Vacuum Techniques

•Gauges
 Vacuum Gauges
• Thermal Conductivity Gauges: (Pirani, TC, Convection)
– Describe the operating principle for each gauge
– Explain the use of the Wheatstone bridge
– Compare the constant current and constant temperature modes of
operation
– Explain why the TC gauges typically have an upper limit of 1 torr
– Relate the lower pressure limit to thermal radiative heat transfer
• Ionization Gauges: (Hot Cathode, Cold Cathode)
– Describe the operating principle and electrical configuration for each
gauge
– Relate the sensitivity of the HCG to the geometry and gas properties
– Explain what is meant by the ‘soft x-ray’ limit
– Describe the role of magnetic field for the CCG
• Absollout gauges??/
 Measurement of pressure

• Mechanical phenomena gauges: measure

actual force exerted by gas (e.g. manometer).
• Transport phenomena: measuring gaseous
drag on moving body (e.g. spinning rotor
gauge) or thermal conductivity of gas (e.g.
thermocouple gauge).
• Ionization phenomena gauges: ionize gas
and measure total ion current (e.g. ion
gauge).
• Partial pressure residual gas analyzers:mass
spectrometers.
• Mechanical guages
Mechanical: liquid column, diaphragm, etc
Real pressure from force measurement
Mechanical phenomena Pressure
Measurement
Mechanical phenomena Pressure
Gauge
Bourdon Gauge
Mechanical phenomena How the
gauge works
Capacitance (diaphragm) gauge:
measure diaphragm bending by capacitance change

A
d C=ε
d
pressure
Absolute pressure
reference to a vacuum cell

Full range: 0.02 torr, 1 torr, 1000 torr, real species independent
10000 torr linear, accurate
Accuracy ~ 0.1 % zero point is not absolute
• Transport phenomena
 Transport phenomena(1)

• Gas molecules colliding with the heated

filament take kinetic energy away from
the filament’s atoms. This cools the
filament down.
• A higher pressure means that none
molecules collide with the filament per
second, so a larger cooling effect occurs.
 Transport phenomena(2)

• When the filament is cooler its resistance

is lower.
• The resistance can be measured
automatically.
• One way of doing this is to use a
Wheatstone Bridge.
 Transport phenomena(3)

Pirani Gauge

+ -

Filament
Thermal conductivity gauges mechanisms
WG

– Four possible mechanisms to Hot wire

take heat away from sensing Heating
current
element: 1/2 WC 1/2 WC
• Radiative heat transfer to Thermocouple
WCNV
surroundings joint

WR
• Conduction along the sensing
element
• Conduction through the
residual gas
• Convective heat flow to the
residual gas
 Thermal conductivity gauges mechanisms

1-Radiative heat transfer transfer:

WR = ε1 (2π r1 L )σ T − T ( 1
4
2
4
)
T2 r1
T1

L
• Conduction along the
wire
1 dT
WC = π r1 kwire
2

2 dl
T1 T2

L
• Conduction through the residual gas:
1/2
 γ + 1  R' 
(
WG = 2π r L Fα 
1
2
)  P 
 γ − 1  8π MT2 
(T1 − T2 )
as properties (M, γ, α) determine variation in
sensor response to pressure

R`: wire resistance,

P: pressure ,
L, r1: Wire length and diameter,
M, γ, Fα: Gas properties.
T1 and T2 Wire and gas temperature respectively
 Thermal Conductivity Gauges
Vbr2
• WT = WG + WR + Wc =
Pirani calibration (and low pressure limit): 4RS
• Platinum wire with r1 = 0.0127 mm, L = 150 mm
• At very low P, Vbr = 0.3907 V, and Rs = 43.61 Ω WR+WC =8.75x10-
4
W
• Subtracting WR+WC from WT yields WG for N2 as shown below:
Thermal Conductivity Measurment
Constant current mode
• Constant current mode:
– As pressure decreases, less heat is
removed by conduction through the gas from
the sensing element, and temperature
increases.
– Measure temperature dependent change of
resistance (or TC voltage).
 Thermal Conductivity Measurment
Constant temperature mode:
• Constant temperature mode:
– Adjust current to heater to maintain constant
sensor property (resistance or voltage)
– Use Wheatstone bridge arrangement to
optimize sensitivity
– Correlate current flow against pressure
– Extends high pressure range (used in Pirani,
not common for TC)
 Pressure Gauges
Gauge
Compensator
to system

