Basic Operations Guide Ultima III - V2

 

 

Rigaku D/Max 2200PC Ultima III Basic Operations Guide  Guide 

Manual No. BOG-U3-v2 February 2006

 

Table of Contents Section 1:

Cooling System Maintenance and Operation……………………..…...1-12

Addendum:   Addendum:

Water Quality Documentation……………………………..…………13-15 Documentation……………………………..…………13-15

Section 2:  2: 

System Power-up…………………………………………..…………16-20 Power-up…………………………………………..…………16-20

Section 3:

Configuration of Hardware and Software with Focusing Optics…………………………………………………… Optics………………………………………………………21-30 …21-30

Section 4: 4:  

Automatic Alignment with Focusing Optics………………………....31-45 Optics………………………....31-45 Optional Instrument Configurations

Section 5: 5:  

System Configuration and Alignment with Parallel Beam Optics…………………………………………...…………… Optics…………………………………………...……………..46-60 ..46-60

Section 6: 6:  

System Configuration and Alignment with Focusing Optics and Diffracted Beam Monochromator……………………… Mo nochromator……………………………......61-71 ……......61-71

Section 7:  7: 

System Configuration and Alignment with Parallel Beam Optics and Diffracted Beam Monochromator……………………… Mo nochromator……………………………......72-73 ……......72-73

Service Evaluation Record…………………………..………………………….……………...74 Record…………………………..………………………….……………...74

 

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Section 1: Cooling System Maintenance and Operations   Operations

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Before we power up the generator, always always check the condition of the water in the chiller. The reason for this is that we would like to catch any water quality issues before pumping contaminants through the x-ray tube. For sake of illustration illustration this section addresses the routine chiller maintenance issues using a small small water-to-water chiller. The same methodology can be applied to air-to-water chillers and larger chillers, as the water quality issues are essentially the same.

Step 1.  Cooling System Inspection a.  Remove the reservoir cover and visually inspect (see Figure 1.1)  b.  Water level – the water level should be above the float switch level. c.  Water quality: the water in the reservoir should be clean and clear, free of algae-like substances, bacteria, corrosion debris. d.  In-tank filter: the nylon filter elements should be white and free of particulate and all other forms of debris. e.  Reservoir sediment: blue CuS chips in the bottom of the reservoir can help suppres suppresss algae growth however, a few chips is plenty. Otherwise the bottom of the reservoir should be free of all particulate matter.

Figure 1.1.  1.1.  The reservoir cover has been removed removed in this picture to all allow ow for inspection of the the reservoir, filter, and general water quality.

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In the case shown below (Figure 1.2), the filter is significantly discolored due to the accumulation of algae-like debris and a fair amount of particulate debris has accumulated at the  bottom of the reservoir (Figure 1.3).

Contaminated Filter  Figure 1.2. 1.2.   The in-tank filter has turned black as a consequence of accumulated algae-like debris.

Particulate debris accumulation at the  bottom of the reservoir 

Figure 1.3. 1.3.   Organic debris has accumulated at the bottom of the chiller reservoir.

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For cases where the water in the reservoir is found to be clean and clear skip ahead to Step 3.

Step 2. Flush the Cooling System. a.  Drain the contaminated water into a suitable container (see Figure 1.4)  b.  Disconnect and clean the in-tank filter – rinse under running water and/or gently  brush with a soft bristled brush to remove attached debris. You can safely soak the filter in warm soapy water with a little household bleach bleac h to kill algae while cleaning the reservoir out. The filter is made of nylon and won’t be harmed by soap or bleach.  c.  Flush the system with with TAP water. Depending upon how dirty the reservoir and cooling system are you may have ha ve to flush the system several times to eliminate water  borne contaminants. {The reason for flushing the system with tap water is twofold. twofold. First, tap water is typically less expensive than distilled water, which matters more when the system has to be flushed several times. Second, tap water usually (not always) contains some residual chlorine, which can help to kill most type of algae and waterborne bacteria.}

Figure 1.4.  1.4.  Disconnect the reservoir hose and drain the reservoir contents into a suitable container. d.  Wipe debris out of the reservoir after each flush using paper towels (see Figures 1.5 and 1.6 below). This will help to minimize minimize the number of flush flush cycles required to clean out the cooling system.

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Figure 1.5.  1.5.  This image shows the the debris remaining on the bottom of the reservoir after the tank has been drained. In some cases, algae may adhere to the walls and condenser plumbing sso o it is a good idea to wipe down these parts too.

Figure 1.6. 1.6. This image shows that that a significant amount of residue residue can be removed quickly with  paper towels.

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e.  After reattaching the drain hose, in-tank filter and refilling the reservoir start the chiller again. In many cases, contaminated water that was trapped in the lines will  pollute the new water in the reservoir (see Figure 1.7). Let the system run for a few minutes then repeat the flushing process described above. If the cooling system system is severely contaminated you may choose to add APPROVED chemicals to the cooling system to help speed along the flushing process. DO NOT USE unapproved chemicals in the cooling system as even a few minutes of exposure can be sufficient to destroy components in the water path p ath (e.g., pump seals, hose materials, flow sensors). Approved water additives are described in the addendum to this section.

Figure 1.7. 1.7.   This image shows the water in the reservoir after the first flush cycle and a few minutes of operation. Sometimes it takes several several flush cycles before the the chiller will run clean.

Step 3. Inspect and Clean the Internal Filter (X-ray Tube) It is assumed that the instrument has power at this point and a nd that the control PC has been bootedup. If this is not the case, power up the instrument instrument (NOT the generator though) and PC. To  power up the instrument make sure that the “Emergency Stop” is fully released, the main breaker (lower right-rear corner) is closed (full up position) and that the power “ON” button (left side of control panel on the instrument). The green “Ready” LED (below the “XRAYS” label) sshould hould  be on. Drive the tube axis to 75 degrees using “Manual Measurement” (see Figure 1.8) a.  Double click on the Rigaku folder located on the PC desktop.  b.  Double click on the Right Measurement folder c.  Double click on the Manual Measurement icon d.  Under the Control Axis pull down menu select the “Theta S” axis.

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e.  Under the “Control” pull down menu select “Initialize” then click “Execute”. f.  Under the “Control” pull down menu select “Move”. g.  Type 75 in the position window then press the “Execute” button. Figure 1.9 shows the final position of the tube arm prior to removal of the x-ray tube. h.  Remove the X-ray tube (See Figure 1.10).

