10-610 monochromator x-ray source anode replacement procedure

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

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

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.

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X-ray source arcing

X-ray source arcing results in unstable XPS data and can also damage the x-ray source power supply or high voltage control.

Typically X-ray source arcing is caused by contamination on the anode, a coated anode support ceramic (the football ceramic) or a loose filament.

However one unseen cause of x-ray source arcing is when the high voltage cable to the x-ray source is not tightened all the way down until it snaps in. The procedure is simple – line up the slot on the cable with the two little tabs on the source connector. Then press down all the way and turn the cable collar clockwise until it snaps in.

On the newer 04-548 15kV dual anode sources this is easy to do as the connector is exposed. But the connector is recessed on the older dual anode sources and all of the mono sources.

To properly connect the high voltage cable on the older dual X-ray sources or a mono source you need to remove the cover on the source so that you can see the connector and make sure that the cable slots line up and that the cable locks down when the collar is turned fully clockwise.

high-voltage-connector-slots

high-voltage-connector-slots

high-voltage-connector-snapped-in

high-voltage-connector-snapped-in

If the high voltage cable is not snapped all the way down then it can arc at higher voltages and damage the cable connector, the source connector, or more typically both connectors.

The pictures below show damaged cable and source high voltage connectors.

melted x-ray source connector

melted x-ray source connector

 

 

burnt x-ray source connector

burnt x-ray source connector

 

Once arcing damage occurs the cable end and or source connector need to be replaced.

RBD Instruments provides the source connector and we can also repair or exchange your cable. Visit our website and look under Parts – Optics – X-ray Photoelectron Spectroscopy Model 04-500 and04-548 X-ray source parts or call us at 541 550 5016

Revised outgas procedure for PHI dual anode x-ray sources and single anode mono sources.

Out-gassing the filaments and conditioning the anode are essential steps needed to remove adsorbed gases from the filament area of any PHI X-ray source.

Recently I have seen a couple of instances where a 10-610 monochromator source was not properly out-gassed and the result was a contaminated anode and very low counts. So degassing the anode is essential for proper operation.

To prevent anode contamination, the anode needs to be degassed per the PHI manual. However I have found that by changing the order of the out-gas procedure steps that the amount of time it takes to out gas the source to full power can be significantly reduced.

The manual states that the out-gas procedure sequence is as follows:

  1. Outgas the filaments
  2. Condition the high voltage
  3. Degas the anode

But from a practical standpoint it makes more sense to degas the anode before conditioning the high voltage. The reason is that a degassed anode is less likely to arc.

So the faster way to out-gas an X-ray source is:

  1. Outgas the filaments
  2. Degas the anode
  3. Condition the high voltage

 

Step 1. Outgas the filaments.

You need to out-gas the filaments after new filaments have been installed or anytime the system has been brought up to air and baked out. For this procedure it is assumed that the system has been baked out. (The only bake out exception is if you have just replaced the 04-303 ion gun ionizer and back-filled the chamber with dry nitrogen).

  1. Turn on the 32-095/096 power.
  2. On the 32-095/6, press the Blue Out/Act out-gas activate button.
  3. Select both filaments
  4. Select the Mg filament (or filament 1)
  5. Slowly increase the amps to 3.5
  6. Select the Al filament (or filament 2)
  7. Slowly increase the amps to 3.5
  8. Let the filaments sit there for a few minutes and then slowly increase each filament to 4.5 amps.
  9. Let the filaments sit at 4.5 amps for a minimum of 4 hours (overnight is best).
  10. After out-gassing for at least 4 hours set the filament current to zero on both filaments and turn off the Out/Act out-gas button by pressing it one more time.

Step 2 Degas the Anode

  1. Set the beam voltage to 500V and turn it on.
  2. On the 32-095/6, press the Blue Out/Act out-gas activate button
  3. Select the Mg filament (or filament 1)
  4. Slowly increase the amps to 3.5 and then monitor the anode current (emission current) meter.
  5. VERY SLOWLY 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.
  6. Monitor the ion gauge vacuum reading and wait until the out-gassing comes back down then slowly increase the beam voltage to 1 kV. If necessary reduce the filament current to keep the emission below 2mA.
  7. In steps of 1kV 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 10 minutes to several hours, depending on how much the anode out-gasses. For best results keep the vacuum in the chamber in the low 10-9 Torr range. The higher the pressure from out-gassing, the more likely an arc will occur.
  8. Once the anode has been out-gassed 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.

Step 3 Condition the high voltage

  1. Make sure that the Out/Act button is OFF and that the filament current is set to zero on both filaments.
  2. SLOWLY bring the high voltage up to 10kV while monitoring the vacuum chamber ion gauge.
  3. Step the high voltage up increments of 500V until you get to 16.5kV. When you see some signs of out-gassing (the pressure in the vacuum chamber will come up) then back down the high voltage a little bit and wait until the vacuum recovers.
  4. 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 out-gassing 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.