EXPERIMENTAL TECHNIQUES

CHAPTER – 1
VACUUM TECHNIQUES
Units and basic definitions, Roughing pumps - Oil sealed rotary vacuum pump and Sorption pump,
High vacuum pumps – Turbo molecular pump, Diffusion pump, Oil vapour booster pump, Ion pumps
- Sputter ion pump and Getter ion pump, Cryo pump, Vacuum guages - Pirani gauge, Thermocouple
gauge, penning guage (Cold cathode Ionization guage) and Hot filament ionization gauge, Vacuum
accessories – Diaphragm, Gate valve, Butterfly valve, Baffle and isolation valves, magnetic valves,
adjustable valves, air inlet valves, Traps - Liquid nitrogen trap, Sorption traps, and gaskets and O
rings

VACCUM:
• Vacuum is a region with a gaseous pressure much less than atmospheric pressure.
Vacuum is space devoid of matter.
• The word stems from the Latin adjective vacuus for "vacant" or "void".
• The Latin term in vacuo is used to describe an object that is surrounded by a vacuum.
Types of vacuum:
• Low vacuum
• Medium vacuum
• High vacuum
• Ultra-high vacuum
• Deep space vacuum
• Perfect vacuum
• Hard vacuum and soft vacuum
Uses of vacuum:
 • incandescent light bulb to protect the filament from chemical degradation.
• electron beam welding, cold welding, vacuum packing and vacuum frying.
• Ultra-high vacuum is used in the study of atomically clean substrates.
• High to ultra-high vacuum removes the obstruction of air, allowing particle beams to deposit
or remove materials without contamination.
• Vacuum is the principle behind chemical vapor deposition, physical vapor deposition, and dry
etching which are essential to the fabrication of semiconductors and optical coatings, and
to surface science.

BASIC TERMS & CONCEPTS OF VACUUM TECHNOLOGY

[1]. Absolute Pressure ( Pabs ):
- Specified in vacuum technology so that ‘abs’ index can be normally omitted.
[2]. Partial Pressure ( Pi ):
- PP of certain gas/vapour in the vessel is the pressure which that gas/vapour exert if it
alone was present in the vessel
[3]. Total Pressure ( Pt ):
- Sum of partial pressures for all gases & vapours in the vessel.
[4]. Volumetric Flow ( Flow Volume – qv ):
- ‘flow volume’ – volume of gas which flows through a piping element within a unit of
time, at the pressure and temperature prevailing at the particular moment.
- Even if volumetric flow can be identical, no. of molecules moved may differ depending
on P & T.
- Units: m3/h , cm3/s
[5]. Pumping Speed ( Se ) :
 1. Speed of exhaust:
 Volumetric flow through the pump’s intake port.
 If dt is infinitesimal time span during which an infinitesimal volume of gas dV is
exhausted into pumping line;
𝒅𝑽
𝑺𝒆 =
𝒅𝒕
2. Pumping Speed ( SP ) :
 Speed of vacuum pump measured at pump inlet.
 Volume of gas entering the pump per unit time where prevailing pressure is Pp
 If dt is infinitesimal time span during which an infinitesimal volume of gas dVp where
prevailing pressure is Pp is entered into pumping line;
𝒅𝑽𝒑
𝑺𝒑 =
𝒅𝒕
3. Pumping Speed at any intermediate point ( Si ):
 Volume of gas dVi passing through any point in system at time dt measured at
prevailing pressure is Pi.

𝒅𝑽𝒊
𝑺𝒊 =
𝒅𝒕

• If S remains constant during pumping process, then one can use the difference quotient
instead of differential quotient.
∆𝑽
𝑺=
∆𝒕
[6]. Pump Throughput ( qpV ):

- The pump capacity ( throughput ) of a pump is equal either to the mass flow through the
pump intake port :
𝒎
𝒒𝒎 =
𝒕
Or to the pV flow through the pump’s intake port:

𝒑. 𝑽
𝒒𝒑𝑽 =
𝒕
𝒒𝒑𝑽 = 𝒑 . 𝑺
where S is the pumping speed of the pump at intake pressure of p.

[7]. Pump Compression Ratio:

- Ratio of exhaust pressure to inlet pressure
- Directly indicates amount of work to be done by the vacuum pump to drive away the gas
molecule from system.
- Smaller the ratio, easier for the pump to achieve smaller ultimate pressure on exhaust
side.

TYPES OF VACUUM PUMPS

 Positive Momentum
Displacement Transfer type Cryo Pump Sorption Pump Ion Pump
Pump Pump

I. ROUGH VACUUM PUMPS:

Pressure ranges:

RANGE PRESSURE
LOW VACUUM PUMP 759 to 1 x 10-3 (mbar)
HIGH VACUUM PUMP 1 x 10-3 to 1 x 10-8 (mbar)
ULTRA HIGH VACUUM PUMP Less than 1 x 10-8 (mbar)

Types of Rough Vacuum Pumps:

Rotatory Vane Rotatory Piston

Dry Mechanical Blower/Booster
Mechanical Mechanical Sorption Pump
Pump Pump
Pump Pump

OIL-SEALED ROTARY VANE PUMP:

- Rotary pump
- Positive displacement class (operation based on periodic variation in volume of Pump chambers)
- Main parts: Stator, eccentrically positioned Rotor
Stator:
▪ Also called casing
▪ It is a steel cylinder with ends enclosed by
plates that hold the shaft of rotor.
▪ Pierced by inlet & exhaust ports positioned on
either side of vertical.
▪ Inlet port →connected to vacuum system.
▪ Exhaust port → provided with an outlet valve
( a metal plate moving vertically between
arrester plates or a sheet of neoprene which is constrained to hinge between stator and a metal
backing plate.
Rotor:
▪ Consists of a steel cylinder mounted on a driving shaft
▪ Its axis is parallel to that of stator. Axis is placed such that it makes contact with top surface of
stator → line of contact lies between 2 ports.
▪ The line of contact is known as the top seal between the stator and the rotor has a clearance of 2-3
microns.
Vanes:
▪ A diametrical slot is the cut-through length of the rotor and carries the two vanes.
▪ Rectangular steel plates which make a sliding fit in the rotor slot and are held apart by a spring.
▪ Diametrical slot ensures that the vanes of the rounded edge are always in good contact with the
stator wall.
Significance of Oil:
▪ The stator rotor assembly is submerged in suitable oil.
▪ It is usually a low vapor pressure hydrocarbon oil (poly-phenyl ether or alkyl – naphthalene)
▪ Desirable properties of rotary pump oil are:
 High viscosity
 Low vapor pressure
 High temperature resistance
Working of Rotary Pump:
Three stages of working of a rotary pump are:

SUCTION COMPRESSION EXHAUST

• As one of the vanes passes the inlet port, the vacuum system is connected to the space limited by
the stator, the top seal, the rotor and that vane.
• The volume of this space increases as the vanes sweep round and produce a decrease in system’s
pressure.
• This continues until the time the other vane reaches the inlet port, when the volume of the gas is
evacuated is isolated between the two vanes.
• Further rotation sweeps the isolated gas around the stator until first vane passes to the top seal.
• The gas is now held between the second vane and the top seal and by the further rotation it is
compressed until the pressure is sufficient (about 850 torr) to open the exhaust valve and the gas
is evacuated from the pump.
• During the operation of the pump, the oil seals the small clearances between the moving parts to
prevent leakage of pumped gas.
• At the very end of each compression stage the cavity under the valve and the volume vacated by
the pumped gas are completely filled with oil.
• In this way the effect of clearance space on the ultimate pressure is minimized.
• In addition to sealing, the oil lubricates and partly cools the pump.
• Oil circulates continuously into the pump chamber from a reservoir where it is held under
atmospheric pressure.
Mathematical part: -
Since both vanes are in operation, during
one rotation of the rotor a volume of gas is
displaced by the pump. Hence the volume
rate at which the gas is swept round the
pump, referred to as pump displacement
(St) is
St = 2 vn
v - volume between vanes, n - number of
rotations per unit time .