Figure 1.8.  1.8.  This screen shot shows the mouse operations used to open the Manual M Measurement easurement  program and move the tube axis (named Theta S) to 75 degrees.  degrees. 

Figure 1.9.  1.9.  This photograph shows the tube axis inclined at approximately approximately 75 degrees. This will make it easier to uninstall the X-ray tube and will also help to prevent water from dripping down into the tube tower.

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Figure 1.10.  1.10.  Left: the X-ray tube before being removed from the tube tower.  Right: A standard screwdriver is used to remove the two screws that attach the tube to the tower assembly. Note: The X-ray tube should be handled carefully. Note: The carefully. Whenever possible it is best practice to hold the tube by the stainless steel water jacket. For example, when the tube is being removed from the tube tower it is natural natural to hold the tube by the the stainless steel water jacket. However, in order to inspect the internal filter inside the water jacket an alternate method of holding the tube is required. Under no circumstance should should human hands touch the Beryllium windows. Furthermore, it is highly undesirable to touch the body of the x-ray tube with bare hands as the oils and other debris transferred to the tube body bod y can cause electrical arcing when the tube is energized. Powder-free latex gloves can be used when handling the x-ray tube or alternately lint free paper wipes can be used as shown in Figure 1.11 below.

Be X-ray windows Figure 1.11.  1.11.  Left: shows lint-free paper being used to keep the tube clean during handling.  Right: the t: the four Allen screws are removed to release the water jacket from the b body ody of the x-ray tube. i.  Release the four Allen screws attaching the water jacket to the body of the x-ray tube.

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 j.  Inspect the individual parts – look for dirt, d irt, debris, corrosion, excessive oxidation of the cooled anode surface, flat spots on the O-rings, evidence of water leakage, etc. (see Figure 1.12). Replace O-rings as needed (replacement OO-rings rings are normally included in the accessory kit delivered with the instrument).

Figure 1.12.  1.12.  Left:  shows modest oxidation of the wet side of the anode. The direction of the oxidation patch matches the line direction of the x-ray source.  Right:  water jacket assembly with spray nozzle. k.  Remove the spray nozzle by gently pulling the brass nozzle straight up and remove the brass mesh filter inside (see Figure 1.13). l.  Inspect and clean the filter as needed (see Figure 1.14). The water treatment document appended to the end of this section offers some suggestions as to how to go about cleaning the internal filter. Needless to say, handle and clean the ffilter ilter with due care as this part is not normally considered to be consumable (no extra filters are included in the accessory kit delivered with the instrument).

Figure 1.13.  1.13.  This image shows the spray spray nozzle being removed from the water jacket assembly.

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Figure 1.14.  1.14.  Left: Substantial blockage of the internal filter.  Right: The same filter is shown after cleaning. m.  Reassemble the water jacket (see Figure 1.15). a.  Insert brass mesh filter  b.  Install spray nozzle

Figure 1.15.  1.15.  Left: re-install brass filter inside nozzle mount.  Right: align notch in the base of the nozzle with locator pin at base of nozzle mount. n.  Attach the water jacket to the tube body (see Figure 1.16). a.  Reseat O-rings to ensure a good water seal  b.  Rotationally align the screw holes in the water jacket with the corresponding holes in the tube body. c.  Tighten the attachment screws just enough to slightly compress the O-rings (Note: over tightening the screws can damage the O-rings). o.  Install the tube in the tube tower (see Figure 1.17) a.  Align the pin & corresponding pinhole on the tube assembly.  b.  Tighten the attachment screws enough to achieve a good water seal.

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Figure 1.16.  1.16.  Left: the screw holes in the water jacket are not lined up with the holes in the tube  body.  Right:  the water jacket was rotated 90 degrees clockwise so that tthe he screw holes in both  part lined up then the attachment screws were attached.

Figure 1.17. 1.17.   Left: the pin hole on the tube assembly is aligned with the pin on the tower.  Right:  the attachment screws are tightened just enough to provide a good water seal.  p.  Refill the chiller reservoir with distilled water and reinstall the in-tank filter (if not currently installed) (Figure 1.18). q.  Consult the operators manual for proper temperature (~68 F) and pump pressure (4055 psi) settings. r.  Turn the chiller power switch on. s.  Check to make sure that there are no leaks around the x-ray tube. t.  Check to make sure that the chiller is performing within the specified operational limits. u.  Re-install the reservoir cover and replace side panels pane ls and top cover of the chiller unit.

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Figure 1.18.  1.18.  This photograph shows the chiller reservoir after being fl flushed ushed and cleaned several times. The in-tank filter has also been cleaned and re-installed.

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ADDENDUM

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Section 2: System Power-up  Power-up 

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Prior to beginning this phase in the procedure it is assumed that the chiller and x-ray tube have  been inspected and cleaned (as needed). The instrument PC should be already on before  proceeding.

Step 4.  Power Up the X-ray Generator. a.  Use the mouse to double-click on each of the numbered programs shown in Figure 2.1 below.

operations used to open the x-ray generator Figure 2.1  2.1  The image above shows the mouse operations control software (named “XG Operation”).  b.  Click on the icon shown in Figure 2.2 to change the view displayed for the generator control.

F Figure 2.2. 2.2. Click on the third icon as shown above.

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c.  Verify that the Hand icon is highlighted in Yellow ((see see Figure 2.3). If it is not use the mouse to click on it. it. This will turn on instrument instrument power (power to move move the goniometer axes)

already active (yellow highlights will appear on Figure 2.3.  2.3.  Click on the Hand icon if it is not already the button when instrument power is “ON”. d.  Click on the radiation icon (see Figure 2.4) – this will power up the generator to 20kV and 2 mA.

Figure 2.4. 2.4.   Left: Click on radiation symbol.  Right: Radiation icon changes color when the generator is on and the power settings are displayed in the horizontal scroll bars. e.  Click on the “Option” menu then select “Property (see Figure 2.5). f.  Select the Tab labeled “Aging data”. Note:   At this point you will start to make decisions based upon the details of the instr Note: instrument ument that you are working on. For new tubes (or tubes that haven’t been used for a month or more) you will select or setup setup an aging program that will gradually outgas the filam filament. ent. Alternately, for Xray tubes that have been used recently, the goal of the aging process is to gradually ramp the  power up in order to achieve thermal equilibrium at measurement power (e.g. 40kV and 44mA). When out gassing a new tube typically the kV settings will be inc incremented remented in sequential time steps with the mA setting setting being left at a relatively low value initially. This procedure allows adsorbed gasses time to release release from the surface of the filament. The kV and mA values can be increased in an alternating time steps (e.g. kV first, then mA) when thermally aging a tube for every day use since both bo th power settings contribute to the overall operating temperature of the tube. Examples of each type of aging cycle are given in Figures 2.6 & 2.7.

