for the seat. They find applications as
f l
foreline valves,
l UHV shut-off
h ff valves,
l
sorption trap valves
and high temperature bakeout valves (for
production
d ti off night
i ht vision
i i goggles).
l ) Their
Th i
conductance for a given bore size is
about half that of the straight-through
valve A popular version of the O-ring
valve. O ring
sealed right-angle valve is known as the
block valve because of its shape.
 Valves

Straight-through Valve: A distinction

must be made between straight-through
and inline valves.
valves In common
descriptions, only the straight-through
valve has a line of sight through it. The
primary application for straight
straight-through
through
valves is to transfer samples or radiation
from one section of a system to another.
These valves have good gas
conductance, since the bore is neither
obstructed nor bent.
 Valves
Ball Valve: This is a low-cost valve used
only at foreline pressures. Ball valves
should not be used at HV pressures
because the potential for gas evolution
and leak is too high. They are useful
valves,, however,, providing
p g good
g service
at rough vacuum pressures.

Inline Valve: Inline valves have their

inlet and outlet flanges on 'opposite
sides' of the valve,, but the center
lines of the ports are parallel rather
than coincident. This type of valve is
used where the `plumbing' cannot
accept a right-angle turn.
Conductance for a given bore is low,
because the gas must make two
right-angle
h l turns in the
h valve
l body.
b d
 Valves

Butterflyy Valve: These simple

p valves
open to give a high conductance, but
obstructed, path as the flapper remains
in the valve bore. They are used above
diffusion pumps and in forelines. When
mounting this type of valve, remember to
leave room above and below for the
flapper to rotate.
 Valves

Variable Conductance Controller: It

may be argued that this device (VCC) is
not a valve. As its name states, it controls
the conductance between two vacuum
sections most often between a HV pump
sections,
and a sputtering or etching chamber
where the operating pressure is in the
10-2 Torr range during operation,
operation but 10-6
Torr during pumpdown. Since HV pumps
cannot operate at 10-2 Torr and process
gas loss from the chamber would be
unacceptably high with a direct
connection, the VCC throttles the port
duringg sputtering/etching
p g/ g and is opened
p
for high conductance during pumpdown
to remove contaminants.
 Valves

Leak Valve: These are sometimes

called gas control valves. They have a
specific application: admitting small
amounts of gas into the system at a
controlled leak rate. The conductance
of a leak valve is extremely low even
when fully open
open.
 Gas and Liquid management
Mass flow controllers
All vacuum processes using low pressure gases are sensitive to `number density' (the number
of molecules per cm-3) of gas. Attempts to regulate the vacuum process by adjusting
volumetric flow are ineffective since number density changes with pressure and temperature.
Mass flow -- a measure of the number of molecules flowing past a point - is directly related
to number density and, hence, process rate.
Mass flow controllers (MFC) operate by measuring the heat input required to maintain a
temperature profile along a laminar flow sensor tube. One patented type has a sensor with
three heaters that maintain the profile with an auto-balancing bridge circuit. Its response time
(less than 0.5 sec) gives fast control without overshoots or oscillations. The straight, large-
b
bore sensor tubes
b off some controllers
ll ensure laminar
l flow
fl and
d minimize particulate
l clogging,
l
condensation and the effect of ambient temperature fluctuations.
For mass flow measurement, the sensor simply monitors the flow and displays it either on an
external or integral display meter. For mass flow control, the metered flow rate is continuously
compared with a user-defined setpoint and generates an out-of-balance feedback signal that
proportionally regulates an electromagnetic valve.
In modern gas handling, low contamination and particulate content is critical. The materials
wettedd by
b the
h gas stream inside
i id the
h MFC,
MFC the
h regulating
l i valvel characteristics,
h i i assembly bl under
d
Class 100 clean room conditions and double-bag packing are vital considerations when
choosing an MFC.
 MFC

T1 T2
sensor tube (n)

p1 p2
T2 T1 = Bc p Q
B Proportion
p alityy Constant
c p heat capacity per mole at constant pressure
Q mass flow rate
 Kinetic theory of gases

yields an atomistic picture of all processes in a closed gas volume

explains macroscopic properties by (e.g. pressure) by microscopic processes
closed gas volume:
high number ( 1023) of gas molecules
permanent random motion
p
details of the motion primarily depend on temperature T
molecules collide with each other and the container walls
rate of collisions (#/s) depends on number density n (#/m3) or pressure
p (N/m2)

ideal gas:
no attractive or repulsive interaction of the molecules (except
during collisions)
molecules behave like independent elastic spheres with
sphere
h diameter
di t <<< average distance
di t between
b t two
t spheres
h
permanent exchange of kinetic energy by elastic collisions is essential for
reaching the thermodynamical equilibrium
 Kinetic
equilibrium distribution of molecular velocities: Maxwell- Boltzmann formula
Mv 2
3/ 2
1 dn 4 M
f (v ) = = v exp
2

n dv 2 RT 2 RT
M: molecular weight (kg)
T: absolute temperature (K)