SORPTION PUMP
• Dry pump which operate without the use of oil.
• Provide an alternative to the oil-sealed mechanical
pumps.
• Suitable for small and medium sized systems with
very light gas loads.
• For pumping systems from atmospheric pressure
down to 10-2-10-3 Torr.
➢ Whenever a gas comes in contact with a solid, the
solid takes up some of the gas and this process is
known as sorption.
➢ Solid can give up some of the gas and this process is
referred to as desorption.

Factors of Sorption & Desorption:

✓ Temperature of the solid
✓ Nature of the gas
✓ Gas pressure

SORPTION SORPTION

ADSORPTION PHYSISORPTION

ABSORPTION CHEMISORPTION
 ❖ Adsorption - formation of the gaseous layer on the surface of the solid.
❖ Absorption - penetration of the gas into the bulk of the solid.
• Solid which takes up the gas is known as adsorbent or absorbent and the gas removed is known
as adsorbate or absorbate.
• The forces attracting the gas molecules to the solid may be of physical or chemical origin.
Accordingly sorption may be physisorption or chemisorption.
• In a sorption pump the gas molecules are held on the adsorbent surface by physisorption.
• The idea of sorption was put to use for creating vacuum in 1875 by Dewar. He used porous
charcoal as the adsorbent.
• Nowadays charcoal has been partially replaced by naturally occurring and synthetic zeolites.

Zeolites:
o DEFINITION: Porous aluminum silicates combined with one or more other metallic
elements, having the composition Na2O.Al2O3. nSiO. XH2O, in which the atoms are
arranged in tetrahedral forms about the Al and Si atoms.
o Have large surface areas on which the gas could be adsorbed.
o Known as molecular sieves.
o The tetrahedra are arranged in complex three-dimensional forms by sharing oxygen atoms
so that there are vast number of cavities formed which are joined by pores.
o These materials adsorb large amount of gas when cooled with liquid nitrogen and hence
all sorption pumps need liquid nitrogen to operate.

CONSTRUCTION:
➢ Consist of a cylindrical canister [Stainless steel/ Aluminum /Borosilicate Glass] that is filled
with the adsorbent in the form of pellets.
➢ The canister is placed in a Dewar (Pyrex flask) cooled by liquid nitrogen.
➢ Since zeolite is a poor heat conductor an array of aluminum fins inside the pump is used to
improve the thermal contact with the sieve material.
➢ There is a Pressure relief valve.

This design influences only pumping speed.

WORKING:
❖ Gas molecules are actually trapped on the surface of the sorbant material cooled to liquid
nitrogen temperature.
❖ Gas is subsequently released when the sorbant material is returned to the ambient
(surrounding) temperature.
❖ Since it is a cyclic pump, working has 3 phases:
1. Sorption:
- Used to create vacuum.
- Achieved by cooling the body to lower temp. using Dewar flask.
- Gas will neither condense nor get absorbed.
2. Desorption:
- Pump warm up to room temperature.
- Gases escape through pressure relief valve.
- This step should be careful while pumping Toxic/Inflammable gases.
3. Regeneration:
 - Pump is heated to 3000C to drive off water vapour.
- Vapour accumulates on molecular sieves.
- Takes around 2hrs to fully regenerate the pump.

When the pump is not used, it should be closed from atmosphere to avoid vapour saturation.
Need of Pressure relief valve: Saturated pump contains sufficient gas to develop a pressure of many
atmospheres in the pump volume during warm up => a pressure-relief valve on the pump to avoid
over pressure during either a routine or accidental regeneration.
ADVANTAGES:
✓ Absence of oil/contaminants
✓ Low cost maintenance
✓ Vibration free operation (since no moving parts)

DISADVANTAGES:
✓ Cannot operate continuously.
✓ Cannot pump H2, He & Ne (due to low condensation temperature than liquid N2

APPLICATION: Roughing pump for sputter ion pump in UHV experiments.

II. HIGH VACUUM PUMPS:

OIL DIFFUSION PUMPS
It is most commonly used high vacuum pump in industrial vacuum processing.

Structure of Diffusion Pump:

➢ Consists of a cylindrical body fitted with a flanged inlet for

attachment to the system to be evacuated.

➢ It is a stainless-steel chamber that vary in size based on the

application.

➢ Interior of diffusion pumps:

o Consist of three varying sized, cone-shaped pressure jets stacked

vertically.

➢ Lowest stacked cone:

o Largest, decreases in size as you move upwards (like an upwards

pointing arrow).

➢ The upper two thirds of the body are surrounded by cooling coils.

➢ An outlet duct or foreline is provided at the side of the lower pump

body for discharging the pumped gases and vapours to the mechanical fore
pump.

➢ Bottom of the chamber:

o Heater → Silicone-based diffusion pump oil is heated until it reaches gaseous state
(180 – 270°C).
 o Closed, forming the boiler which is
fitted with a heater.

o A suitable oil called pump fluid or

working fluid is at the bottom of the
boiler.

➢ Jet forming structure:

o Consists of a concentric cylinder

partially capped and fitted with flared
ends to form umbrella shaped jets
through which the pump fluid vapours
can emerge at supersonic speeds.

o This portion is called the chimney.

o The chamber to be evacuated and the diffusion pump are separated by the baffle
valve.

Pump fluids commonly used:

❖ DC704 and DC705 (phenyl siloxane compounds)

❖ Neovac-SY and Santovac-5 (Phenyl ethers)

❖ Fluorinated poly-phenyl ethers

Working Principle:

The chamber and the diffusion pump can be

independently roughed by closing the appropriate valve
to the fore pump. After the initial pumping of both
sides to nearly 10-1 Torr, the valve connecting the
chamber to the fore pump is closed and simultaneously
the baffle valve is opened. Now the diffusion pump is
ready for operation.

1. Working fluid in the boiler of the pump is heated by

means of an electric heating coil clamped to the lower
body and a vapour stream is created.

2. The excited gas vapour travels upward and exits

through the pressure jets that are pointed at downward
angle ( They travel at an incredible 750 miles per hour
sometimes breaking the sound barrier).

