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Gettering and Ion Pumping
Per gentile concessione di Varian S.p.a.
Tratto da : "High Vacuum Technology: A Practical Guide"
di Mars Hablanian
Ultrahigh-vacuum techniques and system components have evolved
together with special pumping methods uniquely adapted to the requirements of
extreme cleanliness, bakeability, and pumping speed. The principal pumping mechanisms
employed are chemical transformation, whereby gases are chemically combined
into solid compounds having very low vapor pressure, and a method involving
an ionization step that permits acceleration of the atoms or molecules in an
electric field to drive the ions directly into a solid surface, where they remained
captured.
1. GETTERING PUMPS
At high-vacuum conditions a surface can hold
large quantities of gases compared to the amount of gas present in the space.
This produces a pumping action either by physisorption or gettering, which refers
to a chemical combination between the surface and the pumped gas. Many chemically
active materials can be used for gettering. In vacuum systems the material commonly
used as titanium because it is chemically reactive with most gases when it is
deposited on a surface as a pure metallic film, but it is rather inert in bulk
form because of the tenacious oxide film covering its surface.
To produce a pumping action, all that is needed is a
source of titanium and a means of producing a fresh (unoxidized) layer preferably
on a large surface. Various forms of heating can be used to deposit a titanium
film by evaporation or sublimation. The fresh titanium, deposited on surfaces
surrounding the source, forms stable, solid compounds with chemically active
gas atoms or molecules that strike the surface. This capture process can be
continuous if new layers al titanium are constantly produced.
Figure 1 shows a typical arrangement.
The pumping speed versus pressure curve for any titanium pump is shown in
Figure 2. Pumping speed is maximum when a complete film of titanium is maintained
on the pumping surface. Pumping speed, then, is maximum at low pressure. The
number al gas molecules striking the titanium surface decreases with decreasing
pressure. Therefore, below some pressure point a particular titanium source
is able to supply titanium fast enough to sustain a complete film of fresh titanium.
In this pressure range, the pumping speed is limited only by the intrinsic speed
Sj of the titanium surface area and the gas conductance from the chamber into
the pump.
It should be noted that at law pressure.
periodic sublimation is employed to allow greater saturation of the titanium
film before more titanium is deposited. The life of a titanium source is finite,
but with judicious use (to be discussed later) it can be made to serve for a
relatively long period. When pressure increases, and hence the density of gas
molecules per unit volume is greater, pumping speed decreases and is dependent
on the rate of continuous titanium sublimation.
At higher pressures, the impinging gas
molecules combine with the titanium virtually as fast as it is deposited and
a complete film of fresh titanium is never formed. Consequently, the probability
of capture for gas molecules decreases. Throughput is constant in this pressure
region because the pumping action is limited by the rate of titanium deposition.
As in the case of cryopumps, the pumping
speeds of gettering pumps cannot be defined precisely because it depends somewhat
on the mixture of gases, the presence of gases that are not chemically pumped,
the temperature, and the previous history of a surface.
The following method can be used for
computing an approximate pumping speed. Surface area, speed for specific gases,
and the conductance of the titanium sublimation pump inlet aperture are the
variables considered (see Table 1).
The area-limited speed for specific gas is:
 |
l/s
|
where A is the area of gettering surface
in square centimeters and Sj is the intrinsic speed per square centimeter
of titanium surface for a specific gas, in liters/second.
To use titanium economically, it is essential
to determine the time required to deposit a complete but nonwasteful film and
then cycle power to the filament accordingly.
Figure 3 shows typical pressure rise characteristics
for a system in which the titanium sublimation pump yields a pressure reduction
of a factor of 10 before saturation of titanium causes the pressure to rise.
At successively lower pressures, saturation occurs often a longer period of
time because the number of reacting gas molecules is decreased proportionally.
