A blog on the repair, operation and calibration of surface analysis systems and components including electron spectrometers, sputter ion guns and vacuum related hardware. Click on the Index tab below to see a list of all posts. Visit our website at http://www.rbdinstruments.com
This blog post shows the steps required to install a
monochromator upgrade on a PHI 5600 XPS system.
The components of a monochromator upgrade include the monochromator housing, the crystal substrate and aligner, the mono X-ray source, and the X-ray source aligner. If your X-ray source is a 32-095 then you will need to replace that with a 32-096 that can drive two x-ray sources (standard dual anode and mono source). An additional water line is included to complete the cooling circuit between the standard and mono X-ray sources.
Step by step procedure:
First, vent the vacuum chamber.
Use a new 4 5/8” copper gasket and install X-ray source X Y Z aligner to the monochromator housing. It is much easier to install the X Y Z aligner onto the mono housing before the mono housing is mounted to the chamber.
Use a new 6” copper gasket and Install the monochromator housing to the chamber on the flange that is opposite of the hemispherical analyzer. It is heavy and so you will need at least two people to mount the monochromator housing to the flange on the chamber.
Once mounted tighten the nuts on the flange. In my experience, going in a circular pattern is the best way to tighten flanges on UHV chambers. The trick is to not over-tighten the nuts or bolts as you go around. Start out with just a little bit of torque and gradually increase it as you go around. One or two of the nuts on the back of the monochromator housing are exceedingly difficult to get to. A ½” U-shaped or half-moon wrench makes getting to those nuts easier.
Or you can simply cut a standard ½” wrench in half.
Once the nuts are tight and there is no gap between the flanges it is sealed.
Install the mono crystal substrate into the top mono flange
assembly: Use gloves and very carefully
remove the crystal substrate from its box and unwrap it, being careful not to
touch the crystals. There are 3 recesses
in the crystal block that line up with flat spaces on the mono flange
assembly.
The crystal substrate is held in place with 3 clamps. The clamps mount on a guide screw and then there are two spring loaded set screws that provide tension to hold the crystal substrate in place.
Tighten the set screws to where they just start to tighten up, and then about 1/16” more. Do not over-tighten the set screws. They should be tight enough to hold the crystal substrate in place firmly, but not so tight that the springs inside the set screws are fully compressed.
Next, install a new rectangular Helicoflex type monochromator
gasket into the top of the monochromator housing. It will sit into a recess and
should be centered in the recess.
Put the mono housing shutter in the bakeout position. The chamber will be baked out and so the
shutter will need to be set prior to the bake out. Also, you can see how the shutter works
before the top mono flange is installed.
Install the top mono flange assembly onto the top of the mono housing. This can be done by one person. Make sure that the crystal substrate does not touch the sides of the mono housing as you lower the mono flange assembly. There are two guide pins to hold the mono flange assembly in place. The serial number on the mono flange assembly should line up with the serial number on the mono housing.
Install the bolts into the holes in the mono flange assembly and tighten them. For this flange, use little torque as you tighten the flange in a circular (rectangular) pattern. The bolts are coarse threads and you want to tighten the flange evenly.
Once the bolts are tight and there is no gap between the two flanges then it should be sealed.
Use a new 6” copper gasket and mount the 10-610 mono X-ray source to the 6” flange on the X Y Z aligner and tighten the nuts until there is no gap between the flanges or until the nuts are very tight, which ever comes first.
At this point the chamber can be pumped down and baked out. Make sure that all the housing parts and O-ring seals are removed from the 10-610 mono source prior to bake out.
The pictures below show the components of the 10-610 X-ray source as they are reassembled after the bake out.
After the chamber has been baked out, refer to the 10-610
mono X-ray source and 10-420 monochromator manuals for outgas, operation, and
alignment information.
This post will show how to replace the 10-610 monochromator X-ray source anode and filaments. The 10-610 monochromator X-ray source is used in conjunction with the 10-410 or 10-420 monochromator. When replacing the anode you should also replace both filaments and the deionizer cartridge (located in the 16-0XX heat exchanger).