3. As the gas travels toward the walls of the pump chamber, it traps air molecules along the way
through "diffusion".

4. As the walls of the pump chamber are usually water-cooled, when the gas reaches the
chamber walls, it immediately returns to liquid state releasing the trapped air molecules at a
lower position and at increased pressure creating the vacuum.

5. The condensed oil vapours returned to the boiler get re-evaporated and maintains the vapour
flow to the jet assembly.
 6. The entrained gas molecules continue their flow towards the exit where they are removed by
the mechanical forepump.

Difference b/w Single & Multi-staged Pumps:

▪ Commonly used small multistage pumps often have three stages and large ones five or even
six.

▪ The number of pumping stages or vapour nozzles depends on performance specifications.

▪ Requirements of single stage pump: high pumping speed, high compression ratio.

▪ Requirements of multistage pump: first stage at the inlet has high pumping speed and low
compression ratio and last (discharge) stage vice versa.

Pressure range:
 Normally, 10-1 and 10-10 Torr

 Baking and subsequent cooling of pumped chambers, inlet ducts and baffle valves are
required to extend the pressure range, since they can reduce out-gassing as well as produce
some sort of sorption pumping effects.

 Without the assistance of the cryogenic pumping and without baking the lowest inlet
pressures, pressure conveniently achieved is nearly 10-8 Torr.

 With the aid of cryogenic pumping and liquid nitrogen cooled traps, inlet pressures below
1 x 10-10 Torr can be obtained.

Advantages:
▪ No moving mechanical parts
▪ Reliable
▪ Operates practically without noise or
vibration
▪ Relatively low cost to purchase,
operate, and maintain

Applications:
▪ Analytical and mass spectrometry
▪ Instrumentation
▪ Research development
▪ Nanotechnology

TURBOMOLECULAR PUMP
 ➢ Used to obtain and maintain high vacuum.
➢ Principle: Gas molecules can be given
momentum in a desired direction by repeated
collision with a moving solid surface.
➢ A rapidly spinning fan rotor 'hits' gas
molecules from the inlet of the pump towards the
exhaust to create or maintain a vacuum.
➢ Clean vacuum pump and is the developed
form of the molecular drag pump

Pump concrete:
1) traction molecular pump and high-speed movement of gas molecules collide and get
momentum rotor driven to the pump outlet.
2) turbo molecular pump by high-speed rotation of the rotor blades and the stationary blade
with each other achieves given pumping. Such pumps are typically operating the molecular
flow state.
3) It is composed of complex turbo molecular pump and traction type two series combination
of a complex type of molecular pump.

WORKING:

✓ Gas is drawn into the pump from the inlet

side.
✓ There are a series of disks with a row of
blades, alternately fixed and moving. There
may be as many as 20 - 60 blades in each
disk.
✓ The fixed blades are fitted to the stator and
the moving blades are part of the rotor. In
each disk the blades are inclined with respect
to the disk plane, in one direction for the
blades of the moving disks and in the other
for the blades of the fixed disk. Each rotor and stator disk can be called a compression stage.
✓ A pump may have as many as ten to forty such stages.
✓ The moving disks have a high rotational speed so that the corresponding peripheral speed of
the blades can be of the order of 500 m / s.
✓ Therefore, the speed of the molecules of the pumped gas is also of the same order.
✓ Thus, the turbomolecular pump compresses gases by momentum transfer from the rapidly
rotating blades of the rotor disks to the gas molecules.
✓ The rotor impulse is thus transmitted to the molecules.
✓ The non - directed random motion of the particles is changed to a directed motion, thus
achieving the pumping process.
Mean free path of the particles:

• It should be larger than the spacing between the rotor and the stator blades.
• Hence a turbomolecular pump is not capable of pumping gases against atmospheric pressure
→ backed by a suitable roughing pump.
• The gas is expelled through the exhaust port.

EQUATION PART:

The pumping speed and compression ratio i.e. ultimate vacuum

obtained by a Turbomolecular pump is mainly decided by:
▪ Molecular weight of gas to be evacuated
▪ Rotational velocity of the pump rotor
▪ Flow channel geometry
▪ Total number of rotor and stator blades per
stage
▪ Total number of stages
The maximum compression ratio K is given in terms of the
molecular weight of the gas being pumped and the rotor speed
v as follows:
𝐾 = 𝑒 𝑣𝑔√𝑀
where g is a factor depending on the geometry of the stator and rotor blades.
➢ Essentially this factor depends on the rotor blade angle and the ratio of the distance between
the blades and the blade width.

ION PUMPS:
• Operate on the basis of maintaining a lower gas density within themselves than that of gas
existing in the environment they are pumping.
 net gas migration into the pump (due to the random motion of the molecules)
• Once in the pumps, few gases escape and they are either displaced or captured, depending on
the type of pump.
• Displacement type pump: molecules of gas move through it to the atmosphere.
• Ion pump: captures and stores them.
 pump must be cleaned out and renovated at some point in time.
• The decrease of gas pressure in vacuum devices with an electric discharge has been known
for a very long time.
• This is due to the fact that certain gases react with the cathode and are deposited on the walls
as solid particles.
• Generic name - Sputter Ion Pump (or Ion Getter Pump)
 Reason: some of the gas molecules undergo ionization and cause sputtering of the gettering
agent. This material chemically reacts with the active gases => stable compounds formed =>
deposited on the internal walls of the pump.
• The getter is provided initially by a plate/electrode, which is sputtered away by gas ions
formed under the influence of the high voltage in the range of 3,000 to 7,000 V DC.

Operation Of Ion Pumps:

1) Gas molecules enter a field of high-speed electrons where some are subjected to collisions.
2) In the collision process, a molecule may lose one or more of its own electrons and thereby is left
as a positively charged ion.
3) Under the influence of a strong electric field, the ion is accelerated into the titanium
cathode(getter).
4) The force of this collision causes atoms to be physically removed from the electrode and
"sputtered" onto the adjacent walls of the pump.
5) This particulate titanium is extremely reactive and will chemically unite with the active gases.
6) The resulting compounds accumulate on surfaces of the pump elements and pump walls.

• Active gases - oxygen, nitrogen, CO, CO2, and water

• Non-Reactive gases - Noble gases like helium, neon, argon, krypton, and xenon.
 Pumped by "ion burial," (Ion burial is the "plastering over" of inert gas atoms by the
sputtered getter atoms.)

(1) SPUTTER ION PUMP

The simplest form of ion pump is the Penning cell (cold
cathode vacuum gauge)
Parts:

• Central anode unit (cylindrical):

➢ usually made of stainless steel
➢ upon which a positive voltage is
imposed.
➢ can either be a short section of metal
tubing or a square box-like structure,
open at each end.
➢ Opposite each open end is placed a plate
of titanium metal that is electrically
connected to ground to form the cathode
structure.
➢ A single cell configured in this way is
said to be a single diode pump.
• High vacuum Container:
➢ Anode cell unit is packaged in this.
 unit cell becomes a pump with a pump speed of about a litre per second.

• Higher speed pump = an array of more cells.