milliammeter

Power
Supply
 Thermocouple gauge

For roughing vacuum measurements

• Ionization gauges
 Ionization phenomena(1)
• Electrons emitted from the heated filament
are attracted to the positive grid. Many
electrons follow long looped paths before
striking the grid.
• During this time they collide with gas
molecules, thus creating positive ions.
 Ionization phenomena(2)
• These ions are attracted to the negative
collector and constitute a current into the
gauge circuit.
• A higher pressure results in a higher
gauge current.
• The emission current must be kept within
strict limits as it too affects the gauge
current.
 Ionization phenomena(3)

• Thermionic/hot cathode ionization gauges.

• Energetic beam of electrons (constant I-) used
to ionize gas molecules and produce ion
current.
• e- + M → M+ + 2e-
I+ = p KI -, K: ion gauge sensitivity
• Upper pressure limit (10-3 Torr): secondary ion
ionization excitation, filament burn out.
• Lower pressure limit (10-10 Torr): secondary
electron current from X-ray emission.
 Hot Catode Ionization Gauges –
HCG(1)
• Hot cathode gauge (HCG)
– Thermionic source (electrons)
cause inelastic collisions with gas,
producing ions
– Ions collected at (-) biased surface
– Electrons travel to (+180 V) grid
• Pre-1950 lower limit of 10-6 Pa
– Soft x-rays produced at grid result in
photo-electron flow away from collector
+
collector (same as ion flow to grid
collector)
­
– Bayard-Alpert modification: fine wire
­ filament
collector surrounded by grid range
extended to 10-9 Pa
 HCG(2)

Ionization Gauge +ve

Ion Collector

Heated
Filament

Grid Pressure
Gauge

A.C.

Emission
Current
HCG(3)
 HCG(4)
• 10-11 ~ 10-3 torr
• linear sensitivity Th on Ir has a lower work function,
• absolute zero point so works at a lower temperature
• species dependent

sensitivity ∝ ionization cross section

air, N2, O2 1.0
He 0.15
Ne 0.3
H2 0.4

CH4 1.4
 HCG(5) Gauge sensitivity
• Gauge sensitivity:
– Dependent on rate of ionizing
collisions
σ LA ⋅ n
– Ion collision cross section given by
• σ = cross section per molecule
• n = molecule density = P/(kT)
• L = length of ionizing space
• A = cross sectional area of
electron beam
 HCG(6) Ion current
– Ion current is then:

P
= Nq ⋅ σ LA
kT
• N = arrival rate of electrons
• q = charge per electron
– With Nq = ie, we have i+ = P K ie + ir,
– Gauge sensitivity S = K ie
σ LA
K=
kT

– Typical range for K: 0.02 Pa-1 to 0.2 Pa-1 (bigger is better)

Cold Cathode Ion Gauges: CCG(1)
• Cold Cathode Gauge (CCG)
Invented by Penning in 1937 -
electrical configuration like diode
SIP
• 1952 design of wire-in-cylinder
with reverse polarity (+ wire)
provides key performance
improvement
• “Inverted Magnetron” - Magnetic
field produces long helical path for
electrons & ions many collisions
• Ionizing electrons part of self-
sustaining gas discharge
• No background current to mask
the ion current
• Power into CCG ~ 0.1 W
Cold Cathode Ion Gauges: CCG(2)
similar to hot cathode ion gauge
more robust
less accurate
hard to ignite at low pressure
magnet

Hot Cold
 CCG(3)
• “Striking time” is delay
before discharge starts. At
10-4 Pa, ts ~ seconds; at
10-8 Pa, ts ~ hours or days
• Nearly linear dependence
of ion current with
pressure:
ig = KP n ; n = 1.05 − 1.2

• Typical anode voltage +3

kV
• Typical current 0.1 mA
 Pressure Measurement
Convectron Gauge:
Initial pumpdown from
1 atm, and as a
foreline monitor
Thermal Conductivity of Gas

Baratron:
True Pressure
(diaphragm displacement) Insensitive to gas
composition,
Good choice for
process pressures
Ionization of Gas

Ion Gauge:
Sensitive to gas
composition, but
RGA: a good choice for
A simple mass base pressures
spectrometer
Vacuum Gauge Selection adapted from Lesker.com
 Residual gas analyzers

• More compact with higher sensitivity.

