Ultra-high Vacuum and good vacuum

practices
K. P. Subramanian and B. Bapat
Physical Research Laboratory, Ahmedabad 380009
E-mail: bapat@prl.res.in
24 August 2012

Introduction

Vacuum technology is part of modern times in many ways, finding application

in electronics, chemical, pharmaceutical and food industries. In research laboratories, vacuum conditions are often necessary due to many reasons. When one
needs to study various reactions, it is necessary to prepare the samples isolated
from their neighbours. This is achieved by manipulating the samples in vacuum
in controlled conditions. Many surface scientists work with their samples in a
vacuum system. The reasons for this are several. First, many samples react with
the gases in ordinary room air which means they must be kept in a clean environment. Second, the experimental probes used to measure sample properties
may get influenced by the ambient environment, to the extent that might not exist
outside a vacuum.
This short note will introduce you to basic terminology and technology for
producing and maintaining vacuum conditions. Ambient pressure is defined as
the current atmospheric pressure which is usually around 1.01 105 Pa, or 1.013
bar, or 760 Torr (which is the pressure corresponding to a 760 mm Hg column).
The composition of air is approximately 78% nitrogen and 21% oxygen with the
remainder consisting of a mix of Argon, CO2 , H2 O and trace gases. At atmospheric pressure there are roughly 1019 of these molecules per cubic centimeter1
which is very high for doing most of the atomic and molecular experiments in
1 Loschmidt

number is Avogadro No. divided by molar volume at NTP, and has a value 2.7

1019 /cc.

gas phase. Kinetic theory of gases states that the pressure exerted by a gas (on
the walls of the enclosure) is proportional to the number density of gas and the
equilibrium temperature of the enclosure.2 It also states that the molecules are colliding themselves. The average distance traveled by two molecules between collisions is called the mean free path3 . In gas phase AMP experiments (mostly, unless
otherwise specified), it is customary to pump down the experimental chamber to
low pressures such that the mean free path of molecules inside the chamber is
larger than the dimensions of the chamber. This would satisfy the primary condition that the investigated molecule on its way to the detector is hardly perturbed
by external sources. However, in many experiments, where purity, noise and detector performance etc. are also important issues, ultra high vacuum conditions
are essential, where the corresponding mean free path would be tens of km or
even larger.

Domains of vacuum

Different pressures ranges are given names in vacuum practice, and these are
rough, low, high, ultrahigh, and extreme high vacuum. They correspond roughly
to the ranges (i) 100 to 103 mbar, (ii) 103 to 106 mbar (iii) 106 to 108 mbar
(iv) 108 mbar to 1011 mbar (v) less than 1011 mbar. This classification is based
on the nature of fluid flow in these three domains of vacuum.
In rough vacuum (as well as at higher pressures), where collision frequency
of gas molecules are large, the fluid flow is viscous. In this region, the imposed
pressure gradient is sufficient to cause a flow of fluid from the chamber to the
mouth of the pump.
On the contrary, in ultra high vacuum conditions, the pressure difference has
little influence in directing fluid flow towards the pump. Mean free path of molecules
are many km in this region, and the gas molecules are perpetually bouncing on
the walls of the chamber and are seldom deflected towards the pump port. The
flow in this region is said to be molecular flow, where viscous character of the
fluid ceases completely.
In the high vacuum range the fluid flow is characterized by both viscous and
molecular properties of the fluid. Because of this mixture of flow types, there may
2 Pressure

P = nk B T where n is the no. density, T absolute temperature and k B the Boltzmann

constant.
3 As a rule of thumb, the mean free path [in c.m.] could be estimated as 0.007/p where p is the
pressure in mbar. However, for exact values, one must use more accurate formulae.

be zones within the same vacuum system with widely varying mean free paths,
on the scale of the vacuum vessel. This is common when there is a steady gas flow
into the chamber.