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Figure 2.5. 2.5. The image shows the numbered mouse operations shown above are used to gain access to the Aging data tables.

he pull down menu so Figure 2.6.  2.6.  The mouse is used to select ”The Present condition” from tthe that the generator remains at the last power level programmed into the “Aging data” table.

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Figure 2.7.  2.7.  Left: The image shows the name of the aging table (New Target 2) along with  power and time step values for a typical out gassing aging cycle. Right: The image shows typical  power and time step values for a thermal aging cycle used to bring the tube into thermal equilibrium at operating power for standard measurements. Note:   Tube suppliers will typically Note: typically provide an out gassing power/ti power/time me schedule in the  paperwork associated withisthe replacement tube. It is always preferable to use the manufacturers aging schedule when one available. (or infrequently used tube) has been through an out gassing aging cycle Note:   After a new tube (or Note: once it can be aged using a thermal aging cycle provided that the tube is used regularly. Note: Any Note:  Any tube that has not been used for a period of several weeks (or longer) should be aged using an out gassing power/time power/time schedule to reduce the risk of damaging the tube (filament). In general, the longer the period of inactivity the longer the dwell time for each power step.  New aging programs can be created by clicking on the “New” button and entering a name in the text field of the dialog box that appears. Correspondingly, any user created aging schedule can  be removed from the pull down menu by first selecting the program then clicking on the “Delete” button. The default aging schedules can be edited but can not be deleted. Aging data table entries can be edited by using the mouse to select a cell, then type the new value and press the “Enter” button on the keyboard to register register the changed value. Once a suitable aging program has been defined and selected click the “OK” button at the bottom of the dialog box.

Figure 2.8.  2.8.  Left: Click on the aging icon to initiate the aging cycle.  Right:  The aging icon changes color while the program is running and the power levels changes automatically.

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Section 3: Configuration of Hardware and Software with Focusing Optics  Optics 

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At this point in the procedure the instrument and control PC should be on and the X-ray generator should be at normal operating power (e.g., 40kV, 44 mA). It is advisable to power down the generator however, if you need to remove any of the incident beam optical components in order to prevent accidental exposure to x-rays. In this section hardware configuration will be verified. Not all Ultima III’s will have exactly the same configuration as shown shown in the  photographs below. In some instances the detail of how components are attached will be a little different depending upon the components installed on a particular instrument (e.g., either thumb screws or Allen screws may be used to attach the detector box to the detector arm depending upon whether the in-plane arm has been installed on the goniometer). However, in all cases the same basic sequence of steps should be followed in terms of checking/setting up proper hardware and software configurations. Proper Mechanical Positioning of All Optical Components. Step 5.  Verify Installation and Proper a.  Open the lower left door on the instrument and turn “OFF” the RCD 3 controller power (SERVO AMP unit on left side of left cabinet). This will ensure that none of the motorize electrical connections are live while we check connections.  b.  Check the power/communication cables cab les for the CBO (2 connections), Div Slit (1 connection), detector optic box and Scintillation detector (1 connection – always live 700V, DO NOT disconnect unless the “Emergency Stop” button has been depressed.) as shown in Figure 3.1. The incident beam optical components are shown in in Figure 3.2.

Ultima III with the following accessories attached: attached: Cross Figure 3.1.  3.1.  This image shows an Ultima Beam Optic, computer controlled slit assemblies, standard sample stage, in-plane arm goniometer and Scintillation detector.

Figure 3.2. 3.2.   Left: shutter assembly and tube arm with all other optical components removed. Mechanical reference surfaces used to mechanically mechan ically position the incident beam optics assembly are highlighted in RED.  Right:  Labeled incident beam optical components are shown.

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c.  Make sure that the incident beam optic is  properly inserted into the shutter *. The external shutter is assembly* assembly normally open when a primary optic is  properly installed. In Figure 3.3 the external shutter was manually opened half way to demonstrate the function of EVER   the external shutter. DO NOT EVER attempt to mechanically open the secondary shutter while the generator is turned ON as this would be a HAZARD. If RADIATION SAFETY HAZARD. the generator is currently at measurement  power (e.g., 40kV, 44mA), place your hand on top of the tube. If the top of the tube is noticeably warm/hot power down the generator and clean the X-ray tube filter (see STEP 3 for further details). *The X-raytogenerator always be powered OFF prior OFF  prior removal should of the primary incident  beam optic.

Figure 3.3.  3.3.  The external shutter aperture is being opened by pressing the springloaded button down. The entry aperture of the primary incident beam optic (Empty  beam path or CBO) has to be inserted into the shutter opening to hold this outer shutter open. The optic reference surfaces should be in contact with both of the reference surfaces highlighted in RED in RED in Figure 3.2.  3.2. 

d.  Verify that the incident beam PSA box is fully attached to the primary optic (check to make sure that the Allen screws are snug).

Figure 3.4.  3.4.  The incident beam PSA box is attached to the primary optic using two Allen screws. The PSA optic does not have to be uninstalled to check the tightness of the screws but the Div Slit assembly will have to be removed.

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e.   Now the BB selection slit and 5 degree PSA should be installed in the positions shown in Figure 3.5.

Figure 3.5.  3.5.  Left: BB selection slit, PSA, 10 mm H.L. Slit. Right: the Bragg-Brentano (BB) selection slit and incident beam PSA are installed. f.  Install/check the Div Slit assembly. There are two different designs the older design is shown in Figure 3.6. Here you set/check the reference mechanical positioning aligning two marks (circledby in Red) then tighten the thumb screw using the J-bar tool shown. On the newer design there are two flat reference surfaces similar to those on the CBO assembly that match two perpendicular reference surfaces on the detector arm. arm. To properly align the newer Div Sit assembly just slide the assembly along the horizontal reference surface until it engages the vertical reference surface, then tighten the Allen screw.