R:gas
g constant = 8.314 J/mole-K
/
n: number density of molecules (m-3)

f(v)dv is the probability to find an

arbitrary
b molecule
l l with
h
a velocity in [v, v+dv]


f (v)dv = 1
0 average velocity; v

most p
probable velocity;
y; vm
v f (v)dv
d
8RT
d 2 RT v =0= 0
=
f ( vm ) = 0 ; vm =
M
dv M f (v)dv
0

root mean square (rms) velocity; kinetic energy

gy of a mole onlyy

depends on temperature
v f (v)dv
2

2 1/ 2 3RT 1 3
v = 0

= M v 2 = RT
M 2 2
f (v)dv
2 1/2
vm < v < v
0

The sound velocity is always close to these velocity:

Sound = pressure waves = molecular collisions
 Typical molecular velocities: several 100 m/s

High rate of molecule-wall collisions
Pressure = ((momentum change g per
p s)/(unit
)( area))
1 nM 2 nRT N RT
" p = v = =
3 NA NA NA V
N (perfect gas law)
pV = RT
NA

Pressure is the most important system property in vacuum technology

SI unit of pressure:
F N
[ p ] = = 2 = Pa
A m
O h frequently
Other f l used
d units:
i

1 atm = 1.013 105 Pa 1 torr = 133.3 Pa 1 bar = 750 torr

 Mean-free path, :
Average distance traveled by molecules
Between successive molecule/molecule collisions
Smith 2.6
d 2 n = 1
Collision: RT
vN A vN A p =
n= = N A d 2
p
V RT
vRT

Air,, ambient pressure,
p , 300K,, d = 3 1500
Air, 1 Pa, 300 K, d = 3 1.5cm
Rule of thumb for small molecule, 300 K, 1 Pa 1cm
Air 300 K
Air, 6.6 10 3 Pa
P / pm

Collisions with the container walls p

prevail at pressures
p below 10-10 Pa
Time between 2 successive collision: = / (10-10 s for air molecules)
Gases mix together rather slowly, gas molecules execute a zigzag motion
with little net displacement
 Gas Impingement on Surfaces

# of molecules per second and unit area collide with a surface at a pressure p:

p
gK
Gas impingement flux: = pN A Pa molecules
= 2.63 10 20
2MRT MT cm 2 s

Knudsen equation

n A molecules leave the container

per s volume flow per s (300 K,
K air):
gas
A A 1
Oriflice area A
V = 11.7 2
n cm s
vacuum
 How long does it take until an initially clean surface is coated by and
contaminated with a monolayer of gas molecules (assuming all arriving
molecules stick to the surface)? )

Very important issue for

Preparation of thin films under clean conditions
(inverse growth rate (ML/s)-1 >> monolayer formation time)
Surface analysis (analysis time << monolayer formation time)
molecules
ML = 1ML 1019 (atom = 3A diameter)
m2
MT Pa
ML = 3.8 10 6 ( ).s
gK p
air, 105 Pa ML~ 3.510-9 s
UHV, 10-8 Pa ML~ 9.5h
Rule of Thumb ML~ 1s at 10-6 mbar
 Gas transport

some facts that are necessary for a successful design of vacuum systems
benefits
f off a good design: short pumping times, low costs
gas flow: net directed movement of a gas, combined with a pressure drop

ttwo main
i gas flflow regimes
i (D:
(D system
t dimension):
di i )
molecular flow, >>D
low pressure, HV, UHV, collisions with container walls prevail
flow <<D
viscous flow,
CVD, molecule-molecule collisions prevail
laminar for low flow velocities, turbulent for high flow velocities

Knudsen number Kn=D/:

molecular flow Kn<1 air: Dp < 3.7 10-7m Pa
intermediate flow 1<Kn<110
viscous flow Kn>110 air: Dp > 3.7 10-5m Pa
The gas flow mechanisms may differ in various parts of the same system

