Agilent Technologies - High and Ultra-High Vacuum For Science Research PDF
Agilent Technologies - High and Ultra-High Vacuum For Science Research PDF
Agilent Technologies - High and Ultra-High Vacuum For Science Research PDF
HIGH/ULTRA-HIGH VACUUM
Seminar Outline
Vacuum introduction
Cryopump
Applications of physics
Materials selection
System pumping speed
Vacuum pumps
UHV applications
selection criteria
Gauges
System operation
Case studies
Pumpdown calculations
Vacuum Introduction
Overview
Pressure
Levels of vacuum
Gas characteristics in vacuum
Flow regimes: viscous/molecular
Agilent Technologies 1
Notes
Gas Composition
Pressure (torr)
10-3
10-6
10-9
10-10
10-11
Rough
High
Ultra High
Atm
Wet Air
Notes
Surface area, material type, pump speed and temperature determne ultimate pressure and pumpdown times
Agilent Technologies 3
Notes
Flow Regimes
Viscous flow:
Distance between particles is small; collisions between
gas particles dominate; flow through momentum transfer;
generally P greater than 0.1 torr (100 millitorr)
Transition Flow:
Region between viscous and molecular flow
Molecular flow:
Distance between particles is large; collisions between
the gas particles and wall dominate; flow through random
motion; generally P smaller than 10-3 torr
Notes
Moving Particles
We use a vacuum when we want to move
a particle through space in a specific way.
In a television set cathode ray tube, electrons
generated at the back of the tube in the electron gun have to move to a particular spot on
the phosphor screen that coats the front of
the tube. If there was air in the tube, the electrons would be deflected and blocked from
reaching the screen.
A very common application is to deposit a material on a substrate. In a vacuum system, a
material is heated and evaporated. The atoms
have to move from a source to a
substrate over a certain distance. If there was
gas in the chamber, the gas particles (atoms
and/or molecules) would prevent
the evaporated material from reaching the
substrate. Also, if the gas in the chamber contains oxygen, it could oxidize the material we
are depositing.
Agilent Technologies 5
Notes
Mean Free Path
As we lower the pressure in the vacuum
chamber, the amount of space between the
gas molecules increases. The particles bump
into each other less frequently. The average
distance a molecule moves before it bumps
another particle is called the mean free path.
At atmosphere, the mean free path is extremely short, about 2.5 millionths (2.5 x 10-6)
of an inch. Under vacuum, fewer molecules
remain, and the mean free path is longer. Its
length depends on the number of molecules
present, and therefore on the pressure. When P
is expressed in torr, the mean free path for air
can be estimated from the relationship:
Mean Free Path = 5______
x 10-3 (cm)
P
From this we can see that as the pressure gets
lower the mean free path gets longer. Likewise,
as the pressure gets lower, there are fewer
molecules of gas present, so there is less
chance of them striking each other.
In 1 cc of gas at standard conditions (760 torr
at 0OC), there are about 3 x 1019 gas molecules and the mean free path is about
2.5 x 10-6 cm (a few millionths of an inch).
At 1 x 10-9 torr, there are about 4 x 107 (ten
million!) molecules per cc, and the mean free
path is about 31 miles or 50 kilometers. The
number of molecules per unit volume (in this
example cubic centimeters) is called the gas
density or molecular density.
Notes
Adsorbed Gas
The diagram above illustrates the fact that
once the pressure in a high vacuum system
has reached high vacuum levels, most gas resides on the walls of the system. At a pressure
of 1 x 10-6 torr there are 500 molecules residing on the walls of the system for every molecule moving through the system.
This highlights the fact that at high vacuum
and ultra-high vacuum levels, the pressure
in the system is determined by the surface gas
in the system. The right column in the diagram
shows that it only takes 2.2 seconds to coat
a perfectly clean system (a system without
a single molecule in it!) with a monolayer of
gas when it exposed to that gas at a pressure
of 1 x 10-6 torr. At 1 x 10-9 torr it will take
2,200 seconds to coat the system with one
monolayer. This explains why surface analysis
equipment usually operates at ultra-high
vacuum pressures.