Since the mechanism of titanium pumping is
chemical combination, the theoretical maximum throughput can be found by using
the appropriate chemical formula and the rate of titanium sublimation in atoms
per second. To use as an example pumping nitrogen (compound: TiN), the typical
sublimation rate from a titanium source is 3x1017 atoms/s since one
titanium atom can combine with one nitrogen atom, the theoretical maximum nitrogen
throughput is
A = 3x1017 atoms/s
However, nitrogen forms molecules with two
atoms. Therefore, the throughput in molecules per second is 1.5x1017
mol/s, which is converted to the normal units for throughput by using
Avogadro’s number:
There are 6.023 x 1023 molecules
in a mole of gas that at atmospheric pressure (760 torr) has a volume of 22.4
l. Titanium evaporation can be of great assistance in vacuum systems
by providing high pumping speeds at relatively high pressures. Typical pumping
speeds for pumps al different diameters are shown in Figure 4.
In Figure 1 the source al titanium is shown
in the form of a wire. In practice, there are several ways to produce a mechanically
stable evaporating surface. For example, molybdenum-titanium alloy wire will
retain its shape at an elevated temperature while preferentially evaporating
titanium because it has a higher vapor pressure compared to molybdenum. One
or more filaments can be used. If one al the filaments has been depleted, the
other can be used by external switching. To provide a larger storage of titanium,
a hollow titanium spheroid piece can be heated by an internal heater (Figure
5).
The titanium piece is removable and should
be replaced before it gets too thin to retain its shape.
A titanium sublimation control unit provides
a regulated power source for operating either a filament sublimation cartridge
or a radiation-heated titanium sphere. Essentially, it is a current-regulated
power supply (low-voltage ac power) which is applied directly to the filaments
of the sublimation cartridge or to the heaters inside the Ti-Ball sphere. Power
is adjustable according to the desired evaporation rate.
In the manual mode it can provide 0 to 50
A either continuously or periodically (a maximum of 10 V). In the automatic
mode the current is supplied for a period of a few minutes and then switched
all or reduced to a standby value for a period that depends on the pressure
in the vacuum system.
This period is adjusted according to the
signal received from the pressure gauge. Often, a life indicator is used to
show the amount of titanium expended as measured through an ampere-hour integrator.
When a new filament is put in operation,
it must be degassed to reduce the initial burst of gas, which is released when
the sublimator is heated. For pressures above 5x10-6 torr, it is
recommended to maintain sublimation continuously.
Manufacturers usually recommend a certain
waiting period between evaporations, in the manual mode, according to a system
pressure. However, the optimum “off” period may vary for different systems because
it depends on the geometric relationships and the size of the surface receiving
the evaporating gettering material. Typically, a monolayer of titanium is evaporated
during 2 min of sublimation time. Typical sublimation rates for a filament and
a Varian Mini-Ti-Bali are shown in Figure 6 and 7. Chemical gettering is not
possible with inert gases and it is almost useless with a gas such as methane
(Table 1).
A technique has been developed to pump inert
gases which includes an ionization process. Usually, the ionization is produced
as a result of a collision with electrons. The electrons may be produced either
by cold cathode field emission or thermoionic emission from hot filaments. The
electrons and then the ions are accelerated through an electric field of a few
thousand volts. The velocities obtained are sufficient to drive the ions into
a solid metal surface. They are “buried” a few atomic layers deep and they remain
captured in the surface more or less at room temperature, and it the diffusion
rates are low, they will not reappear in the gas phase for a long time.
2. SPUTTER-ION PUMPS
Pumps utilizing chemical and ionization pumping
effects can generally be called ion-getter pumps. Early designs (after 1955)
had a variety of arrangements for electron sources and for titanium evaporation.
Later designs, which are used almost exclusively now, are called sputter-ion
pumps because the supply of a fresh titanium film is produced by a process called
sputtering. The basic structure consists al two electrodes, anode and cathode,
and a magnet (Figure 8).
The anode is usually cylindrical and made
of stainless steel; the cathode plates positioned on both sides of the anode
tube are made of titanium, which serves as gettering material. The magnetic
field is oriented along the axis of the anode. The basic cell resembles a cold
cathode ionization gauge.