Conductance, throughput and pumping speed

Quite analogous to electrical circuits, we can imagine that any vacuum line offers impedance to the fluid flow. Ignoring the change in impedance due to the
(chemical) nature of the gas, we can conclude that the resistance is proportional
to the length of the conducting line and is inversely proportional to its area of
cross section. Conductance is the reciprocal of impedance. As resistances add in
series, the conductance of various sections in a vacuum system adds reciprocally.
Also, it has to be noted that the speed of a pump and conductance has same dimensions and is usually represented in lit/sec. Conductance of vacuum lines of
various geometries (such as circular,. Oval, rectangular sections) can be derived
from kinetic theory of gases. The formulae for computing conductance in viscous
and molecular flow regions are different 4 . The quantity of a gas is a measure of
the number of molecules in the gas. This measure is the product of the pressure
times the volume and is also determined by the temperature of the gas. Common
units are mbar-l; though one may use any other convenient unit to express the
quantity. A more useful quantity is the throughput of gas, defined as the quantity
of gas at a specified temperature passing an open cross section of the vacuum system in unit time. Thus, throughput = quantity/time, and has units mbar-l/s. At
high pressures and in rough vacuums, pumping speed is the rate of displacement
of the mechanical pump. However, the concept of displacement fails at high and
ultra-high vacuum and one has to look for other definitions. The pumping sped
at any point in a vacuum system can be defined as the ratio of the throughput
to the pressure at that point. Therefore, it can be written as Pumping Speed =
throughput/pressure. Obviously, pumping speed will have dimension [L3 T 1 ].
4 Formulae

for conductance of vacuum lines with various geometries can be found in the text
book by Dushman, Chapter 2, sections 14

Measurement of vacuum

Measurement of low vacuum

Loss of heat due to conduction of surrounding gas depends on the gas density,
hence pressure. This principle is used in vacuum gauges that are useful in the
lower range of vacuum (typically, 101 to 104 mbar). a. Thermocouple gauge
As the name suggests, a thermocouple junction is used in a thermocouple gauge.
One junction is situated in the vacuum enclosure, whereas the second junction
is held in air in a constant temperature bath at a lower temperature. A steady
DC current flows through both these junctions. If the gas density is larger, heat
loss due to conduction will be more, which will lower the temperature difference
between the junctions. Similarly, the thermoelectric current will increase at higher
vacuum. The ground-free thermo-electric current is monitored and is amplified
using a suitable amplifier. The output signal of the amplifier is calibrated, and is
used to display the vacuum measured directly on a dial gauge.
It should be noted that the heat conductivity also depends on the gas being
used in the system. Therefore, the thermocouple gauges are separately calibrated
for air and commonly used gases such as nitrogen, argon etc. and the calibration charts for each gas is made available for the user. The range of operation
of thermocouple gauge is typically 1 to 103 mbar. b. Pirani gauge While the
thermocouple gauge uses the thermoelectric property, the Pirani gauge uses variation of resistance of a resistor as a function temperature as the principle behind
its operation. The construction of Pirani gauge is fairly simple; it consists of four
resistances wired in the configuration of Whetstones bridge, where one resistance
in vacuum and the others are in air. The temperature of all three resistors (other
than the measuring one) is stabilized. A constant current flows through all resistors. The resistor on the measurement arm exchanges heat with the gas through
conduction. Thus the equilibrium temperature of the resistor on measurement
arm will be higher, and correspondingly its resistance also will change. This will
upset the balance of the Whetstones bridge and the galvanometer will register the
difference. Similar to the case of thermocouple gauge, this signal can be calibrated
against the vacuum. Pirani gauge is also sensitive to the type of gas, and it needs
separate calibration for each gas.
The range of operation of Pirani gauge is typically, 10 to 104 mbar.

Measurement of high vacuum

a. Cold cathode (Penning) gauge Beyond 104 mbar, we need other gauges to measure vacuum. The cold cathode gauge or Penning gauge is the most commonly
used gauge in 103-106 mbar pressure region. Its configuration is very much similar to the sputter ion pump, where an anode, in the form of a wire loop is sandwiched between two cathode plates. Magnetic field, like in a sputter ion pump, is
used to make electrons spiral and enhance ionization of the gas molecules.
The ion current produced in the gauge is measured using an electrometer. This
current is proportional to the number density of gas, hence inversely proportional
to the vacuum. Penning gauge is also a relative gauge, as its operation depends on
the nature of gas. b. Hot ionization (Bayard Alpert) gauge The operation of Penning gauge ceases at around 106 mbar, where the number density is lower than
the density required sustaining Penning gauge. This problem is circumvented in
hot ion gauge, where a constant ionization current is provided by the thermionic
emission of a hot filament. This gauge works on the principle that the ratio of
ion-current (measured) to ionization current (thermionic, maintained a constant)
is proportional to the gas density (vacuum). i+/i- = k p, or i+- = k p., when i- is
kept a constant. The electrons from the filament are accelerated to about 100 eV
by means of a spiral grid. The ion collector is a bare thin metal wire placed along
the axis of the tube.
Earlier BA gauges, which used anodes with larger area suffered a peculiar
problem. The 200 eV electrons (accelerated by the grid) were found to produce
soft Xrays when they were incident on the grid. These Xrays, when absorbed by
large area cathode emitted photoelectrons, which is equivalent to collection of a
positive charge. This error becomes very large at lower vacuum (below 108 mbar),
causing departure from linearity of the i+- = k p relation. This problem is greatly
reduced by Bayard and Alpert, who replaced large area anode to a thin wire. This
modification enabled operation of the gauge up to 1012 mbar.

