III.

Vacuum fundamentals & technology

Why we need vacuum?

In materials characterisation:

•Keep surfaces free of contaminants.

•Large mean free path for particles (electrons, ions).

•Analysis of gaseous samples without air contamination.

In industrial applications and material preparation:

•Process films with low density of impurities.

•Maintain plasma discharge for sputtering sources.

•Evaporate reactive compounds.

Mean free path for air at

20 ºC:
λ= 7 x 10-5 m / P(mbar)
At pressure 1 bar:
λ=70 nm only
λ
 Pressure ranges and units
• Rough vacuum p >1 mTorr Mean free path for air at
– Rotary vane pump 20 ºC:
– Thermocouple, Pirani or Capacitance Manometer λ= 7 x 10-5 m / P(mbar)
• Medium Vacuum 10-8 Torr < p < 1 mTorr At pressure 1 bar:
– Cryo pump, Diffusion Pump, Turbo Pump, Ion
λ=70 nm only
pump
– BA Ion gauge, mass spectrometer
– Viton seals
• High to Ultra High Vacuum
10-10 Torr < P < 10-8 Torr
– Turbo, Ion, Titanium Sublimation Pump,Cryo pump
λ
– All Metal Seals, Baked system λ> apparatus dimensions:
– BA Ion Gauge, mass spectrometer the flow is free molecular
λ< apparatus dimensions:
the flow is viscous
SI unit
 Monolayer time and gas exposure

Degree of Pressure Gas Density Mean Free Path Time / ML

Vacuum (Torr) (molecules m-3 ) (m) (s)
Atmospheric 760 2 x 1025 7 x 10-8 10-9
Low 1 3 x 1022 5 x 10-5 10-6
Medium 10-3 3 x 1019 5 x 10-2 10-3
High 10-6 3 x 1016 50 1
UltraHigh 10-10 3 x 1012 5 x 105 104

• Monolayer time: the time for one atomic layer of gas to adsorb on the surface.
• Sticking Coefficient: S = number of adsorbed / number of incident
• At 3 x 10-5 Torr, it takes about one second for a monolayer of gas to adsorb on a
surface assuming a sticking coefficient, S = 1.
• At 10-9 Torr, it takes 1 hour to form a monolayer for S = 1.
• For most gases at room temperature S<<1, so the monolayer time is much longer.
• The gas exposure is measure of the amount of gas which a surface has been
subjected to. In is usually measured in the units of Langmuir (L):

Exposure(L) = 106 x Pressure(Torr) x Time(s)

(if the pressure is constant, otherwise it is an intergral of pressure over time)

 Creating vacuum - concepts
Pumping Speed
Pumping speed is defined as the ratio of the throughput of a given gas to the partial pressure of that
gas at a specific point near the inlet port of the pump.
Less formally, it is the volume of gas (at any pressure) that is removed from the system by the pump
in unit time.
Pumping speed is a measure of the pump's capacity to remove gas from the chamber.
Units: liters per second (L/sec) or (m3/sec).
Conductance

Conductance is the ratio of throughput, under steady-state conservation conditions, to the

pressure differential between two specified isobaric sections inside the pumping system.
Informally, the conductance of a tube is its capacity to let a volume of gas (at any pressure) pass
from one end to the other in a unit of time.
Conductance is a property of a passive (non-pumping) component of a vacuum system, similarly as
pumping speed is a property of a pump.
Units: liters per second (L/sec) or (m3/sec).
Throughput and gas load
Throughput and gas load can be defined as the quantity of gas in pressure-volume units flowing in unit
time past some location in the system.
Units: (torr x liters / sec) or (Pa x m3 / sec)
Knowing temperature and throughput, we can calculate the mass of gas flowing past some point in 1 sec.
Although throughput and gas load are sometimes used interchangeably, it is preferable to reserve throughput
as a property of the pumping system and gas load as a property of the chamber. Then we can state that at a
dynamic equilibrium:
Gas in = gas out
or
Gas load = throughput
 Creating vacuum - concepts

Gas load from the chamber means gases entering the gas phase from all sources: gas leaks (deliberate
and accidental), wall outgassing, permeation through gaskets, evaporation of volatile material and back-
streaming of gases and vapors from pumps.
In operation, the pump's throughput is found by multiplying the effective pumping speed from the chamber
by the pressure in the chamber. The effective speed of a pump is smaller than its nominal value, quoted
by the manufacturer, since it is reduced by the limited conductance of the passive components attached
to it (tubes, grids, ports)