Electrons are emitted from the cathode due
to the action of an electric field, typically 5000 to 7000 V applied between
electrodes. The presence of the magnetic field produces long, more-or-less helical
trajectories for the electrons. The long travel path of electrons before reaching
the anode improves the chances of collision with the gas molecules inside the
pumping module. The common result of a collision with the electron is the creation
of a positive ion. In other words, when the electron collides with a gas molecule
(with the velocity or energy attained due to the high-voltage field), it tends
to knock out another electron from the molecule. The positive ions travel to
the cathode due to the action of the same electric field. The collision with
the solid surface, when the velocity or energy is adequate, produces a phenomenon
called sputtering (i.e., ejection of titanium atoms from the cathode surface).
The fresh titanium film covers various surfaces
in the pump, where it reacts with gas molecules as illustrated in Figure 8 (black
layer inside the anode). Some of the ionized molecules or atoms impact the cathode
surface with high enough force to penetrate the solid and remain buried.
The detail pumping mechanisms in sputter
ion pumps are more complex than outlined here. It may be appreciated that different
gases are pumped in a different way and at different pumping speeds. Also, there
exists the possibility of previously pumped gases to be reemitted: for example,
when the cathode surface is eroded, as illustrated in Figure 9. Sputter-ion
pumps are generally associated with ultrahigh vacuum, although they can be used
successfully in the high-vacuum region. Also. other pumps can produce an ultrahigh
vacuum. The unique advantage of sputter-ion pumps, aside from their relative
cleanliness, is their complete isolation from the atmospheric environment. Like
cryopumps, they do not have an exhaust. They accumulate the pumped gases inside
the pump. Unlike cryopumps, they are not regenerated periodically. They are
used until the cathode is exhausted. Naturally, their life depends on the amount
of pumped gas, and therefore they should not be used at higher pressures for
extended periods.
3. BASIC PERFORMANCE OF SPUTTER-ION PUMPS
The general pumping speed characteristics
of sputter-ion pumps are similar to other vacuum pumps. There is a more-or-less
constant-speed region at intermediate pressures, the net pumping speed is reduced
to zero at low pressure, and it decreases to very low values at higher pressures.
Due to practical engineering considerations sputter-ion pumps are not designed
for high continuous-gas-throughput conditions. Compared to other high-vacuum
pumps of equal pumping speed, sputter-ion pumps have approximately 100 times
lower maximum throughput values. The pumping speed begins to decrease near 1x10-5
torr rather than near 1x10-3 torr.
A typical pumping speed characteristic is
shown in Figure 10.
The ultimate pressure of an isolated pump
is the 10-12 torr range. There is not single, simple, specific reason
for the particular ultimate pressure. Presumably, it is due partly to the equilibrium
between the residual gas evolution inside the pump and the pumping speed. This
is similar to other pumps.
Partly, however, it may be due to the tendency
for the electric discharge in the gas to extinguish at very low pressures.
The pumping speed of ion-getter pumps depends,
as in cryopumps. on the arrival rate of the gas molecule (i.e., their molecular
weight and temperature) and the sticking coefficient or the probability of capture
upon arrival at the surface. The pumping speed per unit area, S (liters per
second per cm2), can be expressed as:
where s is the sticking coefficient,
T the absolute temperature (K), and M the molecular weight.
This equation is not very useful unless the sticking coefficient is known. Unfortunately,
it can vary within a factor of 2 or more. The initial sticking coefficient for
nitrogen on titanium surface has been quoted in the technical literature at
values ranging from 0.1 to 0.7. For sputter-ion pumps an additional variable
is the efficiency of the sputtering process or the sputtering yield.
At the present time there are five varieties
of industrial sputter-ion pumps: the diode pump (Figure 8), in which the cathodes
are attached to the body of the pump and a high (positive) voltage is applied
to the anode; the triode pump, where the cathodes are separated from the pump
body and a high (negative) voltage is applied to the cathode (Figure 11); “differential”
pumps, where one of the cathodes is made of a metal other than titanium; StarCell
pumps (Varian Associates), which are triode pumps with a distinctive star-shaped
configuration; and pumps that include a non-evaporative gettering module. The
latter provides a high speed for hydrogen and consists of a corrugated strip
of constantan into which is sintered a special alloy (zirconium, vanadium, iron).
