Measurement of Vacuum

Given the very large range of pressures produced in vacuum systems (up to 19 orders of magnitude
in some systems) there is no single gauge capable of measuring the full range of pressures. Most
vacuum systems must have at least two different types of gauges, or even three.
Gauges can be divided into three categories:
1.) Direct Pressure/Force Methods
2.) Thermal Conductivity Gauges
3.) Ion Gauges

1.) Direct Pressure/Force Methods

The most straightforward method of measuring pressure is to measure the force exerted
on
the wall of the container or on the surface of a liquid. Mechanical force-measurement
gauges usually involve measuring the deflection of a diaphragm supported between the
vacuum system and either atmosphere (Bourdon gauge) or a chamber evacuated to a
pressure significantly less than lowest pressure range of the gauge(Capacitance Diaphragm
Manometers).

1.1) Capacitance Diaphragm Manometers

Operating Principles:
These gauges use a thin metal, or in some cases, ceramic diaphragm, which separates two
chambers, one connected to the vacuum system and the other providing the reference pressure.
The reference chamber is commonly evacuated to well below the lowest pressure range of the
gauge, and has a getter to maintain that pressure. The term “capacitive measurement” means that a
plate capacitor is created by the diaphragm with a fixed electrode behind the diaphragm. When the
distance between the two plates of this capacitor changes, a change in capacitance will result. This
change, which is proportional to the pressure, is then converted into a corresponding electrical
measurement signal. The deflection of the diaphragm is measured using a very sensitive electrical
capacitance bridge circuit that can detect changes of ~2 x10 -10 m. In the most sensitive gauges the
device is thermostatted to avoid drifts due to temperature change; in less sensitive instruments
there is no temperature control.

Operation:
The bridge must be periodically zeroed by evacuating the measuring side of the diaphragm to a
pressure below the lowest pressure to be measured.
The simplest form of the capacitance manometer uses a
capacitance electrode on both the reference and measurement
sides of the diaphragm. In applications involving
sources of contamination, or a radioactive gas such as tritium,
this can lead to inaccuracies, and a manometer with
capacitance probes only on the reference side should be
used.

Precautions:
1.) When a gauge is used for precision measurements, it
must be corrected for the pressure differential that results when the thermostatted gauge head is
operating at a different temperature than the vacuum system placed in such a way as to avoid
drastic temperature
2.) Any gauge that is not thermostatically controlled should beplaced in such a way as to avoid
drastic temperature changes, such as periodic exposure to direct sunlight.

2.) Thermal Conductivity Gauges

Applications:
Thermal conductivity gauges are relatively inexpensive. Many operate in a range of ~1x10-3 to 20 torr.
This range has been extended to atmospheric pressure in some modifications of the ‘‘traditional’’ gauge
geometry for monitoring and control during the processes of roughing down from atmospheric pressure
and for the cross-over from roughing pump to high-vacuum pump.

Operating Principles:
Once a volume changes from the viscous regime to the free-molecular regime, the heat
transport capacity of the gas falls in proportion to the number of gas molecules in the
volume. The measurement of this effect is the basis of the thermal conductivity gauge. For a
wire in a cylindrical envelope, the heat transport Qc is

Qc = Kqp(Ts−Te)2prsl

where p is the pressure of the gas, Te is the temperature of the envelope, and Ts is the
temperature of the heated wire or source. Geometrically, re is the radius of the envelope,
rs is the radius of the wire, and l is the length of the wire. The term Kq is the thermal
conductivity of the gas and is gas-dependent. The ultimate low pressure limit for thermal
gauges is set by the radiative heat loss

Qr = Kr (T4s −T4e)2prsl

which rises very rapidly with increasing temperature.

In most gauges, a ribbon or filament serves as the heated element. Heat loss from this element to the wall
is measured either by
1. the change in element temperature, as in the thermocouple gauge, or
2. as a change in electrical resistance, in the Pirani gauge.
Thermal radiation heat loss from the heated element is independent of the presence of gas, setting a lower
limit to the measurement of pressure. For most practical gauges this limit is in the mid- to upper-10 -4 torr
range.

