rga’s for vacuum diagnostics and - vacuum-uk.org · 2 outgassing measurements /...
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RGA’S FOR VACUUM DIAGNOSTICS AND OUTGASSING MEASUREMENTS
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Outgassing measurements / Vacuum-Diagnostics
P*V = Q (amount of gas included in a vacuum-chamber)
dQ/dt = - Seff*Pressure (Seff effective pumping speed)
P = P0 * exp (- (Seff/V)*t)
[Seff/V] = s-1 vacuum time constant
Start with a very simple picture:
Why Vacuum-Diagnostics?
Dr. Günter J. Peter Coventry Oct 2014
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20 40 60 80 100 120
0.0
2.0x10-5
4.0x10-5
6.0x10-5
8.0x10-5
1.0x10-4
Volume of the chamber = 1'000 liters
Effective pumping speed = 100 l/sec
P = Po * exp(- (V/
Seff)*t)
5*10-10
mbar ???
Pre
ssu
re[m
ba
r]
Time [ seconds]
what happens in reality
Basic calculations are right, every time, however,…
Outgassing measurements / Vacuum-Diagnostics
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That’s what we might get in
reality.
both curves start at approx. same time
Outgassing measurements / Vacuum-Diagnostics
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Pump-down curve:
time / arb. units
pre
ssu
re /
arb
. u
nit
s l
og s
cale
base pressure of the pump
theory 1st order approximation
desorption, leak, permeation
Preal
Preal = Q(desorption,permeation,leak) / Seff
Outgassing measurements / Vacuum-Diagnostics
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Just to save time to start a process
The influence of the residual gas on the
result
Sometimes the residual gas even can have a
negative impact on the whole equippment.
Motivation: Why?
Outgassing measurements / Vacuum-Diagnostics
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This is an issue since decades!
Outgassing measurements / Vacuum-Diagnostics
I like to show this old equippment. It’s delivering valuable results since decades and physics
doesn’t change.
elevated temperature
possible sensor too.
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Outgassing measurements / Vacuum-Diagnostics
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Outgassing measurements / Vacuum-Diagnostics
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Outgassing measurements / Vacuum-Diagnostics
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1. Introduction
2. RGA’s for UHV / XHV
3. Outgassing Measurements Basics
Partial Pressure Gauges
Calibration, Limitations
4. Examples for routine measurements
(In situ cleaning and endpoint detection are out of the scope
of this talk. We are willing to discuss such applications later.)
Agenda:
Outgassing measurements / Vacuum-Diagnostics
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0 20 40
0.00E+000
1.00E-010
2.00E-010
3.00E-010
4.00E-010
C
H2
CO2
CO
pressure = 1.5*10-11
mbar
Residual Gas SpectrumS
ign
al S
EM
-cu
rren
t
mas number [amu]
Outgassing measurements / Vacuum-Diagnostics
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0 10 20 30 40 50
0.00E+000
5.00E-011
1.00E-010
1.50E-010
2.00E-010
2.50E-010
3.00E-010
The signals at mass 16 and 19 are clearly identified as EID-Ions
The fact that there is still nitrogen and argon in the residual gas
spectrum indicates a leak!
However at an integral leak test no leak could be detected;
the conclusion is that there is a very small virtuel leak.
N2
+
at a total pressure of 1.5*10-11
mbar
F+
O+
Ar+
N+
Virtuel Leak
CO2
+
CO+
H2
+
Inte
nsity [S
EM
cu
rre
nt]
mass number [amu]
Outgassing measurements / Vacuum-Diagnostics
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Specs for such «RGA’s»
• bakeout temperature 4000 C
• detection limit < 5*10-15 mbar
• outgassing rate < 10-10 mbar*l*S-1
• radiation resistivity / screening of the
electronics
Outgassing measurements / Vacuum-Diagnostics
more details see, Partial Pressure Gauges CAS proceedings 16-24
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The outgassing rate of the test-chamber has to be
low compared to the outgassing rate to be determined.
clean (UHV) environment without sample is required?
P = Q / Seff
Low pumping speed to achieve a high pressure
mass spectrometer to be operated below 10-5 mbar
adjust the pumping speed?
Outgassing measurements / Vacuum-Diagnostics
General Remarks
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Partial pressure = Qpartial / Seff
Example: 1.0*10-4 mbar*l*s-1 and Seff = 500 l*s-1
P = 2.0*10-7 mbar
If the base pressure of the pump << 10-7 mbar,
and if the outgassing of the chamber is
lower than the outgassing of the sample, then
this can be measured.
Outgassing measurements / Vacuum-Diagnostics
General Remarks
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Model spectrum (Origin of peaks)
0 5 10 15 20 25 30 35 40 45 50
m/e
Hydrogen Nitrogen Oxygen Water
Carbon dioxide Argon Carbon monoxide
nature isn’t always kind!