• Gaseous ions formed in ion source box by
electron bombardment, extracted with
suitable fields, separated in analyzer and
then collected and measured.
• Magnetic sector analyzer: masses
separated by static magnetic and electric
fields.
• Quadrupole mass analyzer: masses
separated in oscillating quadrupolar electric
field.
 Mass Spectrometry
• Quadrupole Mass Spectrometry
– Most commonly used in laboratories
• Least expensive of commercially available mass
specs
• Detects up to 100 AMU commonly
• Can be extended easily to 300 AMU detection
• Downside: fragmentation patterns of molecules
can be complex
• Upside: the simplest and least expensive mass
spec (typically $15,000 to $35,000 depending on
attachments; other types of mass specs can easily
cost a few million)
 Analyzer: Quadrupole Mass Filter
Ion source: Tungsten filament

Gas inlet
Detector:
Faraday/
Channeltron

Gas
Turbomolecular
outlet Diaphragm Drag Pump
Vacuum Pump
 Mass Spectrometer
Basics

Vacuum Requirements
Ion Creation
Ion Filtering
Ion Detection
Mass Spectrometer Basics
Ion Source

Quadrupole Mass
e-
Filter

Ion Detector
 Vacuum Requirements
e-
• Filament Longevity +
H H
 Ion Mobility

 Detector Operation

Typical Vacuum ~ 1 x 10-6 Torr

Gas Density ~ 1010 molecules /cm3

(@ 760 Torr (1 atm) ~ 1019 molecules /cm3 )

The Atomic Model
12
C = 12 A.M.U.
= Proton ~ 1AMU , +1e charge

= Neutron ~ 1 AMU , no charge

= Electron ~ 0 AMU, -1e charge

1 AMU = 1.66 X 10 -27 kg

The Periodic Table
 Ionization

e-

Atom Ion
12
C + 1e- 12
C+ + 2e-
Ionization Source - Open
Gas Atom

Electron

Gas Ion
Ionization Source - Closed or
Gas Tight
Neutral Gas
Atom/Molecule Filaments
Electron

Ion

Ions Out Gas In

10-05 10-04 10-03 10

Pressure (mBar)
 Electron Emission
The emission of electrons from the filament is
carefully controlled to provide consistent ion
formation.
IF e-
Ion
Formation
Camber

IE

SET

IF =Filament Current ~ 3 Amps d.c.

IE =Electron (emission) Current ~ 1 mAmp d.c.
 Ionization
Double Ionization m/e = 6
1 e- + 12
C
12
C++ + 3e-

Fragmentation - Ionization

1 e- + 18
H2O 1 e- + 17
OH 1 e- + 17
OH
17
OH+ +2 e-

m/e = 17
 Ionization Products
Ionization can produce more than
one ion type.
E.g. Argon , 40
Ar

40
Ar + 1e- 40
Ar+ + 2e- (m/e = 40)

40
Ar2+ + 3e- (m/e = 20)

40
Ar3+ + 4e- (m/e = 13.3)
 Ionization - Isotopes
Argon Isotopic
Masses
P=Proton, N=Neutron
18P+22N=40AMU -1e

Log (Intensity)
18P+20N=38AMU -1e

18P+18N=36AMU -1e M/Z

Ionization Products – UHP
Argon
Mass scan of ultra pure argon - showing singly and doubly
charged isotope peaks
 Ionization Products
Molecules can fragment in the
ionization process.
ABC + e- ABC+ + 2e-
AB+C+ + 2e-
AB+ + C + 2e-
A + BC+ + 2e-
A+ + BC + 2e-
AC+ + B + 2e-
AC + B+ + 2e-
In addition to the above it is possible for other combinations to be formed
 Typical Ion Formation
Spectrum of CO2 showing the 11 most
intense ions
Natural
Abundances

18
O = 0.2%

13
C = 1.1%
 Mass Filter

• Cylindrical Rods.
• Stainless Steel or
Molybdenum.
•Opposite Rods are
Connected Electrically.
+ - •Alignment is Critical
not adjustable.
- +
U + V cos wt
 Mass Filter
y
z

QUADRUPOLE ROD x
ION SOURCE

QUADRUPOLE ROD + + e-
+ + +
++
+
+ + +
QUADRUPOLE ROD
SEM

Lower m/e ion - deflected in y-axis

Ii
+ Higher m/e ion - deflected in z-axis
Selected m/e ion - reaches detector
 Resolution

10

Valley height
1

1 AMU 1 AMU 1 AMU

Over Resolution 10% Valley Under Resolution

Resolution
 Ion Detectors -
Faraday
Ii
e-

I i ~ 10-14....10-9 A
= Selected ion - positive charge

Indestructible Detector but gain = unity.