Figure 3.6.  3.6.  This image shows shows the mechanical reference marks used to mechanically align the divergence slit assembly.

g.  Install/verify the 10mm H.L. slit in the top part of the Div Slit assembly. A  properly assembled incident beam optical assembly should look similar to one of the captions in Figure 3.7

Figure 3.7.  3.7.  Left: CBO incident beam optical assembly with position of the H.L. slit circled in RED. RED.  Right: Empty Beam Path incident  beam optical assembly.

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h.  Verify that the standard stage has been installed properly (see Figure 3.8) a.  The stage inserts into the goniometer and is attached using three thumb screws.  b.  A flat support should be installed in the sample position and the rotational orientation of the stage should should be adjusted using a level. Tighten the thumb screws to preserve the level orientation of the stage (see Figure 3.9).

Figure 3.8.  3.8.  Left: this photo shows the attachment mounting surface on the goniometer.  Right: Standard sample stage, (3) thumb screws and J-bar screw tool tightening tool.

Figure 3.9.  3.9.  After the stage is leveled, the thumbscrews are cinched up to provide enough friction to preserve the rotational positioning of the stage. i.  Verify the mechanical positioning and electrical e lectrical connections for the detector optics (see Figures 3.10 & 3.11).  j.  Adjust the position of components as needed (see Figure 3.12).

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Figure 3.10.  3.10.  Left: Important reference marks on the detector arm.  Right: Detector optic box and Scintillation detector.

Figure 3.11.  3.11.  The captions in this figure show the bottom of the detector optic box while mounted on the detector arm. Left: Mechanically misaligned.  Right: Mechanically aligned.

Figure 3.12.  3.12.  Left: Loosen/tighten screws to adjust mechanical location of detector box.  Right:  Loosen/tighten Allen screws to adjust location of detector.

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k.  Open detector box and verify that the 5 deg PSA has been installed with the parallel foils vertically oriented (see Figure 3.13). Also make sure that the notch in the PSA properly engages one of the two pin positions within the detector box.

Figure 3.13.  3.13.  Left: Flex the latch in the direction indicated to open the detector box.  Right:  Insert the PSA in the forward or aft position making sure that the notch in the PSA housing engages the alignment pin in the optic box base. Settings Match The Hardware Configuration Settings. Step 6.  Verify That The Software Settings a.  Double click on the Rigaku icon. This will open a dialog box containing four programs (see Figure 3.14).  b.  Double click on “Control” which will open another dialog box containing another four  programs. c.  Double-click on “Rigaku Control Panel” which opens a third dialog with four programs. d.  Double-click on “RINT 2200 Right System” (see Figure 3.15). Note: the fourth icon in the “Rigaku Control Panel” has a very similar name but the icon looks Note: the like a wrench. This is a utility utility program used by installation installation engineers to install ssoftware oftware modules corresponding to physical pieces of hardware purchased with the system. This utility only needs to be used when new ne w hardware is added to the system or in instances where the software has  been reloaded from the installation CDs. e.  Check/set all of the system construction settings (settings on the first tab of the dialog  box) to the values shown in Figure 3.16. As you select each component you will notice that the picture in the lower right corner changes accordingly. Pay particular attention to the following items: a.  “Differential” and “Do Not Execute” MUST  be selected in the “Detector MUST be Property” dialog – these settings will impact the automated alignment  procedure to be performed shortly.

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Figure 3.14. The arrows and numbers indicate the sequence of mouse operations used to pen the “Rigaku Control Panel” utility.

icon.  Figure 3.15. Double-click on the RINT 2200 Right System” icon. 

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symbols indicate mouse operations that you should perform Figure 3.16.  3.16.  The gold arrow cursor symbols in order to verify that all software settings are correct.  b.  If a CBO is mounted on the instrument, the “Incident monochro” pull down menu must be set to “Use” and “CBO unit” Must be set in the Property window. When the Empty beam path optic is installed the “Not used” option should be selected. c.  In the ”Slit” pulldown menu select Auto Variable slit (Focus), then click on the “Property” button to the right. right. Verify that the “DivSlit and “SctSlit tables have all of the same same angular settings. The RecSlit table should have different values all of which are listed in units of (mm). f.  Click on the second tab (labeled “X-ray beam type”) and select the settings shown in Figure 3.17. g.  Click on the third tab (labeled “Geometry system”) and select the settings shown in Figure 3.18 then click the “OK” button at the bottom of the dialog box. h.  The RINT 2200 Right…. Dialog will close and an d another small dialog box will open asking whether you want to write the configuration changes to the Registry. Click on the “Yes” button.

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or specifying the proper Figure 3.17.  3.17.  The gold arrows in this figure indicate mouse operations ffor settings.

or specifying the proper Figure 3.18.  3.18.  The gold arrows in this figure indicate mouse operations ffor settings.

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Section 4: Automatic Alignment with Focusing Optics  Optics 

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The instrument should be on and the generator should have been at measurement power (e.g., 40 kV & 44 mA) for at least 30 minutes. In addition, the PC should be on and the x-ray optics should be set for focusing measurements. measurements. Inspect cabling – make sure that arms can move freely Step 7.  Focusing Optics Alignment. a.  Open the “Automatic Alignment” program using the mouse operations shown in Figure 4.1.

Figure 4.1. The numbers and gold arrows indicate the mouse operations used to open the “Automatic Alignment…” program.  b.  The “Automatic Alignment” program uses Active X components which MS Windows XP automatically blocks. Thus, for the “Automatic Alignment” Alignment” program to work you have to follow the numbered sequence of steps shown in Figure 4.2. c.  Verify that the software settings displayed in the log window (lower right corner of the Automatic Alignment dialog) are set correctly (see Figure 4.3). d.  Select the 2Theta, Theta and Profile Measurement check boxes (1), set the power settings to standard measurement values *# and click “Execute”(see Figure 4.4). #

*  The default power settings used by Rigaku are (40kV, 44mA). However, the instrument can be used at any power setting between (20kV, 2mA) and the upper limit power rating for the tube ((e.g., 2kW for normal focus Cu tubes). The power settings used during alignment should match the power settings used for routine measurement. Aligning the instrument with generator settings other than those used for standard measurements can lead to systematic sources of error in diffraction data. There are two reasons reasons for this. this. First the power settings directly influence the

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Figure 4.2.  4.2.  The numbered mouse operations indicate the steps steps required to enable the “Automatic Alignment” program.  program. 