Source of errors:
1.) Thermal conductivity gauges are commonly calibrated for air, which changes significantly
with the gas. The gauge sensitivity is higher for hydrogen and lower for argon. Thus, if the
gas composition is unknown, the gauge reading may be in error by a factor of two or more.
2.) Some gauges are subject to drift over time, for example, as a result of contamination from
mechanical pump oil, but others remain surprising stable under common system conditions.
Two common sources of drift in the pressure indication are
 2.1) changes in ambient temperature and (It can be minimized by operating the heated
element at 300°C or higher. However, this increases chemical interactions at the element, such as
the decomposition of organic vapors into deposits of tars or carbon; such deposits change the
thermal accommodation coefficient of gases on the element, and hence the gauge sensitivity. More
satisfactory solutions to drift in the ambient temperature include a thermostatically controlled
envelope temperature or a temperature-sensing element that compensates for ambient
temperature changes.)
2.2) contamination of the heated element.

2.1) Thermocouple gauges:

In this gauge, the element is heated at constant power, and its change in temperature, as the
pressure changes, is directly measured using a thermocouple. In many geometries the
thermocouple is spot welded directly at the center of the element; the additional thermal mass of
the couple reduces the response time to pressure changes. In an ingenious modification, the
thermocouple itself (Benson, 1957) becomes the heated element, and the response time is
improved.

2.2) Pirani Gauge:

In this gauge, the element is heated electrically, but the temperature is sensed by measuring its
resistance. The absence of a thermocouple permits a faster time constant.

Figure 2: Pirani gauge. The filament is heated by a current and the resistance is measured
with the bridge.

The gauge can be operated in either constant temperature or constant current mode. In the
constant current mode, the temperature of the wire provides the measurement, while in constant
temperature mode, the current going to the gauge head is modulated to keep Ts constant. In a
constant temperature gauge, the pressure proportional to the power (I2R). The constant
temperature mode has the advantage of avoiding burning out the element, since the maximum
temperature is limited. Additionally, the low-pressure limit for a constant temperature gauge is
lower than for a constant power gauge because of the rapid growth of Ts4 at high temperatures. A
further improvement in response results if the element is maintained at constant temperature, and
the power required becomes the measure of pressure. This measurement principle utilizes the
thermal conductivity of gases for the purpose of pressure measurements in the range from 10-4
mbar/Torr to atmospheric pressure.
 3.)Ion Gauges

At very low pressures, neither force nor thermal gauges function effectively, and yet
another type of gauge is required. High vacuum (low pressure) gauges are nearly always
some form of ion gauge. As a general type, ion gauges function by ionizing the gas atoms in
the vacuum volume and collecting and measuring the ion current produced. Because ionization is
inherently a gas-type-dependent process, ion gauges are never gas-independent.
Ion gauges are of two types
1.) Hot cathode type
2.) Cold cathode type

3.1) Hot-cathode gauge

The standard hot-cathode gauge contains a heated filament(cathode) which produces electrons.
These electrons are accelerated by a grid voltage of ~200V.
They are of two types:
1.) Triode ion
2.) Bayard-Alpert

3.1.1) Triode ion

These sensors commonly use three electrodes. A hot cathode
emits electrons which impinge on an anode. The gas, the
pressure of which is to be measured, is thus ionized. The
resulting positive ion current is detected through the third
electrode - the so-called ion detector - and this current is used
as the signal which is proportional to the pressure. These
electrons are accelerated by a grid voltage of ~200V. Most
electrons miss the wire grid and pass through to the other side.
The anode is at a small negative voltage relative to the cathode
(~10V) so the electrons come to a stop and return back
towards the grid. They will oscillate across the grid several
times before being captured by a wire. If they encounter a gas
atom in their travels, they may ionize it. The ions will drift to
the anode and the current observed here gives the pressure.

Fig. 3(a) Triode ion configuration (Top view)

The original design of the ionization gauge, the triode

gauge, shown in Figure 3B, cannot read below ~1 x
10-8 torr because of a spurious current, known as the x-
ray effect. The electron impact on the grid produces soft
x rays, many of which strike the coaxial ion collector
cylinder, generating a flux of photoelectrons; an electron
ejected
from the ion collector cannot be distinguished from an
arriving ion by the current-measuring circuit. This
limitation of the triode ion gauge leads to the development of the Bayard-Alpert gauge.
3.1.2) Bayard- Alpert Gauges
Bayard-Alpert gauge, has simply inverted the geometry of the triode gauge. The Bayard-Alpert
gauge reverses the location of the filament and anode, which greatly reduces the area of the anode
and hence the area for X-rays to hit The sensitivity of the gauge is little changed from that of the
triode, but the area of the ion collector, and presumably the x ray induced spurious current, is
reduced by a factor of 300, extending the usable range of the gauge to the order of 1 x10-10 torr.

