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Cleaning for Ultra- High Vacuum (UHV)

Cleaning for Ultra- High Vacuum (UHV)

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<strong>Cleaning</strong> <strong>for</strong> <strong>Ultra</strong>-<br />

<strong>High</strong> <strong>Vacuum</strong> (<strong>UHV</strong>)<br />

Keith Middleman<br />

<strong>Vacuum</strong> Science Group<br />

ASTeC<br />

CCLRC Daresbury Laboratory


Outline of Presentation<br />

• <strong>UHV</strong> Limiting Factors<br />

• Why Do We Need To Clean <strong>for</strong> Accelerators<br />

• Methods to Reduce Outgassing<br />

• SRS <strong>Cleaning</strong> Procedure<br />

• Methods of Testing<br />

• Search <strong>for</strong> New <strong>Cleaning</strong> Solvents


Limiting Factors <strong>for</strong> achieving <strong>UHV</strong><br />

• Material Choice<br />

• Gas Sources<br />

• Contaminant: prevents vacuum system reaching required base pressure or<br />

introduces unwanted species into the residual gas.<br />

• Outgassing: The outgassing rate is the time-dependent rate at which gases<br />

and vapours are released under vacuum. This limits the ultimate pressure<br />

achievable and can introduce contamination into the vacuum system.


Why Clean <strong>for</strong> Accelerator <strong>Vacuum</strong> Systems<br />

• <strong>UHV</strong> Total Pressures Required ~ 1x10 -9 mbar<br />

• Maintain Satisfactory Lifetime Stored Electron Beam<br />

• Electron Scatter ∝ Atomic Number 2<br />

• Low presence of high mass species<br />

• Hydrocarbons < 0.1% Pump Lubricants < 0.01%<br />

• Stimulated desorption<br />

• Electron or Ion induced - Major gas source<br />

• Desorption Yield (Number of molecules per incident photon)<br />

• Maintain Clean In-<strong>Vacuum</strong> Surfaces<br />

• Prevent Particle Target Poisoning<br />

• Maintain Efficient Optical Properties <strong>for</strong> EM Radiation Transport


Methods to Reduce Outgassing<br />

• Bakeout - If the pressure is not low enough we can<br />

reduce the thermal outgassing rates by reducing the<br />

surface coverage N or the temperature T.<br />

• Beam <strong>Cleaning</strong><br />

• Passivation<br />

Oxide films<br />

Nitride coatings (TiN, BN)<br />

Active films (NEG coatings)


Methods to Reduce Outgassing<br />

• <strong>Ultra</strong>sonic <strong>Cleaning</strong> - widely used<br />

• Glow discharge<br />

• Electropolishing


SRS <strong>Cleaning</strong> Procedure<br />

CLEANING PROCEDURE<br />

EX-SITU BAKEOUT<br />

• Hot water jet with detergent<br />

• Surface stripping with alumina<br />

beads<br />

• <strong>Ultra</strong>sonic wash in hot Triklone<br />

• Vapour Wash in hot Triklone<br />

• Rinse with de-min water<br />

• Immerse in hot alkaline bath of P3-<br />

Almeco 36 at 60°C<br />

• Rinse in de-min water<br />

• Dry in warm, dust free air, bag and<br />

seal.<br />

• Leak check (< 10 -10<br />

• Bake to 250°C <strong>for</strong> 24 hours<br />

• Record RGA scan<br />

mbar l s -1 )<br />

Effective pre-treatment<br />

ensures outgassing rates<br />

are reduced to < 10-11 mbar<br />

l s -1 cm -2


<strong>Cleaning</strong> Facilities<br />

Water Jet and Detergent Phase


<strong>Cleaning</strong> Facilities<br />

Vapour wash


Testing - Is it ‘Clean’<br />

• Surface Analysis Techniques (Detailed Surface Composition)<br />

• AES - Auger Electron Spectroscopy<br />

• SIMS - Secondary Ion Mass Spectrometry<br />

• Scanning Electron Micrograph<br />

• Phenomenological Testing (Surface <strong>Vacuum</strong> Per<strong>for</strong>mance)<br />

• Measure Total Outgassing Rates - Total Pressure Gauge<br />

• Measure Partial Pressures - RGA<br />

• Stimulated Desorption (Friction, Electron or Ion Induced, Thermal)


Replacement of 1,1,2-Trichloroethylene<br />

• Why Change - Reclassification of 1,1,2-Trichloroethylene (Trike TM )<br />

• What is important to us - Thermal outgassing and ESD<br />

• Throughput method of measuring outgassing rates<br />

Q<br />

=<br />

P1<br />

− P2<br />

A<br />

⋅C<br />

• Comparative Tests - existing procedure proven <strong>for</strong> 20 years


Outgassing Measurement Facility


Thermal Outgassing Results<br />

Experiment In<strong>for</strong>mation<br />

Thermal Outgassing Rate<br />

Q (mbar l s -1 cm -2 )<br />

Blank Run<br />

No Contamination Cleaned with Trike<br />

Full Contamination. Cleaned with Trike<br />

Full Contamination. Cleaned with Lenium<br />

Full Contamination. Cleaned with Leksol<br />

Full Contamination. Cleaned with Novec HFE<br />

Full Contamination. Cleaned with IPA<br />

Full Contamination. Cleaned with Micro 90<br />

Full Contamination. Cleaned with Lancerclean<br />

9.3E-14<br />

7.9E-13<br />

9.3E-13<br />

2.8E-12<br />

9.3E-14<br />

7.5E-13<br />

7.5E-13<br />

3.7E-13<br />

4.6E-12


RGA Data - Thermal Outgassing<br />

Acceptable <strong>UHV</strong> Scan<br />

Hydrocarbon < 0.1%<br />

Pump lubricants < 0.01%<br />

Unacceptable <strong>UHV</strong> Scan<br />

Hydrocarbon ~ 25%<br />

Pump lubricants ~ 5%


RGA Data - Electron Stimulated Desorption<br />

Desorption Yield ~ 10 -3 molecules / e -<br />

Desorption Yield ~ 4 molecules / e -


Summary<br />

• Accelerators (storage rings) require <strong>UHV</strong><br />

• Need to minimise thermal outgassing and<br />

stimulated desorption<br />

• Requires a detailed cleaning recipe<br />

• Phenomenological Testing

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