4.1

Absolute vacuum measurement

McLeod gauge
We have seen that all the above gauges, without exception, depend on one property or other of the gas, and can not be regarded as the absolute gauge. An absolute gauge should measure the pressure purely based on gas kinetic properties,
so that the relation p = nk B T could be used to determine the number density in
absolute way.
5

The first absolute gauge was built by McLeod, which is essentially a mercury
manometer. The mercury manometers are absolute gauges, however, they loses
sensitivity at higher vacuum due to loss in resolution in the determination of mercury column length accurately. In 1874, McLeod devised and ingenuous way,
wherein a larger volume (of the measurement gas) is trapped and squeezed into
a capillary. This increased the sensitivity many fold, and McLeod gauges could
accurately determine absolute pressures down to 105 mbar.
Capacitance manometers
In a capacitance manometer, a chamber of small volume is divided into two regions by a flexible metal membrane. The deflection of the membrane is proportional to the pressure difference across the membrane. If one compartment (reference side) is sealed at a very low vacuum (as compared to the vacuum to be
measured), the deflection of membrane will be proportional to the pressure in the
measurement side. The membrane is included as a capacitor element of an AC
Wheatstones bridge, and the minute deflections are very accurately measured.
The signals are calibrated against an absolute gauge, such as McLeod gauge.
The capacitance manometers are qualified as absolute gauge, as its operation is
independent of any gas property. The capacitance manometer is available in two
configurations. As described above, is the reference side is pumped and sealed
off, then it is referred to as an absolute gauge. If the reference side is connected to a
different vacuum region, for example, upstream and downstream of a gas jet in an
experiment, then it can measure the difference in pressure. In this configuration,
it is treated as a differential gauge.

Creation of vacuum: Types of pumps

The choice of pump depends on the range of vacuum needed in a vacuum system.
Thus the principle of operation of a pump that is used to create rough vacuum
and ultra-high vacuum are vastly different However, all pumps can be characterized by certain parameters such as (i) its gas handling capacity (essentially, the
throughput), (ii) compression ratio (defined as the ratio of outlet and inlet pressures, while the pump is in full operation with zero load) and (iii) their dynamic
range of operation. Further to these consideration, there might be other considerations, such as oil-free vacuum, that governs the choice of a pump for a specific
application.

Pumps used to create rough vacuum:

Mechanical pumps
Mechanical pumps are also called rotary pumps. Since they are capable of pumping down from atmospheric pressures, these pumps forms the first stage of any
other pumps used in a vacuum system. Since they operate at high pressure, their
gas handling ability (or the throughput) is substantially higher than any other
pumps.
Rotary pumps are mechanical pumps, working on the principle of physical
displacement of volume from the vacuum system to the atmosphere (vent). The
displacement is done without any valve, and is achieved by the continuous rotary
motion of a solid cylinder mounted slightly off-axis to the stator. One side of the
rotating cylinder is in contact with the stator, while two retracting, gas-tight vanes
mounted on the rotor divides the volume between the rotor and stator, which
perpetually expands and compresses during the rotor motion. As a result, there
is a displacement of volume at a uniform rate from the system side to the air side,
which causes pump down of the system. For lubrication, the stator is immersed in
low vapour pressure oil. Further, the pumps are provided with gas ballast, which
bleeds small amount of air into the rotor while the pump is in operation. Though
the air ballast decreases ultimate vacuum, it is useful to carry away fumes and
toxic gases and water vapor that may present in the vacuum system. The rotary
pumps operate right from atmosphere (1000 mbar) down to 103 mbar, and thus
the compression ratio is typically a million.
Dry (or scroll) pumps
Rotary is associated with the problem of oil vapour contaminated vacuum, which
may be detrimental in some cases. One substitute for rotory pump (in terms of
its ability to pump down right from atmospheric pressure) is dry pump, which is
free from oil vapour. There are two types of scroll pumps available in the market.
The first type is similar to the centrifuge pump used to pump water. The tips of
impeller blade, made of a tough, low-friction plastic, mounted on a fast rotating
shaft pressed against the stator (properly lined) and it causes constant draft of air
from the inlet side to the exhaust.
The draft is boosted by a special construction, employing Bernoullis Principle.
All the coving parts are free from lubricating oil, and thus the vacuum it produces
is free from oil vapour contamination, hence they are called dry pumps. There
is another variant of dry scroll pump, where the rotory motion is replaced by a
7