Once the anode and filaments have been replaced the vacuum chamber needs to be baked out and the new filament and anode need to be out gassed and conditioned. The monochromator may also need to be adjusted slightly to optimize the counts with the new anode and filaments.
Please read the entire procedure first, then watch the picture slideshow at the bottom of the post.
Anode replacement procedure
Vent the chamber.
Remove the water lines from the source.
Remove the safety cover from the source (3 screws).
Remove the high voltage cable
Remove the sixteen 5/16” bolts on the 6” flange and remove 10-610 mono source from the monochromator.
Next, remove the screw that connects the ground wire to the manifold.
Remove the Teflon block from the source base (2 spline cap head screws).
Remove the Teflon block from the source base. Twist it as you slide it off the anode.
Loosen the nut on the high voltage connector (3/4” open end wrench) and remove the high voltage connector.
Remove the silicone rubber insulator and spring. The spring makes electrical contact between the high voltage connector and the anode flange.
Remove the three spline cap head screws that hold the base to the flange and remove base from the flange. Note, this is optional as the base can stay on for bake out.
Remove the two screws that hold the filament cover on and remove the filament cover.
Remove the two screws that hold the filament cover support on and remove the filament cover support. Note the position of the covers as you take them out as they need to go back the same way.
Remove the 6 cap head screws that hold the anode to the base and lift the old anode out of the source housing.
Separate the old anode from the anode flange.
Install a new O-ring on the new anode bottom and slide the anode flange into the new anode. There are 4 O-rings in the anode kit. The anode flange forces the cooling water to the tip of the anode.
Use a new copper gasket and mount the new anode onto the anode flange. Use care as you slide the anode in not to touch the sides of the anode housing (like the old game Operation). The anode surface is coated with a thin layer of aluminum on a copper substrate. Any contact with the top of the anode surface can cause little dents in the anode surface that can cause arc points. Tighten the 6 cap head screws very lightly as the anode will need to be adjusted.
Using plastic tweezers or needle nose pliers, carefully rotate the anode until it is parallel to the filament housing. The idea is that the anode should be parallel to the anode housing and also centered so that there is a maximum and equal distance between the anode and the housing in order to prevent arcing.
Once the anode is parallel, tighten the six cap head screws on the base all the way down.
center the anode
Next, if necessary loosen the 4 screws on the copper pedestal and move it to center the anode for maximum distance between the anode and the filament housing. If available, you can use the anode alignment tool to help center the anode and then tighten the 4 screws on the base of the copper pedestal.
anode alignment tool
The anode surface should be the same level as the fence that is between the filaments and the anode. If not loosen the spline head cap screw that secures the filament housing to the copper pedestal. You can use the anode alignment tool, a straight edge or just eye ball it.
Filament replacement procedure
The filaments are coated with Yttrium so that they can provide sufficient electrons for emission at a lower filament operating current. Be careful when handling the filaments so that you do not knock off any of the coating on the filaments.
Loosen the filament clamp screws on the large 7mm (diffused) area filament and remove the old filament. Note that the large 7mm filament is closest to the filament connector and wires.
Carefully insert the new filament into the filament clamps and lightly tighten them. The filament should be centered with respect to the anode and the top of the filament should be even with the top of the filament cavity (level with the anode guard). It should also be parallel to the anode guard and centered in the filament cavity. If not, remove the filament and carefully bend the legs as needed. Once the filament height and centering is correct, firmly tighten the filament clamp screws.
Repeat this procedure for the small 2mm (focused) filament.
Install the filament cover base and cover. Note that the little cut out goes over the 2mm filament.
Condition the anode and filaments procedure
Once the new anode and filaments have been installed onto the 10-610 monochromator X-ray source, the source needs to be baked out and then outgassed and conditioned.
First, bake out the system.