When heated this alloy undergoes a transformation
producing a very large gettering surface.
In summary, the pumping action in sputter-ion
pumps is thought to be produced by the following processes:
1. Ion burial and entrapment within the metal
lattice a few atomic layers under the surface of the cathode.
2. Gettering of chemically active gases at the
cathode and elsewhere by sputtered deposits.
3. Diffusion of hydrogen into the cathode material.
4. Dissociation of complex molecules into simpler
fractions which are then pumped by one of the mechanisms.
5. Production of neutral atoms of high velocity
(or energy) by neutralization of ions and scattering from the cathode surface.
The neutral atoms can subsequently be pumped by the burial process in areas
of deposited material on the anode, cathode, or pump envelope.
For practical designs of sputter-ion pumps
the anode cells are between 15 and 25 mm. This is suitable for operations with
magnetic fields of 1 to 1.5 kG.
A voltage of at
least 3 kV is necessary to start the pump reliably. The pump current increases
with the voltage until 6 or 7 kV is reached, which is a common range of operation.
These conditions produce pump currents between 5 and 30 A/torr; for the cell,
the pumping speed is between 0.3 to 2 l/s.
Pumps are made normally
up to 200 l/s but can be made larger.
4. PUMP TYPES AND PERFORMANCE WITH DIFFERENT GASES
Ion-getter pumps are capable of pumping any
gas, including noble gases and hydrocarbons. Due to the differences in molecular
weight and chemical activity, the pumping mechanisms and the associated pumping
speeds are different for different gases. The ionized molecules bombarding the
cathode produce different rates of sputtering depending on their molecular weight
and the angle of approach. Small angles (grazing the surface) produce a higher
sputtering rate. For light gases such as hydrogen the sputtering rate is too
low to obtain pumping speeds comparable to those for nitrogen and oxygen.
Titanium is chosen for the chemical gettering
action because it is a highly reactive element that forms stable compounds with
many different gases. Ironically, titanium in bulk form is very corrosion resistant
at normal temperatures because it has a tightly packed oxide layer which protects
its surface. Getterable gases are oxygen, nitrogen, CO, CO2, and
many others.
In addition to sputtering, a fraction of
impinging ions can remain buried in the cathode. However, as noted before, the
depth of penetration is only a few atomic layers. Because the cathode is continuously
eroded, the pumping speed for getterable gases by this mechanism is negligibly
small. Hydrogen, in principle, is also getterable, but by itself, does nor produce
a sufficient sputtering yield. When hydrogen is pumped together with other gases,
an important fraction of hydrogen is pumped at the anode. But the major mechanism
of hydrogen pumping is due to the diffusion into the cathode material. It diffuses
into the cathode to depths much beyond the range of ion implantation and therefore
can be pumped in a stable manner and high amounts. The pumping speed for hydrogen
is typically two times higher than the speed for nitrogen. Cathode structure
should be resistant to, or should accommodate, distortions because of the presence
of large amounts of hydrogen in the lattice. If the temperature increases, the
diffusion rate is increased but a fraction of pumped hydrogen may be released
because the binding energy of titanium hydride is lower than that for nitride
and oxide.
Inert gases cannot be pumped by chemical
reactions. As noted before, they are pumped primarily by burying into surfaces
in various parts of the pump after impinging either as ions or as neutral atoms
at high velocity (or energy). They can then be covered by layers of sputtering
titanium films. The inert gas atoms implanted at the cathode may be released
as the cathode erodes due to continuing ion bombardment. Early diode pumps,
in association with this, had a rather low speed for inert gases and tended
periodically to release previously pumped gas (called an argon instability).
One way to overcome this problem is to increase the portions
of the atom that rebound from the cathode surface as neutrals and then are implanted
into the anode and the walls of the pump, where they are held more or less
permanently. The probability of this reflection depends on the masses of the
impinging ions and the cathode material as well on the incidence angle. The
higher the mass of the target material, the more likely it is that the ion will
rebound and will also retain more energy after reflection. The use of heavier
metals, such as molybdenum or tantalum as an auxiliary cathode material, then
provides the necessary improvement. If both cathodes were made of the heavier
metal, the sputtering yield would be reduced. Pumps with such differentiated
cathodes produce a very substantial improvement in the pumping speed of inert
gases and also improve its stability (Table 2), although the speed for getterable
gases may be somewhat reduced.