Figure 4.3.  4.3.  The “Automatic Alignment” program modifies the alignment process based upon the software configuration of the instrument (circled in RED). RED).

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Figure 4.4. The numbered steps and gold arrows indicate mouse operations used to initiate the Automatic Alignment process.

steady-state operating temperature of the X-ray tube, which influences the positioning of the anode via thermal expansion. Aside from this, the kV setting determines how deeply the electron beam (emanating from the filament) will penetrate into the surface of the anode, which directly influences the characteristic depth into the surface of the anode from which the nominal X-ray beam emanates. Both of these factors contribute contribute to the observed peak positions. Consequently, both of these factors are normally accommodated during alignment operations. e.  A dialog box will appear prompting you to verify that the tube has been at power for 30 minutes, that the BB selection slit has been installed and that a suitable number of Cu absorbers are inserted (see Figure Figure 4.5). Click the “OK” button after completing the requested operations. f.  The next dialog box that appears relates to the HV/PHA test which we have not selected (yet, but we will later). later). Thus, we can ignore this dialog box temporarily and just click “OK” (see Figure 4.5). g.  Read the instructions carefully in the next dialog box. Skipping a step here will likely result in alignment failure (see Figure 4.5). h.  The software is requesting that you install the parts shown in Figure 4.6. Press the “Door” button on the front panel of the instrument. The button should flash on/off then it is OK to open the radiation radiation enclosure doors. Once the Center Slit and Absorbers have  been properly installed and the radiation enclosure door has been closed (flashing light will turn off), click the “OK” button.

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dialogs shown will appear sequentially. Figure 4.5.  4.5.  Each of the popup dialogs Critical details are highlighted in RED. RED.

Figure 4.6.  Left: Center slit being installed in the sample position.  Right:  Cu absorbers  being installed in the detector optics box.  box. 

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i.  The instrument will initialize all motorize axes then immediately proceed to performing the first series of measurements (see Figure Figure 4.7). When these tests are complete the software will prompt you to remove the center slit (see Figure 4.8).

instrument trument initializes each Figure 4.7.  4.7.  Prior to the onset of alignment measurements the ins motorized axis.  axis. 

the first fto irstthe measurement software software stop and prompt prompt the Figure 4.8.  After 4.8.  user to remove the performing center slit prior onset of the the second set ofwill measurements.  

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 j.  Verify that the sample position position is empty as iindicated ndicated in Figures 4.9. This instruction is critical as it relates to the first measurement in the “Theta Alignment” series. series. Any object installed in the sample position will distort the measured beam position.

Figure 4.9.  4.9.  At the end of the 2Theta measurement measurement series the program will uncheck the jig.  2Theta test (circled in RED), RED), then prompt the user to install the Alignment jig.  k.  Press the “Door” button, open the radiation enclosure and install the alignment jig as indicated in Figures 4.10 and 4.11. Close the radiation enclosure door(s) then use the mouse to click on the “OK” button.

Figure 4.10.  4.10.  The direct beam position position is indicated by the blue the blue + in the plot shown above.  above. 

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Figure 4.11.  4.11.  Left: the Alignment jig referred to in the software is normally stored in a box labeled Setting Jig.  Right:  Install the alignment jig jig in the sample positi position on as shown above. l.  Press the “Door” button on the radiation enclosure, open the door(s), open the detector optics box and remove the Cu absorbers (see Figure 4.6). The next test (Profile Measurement) is a diffraction diffraction experiment rather than a direct beam measurement. Thus, if you forget to remove the absorber the displayed data will exhibit a flat intensity profile (i.e. no observable diffraction peak) and the alignment test will fail. m.  Close the detector optics box; verify that the alignment jig is still in the sample position; close the radiation enclosure door and click on the “OK” button (see Figure 4.12).

Figure 4.12.  4.12.  The “Theta Alignment” series is is now complete and the instructions presented in the dialog relate to the last measurement (Profile Measurement).  Measurement).  

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n.  Using the mouse, follow the numbered sequence shown in Figure 4.13 to save and  print the alignment results.

Figure 4.13.  4.13.  The optical alignment of the instrument is now complete.  complete. 

Step 8.  Calibrate the Detector Electronics. a.  Use the mouse to select the check box next to “HV/PHA Alignment”, verify generator power settings, then click “Execute”.

associated with detector calibration are circled in RED. RED. Figure 4.14. 4.14.   The settings associated

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 b.  Click the “OK” button in the first dialog that appears (see Figure 4.15). These instructions pertain to the optical alignment test series just completed.

preformed Figure 4.15.  4.15.  The instructions in this dialog relate to the optical alignment tests preformed earlier.   earlier. c.  Read and complete the instructions in this dialog prior to clicking the “OK”  button (see Figure 4.16).

Figure 4.16.  4.16.  The instructions in this dialog relate directly to detector calibration. d.  Use the mouse to perform perform the numbered steps shown in in Figure 4.17. The printout should appear similar to Figure 4.18.

Figure 4.17.  4.17.  The numbers indicate mouse operations that that will save and print the alignment results.   results.

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tests are circled in RED. RED.  Figure 4.18. 4.18.   The results of the HV/PHA tests

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e.   Next we will perform the “Counting Loss” correction experiment. The circuit used to count photons (based upon the HV/PHA settings determined above) takes a finite amount of time per photon to process the electrical signal produced as it interacts with the detector. Correspondingly, at very high count rates (e.g. in excess of 100,000 cps) some signals are lost while previously detected signals are still being electronically processed. The “Counting Los” experiment determines correctionbecomes coefficients needed compensate for so initiate that thethis detector response linear up to to approximately 700,these 000 losses cps. To experiment perform the mouse operations indicated in Figure 4.19.

used to perform the “Counting Loss” correction correction Figure 4.19.  4.19.  The mouse operations used experiment are shown above.  above.   The “Counting Loss” button only active when focusing optics and no diffracted beam Note: Note: The monochromator are specified in theis“System Configuration” software. f.  The software will prompt you to install the “counting-loss correction jig” in the sample position (see Figures Figures 4.20 and 4.21). It is critical critical that all absorbers (other than the Ni K beta filter) must be removed remove d as these will distort the “Counting Loss” experiment. During the course of this measurement measurement sequence you will notice that the software will measured several diffraction peaks and change the generator power. This is done to generate a series of intensity values which will subsequently be linearized (see Figure 4.22). g.  To save and print the result of this experimental series follow the steps illustrated in Figure 4.22. The corresponding printout should appear similar similar to the graph Figure 4.22.