Agilent Technologies 7
Notes
Vacuum system gas load results from:
Surface Condition (outgassing/
desorption)
System Materials (diffusion and
permeation)
Leaks (real and internal/virtual leaks)
Pumps (backstreaming)
Practical Application
of Physics
Overview
Processes that use vacuum
Basic HV/UHV system
System pressure
Gas load
Material permiation
Notes
High Vacuum
Chamber
Throughput
Throughput is the actual amount of gas
or the number of atoms and/or molecules
moving through or being removed from
a vacuum system. This is the work really
being done by a vacuum system. Throughput is expressed by the letter Q.
The flow of gas through a pipe is described as the amount of gas (Q) flowing
through a pipe is equal to conductance (C)
of the pipe times the pressure (P1 P2)
over the pipe.
Or: Q = C x (P1 P2)
For the case where a pump is removing
gas from a chamber at pressure P, we can
look at how throughput is related to pumping speed (S) by taking another look at the
definition of speed
Pumping Speed: amount of gas flowing
into a chamber
pressure in the chamber
or: S = Q
_ (liters/second)
P
reworking this formula:
Q = P x S (torrliters/second)
Flow Regimes
Notes
Agilent Technologies 11
Definitions
The gas load is the rate gas enters the system volume
Gas entering the volume through external and
internal leaks
Gas entering the volume through external and
internal leaks
Gas emanating from or passing through materials
by diffusion and permeation
At a known temperature, the gas load is the amount of gas
particles entering the system volume per unit time
Q (gas load, throughput, leak rate) is expressed in units
of pressure volume/time
torrliters/sec, atmcc/sec, sccm, mbarliters/sec,
Pam3/hr
Notes
Notes
Agilent Technologies 13
Notes
QOUTGAS can be hastened and QDIFFUSION can be reduced by bakeout, minimuzing time open to atmosphere,
and by purging with a dry gas while system is open.
Outgassing
QOUTGAS = qOUTGAS x A
Outgassing
Notes
Agilent Technologies 15
Material Permeation
Examples
steels have higher permeation rates with higher
carbon content
copper has low permeation for all gases
aluminum has low permeation for hydrogen
Notes
Materials
Overview
Basic HV/UHV system
Origins of gas
Materials selection
Surface preparation and cleaning
Outgassing rates
Mechanical joining
Valves and seals
Notes
High Vacuum
Chamber
Notes
Vacuum system gas load results from:
Surface Condition (outgassing/desorption)
System Materials (diffusion and permeation)
Leaks (real and internal/virtual leaks)
Pumps (backstreaming)
Materials Selection
Agilent Technologies 19
Notes
Notes
Agilent Technologies 21
Ceramics
Alumina (Al2O3)
Steatite (MgO-SIO2)
Easily machined
Notes
Notes
Techniques
Physical wiping/polishng
Detergent washing
Chemical cleaning (i.e., acids, solvents/degreasers)
Sand/bead blasting
Ultrasonic bath
Electropolishing
Nickel plating
Agilent Technologies 23
Notes
Notes
KF Flange
Another popular type of elastomer flange is
the KF flange, also known as an NW flange.
The flange is of standard ISO 2861/1 design
consisting of two symmetrical flanges, a center ring to support and position an o-ring, and
a clamp that allows assembly without any
tools. KF flanges are quite convenient to use
in rough and high vacuum systems.
O-Ring Seals
Below are useful suggestions for working
with o-rings:
1. When preparing to make a flange
connection, be sure to clean and dry
the groove and the flat mating surfaces.
Check the sealing surfaces for scratches
that cross the seal area.
2. Lightly lubricate the o-ring with a vacuum
grease such as Apiezon-L, then wipe off
most of the grease with lint-free paper before making the connection. Keep in mind
that the o-ring makes the seal not the
grease. The grease makes the o-ring slip
and helps it to conform to its groove.
