Working with Ultra High Vacuum

(UHV) Equipment
Matthew Marcinkowski
Group Meeting
January 23, 2017
Sykes Lab UHV Instruments

LT-STM VT-STM

3 TPD
Chambers
 Outline
• Installation

• Pumping Down

• Bakeouts

• Experiments

• Venting
 Outline
• Installation

• Pumping Down

• Bakeouts

• Experiments

• Venting
 Installation-Cleanliness

Use clean tools.

Wear gloves!

Work on clean aluminum foil.

Cover any chamber openings with foil and red plastic covers.

Finger prints outgas at the rate of 1 X 10-5 Torr

Liters per second! Leaving finger prints on UHV
components may prevent the chamber from
pumping to a low enough pressure. The same
goes for anything else that may leave oil on a UHV
component.
 Installation-Materials Selection
• Materials for use in UHV need to have a low rate of outgassing.
 Installation-Materials Selection
• Materials for use in UHV need to have a low rate of outgassing.
 Installation-Materials Selection
• Materials for use in UHV need to have a low rate of outgassing.
Installation-Conflat Flanges
 Installation- Take Care of the
Instrument!
• Take extra care when handling fragile components!

• Knife Edges

• Bellows

• Feedthroughs

• Wobblestick!

• Small parts including such as sputter gun components.

 Outline
• Installation

• Pumping Down

• Bakeouts

• Experiments

• Venting
 Pumping Down
• Procedure is slightly different for each instrument.

• It is important to follow procedure to avoid damaging pumps, valves,

or other equipment on instrument.

• Generally pumping down involves turning on pumps and opening

valves in correct order.

Rotary pump brings you to rough vacuum. Turbo Pump Brings you to High
Monitor the pump down from the
Monitor this stage with a pirani gauge. Vacuum Regime
high vacuum regime with an ion
(Pre-Bake)
gauge
Pumping Down-Gas Loads
Pumping Down-Curve
 Leak Testing- Rate of Rise

• Shut vacuum chamber off from all pumps and monitor the rise in pressure.

• Helps to identify if a leak is present.

Leak Testing- Residual Gas Analyzer (RGA)

Turbo pumped chamber not baked. Turbo pumped with a leak.

Contaminants- RGA

Chamber contaminated by
hydrocarbons.
Leak Testing- Methanol Leak Test

• Useful for detecting large leaks

(Pressure isn’t going below 1 X 10-6
mbar).

• Squirt methanol onto suspect flanges.

• If there is a large leak methanol will be

sucked into the chamber and the
pressure will increase.
Leak Testing- He Leak Test
• Can detect much smaller
leaks.

• Spray helium gas onto suspect

flanges (helium is lighter than
air, start high end low).

• Using an RGA monitor mass 4.

• When a flange with a leak is

exposed to the gas the RGA
signal will increase.

• Often RGAs have a leak

detection mode with audio
cues.
 Test Equipment after Pump Down
• Before baking it is best to make sure everything you installed or was
previously on the instrument is working/still working.

• Not everything can be fully tested before a bake, but it is best to test
anything that can be.
• Sputter gun!

• Sample heaters, thermocouples

• Mass Specs

• Electrical connections on TSP, EFMS, ect.

 Outline
• Installation

• Pumping Down

• Bakeouts

• Experiments

• Venting
 Bakeout

• Eventually you can reach UHV by pumping overtime with a

turbo pump, but baking significantly speeds up the process.
 To Prepare for a Bakeout
• Remove all non-bakeable items from the chamber
• Plastics
• Electronics
• Magnets
• Sample tubes
• Anything on the instrument table
• Blow out any water lines
• Pump behind leak valves
• Wrap any fragile components in foil. This will allow these parts to
heat up more gradually and not undergo as much strain from heating.
• Windex the chamber
• Attach heaters and thermocouples to the chamber
• Have someone else check your work!
 During a bakeout
• Ensure you have performed all
steps on the previous slide
including having someone else
check your work!

• Cover the chamber using the

appropriate bakeout apparatus.

• Turn on heaters.

• Closely monitor temperature and

pressure. Too high of a
temperature can damage
components (we typically do not
go above 120 °C) and if they
pressure is too high this may
indicate a leak that was missed.

• Pressure should initially increase as

species are outgassed and then
decrease as bake continues. Bake
at least 36 hours or until pressure
decrease levels off.
 Post Bakeout
• Ensure heaters are turned off and remove bakeout apparatus.