A more effective
approach is to provide a more favorable incidence angle for the ions. One way
to achieve this is to slot the cathode surface, providing shallow angles for
incident ions, and to increase both the reflection probability and the sputtering
yield. Such pumps produce inert gas speeds that are 5 to 10% of the pumping
speed for air, and the pumping speed for the inert gases is stable.
The next logical development is to make the
cathode in the form of thin parallel strips with some space between them. This
grid structure is partly transparent for ions and allows the pump wall (behind
the cathode) to be available as a pumping surface. The wall can be considered
as an auxiliary anode. This type of pump is called a “triode pump” (Figure 11),
as expected, the pump walls are kept at a ground potential and the high negative
voltage is applied to the cathodes. In a triode pump the ions that retain their
energy after being neutralized at the cathode may travel to the pump wall and
be buried there or reflect and be pump at the anode. The pumping speed for the
inert gases for triode pumps is 20 to 25% of speed for air and it is very stable
even after a long period of pumping. The pumping speed for hydrogen is somewhat
lower than that of diode pumps with titanium cathodes. Also, distortion of cathode
strips can occur after pumping large amounts of hydrogen or when pumping at
the high end of the pressure range.
To overcome problems with cathode distortions
the cathode has been designed with radial strips or spokes located in alignment
with each anode cell (Figure 12).
This avoids the tendency for distortions
because the spokes are attached only on one end. They are free at the center
arid are symmetric relative to the ion activity in the pumping cell. Because
of the shape these pumps are known under the trademark StarCell (Varian Associates).
An additional important advantage is obtained from the symmetric pattern of
cathode erosion, which begins at the center and progresses toward the periphery.
In this way more titanium can be sputtered before the cathode structure loses
its integrity. In a diode pump, the ion bombardment eventually produces a hole
in the cathode plate after which the pumping action is nearly lost. In a triode
pump the end of the cathode life occurs when a strip brakes, which often causes
a short circuit. Due to the gradual symmetric erosion in the StarCell pump its
life is increases by nearly a factor of 2 compared to a standard triode pump
and by 60% compared to a diode pump, so that the pump can operate continuously
at 1x10-5 torr for a period of 1 year. Pumping speeds of StarCell
pumps for different gases compare as follows: for oxygen, nitrogen, water vapor,
and methane, nearly the same; for carbon dioxide, 10% higher; for hydrogen,
twice as high as nitrogen; for argon, 22%; and for helium, 30% of nitrogen.
The most recent development in ion pump design is the addition of a nonevaporating
getter strip inside the pump. This increases the pumping speed and the maximum
throughput capability of the pump.
5. OPERATION OF ION PUMPS
Sputter-ion pumps are normally shipped to
the user after evacuation, degassing, and sealing under vacuum. This keeps the
pump surfaces clean, unsaturated with adsorbed gases, and makes it easier to
start the pump. The pump inlet is covered and sealed by a flanged plate, which
includes an evacuation tube made of’ copper. After the final processing this
tube is sealed usually by a pinch-off tool that produces a leaktight cold weld
as it cuts off the tube. When constructing a new vacuum system the pump should
be opened only after everything is completed and the system is ready to be evacuated.
The exposure of the pump to atmosphere should be minimized.
Ion pump systems normally have a high-vacuum valve which can
isolate the pump when the system is exposed to air. If ultimate pressure in
the 10-9 torr range is adequate, baking may not be mandatory and
the system may have two Viton O-rings, one under the bell jar (Figure 13) and
one in the valve plate. For lower pressures the chamber and all seals must be
made of metal and the entire system surrounded by a bake-out oven.
When pumping speeds of ion pumps are measured or specified
it should be clearly understood whether the measurements are made with a new,
processed pump or after a certain amount of gas has been pumped. The pumping
speed of new ion pumps decreases during operation until a stable level is reached.
