MiniFlex Diffractometer. Start-Up Manual

Transcription

1

2

3 MiniFlex Diffractometer Start-Up Manual Rigaku/MSC 9009 New Trails Drive The Woodlands, TX Tel: Fax: Web:

4

5 Table of Contents INSTALLING THE SYSTEM... 3 PART 1 - CONFIGURING THE HARDWARE...4 Section 1 - Installing the X-ray Tube... 4 Section 2 - Connecting the Heat Exchanger... 5 Section 3 - Turning the Power On... 7 Section 4 - Configuring the Computer... 9 PART 2 - SETTING UP THE SYSTEM...10 Section 5 - Setting the System Conditions...10 Section 6 - Initializing the Goniometer...11 Section 7 - Optimizing the HV/PHA Value of the Scintillation Counter...12 Section 8 - Adjusting the X-ray Tube Height...16 Section 9 - Aligning the Optical Axis...18 Section 10 - Confirming the HV and Correction Angle...20 PERFORMING MEASUREMENTS...23 Measuring Full Charts...24 Measuring a Series of Selected Peaks/Saving the Results in a Single File...26 TROUBLESHOOTING...31 SECTION 1 - MANUAL MEASUREMENT...31 Errors During Measurement...33 Hardware Related Errors...34 System Failure...36 SECTION 2 - STANDARD MEASUREMENT...37 System Failure...43 GLOSSARY

6

7 Chapter 1 Installing the System This chapter describes the procedures for setting up the Rigaku MiniFlex + Diffractometer. We recommend that you read them over completely, before installation, so that you understand the procedures and can take the necessary precautions. This chapter is divided into two parts: Part 1 describes the steps for configuring the hardware, and is divided up into the following sections: Section 1 - Installing the X-ray Tube. See page 4. Section 2 - Connecting the Heat Exchanger. See page 5. Section 3 - Turning the Power On. See page 7. Section 4 - Configuring the Computer. See page 9. Part 2 describes the steps for setting up the system in preparation for measurements: Section 5 - Setting the System Conditions. See page 10. Section 6 - Initializing the Goniometer. See page 11. Section 7 - Optimizing the HV/PHA Value of the Scintillation Counter. See page 12. Section 8 - Adjusting the X-ray Tube Height. See page 16. Section 9 - Aligning the Optical Axis. See page 16. Section 10 - Confirming the HV and Correction Angle. See page 20. The procedures are easy and uncomplicated and should take about two hours to complete the first time if the software is pre-installed. 3

8 4 - Rigaku MiniFlex + Diffractometer Part 1 - Configuring the Hardware A number of accessories are included with the MiniFlex +. Confirm that all of them have been received when you unpack your equipment. The accessories are shown here for easy verification: Hex screwdriver (double ended) Polystyrene case Sample preparation jig (4 pieces) Pestle Sample retainer Glass plate (round) Sample mounting block Silicon/plastic sample 10 A fuses (3) 2 A fuses (3) Glass plate (square) Solid base sample holder (3) Sample retaining clip Thick aluminum absorber Open ring sample holder (3) Not shown: Wooden box, containing accessories P-8 O-rings (2) Hex wrench for sample holder In addition, a few basic tools are needed: a standard screwdriver, a Phillips head screwdriver, and a knife, blade or scissors. Section 1 - Installing the X-ray Tube 1. Remove the two Phillips screws that secure the cover to the upper cabinet. They are located at the bottom corners of the cover, one on each side of the upper cabinet. After removing the screws, the cover can be tilted back for easy access to the inner components. 2. On the top surface of the tube housing are two screw holes for securing the x-ray tube. Before installing the tube, place O-rings in each of the water circulation port holes. These are the two P-8 O-rings included with the accessories.