Bayard- Alpert configuration

The equation describing the gauge operation is

+ -
where P is pressure, in torr, i is the ion current, i is the electron current, and K, in torr-1, is the
gauge constant for the specific gas.
The gauge and associated electronics are normally calibrated for nitrogen gas, but, as with the
thermal conductivity gauge, the sensitivity varies with gas, so the gas composition must be known
for an absolute pressure reading.

Disadvantages:
The lifetime of all hot-cathode gauges is limited by the lifetime of the filament. Filaments
age rapidly when heated at pressures greater than 10 -2, so a roughing gauge (such as a
Pirani) must be used to monitor the pressure before turning on the hot-cathode gauge.
Also, the presence of certain chemicals in vacuum system (such as chlorine) can very
quickly destroy the hot filament.

3.2) Cold cathode gauges

Cold cathode gauges avoid the filament destruction common to hot-type gauges. One
common type of cold-cathode gauge is the Penning or Phillips gauge. In this gauge, a much
higher voltage (~2kV) is used than in hot-cathode gauges, but there is no heating to the
cathode.
Operating Principles:
The gauge is formed from two cathode plates with a wire loop anode halfway between the two. The
electrons emitted from the cathode are accelerated towards the plane of the anode loop. A magnetic

field of 0.15 tesla is directed along the axis of the cathode.

This field makes the electrons curve in a helix. The electrons curl down through the plane of the
anode loop until they are pushed back by the other cathode and they oscillate a very large number
of times in the field before encountering the ring of the anode. This long path and high kinetic
-2 -7
energy give a very large chance of ionizing a gas molecule. The operating range is from 10 to 10
torr.

Disadvantages:
1.) It can be hard to start the discharge at low pressures. Sometimes a small filament or beta
source is used to start the discharge.
2.) Discharge current in the Penning and other cold cathode discharge gauges is extinguished at
pressures of a few torr. When a gauge does not give a pressure indication, this means that either the
-7
pressure is below 10 torr or at many torr, a rather significant difference. Thus, it is necessary to
use an additional gauge that is responsive in the blind spot of the Penning—i.e., between
-2
atmospheric pressure and 10 torr.
3.) Discontinuities in the pressure indication may also occur throughout the range.

A gauge can affect the pressure in a system in three important ways

1.) An operating gauge functions as a small pump. In systems that are pumped at relatively large
speeds, the gauge has negligible effect, but if the gauge is connected to the system by a long tube of
small diameter, the limited conductance of the connection will result in a pressure drop, and the
gauge will record a pressure lower than that in the system. For example, a gauge pumping at 0.1
L/s, connected to a chamber by a 100- cm-long, 1-cm-diameter tube, with a conductance of
~0.2 L/s for air, will give a reading 33% lower than the actual chamber pressure.

Solution: The solution is to connect all gauges using short and fat (i.e., high-conductance) tubes,
and/or to run the gauge at a lower emission current.

2.) A new gauge is a source of significant outgassing, which increases further when turned on as its
temperature increases. Whenever a well-outgassed gauge is exposed to the atmosphere, gas
adsorption occurs, and once again significant outgassing will result after system evacuation. This
affects measurements in any part of the pressure range, but is more significant at very low
pressures.
Solution: For gauges especially suitable for pressures higher than the low 10_7 torr range, the grid
of the gauge is a heavy non-sag tungsten or molybdenum wire that can be heated using a high-
current, low-voltage supply. Temperatures of _13008C can be achieved, but higher temperatures,
desirable for UHV applications, can cause grid sagging; the radiation from the grid accelerates the
outgassing of the entire gauge structure, including the envelope.

3.) The high-temperature electron emitter can interact with gases in the system in a number of
ways. A tungsten filament, operating at 10 mA emission current, has a temperature on the order of
1825°C. Effects observed include the pumping of hydrogen and oxygen at speeds of 1 L/s or more;
decomposition of organics, such as acetone, produce multiple fragments and can result in a
substantial increase in the apparent pressure. Oxygen also reacts with trace amounts of carbon
invariably present in tungsten filaments, producing carbon monoxide and carbon dioxide.

Solutions:
low-work-function electron emitters such as thoria-coated or thoriated tungsten and rhenium can
be used, typically operating at temperatures on the order of 1450°C.

Advantages:
The power used by a thoria-coated emitter is quite low; for example, at 10 mA mission it is ~3 W
for thoriacoated tungsten, as compared to ~27 W for pure tungsten, so that the gauge operates at a
lower overall temperature and outgassing is reduced.