Agilent Technologies 25
Notes
Notes
Tungsten and metal inert gas welding (TIG & MIG) are
the most widely used techniques for vacuum systems
Agilent Technologies 27
Notes
Notes
Valves
A variety of valves are manufactured for various vacuum requirements. Each of these
takes into consideration factors such as operating vacuum levels, degree of cleanliness
needed, need for bakeout, and materials construction. Above, a small right angle block
valve made of aluminum and using o-ring seals is used as an illustration.
Valves can be separated into several types based first on whether they are elastomersealed or all-metal; then whether they are small or large valves. Valves also come in
hand-operated, pneumatically-operated, and solenoidoperated varieties. Small valves
will be defined as valves with inside diameters less than 2 inches. Large valves will be
defined as valves with more than 2 inches inside diameter. Valves can also be classified
as rightangle, tee, straight-through, back-to-air, variable-leak, gate and slide valves.
Large Elastomer
Sealed Valves
Agilent Technologies 29
Valve Design
Valve Design
The valve seal plate opens and closes as
with a gate. That is, the seal plate drops and
retracts from the port. In some designs, the
plate does not fully clear the port and, therefore, does not give maximum conductance.
Also, debris can fall on the seal and
cause leaks.
Valve Operation 2
Valve Operation
After forward motion stops, further driving
motion moves the seal plate up into the
sealed position.
The over-center mechanism and second
mechanical stop insure that the seal plate is
positively locked in the sealed position.
Valves are often air-operated and close with
considerable speed and force. It is important
to remember to disconnect both air and electricity when maintenance has to be done.
O-Ring Seals
In a valve having an o-ring-sealed shaft,
the seal is usually quickly rolled and
scuffed. This seriously reduces its life. The
o-ring must be lubricated in order to minimize wear.
Valves with this type of design should be
one of the first items to check when
troubleshooting a vacuum system.
Differential Pumping
Maintenance
The valve should be in the open position for maintenance and
cleaning. Air and electrical lines should then be removed. Next, remove
the whole actuator sealing-plate assembly by taking off the body
flange and its o-ring.
The body flange o-ring is held in its position over a large, rectangular
o-ring retainer. Re-assembly of this flange can be time-consuming if
the o-ring continues to slip off its retainer during the bolt-on process.
Bolting on is made much easier by using a seal positioning tool.
Once out of the valve body the mechanism can be cleaned, adjusted,
or repaired. Full removal of the valve and valve body from the vacuum
system is usually required to perform proper cleaning and refurbishing. See instruction manual for proper maintenance procedures.
The cleaning procedure is similar to the small elastomer-sealed
valves. Do not attempt to spray cleaning solutions or solvents into
the valve body or port area while the valve is on the vacuum system. Serious pump or system contamination could result.
Agilent Technologies 31
Notes
Small Metal-Sealed Valves
Small valves are 3 4 in. to 21 2 in. in diameter.
The construction of the valves is entirely
metal. There are no elastomers used. The
seal is accomplished using a copper gasket.
Therefore, metal-sealed valves provide reliable seals under repeated bakeout conditions.
A cross-section of an all-metal valve, made
entirely of stainless steel and copper is
shown above.
The sealing surface inside the valve has a
knife edge which cuts into the copper button
to seal the valve closed. The same capturing
principle is used as described previously.
This type of valve can be baked to 450C,
if necessary.
Notes
Sealing Torque
Knife edge grooves can produce vacuum
leaks where the grooves crisscross if the sealplate position is not exactly maintained. If the
grooves do crisscross, a leak can be avoided
by using greater sealing pressure each time a
closure is made. This limits the life of the gasket, however. The torque used to seal the
valve must be increased with each closing as
closing repeatability has some slight tolerance.
The initial sealing torque ranges from about
1 to 13 ft-lbs to a maximum of 6 to 46 ft-lbs,
again depending on valve size.
Maintenance
Some maintenance suggestions for all-metal
valves are outlined below:
1. Metal sealed valves require more sealing
force than elastomer valves. When the valve
is opened or closed, support the valve so the
attached plumbing is not bent or kinked.
2. After baking at high temperatures, the
threads on the valve need to be lubricated
to prevent galling. Use a suitable high- temperature lubricant such as Fel-Pro C-100.