9 Installing the System - 5 Screw holes Water circulation port holes Guide pin 3. Occasionally, the tube is packed in a plastic sheath. If so, remove it. Do not attempt to remove the rubber seal that protects the vacuum seal on the glass. Be careful while handling the tube. Do not touch the tube glass or the beryllium windows. If you do inadvertently touch them, clean the glass with alcohol and the beryllium window with acetone. 4. Set the tube in place. There is a guide pin on the top surface of the tube housing, to be placed in the hole on the bottom of the tube-mounting surface for proper positioning. 5. Once positioned, carefully push the tube in so that it is seated firmly, and the bottom end of the x-ray tube receives the post at the base of the tube housing. This is important, to ensure proper seating of the tube while it is being tightened down with the screws. 6. Insert the two screws into the tube housing and tighten them snugly, alternating between screws, but do not force them. 7. Before closing the cover, check the connections for all of the connectors at the top of the boards in the electronic circuit board panel (ECP). Make sure they are seated properly. There should be a cable running to each connection, except for the INT connector in the CPU-C board. 8. Close the cover and replace the screws. Section 2 - Connecting the Heat Exchanger 1. Connect the pieces of hose together first, without connecting anything to the diffractometer. Before connecting to the diffractometer, the hoses must be cleaned out by running water through them. Connect a length (cut to your needs) of the braided PVC hose to each port of the heat exchanger. Connect a length of the narrower plastic hose to each piece of braided hose, for eventual connection to the diffractometer ports. The quick-release valve should be installed in the line that runs between the diffractometer OUT port, and the heat exchanger IN port.

10 6 - Rigaku MiniFlex + Diffractometer 2. Remove the water reservoir cover and reservoir cap located at the top of the heat exchanger. Fill the reservoir with distilled water (approx. 1 liter). 3. Place both of the diffractometer ends of the hoses in a pail of distilled water (about 1/2 to 1 gal.). Turn the heat exchanger on for a few minutes to rinse them out. Note: Do not run the heat exchanger dry, as it will damage it. After the rinsing is completed, turn the heat exchanger off. Plastic hoses Braided PVC hoses Quick-release valve 4. Using their snap fittings, connect the hoses to the diffractometer. The line that carries water out from the heat exchanger is attached on the back of the MiniFlex + main body to the port marked IN. The inflow line for the heat exchanger is connected to the OUT port on the MiniFlex Now separate the hose at the quick release valve, about midway in the line between the heat exchanger inflow port and the diffractometer OUT port. Put the end of the hose that extends from the diffractometer OUT port in a pail or into a drain. 6. Before the system is fully connected, the lines within the MiniFlex + should be flushed, to remove any sediment that may have collected. Turn the heat exchanger on and run another 1/2 gal. or so through the cooling system. 7. Reconnect the hoses and refill the water in the chiller. Replace the reservoir cap and cover. 8. Turn off the heat exchanger.

11 Installing the System - 7 Section 3 - Turning the Power On 1. Ensure that the heat exchanger is turned off so that there is no water flow, and plug the power cord for the MiniFlex + into a 110 V wall outlet. 2. Turn the MiniFlex + on. The switch is at the back of the unit. 3. Verify that the CW (cooling water) alarm indicator is on in the LED display panel on the front of the MiniFlex +. This indicates that the flow switch is working. 4. Turn the heat exchanger on. 5. Verify that the CW alarm indicator is now off. POWER indicator CW alarm indicator READY light RST (reset) button X-RAY ON/OFF SHUTTER indicator X-RAY indicator 6. Check to see that the POWER, SHUTTER, and SCAN indicators are now illuminated. Open the front sliding door and note that the SHUTTER LED turns off. 7. Push the RST (reset) button at the bottom left of the display panel. 8. Verify that the READY light is lit. 9. Push the X-RAY ON button that is located at the bottom right of the display panel. 10. Wait approximately 8 seconds. Verify that the X-RAY indicator is lit in the display panel. The red light on the top of the MiniFlex + will also light up. 11. If one of the alarm LED s lights up, push the RST button again, and then push the X-RAY ON button again. (Whether you hear the alarm buzzer or can only see a maintenance indicator LED depends on whether the BUZ button is toggled on or off.)

12 8 - Rigaku MiniFlex + Diffractometer 12. If an LED warning indicator remains lit, note which LED is lit and call Rigaku field service for additional help.