Outgassing measurements / Vacuum-Diagnostics
Some use generic factors for calibration, from where does the computer know that it’s only
N2 detected at mass 28???
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Calibration is required anyway.
Question is what can be calibrated how far?
Outgassing measurements / Vacuum-Diagnostics
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Outgassing measurements / Vacuum-Diagnostics
Test-Gas
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Outgassing measurements / Vacuum-Diagnostics
Test-Gas
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Outgassing measurements / Vacuum-Diagnostics
Oops! What happened? Ar/Xe = 174.0 previous and 82.1 now
Test-Gas
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Outgassing measurements / Vacuum-Diagnostics
Ar/Xe = 174.0 previous and 82.1 now???
Our mass spectrometer are very stable in terms of mass resolution,
mass scale and sensitivity.
In order to demonstrate what might happen, I just changed the
mass-resolution settings *) for the next spectrum recorded.
-> mass resolution might be (is) rather different from RGA to RGA
and the sensitivity too.
Calibration is essential !
*) The change in resolution settings isn’t obvious from the peak-width at all. However, it caused a factor of
two change.
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Outgassing measurements / Vacuum-Diagnostics
Residual Gas:
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Task:
measure outgassing rates Q := mbar*liter*S-1
RGA: used for partial pressure measurement (after clever calibration)
P = Q / Seff effektive pumping speed and pressure have to be known
The base-pressure has to be a factor of 100 lower to avoid systhematic errors.
Outgassing measurements / Vacuum-Diagnostics
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Sensitivity of an RGA depends on the gas measured
Interferences (for example m/e= 28 can be N2, CO, fraction of CO2,…
Transmission through the mass-filter
Rem. The outgassing rate of a «normal RGA’s» is about 10-8 mbar*L*S-1
Outgassing measurements / Vacuum-Diagnostics
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Seff the effective pumping speed depends on the gas
S is proportional to (m)-1/2 m = mass of the gas, molecular flow
Use an orifice to throttle the (turbo) pump
Outgassing measurements / Vacuum-Diagnostics
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Sensitivity?
The ionisation cross section versus electron
energy for various gases can be found in text-
books.
Same problem as with an ionisation gauge to be
corrected for different gases.
Outgassing measurements / Vacuum-Diagnostics
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Test-Gas-Mixture : 10% He, 10% N2, 40% Ar, 10% Kr, 10% Xe
Outgassing measurements / Vacuum-Diagnostics
He N2 Ar Kr Xe
contend % 10 10 60 10 10
mass number 4 28 40 84 129
(m)1/2 2.00 5.29 6.32 9.17 11.36
expected partial pressure ratio 20.00 52.90 379.20 91.70 113.60
ionisation efficiency N2 set to 1.0 0.15 1.00 1.20 1.00 2.40
expected signal ratio 3 52.9 455.04 91.7 272.64
measured signal ratio ? ? ? ? ?
---> transmission versus mass
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With this information the results achieved with the «green mass spec» can be
compared with the «red one».
Outgassing measurements / Vacuum-Diagnostics
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calibration of the mass-spectrometer:
Seff at the place of the result = ampere/mbar*l*s-1
sensor has to be known. and with a different Seff, you’ll
get another result.
Both calibrations are gas-specific and there can be a pressure gradient
Inside the test chamber. Seff has to be known anyway for transferable
results.
Outgassing measurements / Vacuum-Diagnostics
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Outgassing measurements / Vacuum-Diagnostics
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Outgassing measurements / Vacuum-Diagnostics
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Outgassing measurements / Vacuum-Diagnostics
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Outgassing measurements / Vacuum-Diagnostics
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Outgassing measurements / Vacuum-Diagnostics
From a test-protocoll of an RGA used
In XHV-applications
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Outgassing measurements / Vacuum-Diagnostics
The RGA has to be calibrated:
Sensitivity A/mbar for an inert gas (Argon)
Transmission versus mass number - precisely speaking : The
ratio for He, N2, Ar, Kr and Xe can be determined.
Then the spectra recorded with various instruments can be
compared.
Spectra still have to be interpreted, because of complex
interferences, «fingerprints» of complex molecules.
Recommendation: create own libaries for specific compounds
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Thank you!
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Outgassing measurements / Vacuum-Diagnostics
The time intervall after re-calibration of the
RGA is required, rather depends on the specific
instrument used and the application as well.
No general advice can be given.
Best practise: Start with a short intervall.
After some time you know,
whether a longer intervall is ok.
I personally check the instrument sometimes routinely after a few month.
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Thank you again!