vibration motion. The pumping is achieved by perpetual displacement caused

by the cyclic vibrational motion of an expanding helix over another static helix.
During the vibration, the contact region between the helices progressively moves
inward along the radius, causing accumulation of the compressed fluid along the
axis of the pump, from where they are vented out. The moving parts are about
70% less than their counterparts, and these pumps offers longer service. Scroll
pumps operate right from atmosphere (1000 mbar) down to about 102 mbar,
and thus the compression ratio is typically one tenth of a million.
Sorption pumps
Sorption pumps are based on the adsorption principle of gases on a porous surface. Special materials, such as zeolite (a chalk-like material) adsorb and retain
gases on its surface and the retention and release of gas is dependent on the temperature of the material. The process of release of adsorbed gas at high temperature (baked in rough vacuum condition) is known as activation. When the activated zeolite is cooled to liquid nitrogen temperature, its adsorption and retention
capacity is increased many times. This is the principle of operation of sorption
pumps.
Unlike rotary and dry pumps, there are no moving parts in a sorption pump.
Even though sorption pumps can start pumping right from atmospheric pressures, the large quantity of gas will soon saturate the sorption pump. Hence, it
is advisable to use a mechanical pump in conjunction with the sorption pump.
The mechanical pump is needed only during the reactivating phase of the sorption pump. The dynamic range of sorption pump is typically 1104 mbar, and it
offers oil-free clean vacuum.
Roots pumps
Roots pumps are mechanical pumps, however designed for higher displacement
at the cost of the dynamic range. Roots pump need a mechanical pump as backing
pump, however they have much higher pumping speeds in the range of 103 to
104 mbar, where the pumping speed of other mechanical pumps falls rapidly.
Therefore, Roots pumps finds application in molecular beam experiments, where
high throughput pumps are required to maintain 104 mbar pressure in the beam
source region.
Roots pumps have two counter-rotating lobes, each in the figure of 8, cased
inside a stator. The phase angle between these two lobes is 90 , which interlocks
8

a displacement volume, that is perpetually swapped from inlet to outlet port..

The pumping speed is maximum at around 103 mbar range, extending over to
one order lower vacuum. The roots pump requires a high-speed backing pump
during its operation.

Pumps used to create high vacuum

Equipment for generating UHV

At higher vacuum, the mean free path increases, and the pumping by inducing
pressure gradient (by volume displacement technique) ceases. In the molecular
flow region, the molecules bounce back and forth off the chamber wall and are
seldom scattered into the solid angle where pump is placed. The chance that
molecules bounce back to the chamber from the pump body is also very large,
making displacement technique inadequate to pump a system to higher vacuum.
Therefore, from this region of vacuum onwards, techniques to impart preferential
momentum transfer to the molecules in the direction are to be sought. Pumping
techniques for UHV fall into two kinds: active and passive. Active pumps are
diffusion pumps, ion & turbomolecular pumps; Passive pumps are sublimation,
sorption, cryogenic type.
Oil diffusion pump
Historically, the first ever diffusion pump was mercury vapour pump, demonstrated by H. Parameswaran in Rutherfords Cavendish Laboratory. This pump is
known as Warrans Tube. Later, the mercury was replaced by hydrocarbon oils,
and these pumps became an integral part of all laboratories worldwide, until the
Turbomolecular Pumps substituted them in the recent past. They are often the
cheapest pumping solution. Turbo technology has progressed so much, that unless one is interested in extreme high vacuum (< 1010 mbar), one need not look
beyond turbopumps. They operate effectively all the way from 103 to 1010
mbar.
In oil diffusion pump, heavy hydrocarbon oil is brought to boiling point by
an electrical heater. The oil bath is covered with an assembly of inverted, coaxial,
cones with gaps in between, through which the hot oil vapour rises and forms jets
in the downward direction. The oil molecules transfer downward momentum to
the wandering gas molecules, thus gas molecules are dragged to the bottom of
pump, from where they are removed by the backing pump. The body of the
9