• Replace non-bakeable components

• Test all components post bakeout.

• Your pressure may still not be below 10-9 , but that’s ok. You still need to

• Degas any filaments or relevant components (MS, EFMs, IG, TSPs, ect). Filaments tend to
adsorb gases very strongly and need to be locally heated to temperatures higher than
that achieved in a bakeout.

• Start using additional pumps post bake to further improve the pressure (TSPs, Ion
Pumps, Cryopumping).
Post Bakeout-RGA
 Outline
• Installation

• Pumping Down

• Bakeouts

• Experiments

• Venting
 Performing Experiments- Safety

• Be safe! First and foremost for yourself and also for the chamber.
• Wear gloves, eye protection when handling chemicals including cryogens.
• Be mindful of high voltage components
• Take appropriate pre-cautions when handling hazardous gases (CO, H2 especially).
• Treat components of the UHV system with care especially fragile ones. (Manipulators,
any moving parts especially wobblesticks!, feedthroughs, bellows, scanners in STMS!,
Mass Specs, XPS, basically any expensive component ect.)
• Always keep an eye on the chamber pressure.
• In the STM chambers be mindful of when you should be using the ion pumps or the
turbo pump.
• Do not attempt any maintenance when the system is at cyrogenic temperatures.
• Do not flash the TSPs when the chamber is at crygogenic temperatures.
• In TPD chambers especially flashing TSPs at the end or beginning of the day can help to
keep your pressures low.
• In general think and come up with a plan before you do something to ensure you won’t
hurt yourself or break something in the chamber!
 Performing Experiments-Records

• While you are performing experiments you

should be updating the lab notebook as you
work. The notebook should at least be updated
when you finish with the instrument for the day.

• Do not take the notebooks out of the building.

Make copies if you need to look at your notes at
home.

• Make sure to save your data as you work.

• Data should be backed up frequently on the

N:Drive in the folder for the appropriate
instrument in the Data folder.
 Typical Procedure for UHV Experiments
• Clean sample with Ar+ sputtering. This removes gases adsorbed from
the background or contaminants from previous experiments.

• Make any modifications to the sample if applicable (metal deposition,

form an oxide ect.)

• Dose molecule of interest if applicable.

• Perform measurement (TPD, STM, XPS, IR, ect).

• If the sample is unchanged by the molecule or measurement

continue to perform doses and measurements. Otherwise repeat
from the beginning.
 How do Power Outages Affect Experiments?

• The TPD 1 and 2 are on Uninterrupted Power Supplies (UPSs) which

are further plugged into the backup generator.

• If power is lost to your chamber each instrument has a procedure

for safely pumping the instrument back down. It is important to
follow the appropriate sequence of events and not allow a pump or
valve to open too early.

• Be wary of potential pressure differentials when reopening valves

and turning on pumps.

• If there is a planned power outage it is often better to shut down

the equipment in a controlled manner rather than let the power
trip everything off.
 Outline
• Installation

• Pumping Down

• Bakeouts

• Experiments

• Venting
 Venting
While a vacuum chamber usually becomes unavoidable at some point, it
should not be done without good reason. It is very easy for equipment
to break during vents and the subsequent pump downs and bakeouts.

• Venting is often necessary when a require component stops working

(ie sputter gun, thermocouples on TPD, ect).

• Venting is sometimes necessary to install new components.

• Vents can sometimes be avoided by over pressurizing with Ar.

• Think about experiments you can do without the broken or new

component before venting. For example if your EFM for metal
evaporation stops working are there experiments you can do on the
pure crystal surface before venting?

• Vents can sometimes be planned around planned power outages.

 Venting-Procedure
Again, this is different from instrument to instrument but the following
general procedure can be applied to each instrument.

1. Turn off all components that should not be exposed to high

pressures such as ion gauges.
2. Seal the chamber off from all pumps using valves or by shutting off
ion pumps.
3. Shut down remaining pumps in a controlled manner. For example
shut off the turbo pump in the TPDs before turning off the backing
rotary.
4. Vent any backing lines to air.
5. There is a vent valve somewhere on each chamber. Attach plastic
tubing to this valve and insert it into a dewar filled with LN2. Slowly
open the vent valve to vent the chamber to N2 gas. This limits the
exposure of the chamber to air.
6. Once the chamber and backing line is vented you can begin to
perform maintainance/ install new components.