3. A new seal needs to be installed after a
maximum of 300 closures. While the procedure is quite simple, it might be necessary
to remove the valve from the vacuum system
to carry out the seal change. The valves require a torque wrench to increase the torque
by about 1 2 ft-lb per closure.
4. Keep a closure log!
Conical Plate
Another solution to the sealing force requirement is to use a thin lightweight conical
plate. The basic design resembles the elastomer-sealed gate design described earlier.
The seal plate in this valve is also conical,
thin and lightweight. These characteristics
are used to good advantage.
Agilent Technologies 33
Notes
Seal Flexing
When moving into the sealing position, the
seal plate drives against a stop built into
the valve body. When this occurs, further
upward force spreads the plate outward.
This flexing of the seal plate actually multiplies the driving force. It also reduces the
load on the drive mechanism. A goldplated
ridge machined into the seal-plate edge
makes a tight leak-free seal when the plate
flattens out against the seat.
The other two ridges protect the center or
sealing ridge against mechanical damage.
This valve is bakeable in the open or closed
position. Perhaps the greatest advantage
of this metal-seal design is that it isnt at all
sensitive to position repeatability. That is,
there is no possibility of indenting eccentric
circles into the seat and causing leaks as in
the case of other metal seals.
Maintenance
Maintenance should be carried out according to the manufacturers instructions. The
exact dimensional tolerances needed in reassembly require specialized tools and
proper training whenever possible.
Cleaning of the valve body and actuator
assembly is usually the same as discussed
earlier in this chapter. Again, UHV usage
demands that good vacuum practice be
strictly followed. Lint, grease and cleaning
residue can cause excessively long pumpdown time. This is related to the outgassing load produced by contaminants in
the system.
Overview
Definition
Ohms Law correlation
Delivered (net) speed
Throughput vs pressure
Effect of conductance
Notes
Throughput
Throughput is the actual amount of gas, or
the number of atoms and/or molecules,
moving through or being removed from a
vacuum system. This is the work really being
done by a vacuum system. Throughput is expressed by the letter Q.
The flow of gas through a pipe is described
as the amount of gas (Q) flowing through a
pipe is equal to conductance (C) of the pipe
times the pressure (P1 P2) over the pipe.
Or: Q = C x (P1 P2)
In the case where a pump is removing gas
from a chamber at pressure P, we can look
at how throughput is related to pumping
speed (S) by taking another look at the
definition of speed
Pumping Speed: amount of gas flowing
into a chamber
Pressure in the chamber
or: S = Q_ (liters/second)
P
reworking this formula: Q = P x S
(torrliters/sec.)
Notes
Agilent Technologies 37
Notes
Notes
Agilent Technologies 39
Notes
Notes
Agilent Technologies 41
Notes
Addendum B
Conductance Formulas
Notes
Notes
Agilent Technologies 45
Notes
Notes
Agilent Technologies 47
Notes
Vacuum Pumps
Overview
Operating ranges
Rough pumps
Scroll pumps
Diaphragn pumps
Blower/booster pumps
Screw pumps
Pump performance
Pump precautions
Pump comparison
Notes
Notes
High Vacuum
Chamber
Agilent Technologies 51
Notes
Scroll Pumps
Notes
Agilent Technologies 53
Notes
Principle of Operation
Gas is transferred through the pump in three
phases similar to gas transfer occurring in
other types of mechanical pumps shown before. The circular motion of the orbiting scroll
forms crescent shaped spaces into which
the gas enters (1 left) and becomes
isolated (2,3 and 4). The orbiting motion
moves the gas towards the center. The volume of the gas becomes smaller and the
pressure increases. Finally the crescent is
connected to the exhaust port (5 left) and
moved to the second set of scrolls. The gas
is then compressed in an identical way and
exhausted from the the pump
Diaphragm
Notes
Agilent Technologies 55
Notes
Notes
Agilent Technologies 57
Notes
Overview
Basic system
Operating ranges
Vapor jet pumps
Molecular pumps
Historical perspective
Commercial solutions
Turbo pump comparisons
Compression ratio
Cryo pump
High vacuum pump comparison
Notes
High Vacuum
Chamber
Notes
Agilent Technologies 61
Notes
Notes
While turbomolecular pumps achieve high
pumping speeds, drag pumps have high
compression ratios (especially for light
gases) and can therefore discharge against
pressures of up to several torr. A compound
pump design provides both capabilities from
a single pump. The Agilent compound pump
(Macrotorr) configuration is shown. It consists of 8 to 10 turbomolecular stages
(Rotor/Stator) followed by several drag
stages (MacroTorr Rotor/Stator) combined
in a single rotor-stator assembly.