• Function of the anode cell structure:
 ➢ To contain a "cloud" of high-energy electrons, which are constrained by the magnet
field.
➢ This field causes the electrons to move in oscillating spiral paths that increase their
chances of striking gas molecules and thereby create positive ions.
➢ These ions are accelerated by the positive anode voltage and made to smash into the
titanium cathode plates.
• This results in one of two things:
i) These positive ions can be buried in the cathode or get reflected to be buried
elsewhere.
ii) The impact can also result in the removal of titanium atoms by "sputtering".

• The sputtered titanium is deposited on the internal surfaces of the pump where it reacts with
adsorbed active gases to form stable compounds.
• Thus, there is no removal of gases from the system but rather, they are bind down physically
or chemically => They can no longer contribute to the pressure in the system.
• Function of the ions:
 Maintain a fresh supply of "gettering" material.
=>ion pump is self-regulating
 At low pressures cathode plates are not wasted
 Electric power is conserved.
• Some of the noble gas atoms are pumped as the result of being ionized.
• In this case, they are buried in the cathodes by the force of the accelerating voltage.
• Others are pumped by burial in the sputtered titanium film.

Triode Ion Pumps:

• Pumping noble gases does not pose a

problem (since present in small quantities)
• At above average quantities, a pump of the
triode configuration should be used.

Cathode:

• Is at negative potential
• Built with slits that permit grazing
incidence sputtering.
 ions cannot be buried to any appreciable extent
 Un-sputtering of previously buried noble gases is largely eliminated.
(Instead, the gases either react with or are buried by the sputtered film on the walls of the
pump body.)
• Consists of multiple strips of titanium held at -5 kV.

Anode cell array:

- made of stainless steel
- held at ground potential.
• In each cell a cold discharge is initiated by stray electrons or by cosmic rays (by field
emission) because of the high applied electrostatic field.
• Ions – produced by the energetic electrons →electrostatically trapped in each cell.
 • The electrons are injected into each cell with insufficient energy to escape through the grid
and with high angular momentum for them to travel directly to the anode in the center of each
cell.
∴ Injected electron spirals about the anode until an ionizing collision occurs.
• Large amounts of ionization can be produced in this way by small electron currents.
• The positive ions produced in each cell are accelerated away from the positive central
electrode and through the open grid.
• Ions passing through the grid are then post accelerated by a bias voltage between the grid and
pump housing (the cathode) => all ions acquire sufficient energy to be buried in the titanium
covered cathode.
• Post acceleration: Important advantage of the triode design - results in higher ion pumping
speeds with correspondingly lower ultimate pressures.
• The pump retains the gas it has previously pumped by continuously evaporating fresh
titanium layers onto the gas covered surface => previously pumped gas is covered over
deeper and deeper rather than being exposed and sputtered off as in sputter-ion pumps.

Sputter Ion Pump with Roughing Pumps:

• Invariably operated in combination with a roughing pump.

• Can be:
➢ Two-stage mechanical rotary pump
➢ Sorption pumps
➢ Combination of both sorption & rotary pumps.
• Roughing pressures - below 5 x 10-3 Torr.
• When the required roughing pressures have been achieved → sputter ion pump is started.
• Large power will be dissipated => pump warms => previously trapped gases to escapes.
• The roughing pump and the sputter ion pump are operated in parallel until the system pressure
begins to fall.
• Fall of pressure → Roughing pump is isolated.
• Period of parallel operation:
- major gas load involves water vapour released from the pump.
- Hence it is better that a liquid nitrogen cooled sorption pump is used as the roughing
pump.
• No pumping fluid in the ion pump => No contamination by the vapours of it.
• When the pressure falls below about 5 x 10-4 Torr the power dissipation in the pump
decreases and the system pressure starts falling rapidly.
• The initial large power dissipation has the advantage that the cathode surface is cleaned and a
considerable fresh titanium layer is sputtered on the pump interiors.
• We have seen that physical and chemical sorption and also chemical reactions at the surface
of certain materials can be utilized for pumping.

ADVANTAGES:

• No massive, expensive magnets are required to provide electron confinement.

• Ionization occurs without an arc discharge.
• Because of this multi-cell design, the pump can achieve considerably higher ion pumping
speed than other electrostatic pumps with equal diameters, lengths and anode voltages.
GETTERERS:
➢ Substances pumping by chemical adsorption and reactions are called getterers.
➢ Metals in the form of thin film evaporated into the wall of the container acts as getterer.
➢ Titanium is the most extensively used getterer.
➢ It getters all common chemically active gases except methane.
➢ Zirconium, tantalum and molybdenum are also used in ultra-high vacuum.
➢ Certain getters selectively adsorb gases. (E.g.) Evaporated rhodium film adsorbs H2, CO, O2
and simple hydrocarbons but does not adsorb N2.
➢ The getter pumps or chemisorption pumps have the following two advantages:
(i) Pump is clean and there is no pump fluid vapour which may enter the system.
(ii) High pumping speeds can be obtained by depositing the adsorbing layer on
the wall of the vacuum vessel itself.
➢ Even if an area of only moderate size is covered with the adsorbent, the pumping speed can
be large since the pumping occurs in the vessel itself.
➢ Instead of this if we use a separate pump, the speed is reduced by the limited conductance of
the connecting pipe.
(2) GETTER ION PUMP
o In these pumps the gas is ionized and the ions are driven toward an auxiliary pump, generally
a sorption pump like getter pump.
o The ions are captured by metal surfaces such as Ti which also pump by sorption.
o These pumps are called ion- sorption or getter-ion pumps.
o The electrons which are needed to ionize the atoms are generally produced by a hot filament.
o These pumps are most suitable to retain vacuum in systems while unattended.
o If an ion-sorption pump stops due to a power failure, only a small amount of gas may be
reemitted into the system, whereas if a diffusion pump ceases operating, large quantities of
gas enter into the system.

CRYO PUMP
High vacuum pumps which function on the basis of the combined action of condensation and
adsorption of gases and vapours on to solid surfaces held at low temperatures are called cryogenic
pumps.

• clean vacuum pumps

• capable of producing very high vacuum down to 10-10 Torr.
• It can operate over a wide range of pressures, typically from about 5 x 10-3 Torr to 1 x 10-11
Torr.
• Any mechanism that captures gases on a cold surface is a cryopump
• Vacuum pump that traps gases and vapours by condensing them on a cold surface
• Effectiveness depends on the freezing and boiling points of the gas relative to the cryopump's
temperature.
• Usually used in high or ultrahigh vacuum systems (since saturation happens quickly in low
vacuums)
Classification of Cryo-systems:

➢ Open (refrigerant open to the atmosphere) - (E.g.) liquid nitrogen trap

➢ Closed (not exposed) -(E.g.) household refrigerator

PRINCIPLE:

• All solids and liquids give off vapours consisting of

atoms and molecules of the substances that have
evaporated from the condensed forms.
• These atoms or molecules exert a pressure known as
the vapour pressure.
• If the substance is in an enclosed space, the vapour
pressure will reach a maximum value depending on
the nature of the substance and the temperature.
• This maximum value occurs when there is a dynamic
equilibrium between the atoms or the molecules
escaping from the liquid or solid and those that strike
the surfaces of the solid and the liquid and return to it.
• Under equilibrium conditions, the total pressure existing in the region of the cryo surface will
be the sum of vapour pressures offered by the component gases.
• If a gas is contained in a vessel with surfaces maintained at low temperatures and if the
pressure is higher than the vapour pressure corresponding to this temperature, then the gas
will condense on the surface.
 • This occurs when the gas molecules striking the surface lose enough of their kinetic energy to
remain adsorbed on the surface.