pump is cooled by circulating chilled water through coils wrapped over the body
of the pump, which condenses the oil vapour and returns to the reservoir under
gravity. The recycling efficiency is so good, that with a typical 100 ml charge of
the pump oil, the pump can be continuously for several months without breaking
vacuum for oil recharge. The oil used in pumps have the following properties: (i)
The chemical reactivity, especially with oxygen (from accidental leaks), should be
low (ii) The vapour pressure, at around room temperature, should be extremely
low (to avoid back streaming of oil vapour into chamber) and (iii) The molecular weight of the oil should be as high as possible (for high momentum transfer
in each collision with the gas molecule). Ancillary units such as water chiller
and circulation pump are essential for the operation of oil diffusion pumps. This,
along with high power consumption (for heater) makes the operation and maintenance of oil diffusion pump a costly affair. The dynamic range of diffusion pump
is approximately 103 to 108 mbar, and the corresponding compression ratio is
around 100,000 to a million.
Sputter ion pump
The principle of operation of a sputter ion pump is to implant a gas molecule (after ionizing it) on an anode and bury them under a layer of sputtered atoms from
the cathode. A stack of anodes is sandwiched between a pair of titanium cathodes,
holding a potential difference of several kV between them. The entire assembly
is placed inside the vacuum vessel, which is immersed in a strong magnetic field
produced by a pair of permanent magnet pole pieces. There is enough space in the
anode through which electrons produced in Penning discharge (spiraling under
the influence of magnetic field) will bounce back and forth the cathode pairs, like
a simple harmonic oscillator. The function of the magnetic field is to enhance the
path length of electrons by spiraling, thereby increasing probability of collisional
ionization of the remnant gas. The positive ions, upon impingement on the titanium cathode, bounces back after charge neutralization and are buried deep on
the anode plate. The titanium atom sputtered by the gas ion also finally lands up
on the anode, thereby burying the implanted gas atom permanently. This process
goes on continuously till the end of life of the pump, indicated by flaking of the
cathode plates. The typical lifetime of an ion pump is 20,000 hrs., when used at
106 mbar, The life of the pump is dependent on the operating pressure. For example, the same pump, if operated at 107 mbar would provide service for 200,000
hrs.
The dynamic range of sputter ion pumps is 106 to 109 mbar; however, they
10

are recommended to be used from 106 mbar onwards. Use of ion pumps is not
recommended in certain experiments, for example in mass spectrometry, where
the flooding of ions may affect the operation of the mass spectrometer.
Turbomolecular pumps
Turbopumps are based on the principle of mechanically (by means of rotating
blades) imparting momentum in the desired direction to the molecules that enter
it. Clearly, the linear velocity of the blade has to be comparable to the molecular
velocity and the kick must change its direction such that it does not return to
the vacuum chamber. This means that the fan has to move with very large angular
speeds of the order of a kilohertz. As a comparison most common AC motors
such as those in a fan or a water pump spin at only 24 Hz.
A turbomolecular pump in practice consists of several such fan-blades stacked
on a single rotating axis, alternated by static disks of a complementary geometry.
The rotor discs are not all alike. The angle of the blade on each successive rotor
and stator discs and the gaps change from disc to disc. The disc on the vacuum
side have steep pitch and the large gaps, the disk at the air-side end is thicker,
has a shallower angles and smaller gaps. The assembly is a marvel or mechanical
enginnering!
The process of dragging molecules does not entirely remove the randomness
of molecular motion. Collisions with the walls and the blades of the pump keep
occurring. However on the average there are more collisions towards the air-side
end between molecules than at the vacuum end. In effect there is compression
of the pumped gas from one stage to the next. A turboump is specified by its
compression ratio and its pumping speed or throughput. These depend on the
diameter of the rotor, its angular speed and the geometry of the rotor blades. The
compression ratio determines the ultimate vacuum a turbopump is capable of
achieving. The compression ratio is different for different gases (higher for lighter
molecules). Typical values are 1010 for Hydrogen, 108 for N2 , O2 , Ar. Thus to
achieve an ultimate pressure of 1010 mbar, the backing pressure for a turbopump
has to be better than 101 mbar. Pumping using a turbopump is thus a two stage
than affair it needs a backing pump to maintain the 101 mbar backing pressure.
Since a turbopump is an inherently medium-free device it causes very little
contamination. It is therefore prudent to have medium free backing pumps (i.e.
avoid oil-based rotary vane pumps) in conjunction with a turbopump. Current
technology offers three options: diaphragm action, piston driven and scrolling
action pumps. These are in increasing order of performance (and price!) but offer
11