Cannot detect small ion currents <10-14 Amps.

(Limit depends on electrometer only)
 SEM Detector – Continuous
Dynode
MASS FILTER
GAIN ~ 100 106
set by SEM VOLTS

SEM
= Selected ion - positive charge- VOLTS
e-
attracted into SEM by -ve dc volts. ~ - 1500V dc

Ii
e-
Can be destroyed by high currents
>10-5 Amps , or by operation at high
pressure. I i ~ 10-14....10-5 A
SEM Detector – Discrete Dynode
Deflection Unit
Faraday
signal
MASS FILTER

Vdef

HV- Ie
 Data acquisition modes -
Scan Analog

Here a range of masses are scanned and the data appears as

mass vs. intensity. This mode is mainly used for diagnostics
and checking mass spec performance, peak shape etc.
Data acquisition modes - Scan Bargraph

This mode is similar to Analog but it only reports data when a mass
peak is found - this reduces the data for simplicity.
This mode is mainly used for scanning for unknown components.
 Data acquisition modes - MID, MCD
MID = Multiple Ion Current
Determination.
Ion current vs. time

MCD = Multiple Concentration

Determination.
Concentration vs. time

NOTE:
Requires calibration
gas mixes

MID/MDC - here the masses to be monitored are known and the

system will only report back these points. It is the fastest mode and
very useful for trending data over time
Residual Gas Analyzer

QUADRUPOLE
HEAD

CONTROL UNIT
How the RGA works
 RELATIVE INTENSITY
RGA SPECTRUM

NORMAL (UNBAKED)
H2 O SYSTEM

(A)
H2 N2,, CO
CO2

MASS NUMBER (A.M.U.)

 RGA SPECTRUM

N2
RELATIVE INTENSITY

SYSTEM WITH
AIR LEAK
H2 O
(B)
O2
H2 CO2

MASS NUMBER (A.M.U.)

The RGA 100 Residual Gas Analyzer
Quadrupole Mass Filter
Components
Principles of Filter Operation
Residue Gas Analyzer (RGA)
A small quadrupole mass analyzer with an electron impact ionizer

With electron multiplier, sensitivity ~ 10-15 torr

Residual Gas Analysis
Residual Gas
Analyzers
 Learning Objectives
• Identify the 3 primary components of an
RGA and describe the available options
for each component
• Describe three performance parameters of
an RGA and factors that influence the
performance
• Describe the operation of the RF
quadrupole
 RGA Components
• Ion source
– Open ion source
– Closed ion source
• Mass filter (analyzer)
– Magnet sector
– RF quadrupole
• Ion current detection system
– Faraday cup
– Electron multiplier
 Ionization
• Ion production of each
species is proportional to
its density or partial
pressure
– but sensitivity and gain
are not independent of
mass
– Linear dependence on
partial pressure holds
true up to total
pressure of ~ 10-3 Pa
• Ionization voltage typically
70 volts
• Ionization products can be
single or double ionized
molecules, or fragment
ions
 Ionization Sources
• Open Ion Source
– Like the Bayard-Alpert gauge
– High conductance of ion formation region to analyzer region for
composition consistency
– Grid at (+) potential w.r.t. analyzer: defines ion energy
•
5­15 V quadrupole, 100­1000 V magnet sector
 Ionization Sources
• Closed Ion Source
– Process gas flows through ionization region
– Higher pressure in enclosure enables increased sensitivity
(10 to 100 times higher pressure in ionization vs. analyzer
region)
– Avoids effects of electron stimulated desorption (ESD) from
walls when sampling high-pressure chambers
 Mass Analyzers
• Separate ions according to ratio of M/q
 40Ar++ and 20Ne+ produce identical signal
• Magnetic Sectors
– As seen in the helium mass spectrometer
– Separation angles of 60º, 90º, 180º are common
– Mass sweep via acceleration voltage change limited to x25
– Electromagnetic change (0-0.25T) enables 1-100 amu
sweep
Relative Intensity