Equations:

Throughput of a pump: Q=SP where S is the pumping speed and P is the pressure

Throughput of a passive element: Q=C(P1 – P2) where C is its conductance, p1 and p2 the pressure
(for exampe through a tube) before and after the element

For elements of a system connected in series, we must add the conductance of these elements as in
an electrical circuit:
1/C = 1/C1 + 1/C2 + 1/C3 +…

Effective pumping speed: 1/Seff = 1/S + 1/C

C1
gas load p1 C2 p2
Qin
C2
Effective Pumping
Pumping speed Seff < S
speed S
Qout
 Outgassing and vapour pressure

Outgassing Rate
Outgassing means the surfaces of the vacuum chambers releasing gas into the system, which has been
adsorbed on the surface before or coming from the material itself.
Outgassing rate: the quantity of gas released from a unit area of a solid surface in unit time
Units: (torr x liter / (m2 x s)) or (Pa x m / s) = (N/ (m x s)) = (W/m2)
The SI unit is watts per square meter.

For a solid surface such as the chamber wall, the outgassing rate depends on the surface's composition,
vacuum history and temperature.
The outgassing rate of chamber walls and system fixtures is an important factor since, in a leak-free
high-vacuum or UHV chamber, the total gas load (due to outgassing) divided by the effective
pumping speed gives the base (ultimate) pressure.
•It is usually best to use all stainless steel, aluminum, glass and copper.
•Bakeout and plasma cleaning are successful methods of reducing the ultimate pressure
because they remove gas from the walls and lower the outgassing rate.
•Elastomer gaskets and o-rings should be specifically manufactured for vacuum applications.

Vapor pressure
It is the pressure of a vapor in equilibrium with its non-vapor phases. All solids and liquids have a tendency
to evaporate to a gaseous form, and all gases have a tendency to condense back. At any given
temperature, for a particular substance, there is a partial pressure -- vapour pressure -- at which the gas of
that substance is in dynamic equilibrium with its liquid or solid forms.
Vapour pressure depends on the temperature.
Materials of high vapour pressure at room temperatures are not suitable vacuum materials.
For example:
Brass and zinc and most organic materials are have too high vapour pressures.
 Room temp

Medium
vacuum

High
vacuum
 Pumps
It is a common mistake to think a vacuum pump sucks gas from a chamber. There is no such force as
suction. If gas molecules in one "section" of an enclosed volume are removed, then molecules from the
remaining volume, in their normal random, high-speed flight, collide and bounce off walls until they fill the
total space at a lower pressure.
Until a molecule, propelled by random collisions, enters the pumping mechanism of a pump, it cannot be
removed from the chamber. The pump does not reach out, grab a molecule from outside and suck it in.

Type Mechanism of Pumping

Mechanical (roughing) Compression of gas
Sorption Physical or chemical absorption
Diffusion* Intermolecular collisions
Turbo Molecular collisions with surfaces
Ion Ionization and implantation of gas
Cryo Solidification of gas by liquid He
Sublimation Trapping of molecules by reactive coatings

Ultrahigh High Medium Low

(< 10-7 Torr) (10-3 -7 -3
~ 10 Torr) (1 ~ 10 Torr) (760 ~ 1 Torr)
Rotary Rotary
Sorption Sorption
Diffusion Diffusion
Turbomolecular Turbomolecular
Sublimation Sublimation
Sputter ion Sputter ion
Cryogenic Cryogenic
 Mechanical Pumps

•An oil seal between a phenolic vane Flat

and a steel cylinder is used to Spring
remove gas from the vacuum region Vane
and exhaust it to the atmosphere. outlet
•This pump works from atmosphere intake
to about 0.1 mTorr.
•Precautions must be taken at low 3
pressures to avoid oil backstreaming
into the vacuum vessel.
•It is also used as a backing pump
for compression pumps like a Electric
diffusion pump or turbomolecular Motor
pump.