The turbo rotor-stator blade combinations at
the low-pressure side (inlet) of the compound
pump have compressed the gas. So the volume of gas being moved at the high-pressure
side (foreline) of the pump has become much
smaller, and high pumping speed is no longer
needed. Due to the increased compression
ratio provided by the drag stages of a compound pump, the discharge pressure against
which it can operate is higher than that of a
traditional turbomolecular pump. Compound
pump can overlap the pressure range of dry
roughing pumps, such as a scroll or a diaphragm pump, allowing for a totally dry
vacuum system to be built.
Agilent Technologies 63
Notes
Notes
Some manufacturers have developed
magnetic bearings for rotor suspension.
Magnetic bearings use electromagnets to
lift the rotor and hold it in place during operation. Sensors detect any off-center movement of the rotor and, through feedback
circuitry, the magnetic fields are adjusted
to recenter the rotor. A so-called crash
bearing is used to handle inadvertent contact between rotor and stator during power
failures or when the pump is accidentally
vented to atmosphere ("dumped").
Agilent Technologies 65
Notes
The atoms and molecules in a gas are in
constant high-speed, straight-line motion
in random directions. This is called thermal
motion (or the Kinetic Energy of Motion) and
is associated with the temperature of the
molecules. The higher the temperature, the
higher the speed. Thermal motion will tend
to move molecules away from each other
until they collide with something, usual the
walls of the container and with one another.
For a given amount of thermal energy (temperature), the speed of an atom will depend
upon its Mass (or weight) - lighter elements
will travel faster than heavier elements.
The atomic motion can be seen (we cannot really see atoms move) by watching the
collective effect of atoms colliding with a
dust particle, that is, we may watch the dust
particle move and extrapolate what the surrounding atoms must have been doing. The
balance between the electrical dispersion
forces holding molecules together and the
thermal motion which tends to move molecules apart, is very important in a vacuum
system. If the dispersion forces are strong,
as they are with some molecules, the molecule will stick to a wall when it collides with
it. With weak dispersion forces, the molecule
will stay on the wall for a very short period.
A water molecule is surrounded by strong
dispersion forces. When it collides against
a wall, it will stick and its movement through
the system will be delayed.
Gases such as helium, nitrogen and oxygen
have relatively weak dispersion forces.
When they move through a vacuum system
and periodically collide against a wall, they
will not stick and there will essentially be no
delay in their movement through the system.
This results in helium, nitrogen and oxygen
being pumped away much faster than water.
The balance between thermal motion and
dispersion forces can be changed by changing the temperature of the vacuum system,
For instance, in order to speed up removal
of water, vacuum systems are often heated
or baked. This increases the energy of thermal motion, resulting in shorter dwell time
of the water molecule on a wall.
Notes
Agilent Technologies 67
Notes
Notes
High Vacuum
Chamber
Throughput
Throughput is the actual amount of gas or
the number of atoms and/or molecules
moving through or being removed from a
vacuum system. This is the work really being
done by a vacuum system. Throughput is expressed by the letter Q.
The flow of gas through a pipe is described
as the amount of gas (Q) flowing through a
pipe is equal to conductance (C) of the pipe
times the pressure (P1 P2) over the pipe.