WORKING OF CRYOPUMP:

• In general vacuum is created by removing gas from a

closed chamber molecule by molecule.
• Pump is commonly cooled using:
➢ Compressed helium
➢ Dry ice
➢ Liquid nitrogen
➢ Stand-alone versions may include a built-in
cryocooler.
• While alternative methods push molecules through
the pump, cryopumps freeze gases into solids, thereby
reducing vapour pressures to such a point that high vacuum
is created.
• To achieve this, a cryopump uses a closed-cycle helium gas refrigeration system to cool specially
designed surfaces to temperatures of about 15 K and 80 K.
• The random motion of gas molecules brings them into contact with these cryogenic surfaces
where they are condensed or adsorbed.
• Baffles are often attached to the cold head to expand the surface area available for condensation,
but these also increase the radiative heat uptake of the cryopump.
• Over time, the surface eventually saturates with condensate and thus 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 back streaming until it is regenerated.
CRYOPUMP EFFECT:

• Cryo-pumping effect is produced by intimate interaction between the gas particles to be

pumped and a cold surface provided to them in the cryopump.
• Forces involved are relatively weak (primarily van der Waals dispersion type) and do not
include chemical bonds.
• They do not require such high temperatures for regeneration.
• Can pump all gases including noble gas, if the temperature is sufficiently low.
• Number of molecules that can be accumulated depends on a number of physical factors:
➢ Physicochemical properties of gas
➢ Properties of surface (surface energy distribution)
➢ Microscopic roughness of the surface
➢ Temperature of gas and surface,

TERMS RELATED TO CRYOPUMPING:

1. Cryocondensation:
o Surfaces must be cooled to such a temperature as to keep the corresponding saturation
pressure equal to or below the desired vacuum pressure in the chamber.
o The achievable pressure is determined by the saturation pressure at the temperature
chosen for the cold surfaces.
o This principle is the most elementary of all forms of capture pumping.
2. Cryosorption:
o Gas particles impinging on a surface of sufficiently low temperature lose so much of
their incident kinetic energy that they stay attached to the cold surface by weak
intermolecular forces
 o This results in significantly higher molecular concentration on the surface than in the
gas phase.
o This phenomenon is called physical adsorption or physisorption
3. Cryotrapping:
o This is the concurrent pumping of two or more gases by entrainment of gas particles
which are not condensable at the prevailing temperatures and pressure conditions.
o For the purpose of entrainment, a condensing gas is used, so that a mixed condensate
is formed.
o Usually, the small molecules of the gas to be pumped are caught in the open lattice of
the cryodeposit of a more abundant species and are quickly buried by subsequent
layers.
4. Regeneration:
o Just like other capture pumps, regeneration or periodic removal of accumulated gases
is required for cryo pumps.
o To achieve optimum pump performance correct regeneration is essential.
Regeneration is nowadays performed by automatic controllers.

ADVANTAGES:

➢ No fluids are used in these pumps.

➢ High-speed pump especially for pumping out water vapour as it can be condensed and
pumped out at relatively high temperatures.
➢ Cleanliness (only possible source of contamination is from the gases pumped) .
➢ High speed
➢ High throughput
➢ Ability to handle high impulsive gas loads
➢ Freedom from messy accidents
➢ Operating economy
➢ Choice of orientation

DISADVANTAGE:

➢ High capital cost

➢ Requires regeneration
➢ Requires periodic maintenance.
➢ Low capacity for hydrogen and helium

MATHEMATICAL PART:
Heat load onto the cryo surface determines the refrigerative power required.
They arise from three main sources:

1. Thermal conduction of residual gas

▪ Thermal conduction heat load is found to be negligibly small.
2. Condensation load of the pumped gases
▪ The heat load due to condensation of gas is directly proportional to the throughput.
3. Radiation of residual gas
▪ The radiation heat load Wr depends on various factors like the area and emissivity of
the cryo surface etc.

If S is the maximum pumping speed per watt of refrigeration then;

(𝟏 − 𝑾𝒓 )
𝑺=
𝟎. 𝟒𝟗𝒑

VACUUM GAUGES
• Devices which are used for measuring the pressure of the residual gas in any enclosure are
called vacuum gauges.
• Based on some property of the gas which directly or indirectly depends on its pressure.
• The requirement is that the dependence on the pressure is unique and relatively simple one.
• used to convert the measure of the property into an observable reading which gives the
pressure.
• Vacuum gauges can be broadly classified into two types :
i) Direct reading type - transducers that measure the pressure by means of the force
exerted by the gas on a suitable surface are used
ii) Indirect reading type - pressure is determined by a property the gas depends on the
pressure in a unique way.

Direct Reading Vacuum Gauges

1) Liquid Column Manometer

TORICELLIAN BAROMETER:

• Uses mercury or some other low vapour pressure

liquid as the working substance.
• Tube is made of glass so that the mercury level can be seen from outside.
• Mercury: suitable since its vapour pressure is very low and it does not wet glass.
• The space above the mercury column is Torricellian vacuum.
 • The weight of the column of mercury inside the tube is balanced by the force due to
atmosphere pushing from the outside.
• The bore of the tube being uniform, the balancing weight is
measured in terms of the height of the mercury column.
• The standard atmospheric pressure is 760 mm.
• When the liquid column manometer is kept inside a chamber
which is by means of a vacuum pump, the force due to the
outside air decreases => it is needed to balance only a lower
height of the mercury column.
• The height of the mercury column decreases in proportion to
the outside pressure.

THE U-TUBE MANOMETER

• Consists of a glass U-tube which contains a certain amount of

mercury.
• One end of the U-tube is closed permanently. The other side is
open to the atmosphere.
• The space above the mercury in the
closed tube is vacuum.
• Here again the level difference between the mercury columns on the
two sides will be proportional to the pressure of air outside.
• This is true even when the U-tube is kept inside an evacuated
chamber.
• The lowest pressure that can be normally measured with the help of
the liquid column manometer is limited to about 1 Torr.
• If a lower density oil with a low vapour pressure is used, the lower
limit can be extended down to about 0.1 Tor.
2) McLeod Gauge

• Makes use of a mercury manometer in which a volume of gas is compressed before it is used for
measurement of the pressure inside the chamber.
• Principle: Boyle's law.
• The range of vacuum measurement is greatly
enhanced.
• The sensitivity can be increased by increasing
the compressible volume or by decreasing the
diameter of the compression capillary.
• The lower limit is set by the fact that too large
a compressible volume leads to difficulties
because the weight of the mercury becomes
unmanageably large and also the fact that too
small a bore for the capillary leads to sticking
of the mercury on the walls.

CONSTRUCTION:

• The device consists of a glass mechanism.

