Insights into XFEL Cavities Production and Vacuum System Challenges

 
RGAs at the companies during XFEL
cavities production and cavity
performances
 
Paolo Michelato
INFN – LASA
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
General comments on vacuum plants used for
XFEL cavity production
 
 
 
 
Unusual operational conditions: many pumping and
venting operations, in some cases many tens/week.
Consequences and actions
a)
Impact on 
system reliability
, e.g. 
shorter lifetime 
of TMP and
of scroll pumps with respect to usual operative conditions.
 
Service must be done more frequently than foreseen, great
 
attention to precursor of failures (noise, bad vacuum, etc)
 
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
What about RGAs: 2 main effects
 
Companies used quite similar process for cavities production.
Same detergent, similar process for main EP, etc
The two companies used two different firm RGAs and
different w.r.t. the Saclay and DESY ones
Different effects 
were visible in RGA behaviour.
 
a)
In one company “unusual peaks” propagates all over all
RGAs. Peaks are “abnormal 32 mass”, 64, 77, 78, etc
 
a)
In the second company RGA SEM sensitivity large decrease
(at least in one firm, using RGA with MCP electron multiplier).
Sum of the values of pp  doesn't give the total pressure, 
error
could be orders of magnitude!  Signal/noise ratio reduced!
 
Frequent calibration operation or use of RGA as a “percent”
 
meter or ion current meter and normalization is done later.
 
Fixed (partially) using a valve on the RGA.
 
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
Janez Setina, Vacuum Symposium 2011
Well known
 problem!
But not for order
of magnitude in
few months!
Someone had
similar
experience?
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
General comments on vacuum plants used for
cavity production
 
Unusual operational conditions: many pumping and
venting operations, some tens/week.
Consequences and actions
a)
Accumulation of impurities
: all times the system will 
pump a
“new” chamber
, the cavity with its amount of contaminants.
If they are transferred to the vacuum system, for instance
during 800 °C or 120 °C treatment, and 
they have a low vapor
pressure
, 
they could be accumulated on the vacuum system.
Transfer mechanism of these compounds could be intricate,
due to memory effects. Vacuum quality becomes worst.
 
To avoid and / or  control this effect,  a bake out (120°C)
 
could help a lot maintaining the vacuum systems more clean
 
(done in one firm). 
ANY SIMILAR EXPERIENCE IN OTHER
 
LABS?
 
 
 
Rga
No sulfur!
Mass 64?
Phtatales?
Where? Everywhere!
Correlations: no correlations.
Venting EZ Ar 6.0,
Bake out: periodically, typ 1time/week
 
 
 
 
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
SPSV system at the firms for XFEL cavities
 
Both firms use a similar architecture and technique
Dry
 primary pump
Hybrid TMP
 (High compression ratio for He)
Large MFC to control gas throughput in the pumping line
Small MFC for the venting
High quality (6.0) filtered (40 nm) 
gas for venting, Ar or N
2
Diffuser
 on the venting line (3 nm)
Optimized timing strategy for reducing pressure bumps (valves)
RGA
 on the high vacuum side
Dedicated commercial 
He mass spectrometer for leak detection
connected on the TMP discharge line
10
-9
 mbar range 
Cal leak 
(specs leak rate < 1x10
-10
 mbarl/s)
PLC controlled, all data are stored in a server.
 
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
EZ slow pumping slow venting system
Courtesy EZ
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
SPSV system at LASA for the 3.9 cavities
 
Reduced number of cavities: 10 x 3.9 GHz for the
third harmonic system
Different strategy used with respect to usual SPSV: forevacuum
pump is 
stalled 
during first part of pumpdown by the flow
coming through the venting line.
After the 
equilibrium conditions 
are reached (few tens of
seconds, i.e. the same throughput in the pump and in the
venting line, 
no pressure change
) 
the venting MFC start to
reduce its opening and therefore pressure is going
down.
Advantages: reduced pressure bump, MFC are already
operative when the pressure start to decrease.
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
Hydrocarbon free vacuum
, for the XFEL,  is defined when the
ratio
 between the total pressure, as the sum of partial pressures,
and the highest contaminant partial pressure is 
over a factor 1000
.
Drawbacks using this definition
: 
if total pressure is quite low
,
as after the 120 deg heat treatment, the partial pressure of
contaminants is quite low 
as absolute value
, but could be
significant
 with respect to the total pressure (> 1/1000).
Effects of contaminants 
are related to their partial
pressure absolute values 
and not (directly) to their ratio
with the total pressure.
It would means that vacuum 
quality would be better if the partial
pressure of water or mass 28 is higher, maintaining constant the
partial pressure of contaminants!
 