Figure 1: A cross-section through the rotor-stator assembly of a turbomolecular pump.

Figure 2: Scheme of operation of a turbomolecular pump. The backing pressure has to be

of the order of 0.1 mbar or less for optimum performance.

12

clean, contamination-free low vacuum.

Passive Pumps
When pumping to vacua below 108 mbar, it often helps to use a passive pump,
because the efficacy of a turbopump starts falling off rapidly with reducing pressure. There are two basic principles, which may be combined in practice. The first
is to ionise the gas and extract the ions and electrons using a combination of such
a pump. The second technique is based on adsorption (with variations going by
the names of sorption or getter pumps). Certain materials, namely titanium,
certain zeolites, and charcoal or activated carbon are very efficient adsorbers of
molecules in the inner surfaces of their pores. This process is temperature dependent, and also gas-specific.
Cooling a surface to very low temperature increases adsorption (a purely kinetic effect). By maintaining a highly adsorbing surface at temperatures close to
that of liquid helium, it is possible to trap virtually all types of molecules, thereby
creating a vacuum. Clearly the trapped molecules will again move about the vacuum chamber if the temperature of the adsorber rises. The other point is, that
there is a limit on how many molecules a given adsorber can adsorb, so such
pumps can only be useful to improve an already high vacuum and are rendrered
useless if there is a leak.

UHV considerations

Ultra-high vacuum (UHV) refers to a range of pressures between 108 1011

mbar. The mean free paths of the molecules at these pressures are of the order
of kilometers, which means there are no collisions between molecules that can
influence the motion of a given packet of air. So creating and maintaining UHV
implies carrying away molecules that are per-chance favourably directed. There is
no way of forcing them away from the region of interest. This means the pump
has to be very efficient at trapping or keeping in check a molecule that reaches the
pump.
There are several other considerations which can make or break the quest for
UHV. These are collectively labelled as good vacuum practices.

13

Choice of materials
As important as the pump, perhaps even more so, is cleanliness and care in vacuum practice. Many materials of common use simply do not have sufficiently
low vapour pressures to qualify as compatible with vacuum. Even materials that
have low vapour pressure may fail because they exhibit another problem, namely
outgassing. This is a process in which a material that is porous or otherwise is
able to adsorb and store large amounts of gases, will start releasing gases as the
ambient pressure falls. This is a very common and debilitating situation. The
major culprit is hydrogen trapped in the molecular structure of the material and
from decomposition of water vapour, and to lesser extent, trapped CO and CO2 .
It is very important to make a right choice of materials. Metals such as stainless
steel, copper and aluminium and most of the nobler, heavier (titanium, tantalum,
molybdenum, tungsten) metals are are ideal. Metals such as brass and iron or
mild steel are to be avoided. SS, Al, Cu all have outgassing rates of the order or
1012 1011 mbar l/s cm2 after bakeout to 200 C for a long time. However, aluminium will take a longer bakeout time to reach these outgassing rates. Among
non-metals glass & certain ceramics, notably machinable ceramics, such as macor,
are acceptable, as are some specially developed polymers such as viton, delrin,
vespel. It is a prevalent, but bad, practice to indiscriminately use various polymers that exhibit large outgassing rates.
Metals, on account of the processes involved in their manufacture from the ore,
may contain defects of various kinds. While mechanical defects can be serious,
our concern is mainly the trapping of gases in blow holes and cracks developed
during metal forming processes. There may also be undesirable porosity. Metal
forming processes such as electroslag refining are designed to avoid such problems, but there is a higher price to be paid for metal formed by such processes.