 • A spherical bulb B with a length of capillary tube C1 closed at the top end is connected to a
reservoir and to another tube having two sections T and C2 and exposed to the Vacuum to be
measured at the top end.
• The section C2 of this tube is also a capillary with a bore diameter the same as that of the tube
above the spherical bulb.
• Initially mercury is filled into the device such that the level is below the level A which is
below both the bottom neck of the spherical bulb and the entrance to the second tube
assembly.
• In this way a volume V of the gas from the vacuum system at the pressure P (to be measured)
is enclosed in the space in the bulb and the capillary.
• Now the level of mercury is raised by allowing more mercury into the system from the
reservoir.
• The gas in the capillary C1 is now compressed to a much smaller volume .
• If S is the area of cross section of the capillary,

Volume of the compressed gas inside the capillary = l.S

Where ‘I’ is the length of the portion of the capillary tube C1 above the mercury level.
𝑃+𝐿
= 𝑃𝑉
𝑙. 𝑆
𝑆𝑙𝐿
𝑃=
( 𝑉 − 𝑆𝑙 )
Hence by measuring L and I we can estimate the pressure of the gas inside the vacuum system.
In actual practice, the mercury level in the wider tube is brought at the same level as the top end of the
capillary tube.
𝑆𝐿2 𝑆
𝑃= ≈ ( ) 𝐿2
( 𝑉 − 𝑆𝐿 ) 𝑉
since V>> SL.
This leads of course to a quadratic scale.

Indirect Reading Gauges

1) Capsule Type Gauges - Bourdon gauge
• Its action depends on the deformation of the capsule with
changing pressure.
• It is a common type of gauge found on compressors and gas
cylinders.
• The capsule is in the form of a thin walled tube (Bourdon
tube) bent in a circle with the open end attached to the vacuum
system.
• The atmospheric pressure deforms the tube.
• An attached pointer mechanism gets deflected and gives a
linear indication of the pressure on the dial.
• The working is independent of the nature of the gas.
 2) Capacitance Manometer (Capacitance Diaphragm Gauge)
• Consists of a flexible diaphragm which forms one plate of a capacitor.
• A fixed parallel plate forms the other plate of the capacitor.
• A certain volume of gas at an appropriate low pressure is trapped
inside the space in which the probe is situated.
• The other side of the diaphragm is connected to the vacuum to be
measured.
• Changes in the pressure in the vacuum system deforms the
diaphragm thereby changing the capacitance measured by the
probe.
• The capacitance value is converted to a corresponding pressure
reading (after proper calibration of course) by means of an electronic circuit.
• The manometer is useful down to 10-6 Torr.
• One disadvantage of the manometer is that small temperature differences can affect the reading of
the gauge. The remedy is to provide some sort of temperature control also.

3) Pirani Gauge
• The operating range of this type of vacuum gauge is from 200 to 10-4 Torr
• The operation is based on the fact that the heat conductivity of a gas depends on the pressure.
• Device mainly consists of a heated filament (R4) supplied from a constant voltage source and
exposed to the gas at the pressure to be measured. surroundings.
• The temperature of the wire will depend on the balance
between the opposing processes of Joule heating and the heat
conduction by the gas.
• The former obviously depends on the current.
• The latter, in turn, depends on the frequency of molecular
collisions with the filament and the nature of the incident gas
molecules; i.e; proportional to the molecular concentration and
the thermal conduction properties of the residual gas.
• The temperature of the wire thus depends on the pressure P.
• The resistance of the wire is decided by its temperature.
• A measurement of the resistance of the wire thus leads to a
determination of the gas pressure.
• The filament wire is heated to a temperature above the surroundings.
• The filament wire is included in one arm of a Wheatstone's bridge network.
• The resistance is determined from the out-of-balance bridge current.
• The current is measured and it can be calibrated in terms of the pressure in Torr.
• There will be a gauge control unit which will provide the stabilized power supply for energizing
the filament wire, measuring the bridge out- of-balance current and for providing a visual reading
on a suitable calibrated scale.
• Major Application: continuous monitoring of pressures above about 10-4 Torr, particularly in
backing lines.
• A low pressure limit of 10-4 Torr is set by the radiation heat loss which becomes more than the
heat transfer by thermal conduction by the gas and a high pressure limit of 10 Torr is set by the
predominance of thermal conduction which becomes independent of pressure.
 4) Thermocouple Gauge
• In a thermocouple gauge the thermo emf generated in a couple of
dissimilar metals attached to a heated filament provides the basis for
pressure measurement.
• The thermocouple made of two dissimilar metals has one junction (H
- hot) attached to a filament (F) supplied with a constant voltage source
and the other junction (C - cold) kept at ambient temperature of the gas.
• The filament temperature and thereby the hot junction temperature is
controlled by the resistance R.
• As in the case of the Pirani gauge, the filament temperature is
dependent on the pressure.
• Thus, the hot junction temperature and consequently the thermo emf
generated in the couple are also dependent on the pressure, which can
therefore be measured by monitoring the thermo emf by means of a milli
voltmeter.
• A single thermocouple is less sensitive than the Pirani gauge.
• However, the sensitivity can be considerably improved by using multiple thermocouples- an
arrangement called the thermopile gauge.

5) Ionization Gauges

There are two types of ionization gauges –

(a) Penning Gauge (Cold Cathode Ionization Gauge)

• The pressure range is from 10-2 to 10-4 Torr
• The basis of the operation is measurement of the D.C. current
due to the positive ions produced by electron impact ionization
in the residual gas.
• This ion current depends on the molecular concentration and
the ionization probabilities of the residual gases.
• Two plane parallel electrodes forming the cathodes (C and
C') and a central ring anode (A) are used inside a vacuum tight
enclosure.
• A cold discharge initiated by applying several kilo Volts voltage across the cathode and the
anode.
• A suitable magnetic field is applied perpendicular to the plane of the electrodes by means of a
horse shoe magnet.
• The electrons make many oscillations in the magnetic field before reaching the anode.
• This produces large ionization of the residual gas.
• The positive ion current collected at the anode is almost linearly dependent on the pressure of
the residual gas.
• There is a possibility of the gauge acting as an ion pump under favorable.
• Therefore, the gauge electrode materials are made of stainless steel which does not sputter
easily and is comparatively inactive chemically.
• The high-pressure limit of 10-2 Torr is set by the initiation of a glow discharge when the
positive ion current becomes independent of the pressure.
 • The low-pressure limit is set by economic considerations.
• The ion current at the low-pressure limits are rather small and will require expensive
amplifier circuits for measurement.