M/q
 Mass Analyzers
• RF Quadrupole
– Two pairs of rods, one (+) pair, one (-) pair
– DC plus AC(rf) potentials applied to all rods:
• (+) pair: U + V cos ω t
• (-) pair: −(U + V cos ω t)
– (+) pair creates ion valley most of the time: high mass, high
inertia molecules pass through
– (-) pair creates ion hill most of the time: low mass, low inertia
molecules pass through
 Mass Analyzers
• RF Quadrupole (cont.)
– The width of the band pass,
or resolving power (M/∆M),
is adjusted via ratio of U/V,
length of the rods, or ion
energy
– Resolving power measured
by peak width at 10% height
– Detector on axis at the end
of the filter counts the
transmitted ions
– Linear sweep of rf & dc
potential produces linear
sweep of amu’s
 Ion Detectors
• Ion current, in, sensitivity S’n and partial pressure Pn are related by in
= S’n Pn
– Sensitivity determines smallest detectable signal (peak height)
– Typical sensitivity for nitrogen: S’n = 5x10­6 A/Pa
• Faraday cup
– Measures electric current flowing to neutralize ion arrival
– Incorporates means to avoid secondary electron release
– Should be followed by stable, low-noise, high-gain FET amplifier
– Commercial detector limit of 5x10-14 A (10-8 Pa, or 106 ions/sec)
– Higher sensitivity (down to 10-12 Pa) requires an electron
multiplier
 Ion Detectors: Electron Multiplier
• How does it work?
– Secondary electrons from ion impact generate multiple
electrons upon each successive impact as they are
accelerated toward the anode
G = G1G2 n
• Gain
# electrons generated by ion impact
– G1 =
# electrons generated by electron impact at each stage
– G2 =
• Inlet voltage typically -2000 V
• Glass tube is curved to prohibit (+) ions generated at anode
from traveling back full length of tube and generating out-of-
phase secondary electrons
 Operation
• Mount a valve between RGA and chamber
• Mount the RGA in a non-remote location
• If pressure > 10-3 Pa:
– reduce electron multiplier voltage
– use simple Faraday cup
– use differentially pumped sampling configuration
• If spectrum changes when ion energy is varied, then ESD is present
(reduce ion energy)
• Select appropriate filament (ThO2, W, Re) and precondition it by
heating above normal operating temp.
• Turn off any Bayard-Alpert gauge
• Save background spectrum for later comparison
 Calibration
• Do not accept partial pressure results
unless instrument has recent
calibration for several useful gas
mixtures
• Calibration procedure standards
available from AVS
• Pulse injection method (quick, in-situ
method)
– Isolate small quantity of gas in
pipe (volume Vi, pressure Pi )
between two valves
– Calculate instantaneous pressure
rise in chamber Pc = (PiVi/Vc)
– Determine sensitivity from peak
ion current at t=0
I peak I peakVc
S' = =
Pc PiVi
 Did you catch it?
• Identify at least 3 important features of an RGA
» Range (1-800 amu)
– Sensitivity (10-5 A/Pa, G ~ 106, 10-12 Pa)
– Resolving power (1 amu)

• Identify the approximate voltage between each of these stages:

– Electron filament and grid
– Grid and quadrupole analyzer
70 volts
– Ion detector inlet and ground
5 ­ 15 volts

­2000 volts
 Gauge Operating Ranges
Ultra High
High Vacuum Rough Vacuum
Vacuum
Bourdon Gauge
Capacitance Manometer
Thermocouple Gauge
Pirani Gauge
Hot Fil. Ion Gauge
Cold Cathode Gauge
Residual Gas Analyzer
McLeod Gauge
Spinning Rotor Gauge

10-12 10-10 10-8 10-6 10-4 10-2 1 10+2

P (mbar)
 Vacuum gauges must
calibrated by
• Comparison with absolute standard
calibrated from its own physical properties.
• Attachment to calibrated vacuum system.
• Comparison with calibrated reference
gauge.