The initial pumping speed for nonsaturated pumps (StarCell types) is shown in
Figure 14. This should be compared with Figure 10, which shows the saturated
pumping speeds for the same pumps. The higher pumping speeds at pressures above
10-7 torr (Figure 14) may or may not be utilized, depending on the
operation of the system. For example, to saturate a 60 l/s StarCell pump 2.5
torr l of gas is normally required.
Sputter-ion pumps are sometimes difficult
to start if the pressure is too high or too low when the high voltage is applied.
At the higher pressures near 10-2 torr, particularly if the pump
has been exposed to the atmosphere for a few days, the initiation of’ the electric
discharge may produce enough current drain from the power supply to increase
the temperature of the internal electrodes. This, in turn, produces increased
outgassing, which may cause a runaway condition. At the same time the voltage
may drop, which reduces the pumping speed, making the starting condition even
more difficult. If the pump is not clean, more gas may be driven from it than
is pumped. Sometimes it is necessary to start and stop the pump a few times
before it finally begins to reduce the pressure in a stable manner. Triode and
diode ion pumps exhibit different behavior during starting. These differences
depend on the design of the power supply and its polarity as well as the cathode
shape and material.
At very low pressures the initiation of the pump may take
a long time. If a system had been evacuated to 10-9 torr by some
other means, the ion pump will start in a few seconds; at 10-12 torr
it may take half an hour. As mentioned before, the performance of the pump at
the higher pressures depends to a great degree on the power supply characteristics.
One of the important aspects is the requirement for maintaining a current sufficient
to obtain higher throughput without overheating. The best performance is obtained
when a pump is properly matched to a power unit. A power supply that is too
large for a given pump will cause overheating and may damage the pump at high
starting pressures. A power unit that is too small will reduce the maximum operating
pressure of the pump or, in other words, reduce its maximum-throughput capability.
The power unit must supply voltage and current required under different working
conditions, automatically limiting the delivered power at high pressures to
facilitate starting of the pump under different conditions. The power consumption
of the pump strongly depends on pressure and becomes essentially negligible
at pressures below 10-6 torr (Figure 15).
One interesting and useful characteristic
of sputter-ion pumps is the approximately linear relationship between the electrical
power used by the pump and the pressure. The pump automatically adjusts the
intensity of the pumping activity to the number of molecules present in the
system, This should not be surprising because the basic pumping mechanisms of
the pump depend on the number of available molecules. The electron “cloud” rotating
in the cell of a sputter-ion pump under the influence of a magnetic field (somewhat
analogous to a rotor of an electric motor) is relatively stable and is not strongly
dependent on pressure. Therefore, the current of the pump. similar to cold cathode
gauges can be used as a measure of pressure, as shown, for example, in Figure
25.
It should be understood that this is
only an approximate indication and should not be thought of as a substitute
for an ultra-high-vacuum gauge of good quality. The measurement becomes more
uncertain as the pressure is reduced below 10-8 – 10-9 torr.
This is due to leakage currents and other effects that are independent from
pressure.
6. NONEVAPORATED GETTER (NEG) PUMPS
There is a class of gettering pumps in which
the active material is not evaporated or sputtered on a pumping surface but
remains in a specially prepared very porous intermetallic compound. Such pumps
were pioneered the by SAES Getters company in Milan, Italy and are often called
NEG pumps. The pumping action initially involves an adsorption event followed
by diffusion inside the material. (It is ironic that these pumps can be called
“diffusion pumps” more than the vapor jet pumps, for which the common name is
a misnomer). The most comprehensive treatment (in high-vacuum textbooks) of
the physical basis of the pumping action and properties of various materials
was presented by O. Saksaganskii, who devotes 47 pages to this subject in his
book.
Usually the pumping material is in the form
of thick films or layers deposited on a substrate strip or ribbon, typically
a nickel-iron alloy such as constantan, nichrome, or stainless steel and others.