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Figure 4.20. 4.20.   The numbered steps indicate the mouse operations to be performed.

Figure 4.21.  4.21.  Left: Polycrystalline quartz sample used for the counting loss correction measurement.  Right: Counting loss jig installed in sample position.  position. 

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Figure 4.22.  4.22.  The numbered steps indicate the mouse operations required to save and print the counting loss results.  results.  h.   Now we need to tell the software to use the counting loss correction values that were just determined. To do this close the Automatic Automatic Alignment program then follow the numbered steps shown in Figure 4.23. i.  Since changes were made in the system configuration, the program will prompt you to decide whether or not to save the changes – click “YES” as indicated in Figure 4.24.

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Figure 4.23.  4.23.  The numbered steps indicate mouse operations used to activate the counting loss correction for all subsequent measurements.  measurements. 

system configuration information information by selecting the the “Yes” Figure 4.24.  4.24.  Save the updated system  button.    button.

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Section 5: System Configuration and Alignment with Parallel Beam Optics  Optics 

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The instrument should be powered up and the generator should have been at measurement power for at least 30 minutes. minutes. The detector electronics should have been calibrated (HV/PHA and Counting Loss experiments – see Section 4, step 8 for fur further ther details). This section will address the procedural sequence used to reconfigure the Ultima III hardware and software with parallel  beam optics. Step 9.  Install Parallel Parallel Beam Optical Hardware. o. 

 p.  q. 

Remove the BB selection slit and install the PB selection selection slit. The beveled edge of the selection slit should be located at the bottom edge and the slit should be inserted behind a spring clip (See Figures 3.5 and 5.1). Verify that the sample stage is level (see Figure 3.9). Open the detector optics box and install the PB optic (see Figure 5.2).

Figure 5.1.  5.1.  The PB selection slit slit is shown above.

Figure 5.2.  5.2.  Diffracted beam parallel beam optics configurations are shown. Left: High flux configuration - 5 deg PSA (axial divergence) and 0.5 deg (radial divergence).  Right: High Resolution Configuration – Thin film PSA with a 0.11 deg. acceptance angle (radial divergence).   divergence).

Step 10.  Change Software Configuration. a.   b.  c.  d. 

Use the mouse to perform the numbered steps shown in Figure 5.3. Change the slit setting to “Auto Variable slit (Parallel)” (see Figure 5.4). Select the “Geometry System” tab then select the Parallel Beam Method radio  button. Click the “OK” button, then click the “Yes” button (see Figure 5.5).

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oftware utility where the ssystem ystem Figure 5.3.  5.3.  This figure shows the steps used to open the ssoftware configuration is specified.  specified. 

Figure 5.4.  5.4.  This figure shows the the steps used to specify parallel parallel beam settings.

Figure 5.5.  5.5.  To implement changes made to the system configuration select the “Yes” button.

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Step 11.  Prealign the X-ray Mirror. a.   b. 

Press the “Door” button on the front of the radiation enclosure. Wait for the light light on this button to flash then open the radiation enclosure doors (see Figure 5.6). Install the fluorescent screen in the sample position as shown in Figure 5.7.

Figure 5.6. This 5.6. This photo shows the “Door” button flashing after being pressed.

Figure 5.7.  5.7.  The fluorescent screen is installed in the sample position.  position. 

c. 

Turn off the fluorescent light inside the enclosure, close the doors (the button

d. 

should stop flashing) and turn off or reduce the room lighting. Perform the mouse operations in Figure 5.8 in order to position the source in front of the fluorescent screen.

Figure 5.8.  5.8.  This image shows the mouse operations required to properly position the x-ray source in front of the fluorescent screen.  screen.  

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e.  Verify that the communication cable between the DC motor Controller (see Figure 5.9) and the CBO assembly is properly connected at both ends. f.  Open the shutter by pressing the “Close” (the green LED will go out on the EXT button) and then “Open” button. You should hear an audible click click from shutter solenoid and theRed Shutter op en lights (Goldthe LED on the Open button, tubeopen tower light and gold Shutter R light on the safety light stack) activate (see Figure 5.10). g.  Turn “ON” the power switch to the DC Motor Controller then while looking through the window of the radiation enclosure at the fluorescent screen adjust the joystick until a bright green line appears at the center of the screen. h.  Turn the power switch “OFF” and verify that the green line still appears in the center of the fluorescent screen.

Figure 5.9.  5.9.  The DC Motor Controller shown above is used to align the tilt orientation of the x-ray mirror optic.  optic. 

i.  Press the shutter “Close” button, then press the “Ext.” button (the green LED should light).  j.  Press the “Door” button (light should flash) and open the radiation enclosure doors. k.  Remove the fluorescent screen and close the enclosure doors. Figure 5.10.  5.10.  Manual shutter controls are circled in RED in this photo.  photo.  

Step 12. Parallel Beam Alignment. a.  Open the “Automatic Alignment” program as indicated in Figure 5.11.  b.  Verify that the software settings indicated in the lower left corner of o f the alignment window are correct (see Figure 5.12). c.  Use the mouse to specify the settings shown in Figure 5.13. d.  A sequential series of dialog windows will appear with instructions that you should perform PRIOR to clicking the “OK” button. Figure 5.14 shows the first three and critical instructions have been underlined and annotated in RED RED.. The alignment parts referred to in the third dialog ar aree shown in Figure 5.15. After clicking on the “OK” button the instrument will perform a scan to find the angular  position of the detector relative to the X-ray source. Once this has been determined you will optimize the mirror tilt orientation to maximize the flux scattered toward the detector.

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Figure 5.11. Launch 5.11. Launch the Automatic Alignment” program by double clicking on the icon shown above.  above. 

software settings indicate parallel beam (see Figure 5.4). Figure 5.12. 5.12.   Verify that the software

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Figure 5.13.  5.13.  The numbered steps indicate mouse operations used to specify and initiate alignment tests.  tests. 