13 Installing the System - 9 Section 4 - Configuring the Computer 1. Install the software. (If you purchased your computer from Rigaku, the software is already installed.) If you are installing the software on your own computer, follow these steps: For Windows 3.11: a. Start Windows. The Windows Program Manager window appears. b. Insert Disk 1 in the appropriate drive. c. From the Program Manager window menu bar, select File > Run. The Run dialog box appears. d. In the Command Line text box, type A:\SETUP, and then click OK. (Substitute drive A with a different floppy drive letter, if necessary.) The MiniFlex + Installation screen appears. e. Type your user name and corporation name, and then click OK. f. Accept the defaults for the directories and follow the instructions on the screen. For Windows 95: a. Click Start on the task bar. b. Click Run. c. Insert Disk 1 in the appropriate drive. d. In the Command Line text box, type a:\setup, and then click OK. (Substitute drive a with a different floppy drive letter, if necessary.) g. Type your user name and corporation name, and then click OK. 2. If you have received and are installing Jade for Windows, follow the installation instructions that are in the Jade manual. 3. Connect the RS-232C cable between the computer and the MiniFlex +. If you purchased your computer from Rigaku, the RS-232C port is COM1. If you are using another computer, you will need to know which port you are using for the RS-232C connection. 4. After installing the software, reboot the computer. This completes setup of the hardware.

14 10 - Rigaku MiniFlex + Diffractometer Part 2 - Setting Up the System Section 5 - Setting the System Conditions Use this window to set up machine conditions: the type of sample holder, the x-ray tube target type, and the port used for communications between the MiniFlex + and the computer. 1. Double-click the Rigaku group icon in the Program Manager window, and then double-click the Condition Setting icon in the Rigaku window to access the Condition Setting window. 2. If you have an attachment (MiniFlex 6 sample changer or Specimen rotation attachment), select it in the Attachment drop-down list box. Otherwise, select Standard sample holder. 6-position sample changer (ASC6) Specimen rotation attachment (spinner)

15 Installing the System Select the correct XG target (usually Cu). 4. Leave the defaults in the remaining fields. 5. Select Edit > Port setting from the menu bar. The Port setting dialog box appears. 6. Select the correct port from the Serial port list that is used to communicate with the MiniFlex +. If Rigaku installed the software, select COM1. 7. Click OK in the Port setting dialog box. 8. Click Exit in the Condition Setting window. A Condition Setting dialog box appears, asking for verification that you wish to save your settings, Do you save the set condition? Click Yes. Section 6 - Initializing the Goniometer 1. Double-click the Manual measurement icon in the Rigaku window to access the Manual measurement window. 2. If you receive the error message, An error occurred in the RCD. Reset is not executed. Please reset. click OK. Note: This statement always occurs if you have lost communication for any reason. Routinely take the following steps: 3. Press the Reset button on the screen.

16 12 - Rigaku MiniFlex + Diffractometer If you continue to receive the RCD error message, the INI files of the Windows software may be disrupted, preventing operation of the MiniFlex + system. To correct these files, it is easiest to rename them and let the system create new ones. The original INI files, located in the path C:\rw\apps are: \manmeas\manmeasr.ini \stdmeas\stdmeas.ini Each module has its own INI files. Rename them in the module that gives problems and try to access the Manual measurement window again after rebooting the computer. Note: If you receive the message, Datum is not executed. Please datum. click OK. Then click the Datum check box under Setting, and press the Execute button. 4. In the Manual measurement window, in the lower portion of the window labeled Setting, click the check box in front of both Initialize and Datum, so that a cross appears in each box. 5. Open the sliding door of the MiniFlex +, so that you can view the movement of the scan axis as it is datumed, when you click the Execute button. 6. Click the Execute button. The MiniFlex + detector arm is now set at a reference 2-theta (2θ) angle of 10 o. Section 7 - Optimizing the HV/PHA Value of the Scintillation Counter 1. Place the silicon sample in the sample holder. Use the silicon sample (silicon powder in plastic matrix) supplied in the MiniFlex + accessory box. Silicon sample Sample holder

17 Installing the System Click Goniometer in the Manual measurement window. 3. Click Independ. mode in the Control drop-down list. The lower half of the Manual measurement window changes, displaying the fields for the independent mode. 4. For Target angle, scroll to, or enter 28.4 for the 2-theta position of the detector to measure the (111) reflection of silicon. 5. If the sliding door has been open so that you could view the movement of the goniometer, Click Execute. The goniometer moves to 28.4 degrees. You can observe it occurring. 6. Close the sliding door. 7. Click the SCHV/PHA button at the top of the window. The Status Display frame and the Control frame change in appearance. Status display frame Control frame 8. Make the following entries in the Control frame: SCHV - Type 700 for the voltage. 9. Click the Execute button. 10. In the Control drop-down list, select Measurement. The Control frame in the bottom half of the window changes in appearance, displaying the fields for the measurement mode.