Disadvantages: The calibration stability is possibly less than that for tungsten filament gauges.
Additionally, thoria is radioactive and it appears possible that it will eventually be replaced by
other emitters, such as yttria . Tungsten filaments will instantaneously fail on exposure to a high
pressure of air or oxygen. Where such exposure is a possibility, failure can be avoided with a
rhenium
filament.

Electron Stimulated Desorption (ESD):

The normal mechanism of gauge operation is the production of ions by electron impact on gas
molecules or atoms. However, electron impact on molecules and atoms adsorbed on the grid
structure results in their desorption, and a small fraction of the desorption occurs as ions, some of
which will reach the ion collector. For some gases, such as oxygen on a molybdenum grid operating
at low pressure, the ion desorption can actually exceed the gas-phase ion production, resulting in a
large error in pressure measurement. The spurious current increases with the gas coverage of the
grid surface, and can be minimized by operating at a high electron-emission level, such that the rate
of electron-stimulated desorption exceeds the rate of gas adsorption.

Technique for detecting serious errors due to ESD:

1.) Change the electron emission. For example, an increase in current will result in a drop in the
indicated pressure as the adsorption coverage is reduced.
2.) Use a gauge fitted with a modulator electrode. This simple procedure can clearly identify the
presence of an ESD-based error and provide a more accurate reading of pressure; unfortunately,
modulated gauges are not commonly available.
Ultimately, low-pressure measurements are best determined using a calibrated mass spectrometer,
or by a combination of a mass spectrometer and calibrated ion gauge.

Stability of Ion Gauge Calibration:

The calibration of a gauge depends on the geometry of the gauge elements, including the relative
positioning of the filaments and grid. For this reason, it is always desirable before calibrating a
gauge to stabilize its structure by outgassing rigorously. This allows the grid structure to anneal,
and, with tungsten filaments, accelerates crystal growth, which ultimately stabilizes the filament
shape. In work demanding high-precision pressure measurement, comparison against a reference
gauge that has a calibration traceable to the National Institutes of Standards and Technology (NIST)
is essential.

Mass Spectrometers
A mass spectrometer for use on vacuum systems is variously referred to as a partial pressure
analyzer (PPA), residual gas analyzer (RGA), or quad.

Applications
Used for monitoring the composition of the gas in a vacuum system, for troubleshooting, and for
detecting leaks.

Disadvantages
Relatively difficult procedure for obtaining quantitative readings.

Magnetic Sector Mass Spectrometers:

Originally it was developed for analytical purposes now mainly used in helium leak detectors,
where a compact instrument using a small magnet is perfectly satisfactory for resolving the helium-
4 peak from the only common adjacent peak, that due to hydrogen-2.

Disadvantages
Generally too large for general application to vacuum systems.
Smaller versions provided excellent performance, but the presence of a large permanent magnet or
electromagnet remained a serious limitation.

Quadrupole Mass Filter:

A quarupole mass spectrometer analyzes the composition of gas in the vacuum system.
Mass selection is accomplished through the application of a combined DC and RF electrical voltage
to two pairs of quadrupole rods. The mass peaks are selected, in turn, by changing the voltage. By
adjusting the ratio of the DC and RF electrical potentials the quadrupole resolution can be changed
to provide either high sensitivity to detect very low partial pressures, at the expense of the ability to
completely resolve adjacent mass peaks, or low sensitivity, with more complete mass resolution.

Advantages:
1.) Rapidly scanning the ion peaks from the gas in a system can often determine the gas
composition.
2.) Interpretation is simplified by the limited number of residual gases commonly found in a
system.
Disadvantegas:
1.) Quadrupole spectrometers is that not all compact versions possess the stability for quantitative
applications.
2.) Very wide variations in detection sensitivity require frequent recalibration, and spurious peaks
are sometimes present.

VACUUM SYSTEM CONSTRUCTION AND DESIGN

1.) Materials for Construction

A vacuum system consists of chamber, pumps and gauges. Stainless steel, aluminum, copper, brass,
alumina, and borosilicate glass are among the materials that have been used for the construction of
vacuum envelopes.

1.1) Stainless steel

The most common material is stainless steel, most frequently 304L.

Advantages:
1.) The material is available in a wide range of shapes and sizes, and
2.) is easily fabricated by heliarc welding or brazing.

Disadvantages:
Any imperfections in this and other metals tend to extend along the rolling or extrusion direction.
For example, the defects in bar stock extend along the length. If a thin-walled flat disc or conical
shape is machined from such stock, it will often develop holes through the wall.