The compound has a porosity of 50 to 70%, may be as thick as a few millimeters,
and can have a real internal physical area 100 times higher than the projected
area (100 to 1000 m2/kg). The active metallic compound is usually
composed of finely dispersed powders of transition metals, which may be sintered,
plasma-sprayed, or rolled into the substrate. A common composition has 84% zirconium
and 16% aluminum. Other compounds include titanium, vanadium, iron, nickel,
and also tantalum, molybdenum, tungsten, and rhenium.
Because of the progressive saturation of the exposed surfaces,
the getter must be reactivated by heating to enhance the diffusion process and
clean the surface. This activation is achieved by raising the temperature to
about 750 °C for several minutes in vacuum. Subsequently, the getter is held
usually at about 400 °C. The performance of the pump is normally judged by its
pumping speed for hydrogen. Most common gases present in high-vacuum systems
are pumped permanently, but hydrogen can be reemitted if the temperature is
raised above 1000 °C. As in other gettering pumps, the total capacity for pumped
gas is limited and after a number of activations, the pumping speed declines
and the pump saturates. Pump specifications provide information about total
accumulation capacity before the getter strip or ribbon becomes brittle and
loses its mechanical integrity.
NEG pumps are available as nude cartridges, as glass-encased
appendage capsules, or as autonomous flanged pumps that can be attached to any
vacuum system. To provide a higher pumping speed in a smaller package, the getter
ribbon is often pleated or corrugated (shown in Figure 16) and provided with
a heater. Water cooling or even air cooling is not necessary for small pumps.
A small pump (2.5 cm diameter, 7.5 cm long), if properly thermally shielded,
can be heated in steady-state operation with a 10 watt heating source, Also,
for pure hydrogen, the pump can be operated at a reduced speed at room temperature.
Pumps are made in many sizes and a nude cartridge may produce 2000 l/s pumping
speed for hydrogen. Typical pumping speeds are 65% for oxygen, 50% for carbon
monoxide, and 17% for nitrogen as compared to hydrogen. The hydrocarbons are
pumped with a speed that is one hundredth of the speed for carbon monoxide.
Such ratios, however, can be misleading because they depend on the quantity
of previously pumped gas. For example, Figures 17, 18, and 19 show the pumping
speeds as a function of the amount of previously pumped gas.
Inert gases and methane are not pumped in
significant amounts. Therefore, usually a small ion-getter pump is required
to provide the pumping speed for these gases In this manner, ultrahigh-vacuum
can be obtained in ultra-high-vacuum systems with the primary pumping done by
NEG pumps, especially, when, after baking. the main residual gas is hydrogen.
NEG pump strips are sometimes included for miles, along the entire length of
tubing in particle accelerators, and as auxiliary pumping modules for enhance
hydrogen pumping speed in autonomous ion-getter (sputter-ion) pumps, which may
be called combination pumps.
7. COMBINATION PUMPS
Non evaporated getter pumps can be incorporated into ion-getter
pumps to provide a higher pumping speed for hydrogen. For this purpose, it is
convenient to select a NEG composition that can be activated at baking temperatures
normally used in the process of obtaining ultra high-vacuum (300 - 400 °C).
An example of such an integrated pump, using the NEG composition St707, is shown
in Figure 20.
The normal range at the activation temperature for this compound
is specified as 600 - 800 °C, but after 12 h bake at 350 °C, sufficient pumping
action is obtained (after cooling in room temperature) as shown in Figure 21.
The combination pump performance, as expected, provides higher
pumping speed for hydrogen, which is usually the main gas in an ion-getter pump
system. The pumping speeds for hydrogen, for three different sized pumps, are
shown in figure 22, where dashed curves represent pumps without NEG addition
and the solid curves represent combination pumps.
The corresponding residual gas measurements are shown in
Figure 23 and demonstrate a sharp reduction of the partial pressure of hydrogen.