Q
Flow conductance C (m3/s
or l/s): C=
With gas throughput Q (pressurevolume/s) p

Conductance of a orifice with area A (molecular flow regime, see above);

A 1
C 11.7 2
cm s

1 1
= conductance joined in series
Csys i Ci

Csys = Ci conductance joined in parellel

i
Conductance of various simple geometries

1/ 2
T
C = 3.64 A = 11.7 A
M

A2 T
1/ 2
D3
C = 6.18 = 12.2
DL M L

D3 T
1/ 2 ( D2 D1 ) 2 ( D2 + D1 )
C = 3.81 = 12.2
L M L

b2c 2 T
1/ 2
b2c 2
C = 9.70 = 31.1
(b + c) L M (b + c) L
Molecular flow of air at 300K
1/ 2
T 1 D2
C = 2.85 D
2
= 9.14
M 1 + 3L / 4 D 1 + 3L / 4 D

1/ 2
T
A

11.7 A0
C = 3.64 =
M 1 ( A / A0 ) 1 A0 / At


D3 T
1/ 2
1 12.2 D 3
C = 3.81 =
L M 4D D 2 4 D D 2
1+ 1 2 L 1 + 1 2

3L Dt
3L Dt

 Vacuum Pumps

Basic function: remove gas molecules and reduce density and pressure
pumping
p p g speed:
p S = Q/p
= gas throughput (pressurevolume/s) / pressure at pump inlet

if Q = 0
Q pp S p = p S = C ( p pp )
p,S Vacuum chamber
Q:throughput
pp pp
Q S = Sp = Sp
p Q
+p
C
Sp Sp
= = Sp
Q Sp
Qp Qp: backflow (outgassing) 1+ 1+
C pp C
pp,S
Sp p mp
pump

a high
g conductance C is desirable
 Q = S p p p Qp
Backflow Qp always limits the ultimate pressure, pend:
Qp
Q = 0; for ; p red =
Sp
Then the pumping speed in the vacuum chamber falls to zero:
Q Qp
S= = S p 1 = S p 1 p 0
S p p pexit
p p p exit

Time required to achieve a given pressure (pump down time):

d dp
Q = ( pV ) = V = S p p p Qp
dt dt
p p (t ) p exit Sp
= exp t
p p (0) p exitit V
Pressure falls exponentially (molecular regime only) with time constant V/Sp
How to achieve clean ultra-high vacuum conditions:

high pumping speed ( a pump cant be too big!), often 2 pumps in series
small vacuum chamber
high conductances (e.g. short & wide tubes, no narrow holes etc.)
special low outgassing stainless steel chamber
low vapor
vapor-pressure
pressure materials (ceramics glass metals)
bake out procedures (250C 400C)
no organic materials
ask your supervisor
switch on your main processor before touching the system
Vacuum Pumps
 Diaphragm Pumps

downward
moving

Lowest
position
iti
Upward
moving

highest
position

Operating principles : Gas Transfer Vacuum Pump (VP), positive displacement VP

Ref: Fundamental of vacuum technology revised and compiled by

Dr. Walter Umrath with contributions from Dr. Hermann Adam , Alfred Bolz, Hermann Boy, Heinz Dohmen,
Karl Gogol, Dr. Wolfgang Jorisch, Walter M.nning,Dr. Hans-J.rgen Mundinger, Hans-Dieter Otten, Willi Scheer,Helmut Seiger, Dr.
Wolfgang Schwarz, Klaus Stepputat, Dieter Urban,Heinz-Josef Wirtzfeld, Heinz-Joachim Zenker
 Rotary Vane Pump

Operating principles : Gas Transfer Vacuum Pump (VP), positive displacement VP, rotary VP, liquid sealed
Rotary Plunger Pumps

Operating principles : Gas Transfer Vacuum Pump (VP), positive displacement VP, rotary VP, liquid sealed
 Root Pumps

Operating principles : Gas Transfer Vacuum Pump (VP), positive displacement VP, rotary VP, dry processing
 Oil Diffusion Pumps

Operating principles : Gas Transfer VP, Kinetic,

fluid entrainment
Turbo-Molecular Pumps

Operating principles : Gas Transfer VP,

Kinetic, drag, molecular drag,
 Sorption Pumps

Operating principles : Entrapment Pump, adsorption pump

 Sputter Ion Pump
Sputter-Ion

Operating principles : Entrapment Pump

 Cryogenic Pump

Operating principles : Entrapment Pump

Vacuum Pump Characteristics