Precautions:
Brazing should be done in hydrogen or vacuum. Torch brazing with the use of a flux should be
avoided, or reserved for rough vacuum applications. The flux is extremely difficult to remove, and
the washing procedure leaves any holes plugged with water, so that helium leak detection is often
unsuccessful. Construction from rolled plate or sheet stock is preferable, with cones or cylinders
made by full penetration seam welding.

1.2) Aluminum

Aluminum is an excellent choice for the vacuum envelope, particularly for high-atomic-radiation
environments.

Advantages:

1. Much easier to machine than stainless

2. Also forms impervious oxide
3. Strength-to-weight ratio is greater than steel
4. Outgassing rate is 5-10x that of stainless

Disadvantages:
Joining by either arc welding or brazing is exceedingly demanding.

1.3) Borosilicate glass

Although outgassing is a serious problem in an unbaked system, a bakeout to as high as 400 °C
reduces the outgassing so UHV conditions can readily be achieved.
1.4) Kovar
It has an expansion coefficient closely matched to borosilicate glass, which is widely used in sealing
windows and alumina-insulating sections for electrical feedthroughs.

1.5) High-alumina ceramic

High-alumina ceramic provides a high-temperaturevacuum wall. It can be coated with a thin
metallic film, such as titanium, and then brazed to a Kovar header to make electrical feedthroughs.

Advantages:
Useful for internal electrically insulating components, and can be used at temperatures up to at
least 1800°C.

1.6) Elastomers
Elastomers are widely used in O-ring seals. Buna N and Viton are most commonly used. The main
advantage of Viton is that it can be used up to 200C, as compared to 80°C for Buna. Polyimide can
be used as high as 3008C and is used as the sealing surface on the nose of vacuum valves intended
for UHV applications, permitting a higher-temperature bakeout.

NOTE:
• Outgassing of materials can be the limiting factor in achieving good vacuum.
– It is usually best to use all stainless steel, aluminum, glass and copper.
– Elastomer gaskets and o-rings should be specifically manufactured for vacuum
applications.
• NEVER USE:
Brass, zinc, or other alloys without first looking up the outgassing rate (should be less than 10 -4
W/m2).

2.) Hardware Components

Demountable seals allows greater flexibility in system assembly and change. Replacement of a
flangemounted component is a relatively trivial problem as compared to that where the component
is brazed or welded in place. A wide variety of seals are available, but only two examples will be
discussed.

2.1) O-ring Flange Seals

The O-ring seal is the most convenient technique for high-vacuum use. Use of O-rings for moving
seals is commonplace; this is acceptable for rotational motion, but is undesirable for translational
motion. In some cases, a double O-ring with a grease fill between the rings is used; this is
unacceptable if a clean, oil-free system is required.

Advantages:
Modern O-ring seal assemblies have the ISO KF type geometry where the two flanges are identical.
This permits flexibility in assembly, and advantage that components from different manufacturers
may readily be interchanged.
Precautions:
Acetone should never be used for cleaning O-rings for vacuum use; it permeates into the rubber,
creating a long-lasting source of the solvent in the vacuum system. The O-rings must be cleaned by
wiping with a lint-free cloth. O-rings may be lubricated with a low-vapor-pressure vacuum grease
such as Apiezon M; the grease should provide a shiny surface, but no accumulation of grease.

Disadvantages:
All elastomers are permeable to the gases in air, and an O-ring seal is always a source of gas
permeating into a vacuum system. The approximate permeation rate for air, at ambient
temperature, through a Viton O-ring is 8 x 10-9 torr-L/s for each centimeter length of O-ring. This
permeation load is rarely of concern in systems at pressures in the 10 -7 torr range or higher.

Solution:
A double O-ring geometry, with the space between the rings continuously evacuated, is a useful
improvement. The guard ring vacuum minimizes air permeation and minimizes the effect of leaks
during motion. Such a seal extends the use of O-rings to the UHV range, and can be helpful if
frequent access to the system is essential.

2.2) All- metal Flange Seals

Application:
All-metal seals were developed for UHV applications. finds application where the absence of
leakage over a wide range of operating conditions is essential. The Conflat seal, developed by
Wheeler (1963), uses a partially annealed copper gasket that is elastically deformed by capture
between the knife edges on the two flanges and along the outside diameter of the gasket. Such a seal
remains leak-tight at temperatures from -195°C to 450°C.

Precaution:
A new gasket should be used every time the seal is made, and the flanges pulled down metal-to-
metal.

Disadvantages:
For flanges with diameters above ~10 in., the weight of the flange becomes excessive, and a copper-
wire seal using a similar capture geometry is easier to lift, if more difficult to assemble.