Moreover there is the problem of SEM degradation…
 
RGA and vacuum quality: some comments
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
RGA spectra interpretation and contaminants
 
In one company many spectra 
anomalous mass 32 high
, wrt air
leak (but no leak!)
Mass 64: may be sulfur, but the relative isotopes abundance for
mass 32 and 34 are not in good agreement with mass 64.
Sulfur concentration in the ethanol is quite low
.
Some “unusual” compounds: around mass 50, 58, 78, 79 and 91
Impurities are “
resident
” in the vacuum system: no significant
change of pp opening and closing cavity valve.
 
Sources: in my opinion some low concentration
contaminants that are accumulated in the vacuum system,
that have a low vapor pressure and that are difficult to be
removed.
As for phthalates, long chain alkanes, etc.
Investigation on UPW and ethanol are under way.
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
RGA spectra: sensitivity loss of order of magnitudes
End of 800°C cycle
P TOT: few E-7 mbar
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
RGA spectra: some example
 
At the end of the 120 °C treatment, total pressure  3x10-8 mbar
 
RGA spectra: some example
 
At the end of the 120 °C treatment, the final treatment.  
Total pressure  3x10
-9
 mbar.
Contaminant level is in the 10
-12
 mbar range.
55, 56
64
77, 78
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
RGA spectra: some example
 
Intermediate leak check, after the 800 °C annealing Total pressure: 5x10
-7
 mbar
50 - 58
64
77, 78
32!
91
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
RGA of one of last XFEL cavity, final clean room pumping
before 120 °C
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
RGA of one of last XFEL cavity, during 800°C
 
RGA of one of last XFEL cavity, during 800°C, end of treatment
 
Effects on cavities?
 
Up to now, we are sure that 
trivial problems as vacuum
system malfunctioning, human error, not correct venting
,
etc 
produces dramatic effects on the accelerating field
.
One cavity 
vented with not filtered air 
had shown an
accelerating gradient of 
few MV/m
 while, 
after HPR
, the
cavity was completely restored
.
Up to now, from preliminary investigations, no correlation
had been found between the partial pressure of
contaminants and the cavity performances.
Why differences between two cavities treated together?
Or one just after the other? While differences in the
accelerating gradient 
could be caused by human factor (FE)
what is the reason for Q
 0 
differences also at low field?
Good question…
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
Effects on cavities?
 
Multivariate analysis had shown no correlation between
contaminants peaks (masses 32, 34, 56, 64, 77, 78)  in the last
pumping and 120 °C with respect to cavities performances.
For instance in one company cavities are 120 °C treated two
by two (twins).
Different behavior also between twins cavities.
No correlation between Q
0
 and max field with
impurities.
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
RGA limits EXFEL (change request accepted)
 
 In order to reduce the number of NCRs, we temporary accepted to
change the rule for RGA acceptance.
 
The 
reference pressure is calculated as the sum
 
of the partial
pressures of the main peaks of the spectrum:
Mass 2, Hydrogen
Mass 18, Water
Mass 28, Nitrogen, CO
Mass 32, Oxygen
Mass 40, Argon
Mass 44, Carbon dioxide
 
Change request accepted for EXFEL:
Lowering the required ratio between partial pressure and
reference value from 1:1000 to 1:300
.
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
RGA done at the end of 120°C final treatment
T: room temperature
Tot pressure (BA gauge): 2.9e-9 mbar
Reference pressure: 3e-9 mbar
1:300
1:1000
 
RGA done at the end of 120°C final treatment
T: room temperature
Tot pressure (BA gauge): 3.5e-9 mbar
Reference pressure
1:300
1:1000
Mass 64, spectra at room temperature end of 800°C furnace treatment
 