(b) Hot Filament Ionization Gauge

• Here the pressure range is lower than that of the
Penning gauge
• In this type of ionization gauge also, the ion current
due to positive ion collection at an anode is used to
measure the pressure.
• Electrons which produce the ionization are produced
by means of a hot filament.
• These electrons possess energy of the order of 100 eV.
• When they pass through the residual gas, ionization is produced.
• The positive ions are extracted by a suitable anode.
• The structure of the gauge is often similar to that of triode valve.
• Usually a cylindrical geometry is utilized although a planar geometry also is not uncommon.
• The filament is a central wire and the anode is a cylindrical one outside
• In between we have a grid mesh. The grid potential is set at about +150 to +300 Volts.
• The collector potential is in the range of -20 to -50 Volts with respect to the filament.
• Low-pressure limit: 10-7 Torr, set by the production of X-rays in the collector anode.
• High pressure limit: 10-2 Torr , a glow discharge, independent of the pressure becomes the major
contributor to the measured current.
• In order to avoid the X-ray production and thereby push the lower limit further down, the
geometry of the gauge can be inverted, with the filament outside and the anode at the centre.
• The X-ray production is minimized in this new geometry because the total area available for the
X-ray production from the anode wire is very small. Such a configuration can be called Bayard
Alpert gauge.
• Applications:
- Vacuum Gauge
- Gas leak detector:
 Especially for helium application (response of the gauge is different for different gases)
 Usually used in conjunction with a Pirani gauge with helium as a probe gas.
 The Pirani indicates higher pressure when sampling helium and the Ionization gauge a
lower pressure. This will confirm the leak.

VACUUM ACESSORIES
• Vacuum set up → chamber or vessel to be evacuated, vacuum pump (to evacuate the
chamber) and a vacuum gauge (measure the vacuum achieved).
• We require many other accessories to go along with the above components.
1. Connecting devices – interconnect the chamber, the gauges and the pump.
2. Valves – isolate or connect certain sections.

Vacuum Valves
For isolating various parts of a vacuum system from one another and inter-connecting them when
required.

Diaphragm Valve (Saunders Type)

• Simplest and more frequently used one.
• Designed along lines similar to a water tap.
• A diaphragm (of a polymer material) is clamped at its edge
and the stem is attached to the center.
• Diaphragm, when pushed against the valve body, isolates the
input and outlet ports.
• Movement of the diaphragm - by turning the handle H at the top.
• The top mid portion of the diaphragm is tightly held to the bottom of the handle so that as the
handle is turned, the central portion of the diaphragm moves up and down.
• When closed, the diaphragm is held tightly against the valve body B.

Gate Valve
• Sealing mechanism of gate valve is a metal disc with "O" rings on
either side.
• It can be pushed down to seal off input and output sides or pulled up,
establishing communication between the two sides.
• The closing and opening can be done either mechanically, manually
or pneumatically.

Butterfly Valve
• Sealing is done by a rotating circular vane, with an "O" ring on
the vane or the valve body.
• There will be a mechanism to force the vane against the valve
body to enforce the sealing.

Baffle Valve

•Consists of a movable disk D with an "O" ring at the bottom.

•Rotating the handle H attached to the disk from outside
forces the disk against the bottom body to form a vacuum seal.
•The "O" ring could be in the valve body bottom also.

Adjustable Valves- The Needle Valve

• Vacuum chamber will have to contain small quantities of a
gas at a low pressure many times, to create an inert
atmosphere.
• Also, a continuous, controlled, flow of the gas may be
required.
 • In such cases, gas will have to be continuously admitted into the system from one side while
it is being pumped from the other side.
• A needle valve is the solution under such conditions.
• Consists of a precision-tapered needle structure (N) moving in and out inside a housing,
thereby adjusting the clearance between the needle and the valve body and allowing varying
quantities of gas to flow from one side to the other.
• The gas flow control is achieved by rotating the knob H.
• The position of the needle and thereby the flow rate (after proper calibration) can be read off
by means of a pointer and scale arrangement attached to H.

Isolation-cum-air-admittance Valve
• Used when the backing pump is oil-filled rotary pump.
• If a running rotary pump stops in between due to power
failure or some pump problem, we are left with a high vacuum
on one side and the atmospheric pressure on the other side.
• The atmospheric pressure may force the oil into the chamber
and contaminate it, a phenomenon known as oil suck back.
• To prevent such an eventuality an isolation-cum-air
admittance valve may be introduced between the pump and the
chamber.
• Consists of a cylinder made of steel which can be moved inside a T-type connector.
• There is a solenoidal winding on the outside, in the upper portion of the straight section of the
T-connector.
• The solenoid is powered from the same power supply as the rotary pump and will hold the
steel cylinder in position I when energized.
• In this position, the steel cylinder holds firmly against the "O" ring on the inner side of the top
flange of the T-connector, thus interconnecting the vacuum chamber and the pump and
isolating them from the atmosphere.
• In the event of a power failure and the pump stops, the solenoid is de-energized and
consequently the steel cylinder drops under gravity onto the "O" ring at the bottom.
• In this position 2, it seals off the vacuum chamber, at the same time establishing a connection
of the pump with atmosphere.
• Air rushes into the rotary pump and thus prevents oil suck back.

Air Inlet Valves

• It may become necessary to open a vacuum chamber for the purpose of changing something
inside.
→ chamber will be first isolated from the vacuum pump by means of a suitable gate
valve and then air is admitted into the chamber gradually with the help of an air inlet
valve.
 • It consists of a certain length of a brass or steel tube closed
at one end with an annular flange having an "O" ring on the
outer face.
• Near the end with the flange there will be threading on the
outer surface to enable a cap to be screwed on, closing the
side vacuum tight.
• The open end of the valve may be coupled to the vacuum
chamber either by direct welding or by some other type of vacuum coupling.
• The screw cap can be opened when required to let in air into the chamber.
• If the air has to be let in at a very small and controlled rate as is the case when the chamber
contains some fragile materials like a very thin target, the air inlet valve can be coupled via a
needle valve.

Flanges
• Used to interconnect vacuum pipes, connectors etc, among themselves as well as to vacuum
pumps, gauges, vacuum chambers etc.
• Usually made of steel or brass.
• 2 categories of flanges - Blank off flanges &
Flanges used to interconnect.

Blank off flanges

o Consist of circular discs of the required diameter
thickness.
o One side may have an "O" ring groove to
provide a sealing
o Used to close one end of a vacuum pipe or a view port etc.

Flange used to interconnect

o Usually an annular disc of the appropriate inner and outer diameters and thickness.
o One or both sides may have "0" ring grooves.
• In both types of flanges, there will be equally spaced through holes along the circumference
of a circle with a diameter larger than the "O" ring groove.
• These holes are meant for tightening of the flanges in order to achieve good vacuum sealing.

Gaskets and "O" Rings

• Used for obtaining good sealing when interconnecting various detachable vacuum
components.
• Located in appropriate "O" ring grooves on flanges - annular with a circular cross section.
• Gaskets have rectangular cross section.
• The "O" rings are seated inside "O" ring grooves.
• When seated inside the groove, about half the thickness will project above the groove.
 • It is a good practice to apply vacuum grease as a lubricant to "O" rings that are associated
with movement, particularly a shearing movement.
• Material used - metals or polymers.
• The polymers are also called elastomers, are rubber like
substances, incompressible, but readily deformed when pressure
is applied and regain their original shapes and dimensions when
the pressure is released
• No elastomer is perfect in the sense of regaining their exact
shape after compression is completely removed.