Cleanliness and contaminants

Cleanliness in vacuum terminology means exclusion of undesired molecules. This
includes, but is not limited to, commonly understood dirt on surfaces and parts
of an apparatus. Oils, greases and other volatile substances deposited on surfaces
exposed to vacuum are to be avoided. Even our own hands generate a conspicuous amount of oily/sweaty secretions, so touching parts exposed to vacuum by
hand can be quite detrimental to vacuum creation. You may think that this is taking things too far, but it is not. A tiny patch of oil will contain more molecules
than the total number of molecules in the vacuum in the vacuum chamber.
14

Table 1: Outgassing rates of common materials in vacuum practice at room temperature. These numbers vary substantially with the exact nature of the treatment and surface
finish, and should only be treated as a guide.

Material

Treatment

Aluminum
Aluminum
Aluminum

none
baked at 200 C
degreased with trichloroethylene, cleaned
with ethyl alcohol, baked 24h
degreased in acetone, methanol rinse, chem
polished, glow discharge in Ar, baked 15h
at 250 C under vacuum
degreased
electropolished
electropolished, baked 30h at 250 C
Degassing 10 h at 20 C
Degassing 24 h at 250 C
24h outgassing
24h outgassing
24h outgassing

Aluminum

Stainless steel
Stainless steel
Stainless steel
Copper
Copper
Nylon
Teflon
PVC
Kapton
Polyimide
Araldite epoxies
G-10
Borosilicate Glass
Macor

Bake at 300C
Cured 150 C for 15h
none
baked at 250 C
none

15

Outgassing Rate
mbar l/s cm2
1106
5109
31010
51013

4107
41010
91013
11010
51015
6106
6108
2108
1107
4108
5108
1108
5109
negligible

Equally important is to reduce the possibility of tiny pockets of trapped gases

such as in joints of two parts or under screws etc. These will hinder pumpdown
to very low pressure as miniscule amounts of air will keep escaping from trapped
volumes for long periods. Trapped volumes can be reduced and often completely
eliminated by clever design.

Types of joints
We now come to the question of how to make reliable vacuum seals. This is a
critical area, because all vacuum systems need opening and closing at short or
long intervals and there are many cases where a single vacuum system consists
of several sub-systems connected together. Not only the quality of the seal as
regards its leak-tightness, but also its interchangeability with other components
and integrity over repeated open-close cycles, are very important.
There are several types of joints in use, and until recently there were confusing
and cumbersome means of creating seals. The situation is much improved now
with worldwide acceptance of a few key standards for circular joints. The situation, however, is not entirely perfect. Joints broadly fall into two types based on
the range of pressures they are meant for. They fall into two very broad and rather
loose categories when based on the size of the joint.
For low and high vacuum, joints are usually made by mating appropriately
prepared (machined) surfaces with a rubber-like, or polymer material compressed
in between. Joints larger than 10 mm diameter are very well standardized in a series that extends to diameters up to 500 mm. These joints (ISO-KF,LF types) made
by compressing an O-ring (a circular ring of circular cross-section) of a soft, stable
material held in place and prevented from collapsing by a metal ring. Compression is applied by a nut-bolt or clamp arrangement. The best choice of material for
O-rings is Viton, a fluorine based organic elastomer. Other choices are neoprene
(a rubber-like material) and silicone (a silicon polymer).
Ultra high vacuum mandates the employment of all-metal joints. A gasket of
a soft metal such as annealed copper, aluminum, indium or lead is compressed
using enormous force with several bolts between stainless steel flanges having
sharp edges or wedges. All-metal joints deform the sealing material plastically,
so they can usually be used only once. O-ring (polymer) joints described earlier
can be reused several times and are also substantially easier to assemble and disassemble. So, unless UHV is really required, it is usually more sensible to use
O-ring joints of ISO-KF,LF type. ISO-KF joints are very practical for low vacuum
applications, such as for foreline components. It should be remembered that all
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Figure 3: Drawings showing flanges and fittings of the ISO-KF,LF and Conflat standards

polymer O-rings can leave undesired contaminants in a vacuum chamber over

the long run. So, it is prudent to never use, even temporarily, an elastomer O-ring
as a substitue for a metal gasket in a system which is intended for UHV.

Ancillary Equipment
A vacuum chamber containing an apparatus is entirely useless if one cannot draw
out signals from the experiment being performed in vacuum. Likewise it is necessary to send signals for controlling processes or making manipulations in vacuum. Thus, means of transferring light, electrical currents/voltages and mechanical manipulation are needed. These are collectively called feedthrus. Various
options are available in the market and these are usually very reliable and robust
techniques.
Other useful accessories are valves of various kinds. These are needed for
either isolating portions of a large system or to seal off and detach smaller units
from a larger one without admitting air. They are also needed to control the flow
of gases into a vacuum system as and when needed.