Next, outgas the filaments
Finally, condition the anode
Bake out the system
Follow the bake out procedure in the PHI manual or search for the RBD Techspot blog- Bake-out procedure to improve base vacuum.
The O-rings on the mono source, HV connector and silicone rubber insulator and Teflon block are all removed from the 10-610 mono source before bake out. After bake out, use a little bit of vacuum grease on the O-rings to help provide a tight water seal when the Teflon block is replaced.
Replace the deionizer cartridge in the 16-0XX heat exchanger. PHI recommends that the deionizer cartridge be replaced each time the anode is replaced to help make sure that the water does not react with the anode.
Outgas the filaments
Prior to outgassing the filaments the system should have been baked out and the mono source housing and water lines reassembled. The deionizer cartridge should also have been replaced. The system should be cool and the base pressure in the low 10-9 to low 10-10 Torr range.
The filaments need to be initially outgassed slowly in order to prevent warping and also to set them.
Select the Outgas/ACT mode on the X-ray source controller.
Select the 2mm focused filament and ramp the current up to 5 amps in increments of .5 amps over a period of 2 to 5 minutes. Wait for the outgassing to subside somewhat as indicated by the ion gauge.
Set the 2mm focused filament current to zero amps and then repeat the procedure with the 7mm diffused filament. Once up to 5 amps, let the 7mm diffused filament sit there for 4 to 8 hours or until the base vacuum returns to the low 10-9 Torr range. Then set the filament current to zero and turn off the Outgas/ACT mode on the X-ray source controller.
Degas the Anode
Set the beam voltage to 500V and turn it on.
On the X-ray source controller, select the Outgas/ACT mode
Select the 2mm focused filament (Mg filament on a 32-095/6)
Slowly increase the amps to 3.5 and then monitor the anode current (emission current) meter.
VERY SLOWY increase the filament current until you get 1mA of emission current. Do not exceed 5 amps of filament current. Do not exceed 2mA of emission current.
Monitor the ion gauge vacuum reading and wait until the outgassing comes back down then slowly increase the beam voltage to 1 kV. If necessary reduce the filament current to keep the emission below 2mA.
In steps of 500V bring the high voltage up to 10kV while adjusting the filament current as needed to keep the emission current below 2mA. Do this over a period of 30 minutes to several hours, depending on how much the anode outgasses. For best results keep the vacuum in the chamber in the low 10-9 Torr range. The higher the pressure from outgassing, the more likely an arc will occur.
Once the anode has been outgassed to 10kV, turn the filament current to zero and set the high voltage to zero. Then switch to the other filament and repeat the procedure.
Condition the high voltage
Make sure that the Out/Act button is OFF and that the filament current is set to zero on both filaments.
SLOWLY bring the high voltage up to 10kV while monitoring the vacuum chamber ion gauge.
Step the high voltage up increments of 500V until you get to 16.5kV. When you see some signs of outgassing (the pressure in the vacuum chamber will come up) then back down the high voltage a little bit and wait until the vacuum recovers.
Once you are able to get to 16.5 kV with no arcing, let the anode sit there for at least 20 minutes.
The X-ray source is now ready for normal operation. For best results, start at a low power and kV such as 100 watts and 10kV. You can step up both the power and the kV over a period of a few hours based on how much outgassing you see when operating in this mode. Once you are up to full power of 300 watts and 15kv the X-ray source can be brought up to full power quickly.
Note that the maximum power that should be applied to the 2mm focused filament is 350 watts and the maximum power that should be applied to the 7mm diffused filament is 600 watts. Personally I do not recommend more than 300 watts on either anode. If you can get by with a lower wattage (such as 250) then both the filaments and anode will last longer.
It is also recommended that you inspect the 10-610 mono anode any time you vent your chamber for maintenance, or at least once a year. If you see indications of melting in the center of the anode you should replace the anode. Otherwise it will eventually develop a water leak and cause potentially catastrophic damage to system components and substantial downtime.