Mass 64 behavior vs number of treatments. Ethanol change (
blue arrow
), cryopump
cleaning (red arrow), cavity with Ethanol + HPR (brow arrow)
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
 
Treatment #
MASS 64
Mass 64, end of 120°C final  treatment, last spectra at room temperature
 
Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016
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The discussions at TTC Meeting in Saclay shed light on companies' experiences during XFEL cavities production, revealing operational challenges related to vacuum plants and RGAs. The use of different firm RGAs resulted in distinct effects on RGA behavior, affecting signal/noise ratio and calibration operations. Accumulation of impurities in vacuum systems raised concerns about maintaining vacuum quality. Similar experiences and solutions were sought from other labs. The SPSV system utilized by firms for XFEL cavities showed a common architecture and technique, emphasizing dry primary pumps and large MFCs.


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  1. RGAs at the companies during XFEL cavities production and cavity performances Paolo Michelato INFN LASA Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  2. General comments on vacuum plants used for XFEL cavity production Unusual operational conditions: many pumping and venting operations, in some cases many tens/week. Consequences and actions a) Impact on system reliability, e.g. shorter lifetime of TMP and of scroll pumps with respect to usual operative conditions. Service must be done more frequently than foreseen, great attention to precursor of failures (noise, bad vacuum, etc) Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  3. What about RGAs: 2 main effects Companies used quite similar process for cavities production. Same detergent, similar process for main EP, etc The two companies used two different firm RGAs and different w.r.t. the Saclay and DESY ones Different effects were visible in RGA behaviour. a) In one company unusual peaks propagates all over all RGAs. Peaks are abnormal 32 mass , 64, 77, 78, etc a) In the second company RGA SEM sensitivity large decrease (at least in one firm, using RGA with MCP electron multiplier). Sum of the values of pp doesn't give the total pressure, error could be orders of magnitude! Signal/noise ratio reduced! Frequent calibration operation or use of RGA as a percent meter or ion current meter and normalization is done later. Fixed (partially) using a valve on the RGA. Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  4. Well known problem! But not for order of magnitude in few months! Someone had similar experience? Janez Setina, Vacuum Symposium 2011 Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  5. General comments on vacuum plants used for cavity production Unusual operational conditions: many pumping and venting operations, some tens/week. Consequences and actions a) Accumulation of impurities: all times the system will pump a new chamber, the cavity with its amount of contaminants. If they are transferred to the vacuum system, for instance during 800 C or 120 C treatment, and they have a low vapor pressure, they could be accumulated on the vacuum system. Transfer mechanism of these compounds could be intricate, due to memory effects. Vacuum quality becomes worst. To avoid and / or control this effect, a bake out (120 C) could help a lot maintaining the vacuum systems more clean (done in one firm). ANY SIMILAR EXPERIENCE IN OTHER LABS? Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  6. SPSV system at the firms for XFEL cavities Both firms use a similar architecture and technique Dry primary pump Hybrid TMP (High compression ratio for He) Large MFC to control gas throughput in the pumping line Small MFC for the venting High quality (6.0) filtered (40 nm) gas for venting, Ar or N2 Diffuser on the venting line (3 nm) Optimized timing strategy for reducing pressure bumps (valves) RGA on the high vacuum side Dedicated commercial He mass spectrometer for leak detection connected on the TMP discharge line 10-9 mbar range Cal leak (specs leak rate < 1x10-10 mbarl/s) PLC controlled, all data are stored in a server. Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  7. EZ slow pumping slow venting system Courtesy EZ Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  8. SPSV system at LASA for the 3.9 cavities Reduced number of cavities: 10 x 3.9 GHz for the third harmonic system Different strategy used with respect to usual SPSV: forevacuum pump is stalled during first part of pumpdown by the flow coming through the venting line. After the equilibrium conditions are reached (few tens of seconds, i.e. the same throughput in the pump and in the venting line, no pressure change) the venting MFC start to reduce its opening and therefore pressure is going down. Advantages: reduced pressure bump, MFC are already operative when the pressure start to decrease. Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  9. RGA and vacuum quality: some comments Hydrocarbon free vacuum, for the XFEL, is defined when the ratio between the total pressure, as the sum of partial pressures, and the highest contaminant partial pressure is over a factor 1000. Drawbacks using this definition: if total pressure is quite low, as after the 120 deg heat treatment, the partial pressure of contaminants is quite low as absolute value, but could be significant with respect to the total pressure (> 1/1000). Effects of contaminants are related to their partial pressure absolute values and not (directly) to their ratio with the total pressure. It would means that vacuum quality would be better if the partial pressure of water or mass 28 is higher, maintaining constant the partial pressure of contaminants! Moreover there is the problem of SEM degradation Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  10. RGA spectra interpretation and contaminants In one company many spectra anomalous mass 32 high, wrt air leak (but no leak!) Mass 64: may be sulfur, but the relative isotopes abundance for mass 32 and 34 are not in good agreement with mass 64. Sulfur concentration in the ethanol is quite low. Some unusual compounds: around mass 50, 58, 78, 79 and 91 Impurities are resident in the vacuum system: no significant change of pp opening and closing cavity valve. Sources: in my opinion some low concentration contaminants that are accumulated in the vacuum system, that have a low vapor pressure and that are difficult to be removed. As for phthalates, long chain alkanes, etc. Investigation on UPW and ethanol are under way. Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  11. RGA spectra: sensitivity loss of order of magnitudes End of 800 C cycle P TOT: few E-7 mbar Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  12. RGA spectra: some example At the end of the 120 C treatment, total pressure 3x10-8 mbar