Or: Q = C x (P1 P2)
In the case where a pump is removing gas from
a chamber at pressure P, we can look at how
throughput is related to pumping speed (S) by
taking another look at the definition of speed
Pumping Speed: amount of gas flowing
into a chamber
Pressure in the chamber
or:
S = _Q (liters/second)
P
Notes
Agilent Technologies 71
Overview
Best Practice
Bakeout procedure
High potting
3. Noble gases
Notes
Notes
Agilent Technologies 73
Notes
Notes
Agilent Technologies 75
Notes
Notes
Agilent Technologies 77
Notes
Notes
Agilent Technologies 79
Notes
Selection Criteria
for UHV Applications
Overview
RGA scan
Selection criteria
Performance vs pressure
Ion pump selection guide
Ion pump characteristics
Leakage
Baking
Potting
Comparison of high vacuum pumps
Notes
Notes
Agilent Technologies 83
Notes
Notes
Agilent Technologies 85
Notes
Notes
Agilent Technologies 87
Notes
Notes
Agilent Technologies 89
Notes
Notes
Agilent Technologies 91
Best to start bake with ion pump off; use turbo pump
to remove gas
When pressure curve is flat, outgas filaments & turn off heat
Allow system to reach base pressure
Notes
When High-Pot?
Notes
When the pump has worked at high pressure for long period (e.g., during a bakeout)
When the leakage current is of the same order of magnitude (or higher) of the current the customer runs the
pump at
Agilent Technologies 93
Notes
Notes
Agilent Technologies 95
Notes
Gauges
Basic system design
Pressure ranges
Heat transfer gauges
Pirani transducer
Capacitance manometer
Hot filament ion gauge
Gauge maintenance
Gauge sensitivity
UHV ion gauge
Cold catheter gauge
Notes
High Vacuum
Chamber
Notes
Vacuum Pumps
Agilent Technologies 99
Notes
Thermocouple Gauge
5 torr to 1 x 10 10-3 torr
Convection Gauge
atmosphere to 1 x 10 10-3 torr
Notes
Notes
Notes
Operating range:
Notes
Overview
System operation
Valve maintenance
System troubleshooting
Virtual leaks
Cleanliness
Vacuum pumpdown
Notes
High Vacuum
Chamber
Notes
Valve maintenance
1. Look at the seals whenever maintenance on
a valve is done. Inspect the seals to see if they
have been warped, or are nicked or scratched.
2. The pistons on pneumatically-actuated
valves need to be lubricated yearly. Most
pneumatically-actuated valves are of the airopen, spring-closed variety. Be careful when
disassembling the valve so that it does not
come apart during disassembly.
3. Lubricate the piston on pneumatic valves
with a lubricant recommended for use with
compressed-air lines. Please remember that
this is not exposed to the vacuum system. This
lubricant, which works well for compressedair pistons, will cause problems (high outgassing) if used inside the vacuum system.
4. Inspect the bellows for dents or cracks.
The brass variety is easy to dent. The dent
will cause the bellows to work-harden and
crack at that location. It should be replaced
while it is disassembled on the bench.
5. Only lubricate the o-rings when necessary
with a vacuum grease such as Apiezon-L or
other lubricant. Grease is a contaminant! Remember that only a very thin film is needed.
6. The valve should be leak-checked on a
helium mass spectrometer leak detector. Do
not forget to check the bellows as well as
the valve seal and bonnet seal. Leak checking before reinstallation on the system can
save a lot of disassembly/re-assembly time
should a leak be present.
Notes
Notes
Notes
Notes
Notes
Notes
Notes
Overview
Basic UHV system design
UHV system cleanliness
UHV system operation
Notes
High Vacuum
Chamber
Notes
Notes
Case Studies
Case Study 1:
High/UHV Vacuum Pumpdown
Overview
Basic system design
System parameters
Calculations worksheet
High vacuum pumpdown
Outgassing rates stainless steel
Pumpdown pressure
Pumpdown calculations
Notes
High Vacuum
Chamber
Notes
Notes
Notes
Notes
Addedum A
Pumpdown Calculations
Notes
Notes
Notes
Notes
Notes
Case Study 2:
Backing Pump
Overview
Selection of forepump
System pressure rough vacuum
Confirmation of ion pump selection/size
Notes
Notes
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