Given below are some common materials used for gaskets and "O" rings:
1) Rubber: Not really suited for good vacuum. Useful only for poor vacuum. Also there is a
danger of undergoing permanent deformation after continuous application of pressure. The
outgassing is abundant.
2) Nitrile: Co-polymers of butadiene and acrylonitride. Mechanically very strong, have high
resistance to compressive set and can be used up to 80 °C.
3) Silicone: High chemical stability, but are mechanically weak.
4) Viton: Co-polymers of perfluoro propylene and vinylidene fluoride. High chemical stability
and low outgassing Maximum temperature: 250 °C.
5) Neoprene: This is a chloroprene polymer.
6) Metals: Copper, aluminum, indium and sometime gold. Metal gaskets - sometimes used in
wire form, usually for UHV applications.

Bellows
• Flexible connectors with flanges fixed on either side.
• Usually made of steel or brass.
• The sides are corrugated and flexible.
• Main use - to interconnect two vacuum components
which may be relatively immovable.
• The bellows can take some degree of deformation /
shearing so as to be accommodated in the space
between the two components.
Wilson's Seal
• Used when it is needed to move some component
inside a vacuum chamber without affecting the
vacuum.
• The movement may be either translational or
rotational.
• In one type of Wilson's seal, two plates with 45° cuts
in them are pressed together.
• This causes the "O" ring between them to be
uniformly shrunk in diameter, pinching the shaft and
creating a vacuum tight seal around it.
• The flange of the vacuum chamber serves as one of the plates and the other plate may be an
aluminum or brass ring.
• They are pressed together by tightening down the three screws placed at 120° apart from one
another.
• The component which is to be moved inside the vacuum can be attached to the right end of
the shaft which is inside the vacuum.
• Both rotary and translational movement can be affected.
• Sometimes the "O" ring setup is repeated once more to ensure better vacuum sealing.

VACUUM TRAPS
• In many situations some unwanted gas molecules may disturb the vacuum.
• Vacuum traps help to condense and trap such unwanted gas molecules.
• It has been found that inclusion of traps generally improves the vacuum achieved.

Liquid Nitrogen Trap

• Standard accessory above mercury diffusion pumps.
• Used above oil diffusion pumps to achieve ultra-high vacuum.
• In backing lines, they are used to suppress pump oil vapours.
• Traps enable enhanced pumping speeds for condensable vapours.
• Pumped gas is allowed to pass through an enclosure which is kept cooled by liquid nitrogen.
• Condensable gases get condensed and are collected at the bottom.
• There are mainly 2 designs of these traps:

(a) Re-entrant Trap

• Used in backing lines to suppress back migration of rotary pump
oil to high vacuum side.
• Also used in backing lines to protect a rotary pump from
condensable vapours which cannot otherwise be tackled by the
rotary pump itself, even on full gas ballast.
• At pressures below about 1 Torr, such a trap is useful to protect
the pump from hydrocarbon and water contamination.
• Disadvantage: low conductance which will reduce the pumping speed.
(b) High Conductance- High Vacuum Trap
• Thermally insulated by the high Vacuum.
• A molecule can travel from pump connection to system connection
after making collisions with the cooled walls only.
• They condense and are trapped.

Refrigerated Chevron Baffle Assembly

• Employed as a primary or secondary baffle
to reduce back streaming above diffusion
pumps.
• Principal function: Condense vapours
coming from the system or from the
diffusion pump.
• When used in conjunction with properly
designed intermediate baffling - condenses
vapours from the system above (acting as a
pump to achieve an ultra- high vacuum).
• Baffle must allow non-condensable gases to
move through it with as little impedance as
possible → baffling must be optically dense
and so constructed, that any molecule entering from the system in any direction will strike a
chilled surface and get condensed.
• Chevron assembly is cooled by conduction from an annular liquid nitrogen reservoir.

Sorption Traps
• Used for backing lines and are very useful
for suppressing migration of oil and water vapour
from a rotary pump.
• Hydrocarbon mineral oils used in rotary
pumps have molecular weights near about 500.
• The volatile molecular weights less than 150
readily migrate from the pump to the vacuum
system.
• The sieve will separate these components.
• A reduction by a factor as large as 50 can be achieved.
• The ultimate pressure achievable decreases from 10-3 Torr to less than 5 X 10-5 Torr.
• The sieve is regenerated by baking at rotary pump vacuum or atmospheric pressure at 300 °C
for about three to four hours.
• Then it is sealed off to prevent re-saturation with oil vapours.
• Some of the more commonly used sorbent materials are Linde molecular sieve 13X and
activated alumina.
• Most critical application -rough pumping cycle of clean sputter-ion pumped systems.
 • High vacuum sorption traps are also used above an oil diffusion pump.
• It will suppress back migration of oil.

Conflact Couplings (KF and QF Couplings)

• We need to couple various vacuum components.
• Demountable flanges would be preferable since these will allow anyone to quickly and easily
design and assemble a complete vacuum system.
• With the help of these, components can be quickly assembled for a particular experimental set
up, then dis- assembled and re-used in another set up.
• Also, when flanges and components are built to international/industry specifications, parts
from different sources / manufacturers can be inter mixed.
• One common flange system is the ISO-KF or simply KF couplings.
• KF stands for the German word Klieneflansche meaning small flange.
• They are also called QF (Quiek Flanges) couplings.
• They come in standard sizes from 3/8" to 2".
• One set consists of a center "O" ring in either side and a clamp which secures the flanges in
place.
• Some clamps are closed with a wignut and others with a toggle lever.
• The clamp holds the system together and provides the sealing force.
• The protruding portions of the flanges are connected to appropriate hoses.
• This can be connected to the vacuum system by means of connecting hoses on either side ring
around which is kept proper groove, two matching flanges on either side.

GENERAL LAYOUT OF A COMPLETE VACUUM SYSTEM

The procedure for achieving good vacuum in the system (chamber) to be pumped is as follows:
1. First the chamber is connected to the roughing pump by opening the roughing valve.
2. The main valve and the baffle valve will be closed. The rotary pump is started.
3. The roughing will be continued until the pressure falls to the range of 10-2 to 10-3 Torr.
 4. Now the roughing valve is closed.
5. The main valve is opened and the inside chamber of the diffusion pump is now evacuated to
roughly the same vacuum level as the chamber.
6. The heater of the diffusion pump is now switched on. Simultaneously water is allowed to
flow with sufficient flow rate through the cooling coils.
7. After giving sufficient time for the oil in the boiler to start boiling profusely, the main valve is
temporarily closed, the roughing valve is again opened and the chamber vacuum re-
established to the earlier level.
8. At this juncture, the roughing valve is again closed, the main valve is opened and the baffle
valve also is opened. At this moment the diffusion pump takes over.
9. The ion gauge should start showing the diffusion range vacuum. Sometimes separate rotary
pumps may be used for roughing and backing.

While shutting down the system, the reverse procedure may be adopted.
1. Baffle valve is closed.
2. The heater is switched off.
3. The cooling water circulation is continued and the inside of the diffusion pump is kept
evacuated by the backing pump for sufficient time till the system has cooled to room
temperature.
4. Main valve is closed
5. Rotary pump is switched off and air is allowed to enter the rotary pump via the isolation-cum-
air-admittance valve.