Figure 5.14. This 5.14. This figure shows three numbered dialog windows with critical instructions RED..  underlined in RED

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Figure 5.15. This 5.15. This image shows the alignment filters to be installed in the filter holder  positions of the detector box for all direct beam alignment measurements.  measurements.  e.  Read the instructions in the next dialog – they indicate how to terminate the mirror alignment test. test. You will be manipulating the joystick joystick to optimize the tilt angle of the mirror while watching the intensity as a function of time. Once the  position of maximum intensity has been achieved you will need to terminate this measurement. f.  Turn on the power to the DC Motor control unit. g.  Click the “OK” button shown in Figure 5.16.

Figure 5.16. The instructions shown in this window tell you how to terminate the test that will begin when you click the “OK” button.  button. 

 

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h.  Make small adjustments to the joystick control to change the tilt of the mirror. Note: The intensity display takes a second or two to respond to joystick perturbations. If you Note: manage to lose the beam click on the the “Pause” button, then repeat STEP 11. After reacquiring the  beam, you can reactivate the mirror alignment. Once the mirror position has been optimized the scan can be terminated as illustrated in Figure 5.17.

Figure 5.17.  5.17.  The numbered steps shown above demonstrate the sequence of mouse operations used to terminate the mirror alignment scan.  scan.   i.  The program will prompt you to remove the Ni K beta filter (see Figure 5.18) in  preparation for the next scan. The objective of this scan is to verify that the measured intensity approximately doubles as a result of removing the Ni filter. Click “OK” after the filter has been removed and the enclosure doors are closed.

  Leftthe critical instructions are underlined in Red.  Right: the Ni K beta filter Figure 5.18.from 5.18.  : The is removed detector box.

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 j.  Once you verify that the observed intensity is approximately double, turn off  power to the DC Motor Controller then terminate the scan using the steps indicated in Figure 5.19.

Figure 5.19. The mouse operations specified in this image indicate the procedure used to terminate the mirror alignment scan.  scan.  k.   Now the software will prompt you to either repeat the mirror alignment (i.e., (i.e., if the observed intensity was not approximately double) by clicking on “Yes” or continue to the next alignment test by clicking on “No”. When the test is successful click “No” as shown in Figure 5.20.

Figure 5.20.  5.20.  Clicking on “No” will allow you to proceed to the next alignment test. l.  Follow the instructions in the dialog (see Figure 5.21) then click on “OK”. Several preprogrammed measurements will take place. m.  Follow the instructions in presented in Figure 5.22, then click “OK”. n.  Verify that the sample position is open and click the “OK” button (see Figure 5.23).

 

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Figure 5.21.  Left: dialog with instructions to be completed prior to clicking on the “OK”  button.  Right: Photograph showing the center ce nter slit being installed in the sample position. position.  

Figure 5.22. Prior 5.22. Prior to clicking the “OK” button, the center slit should be removed and the Parallel beam optic (previously removed in Step 12d, see Figure 5.14) should be re-installed in the detector optics box (see inset photo).  photo).  

 

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test series has been completed. Subsequently, the Figure 5.23.  5.23.  The “2Theta Alignment” test alignment program prompts you to verify that the sample position is open. open.   o.  The first scan in the “Theta Alignment” series is a scan of the detector position relative to the source. Once this measurement is complete, co mplete, the software will  prompt you to install the alignment jig in the sample position as shown in Figure 5.24.

Figure 5.24. The program prompt you to install the alignment jig (see inset photo) in the sample position.  position. 

 

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 p.  The objective of the Theta Alignment” is to make the 0.00 degree orientation of the measurement system parallel to the sample orientation. When this is successfully completed the intensity profile will by triangular in shape (see Figure 5.25) and you will be prompted to remove all of the beam attenuating devices  previously installed. After completing these instructions click the “OK” button. q.  The program will perform a diffraction scan of the 220 reflection of Si and compare the observed peak position and intensity values to internally defined acceptable limits. r.  To save and print the alignment results follow the numbered steps shown in Figure 5.26. s.  An example of the parallel beam alignment printout is given in Figure 5.27.

instructions uctions Figure 5.25.  5.25.  The Theta Alignment” measurement series is now complete and the instr  presented relate to the last test series (Profile (Profile Measurement). Measurement).  

 

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indica ted the mouse operations used to save Figure 5.26. The numbered steps in this image indicated and print the alignment results.  results. 

 

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Figure 5.27. Typical parallel beam alignment results should appear similar to the captions in this figure.  figure. 

 

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Section 6: System Configuration and Alignment with Focusing Optics and a Diffracted Beam Monochroma Monochromator tor  

 

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The instrument should be powered up and the generator should have been at measurement power for at least 30 minutes. minutes. The optical configuration described in Section 3 is the assumed init initial ial hardware configuration. The detector electronics should have been calibrated (HV/PHA and Counting Loss experiments – see Section 4, step 8 for fur further ther details). This section will address the procedural sequence used to reconfigure the Ultima III with a diffracted beam monochromator set for use with focusing optics. Installation. Step 13.  Monochromator  

a. Dismount the detector form the detector arm (see Figure 3.12). 3.12 ).  b.  Disconnect the strain relief support on the High Voltage (detector power) cable.

 NEVER disconnect the HV cable while the instrument Note:  ELECTROCUTION HAZARD! Note:  HAZARD! NEVER is powered up as there will be a live electrical potential of approximately 700V. c.  Remove the two screws attaching the detector to the standard bracket using a “+” head screwdriver (see Figure 6.1). d.  Attach the monochromator  bracket to the detector. Make sure that the screws are tight enough that the detector does not easily rotate relative to the Figure 6.1.  6.1.  This image shows the location of orientation of the bracket the detector bracket attachment screws.  screws.   (see Figure 6.2). e.  Assemble the monochromator (if needed) the relevant parts are shown in Figure 6.3. a.  Carefully remove the monochromator crystal from its shipping box and slide it onto the center-post support as shown in Figure Figure 6.2.  6.2.  This image shows shows the detector along with 6.4. Make sure that the standard bracket and the monochromator bracket.  bracket.  nothing touches the graphite crystal surface as it is quite soft and can easily be scratched or otherwise damaged.  b.  Insert a monochromator receiving slit (e.g., 0.8mm) as indicated in Figure 6.5, then replace the removable cover and tighten the thumbscrew. c.  Before installing the monochromator, flip it over look for WHITE reference line scribed on the bottom surface of theand bracket (seethe Figure 6.6).