8. CLEAN ROUGHING SYSTEMS
The initial evacuation of high- and ultra
high-vacuum systems that are subsequently pumped by ion pumps has two basic
requirements: the ultimate pressure of the roughing pumps should be low (near
1x10-3 torr), and the rough pumps should not contaminate the system
and then the ion pump which can cause starting and operating difficulties. An
additional requirement is to use an ion pump with high-enough pumping speed
or a system with low-enough outgassing rate to be able to reduce the pressure
quickly after the high-vacuum valve is opened. It should be recalled that ion
pumps have approximately one hundredth of the maximum-throughput capability
of other high-vacuum pumps. System design and operation must reflect this characteristic.
With regard to the maximum practically permissible steady-state
gas flow into the pump, the ion-getter pumps must be considered as a different
class of equipment. Compared to throughput-type pumps of the same nominal pumping
speed, they have nearly one thousand times lower throughput capability. This
observation immediately suggests that the starting conditions, after the initial
evacuation, must be different. It is common in textbooks and operating instructions
to specify a pressure level where the pump can be started. This is an unfortunate
choice that leads to errors in system design such as the incorrect selection
of rough pump type or size, or the size of the high-vacuum pump. There are three
items to consider and are illustrated in Figure 24.
The amount of gas initially entering the pump (after the
high-vacuum valve is opened), depends on the volume of the chamber and the pressure
(at the end of the roughing cycle), not the pressure alone. The bypass line
shown in Figure 24 can help in softening the sudden rush of the pumped gas into
the pump, but it does not change the two components of the gas contained and
emanating from it: the gas in space and the gas emitted from the surface. The
selection of the high-vacuum pump size will also depend on the frequency of
evacuation events. With all this in mind, a simple gas accumulation estimate
should be made before deciding on a particular roughing system or the size of
the high-vacuum pump.
Even if some ion pumps can be started at
pressures as high as 10 to 20 mtorr, it is not a good idea to do this too often
because of the accelerated exhaustion of the cathodes. The cathodes of an ion
pump, which are eroded by sputtering, can not be regenerated but must be replaced.
This replacement is not a simple matter because the pump will has to be cut,
open and then re-welded. The cathode life depends on the amount of gas pumped,
on the integral of pressure and time. Typical values for diode pumps are 200
h at a constant pressure of 10-4 torr, 2000 h at 10-5
torr, 20,000 h at 10-6 torr, and so on. Note that at 10-6
torr the life is over 2 years and at 10-3 torr only 20 h! For pumping
nitrogen only the life of a diode pump at 10-6 torr will be about
50,000 h (5.7 years). Corresponding values for a triode pump are 35,000 h, and
for a StarCell pump, 80,000 h.
Ideally, ion pumps should be started at pressures near 1x10-5
torr, although in practice starting pressures near 10-3 torr are
more common. There are several ways to accomplish this. It is possible to use
oil-sealed mechanical pumps with well-designed and carefully operated trapping
arrangement. Such pumps can produce pressures below 10-4 torr with
a liquid nitrogen trap or a carefully degassed zeolite trap. However, oil-sealed
mechanical pumps are rarely used for the initial evacuation of ion pump systems.
Fear of accidental contamination of the system and of the ion pump is sufficient
to discourage their use.
Sorption pumps are commonly used as roughing
systems for ion pumps (Figure 26). To prolong the saturation period, air ejectors
(Venturi pumps) or coarse oil-free mechanical pumps can be used at the beginning.
They can remove about 90% of the air before sorption pumps are engaged. Recently
developed oil-free high-vacuum mechanical pumps can be very useful. They can
produce pressures below 20 mtorr and they can be left pumping on the system
for longer periods of time without any possibility of contamination, allowing
the system to degass. If the ion pump is large and the evacuation object small
(e.g., a microwave tube), the oil-free mechanical pump can be used alone. In
general, they should be used with a single stage of sorption pumping and/or
with a titanium getter pump before the ion pump power is started.
In large, expensive installations it may be useful to
evacuate the vacuum system to 10-5 torr or below using oil-free mechanical
pump followed by cryopumps or turbodrag, or turbomolecular pumps before the
system is switched to ion-getter pumps. One example of successful employment
of these pumps in large vacuum systems is in the field of high-energy physics,
where many of the modern particle accelerators are constructed using ultrahigh-vacuum
techniques and are pumped by ion pumps.
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