Lowest pressure: ca 10-3 torr

 Oil diffusion pumps
Lowest pressure: ca 10-8 torr
•Oil vapor forced through jets in the stack transfer
momentum to gas molecules and force them down
through the pump and out the exhaust
•Economical (no moving parts).
•If used with a cryogenic trap, UHV can be routinely
achieved.
•Problem: oil back-streaming into the vacuum system

There are numerous applications for diffusion pumps,

ranging from high gas volume found in molecular beam
investigation and large-scale vacuum furnace processing
to ultra-high vacuum level needed for surface physics
research and space simulation chambers. Best vacuum
close to 10-9 torr requires an exceptionally good LN2 trap
and additional pumping from a Titanium sublimation pump.

Oil traps are used to reduce the oil back-streaming

 Turbopump (turbomolecular pump)
Lowest pressure: ca 10-10 torr

•Turbine blades rotating at high speed transfer

momentum to gas molecules to force them out
to the exhaust (must be backed).
•UHV can be readily achieved (better if used in
combination with a titanium sublimation pump).
•Sensitive to corrosive gases
•Mechanical wear
 Ion pumps
Lowest pressure: ca 10-11 torr

•A high voltage combined with a magnetic field

causes electrons to travel in a helical path with
an energy sufficient to ionize gas atoms.
•The ions are accelerated so they strike a Ti
plate and become buried in the plate.
•Buries the gas in the plate, so no backing pump
is required.
•A little less expensive than turbo pumps.
•Does not pump rare gases well
•Does not pump hydrogen
•Closed system: very safe against vacuum
accidents

Electrons released from the (cathodic) plates are

constrained by the magnetic field into tight helical
trajectories in the (anodic) tubes. The potential energy
of gas molecules ionised in the tubes is converted to
kinetic energy and the cathode sputters titanium when
struck by an ion. The sputtered material coats the
tubes, the cathode plates and the pump’s walls.
Several pumping mechanisms are possible including A typical ion-pump
chemical reaction, ion burial and neutral burial - the last
two accounting for the pump’s ability to handle inert
gases.
 Other types of pumps

A cryopump is a vacuum pump that traps gases and vapours by condensing them on a cold surface.
They are only effective on selective gases, depending on the freezing and boiling points of the gas
relative to the cryopump's temperature. They are sometimes used to block particular contaminents, for
example in front of a diffusion pump to trap backstreaming oil. In this function, they are called a cryotrap
or cold trap, even though the physical mechanism is the same as for a cryopump. Cryopumps are
commonly cooled by dry ice or liquid nitrogen, or stand-alone versions may include a built-in cryocooler.
Over time, the surface eventually saturates with condensate and the pumping speed gradually drops to
zero. It will hold the trapped gases as long as it remains cold, but it will not condense fresh gases from
leaks or backstreaming until it is regenerated. Saturation happens very quickly in low vacuums, so
cryopumps are usually only used in high or ultrahigh vacuum systems.
Regeneration of a cryopump is the process of evaporating the trapped gases. This can be done at room
temperature and pressure, or the process can be made more complete by exposure to vacuum and
faster by elevated temperatures.

In a titanium sublimation pump, an electrical current passes through a rod or wire of titanium and heats it
until its surface temperature rises enough to slowly sublime the metal. The resulting film of titanium
covering all surfaces within a line-of-sight to the filament, reacts with the active gas molecules striking
them to form nonvolatile compounds. In this context, nitrogen, oxygen, hydrogen, etc. become active
gasses, reacting with the titanium film. After depositing the initial film, the current decreases below
sublimation level. When all the film has reacted, the current increases again, either manually or by
timer/pressure control, to deposit another film. Thus, the Ti sub pump activates repeatedly, not just once.
The titanium sublimation pump rarely works as the only high vacuum pump in a system; rather it works
as a supplementary pump in a number of very specific applications.
 Other components, symbols

Pressure measurement Mechanical components

Gauges: thermocouple, Pirani; ion, Cold cathode Valves
Each type is suitable for a certain pressure range Sample manipulators
Vacuum system generally needs several types of gauges Gas manifolds
Load locks

Hand Operated Valve. Vacuum Gauge

Gate Valve. Rotary Pump

Pneumatic Gate Valve. Turbomolecular Pump

Leak Valve. Ti Sublimation Pump

Ion Pump
Butterfly Valve.
Cryo Pump.
Pneumatic Butterfly.

Bellows.
 Typical vacuum system

Pulsed Laser Deposition (PLD) System