The long march to UHV

With all this information, how does one go about building and actually achieving
a UHV system? It really begins at the beginning. All metal joints using copper
or aluminum gaskets are mandatory. Construction (fabrication) should be done
using internal welding to avoid trapped volumes. Parts placed in vacuum should
have extremely low vapour pressure and outgassing rates and should be free of
trapped volumes as far as possible. Pumping systems should be chosen very
carefully. A turbopump with a large compression ratio combined with a piston
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Table 2: Types of joints, their range of sizes, and range of pressure and temperature over
which they can be reliably used with typical applications.
Type
diameter
Pressure
Temperature Application
(mm)
(mbar)
( C)
KF with neo1050
1000106
080
foreline joints
prene seals
KF with viton
1050
1000107
0150
foreline joints, gas
seals
lines, feedthrus
1000106
080
large ports
ISO-K,L,F with 63500
neoprene seals
ISO-K,L,F with 63500
1000107
0150
large
ports
and
viton seals
feedthrus

13
VCR, Swagelok
316
100010
273450
gas lines

13
273450
feedthrus, large ports
CF (copper gas- 16250 100010
ket)
Aluminium
>100
10001012
273250
very large ports
wire seal
or scroll type dry backing pump is a good choice, at least to begin with. Extreme cleanliness, ensured by meticulous cleaning of all components in degreasing solvents (first degreasing using trichloroethylene, then a detergent, then a few
rounds in water and finally in methanol is good practice; sometimes a single organic solvent, such as propanol or trichloroethylene, may be more appropriate) is
needed. Ultrasonic bath treatment is very effective and must be an integral part
of a UHV lab. Parts should be handled with clean, residue-free gloves and thoroughly dried before installation. All this care is still inadequate, as the vacuum
chamber walls will have lots of adsorbed gas, notably water vapour. To get rid of
this is necessary to bake-out (heat) the entire chamber to 200 C or more for several
hours to days. Water vapour is the largest residue in an unbaked vacuum system.
A well prepared UHV system mostly contains hydrogen, and very little else. It
usually takes a few days to achieve UHV.
It is obvious by now that lot of care is needed for obtaining UHV. It may not
be so obvious that care is needed when admitting air into an evacuated chamber.
This is a non-trivial issue. Ordinary air when admitted into UHV will lead to water vapour and other adhesive molecules quickly settling on the surfaces. These
will hinder the next evacuation. A good practice is to admit dry nitrogen into
the vacuum chamber through a controllable valve. This can be achieved either by
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carefully transferring a fixed amount of nitrogen from a higher pressure cylinder,

or by letting liquid nitrogen evaporate via the valve into the chamber. The latter
is the safer and the recommended method.
A natural question arises: how does one avoid and detect leaks? As mentioned
earlier, strict adherence to standards and plenty of care during assembly helps.
Despite precautions, leaks may be present. Leaks in the range of 102 to 106
mbar can be detected by spraying alcohol over suspect joints while looking for a
rapid pressure rise in the vacuum gauge due to the admission of the alcohol. At
lower pressures, this method fails. In fact as a general and reliable practice, the
use of a Helium mass spectrometer based leak detection is highly recommended.
The device consists of a small vacuum chamber pumped by a turbopump and
contains a miniature mass spectrometer tuned to the detection of He+ ions that are
be formed by electron bombardment on helium atoms entering it. The chamber
to be tested for leaks is connected to the leak detector by a large diameter pipe.
Helium sprayed over the suspected joint reaches the mass spectrometer if there is
indeed a leak. This is an extremely effective and highly sensitive method. A leaky
joint may be fixed by tightening but in some cases replacing the joint may be the
only solution. For UHV systems leak testing of components prior to assembly is
strongly advised, as is leak testing of assembled systems prior to the slow, long
march to UHV.

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References
1. The Physical Basis of Ultrahigh Vacuum P. A. Redhead, J. P. Hobson, E. V.
Kornelsen, (Springer)
2. Review of papers regarding vacuum system and materials M. Wong, 21-Mar02 (Fermi National Laboratory), on the web

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