 

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Figure 6.3.  6.3.  This image shows the constituent constituent parts that comprise comprise the monochromator assembly.   assembly.

Figure 6.4.  6.4.  Left: this caption shows the exposed face of the monochromator crystal.  Right:  the monochromator and support slide onto a brass center post and magnetically attache attachess itself to the top support.  support. 

 

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Figure 6.5. 6.5.   The monochromator receiving slit has been installed behind a 2-pronged spring clip.   clip.

Figure 6.6.  6.6.  This image shows the reference reference mark on the monochromator bracket that will be used to properly position the monochromator on the detector arm.  arm.  

 

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d.  Attach the monochromator assembly to the detector arm as shown in Figure 6.7. You only need to tighten two or three screws enough to support the weight of the assembly. We will need to be able to to laterally slide the monochromator monochromator along the detector arm in the next step so do not fully tighten the screws yet. Note:: The Bragg angle adjustment Note a djustment screw is close to the position of the front attachment screw. Adjustment of this PAINTED screw will misalign the monochromator crystal.

Figure 6.7. This image shows the monochromator monochromator assembly being installed. Two of the five attachment screws were partially tightened to support the weight of the part while final mechanical positioning adjustments are being made.  made.  e.  Adjust the position of the monochromator along the detector arm radius while looking at the reference marks shown in Figure 6.8. f.  Tighten the five attachment screws (see Figure 6.9). Check to make sure that the reference marks are still aligned and that the monochromator assembly does not move when light hand pressure is applied. Configuration and Automatic Alignment. Alignment. Step 14.  Software Configuration a.   b.  c.  d. 

Perform the mouse operations indicated in Figures 6.10 and 6.11. Open the “Automatic Alignment” program as indicated in Figure 6.12. Perform the sequentially numbered mouse operations suggested in Figure 6.13. Press the “Door” button on the instrument, after the button light begins blinking open the enclosure doors and perform the tasks indicated in Figure 6.14. Once finished, close the enclosure doors. e.  Perform the instructions given in Figure 6.15. f.  Perform the instructions given in Figure 6.16.

g.  Perform the instructions given in Figure 6.17. h.  An example alignment printout is given in Figure 6.18.

 

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Figure 6.8. This image shows the two reference marks that have to be mechanically aligned in order to properly position the monochromator.  monochromator.  

Figure 6.9. This image shows the attachment screws being tightened after the reference marks have been aligned.  aligned. 

 

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Figure 6.10. The numbers indicated the sequence of mouse operations used to open the system configuration software.  software. 

the sequence of mouse operations used to specify specify the Figure 6.11.  6.11.  The numbers indicated the current configuration of the hardware.  hardware.  

 

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Figure 6.12. Start the “Automatic Alignment” program by clicking on the icon circled in RED..  RED

  The numbered steps indicate mouse operations used to initiate initiate the Automatic Figure 6.13. 6.13.  Alignment process. process.   

 

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this figure are related to to the labeled components in Figure 6.14.  6.14.  The instructions shown in this the inset photograph.  photograph. 

Figure 6.15.  6.15.  The numbered instructions correspond to to the last measurement in the “2Theta Alignment” test series and the first measurement in the “Theta Alignment” test series respectively.   respectively.

 

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to the labeled component in the inset Figure 6.16.  6.16.  The instructions shown above relate to  photograph.    photograph.

Figure 6.17. The numbered steps indicate mouse operations used to save and print the alignment results.  results. 

 

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Figure 6.18.  6.18.  This image shows a typical alignment result for a system configured with focusing optics and a diffracted beam monochromator.  monochromator.  

 

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Section 7: System Configuration and Alignment with Parallel Beam Optics and a Diffracted Beam Monochrom Monochromator ator  

 

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The instrument should be powered up and the generator should have been at measurement power for at least 30 minutes. minutes. The optical configuration described in Section 5 along with the diffracted beam monochromator installed in Section 6 is the assumed initial hardware configuration. The detector electronics should have been calibrated (HV/PHA and Counting Loss experiments – see Section 4, step step 8 for further details). This section will address address the  procedural sequence used to align the Ultima III with a diffracted beam monochromator set for use with parallel beam optics.

Step 15.  Parallel Beam Monochromator Settings. f.  Press the “Door” button on the the front panel of the inst instrument. rument. After the button light starts blinking, open the enclosure doors. g.  Remove the monochromator receiving slit (see Figure 7.1). h.  Loosen the thumbscrew on the removable monochromator cover and then remove the cover. i.  Rotate the monochromator crystal as indicated in Figure 7.2.

Figure 7.1. This image shows the parts referred to in step 15 b and 15 c.  

Figure 7.2.  7.2.  The monochromator crystal can be rotated rotated 90 degrees to the “FLAT” orientation enhancing the detection efficiency during parallel beam measurements.  measurements.   j.  Replace the monochromator cover and tighten the thumbscrew. k.  Close the radiation enclosure doors. l.  Change and save the system configuration settings as described in Sections 5 and 6. In particular, see Figures 5.3 and 5.4 but also remember that tthe he monochromator 6 in this figure). should be set as indicated in Figure 6.11 (see numbers 2 through m.  Perform the “Automatic Alignment” procedure described in Step 12 of Section 5.

 

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Service Evaluation Record 1.  Cooling system inspected and operating correctly?

Yes/No

2.  Instrument and control PC power-up correctly?

Yes/No

3.  X-ray generator and tube powered up to measurement power?

Yes/No

4.  Good goniometer communication verified?

Yes/No

5.  Focusing optics (BB) properly installed and aligned?

Yes/No

6.  HV/PHA and counting loss calibrations completed?

Yes/No

7.  Parallel beam optics (PB) properly installed and aligned

Yes/No

Optional Diffracted Beam Monochromator 8.  Monochromator installed and aligned for: a.  focusing (BB) optics?

Yes/No

 b.  parallel beam (PB) optics?

Yes/No

Comments: ______________ _____________________________ _____________________________ ___________________________ _____________  ___________________________  _____________ _____________________________ ____________________________ ________________________  ___________   ___________________________  _____________ _____________________________ ____________________________ ________________________  ___________   ___________________________  _____________ _____________________________ _____________________________ ________________________ __________

Rigaku Service Rep __________________ ________________________ ______ Date __________ ____________________ __________ Customer ___________________________ _________________________________ ______ Date __________ ____________________  __________