  13. RGA spectra: some example 77, 78 55, 56 64 At the end of the 120 C treatment, the final treatment. Total pressure 3x10-9 mbar. Contaminant level is in the 10-12 mbar range. Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  14. RGA spectra: some example 32! 77, 78 50 - 58 64 91 Intermediate leak check, after the 800 C annealing Total pressure: 5x10-7 mbar Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  15. RGA of one of last XFEL cavity, final clean room pumping before 120 C Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  16. RGA of one of last XFEL cavity, during 800C

  17. RGA of one of last XFEL cavity, during 800C, end of treatment

  18. Effects on cavities? Up to now, we are sure that trivial problems as vacuum system malfunctioning, human error, not correct venting, etc produces dramatic effects on the accelerating field. One cavity vented with not filtered air had shown an accelerating gradient of few MV/m while, after HPR, the cavity was completely restored. Up to now, from preliminary investigations, no correlation had been found between the partial pressure of contaminants and the cavity performances. Why differences between two cavities treated together? Or one just after the other? While differences in the accelerating gradient could be caused by human factor (FE) what is the reason for Q 0 differences also at low field? Good question Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  19. Effects on cavities? Multivariate analysis had shown no correlation between contaminants peaks (masses 32, 34, 56, 64, 77, 78) in the last pumping and 120 C with respect to cavities performances. For instance in one company cavities are 120 C treated two by two (twins). Different behavior also between twins cavities. No correlation between Q0 and max field with impurities. Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  20. RGA limits EXFEL (change request accepted) In order to reduce the number of NCRs, we temporary accepted to change the rule for RGA acceptance. The reference pressure is calculated as the sumof the partial pressures of the main peaks of the spectrum: Mass 2, Hydrogen Mass 18, Water Mass 28, Nitrogen, CO Mass 32, Oxygen Mass 40, Argon Mass 44, Carbon dioxide Change request accepted for EXFEL: Lowering the required ratio between partial pressure and reference value from 1:1000 to 1:300 . Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  21. RGA done at the end of 120C final treatment T: room temperature Tot pressure (BA gauge): 2.9e-9 mbar Reference pressure: 3e-9 mbar 1:300 1:1000

  22. RGA done at the end of 120C final treatment T: room temperature Tot pressure (BA gauge): 3.5e-9 mbar Reference pressure 1:300 1:1000

  23. Mass 64, spectra at room temperature end of 800C furnace treatment Mass 64 behavior vs number of treatments. Ethanol change (blue arrow), cryopump cleaning (red arrow), cavity with Ethanol + HPR (brow arrow) Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

  24. Mass 64, end of 120C final treatment, last spectra at room temperature MASS 64 Treatment # Paolo Michelato, TTC Meeting at Saclay, July 5 - 8, 2016

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