18 14 - Rigaku MiniFlex + Diffractometer 11. Make the following entries: Start angle - Type 500 for the start voltage for the measurement. Stop angle - Type 850 for the stop voltage for the measurement. Sampling - Type 5.0 for the step size for the measurement. Scan speed - Type 0.5 for the counting time for each step. 12. Click Execute. The Measurement Monitoring (SCHV measurement) window appears, displaying the measurement results in real time. Status Display frame Peak Search frame Profile Control frame 13. When the measurement is complete (approximately 35 seconds), the Manual Measurement window reappears over the Measurement Monitoring (Count monitor) window. Click anywhere in the Profile Control frame of the Measurement Monitoring (SCHV measurement) window. 14. In the Peak search drop-down list in the Peak Search frame, click Peak-top method.

19 Installing the System Click the Execute button under the drop-down list. An X is displayed on the data profile, marking the peak top. The peak voltage and intensity are displayed in the Status Display frame. Make a note of the voltage value, as it will be needed later in the setup. Note: If you wish to retain a picture of this screen on hard copy, turn your printer on, and press the Prnt Scrn key on your keyboard. Open the MS Paint program. Select Edit > Paste from the menu bar. Select File > Print. A picture of the Measurement Monitoring (SCHV measurement) window is printed. Select File > Exit to exit Paint. 16. Click End to close the Measurement Monitoring window. The Manual measurement window reappears. 17. In the Control drop-down list, select Setting. The Control frame in the bottom half of the window changes in appearance, displaying the fields for the setting mode. 18. In the SCHV field, enter the peak voltage value that was determined in step 15.

20 16 - Rigaku MiniFlex + Diffractometer 19. Click Execute. This completes the steps needed to optimize the detector. Section 8 - Adjusting the X-ray Tube Height To obtain the maximum x-ray intensity, the x-ray tube position must be adjusted to maximize the count rate received by the detector. 1. Open the door and remove the silicon sample. 2. Set the aluminum absorber onto the detector arm soller slit box. It fits over the screw holding the nickel filter. Absorber 2-theta soller slit box Note: The absorber is used to prevent the direct beam from damaging the detector. Without the absorber in place, the direct beam will burn out the detector. 3. Confirm that the x-rays are on (LED is lit). 4. Click the Goniometer button at the top of the Manual measurement window. The Status Display frame and the Control frame change in appearance. The Initialize and Datum fields should both have a cross in their check boxes. 5. Click on the option button in front of the Not correct option for Datum condition, and then click the Execute button. 6. In the Control drop-down list, select Independ. mode. 7. In the Target angle scroll list, specify -3 o for the 2-theta detector angle, and then click the Execute button. 8. Again, in the Target angle scroll list, specify 0.0 for the 2-theta detector angle, and again click the Execute button. 9. Click the SCHV/PHA button at the top of the Manual measurement window.

21 Installing the System In the Control drop-down list, select Setting, and then click Execute. 11. Open the sliding door on the front of the MiniFlex +. Note: Adjusting the height of the x-ray tube from the sliding front door is awkward, but it is safe. Opening the sliding front door closes the shutter, which prevents exposure to x-rays. 12. Slightly loosen the two locking screws at the top of the x-ray tube, along the back edge. They are located on both sides of the x-ray tube vertical position adjustment screw. Use the accessory hex key for these adjustments (one end fits the locking screws, the other the adjustment screw). Cu Adjustment screw Rigaku Locking screws X-ray tube head 13. Close the sliding cabinet door. 14. In the Manual measurement window (Goniometer Status), select Monitor in the Control drop-down list. The appearance of the Control frame changes, displaying the fields for the monitor mode. 15. Specify 0.5 seconds for Fixed time. 16. Click Execute. The Measurement Monitoring (Count monitor) window appears, displaying the intensity measurement in real time.

22 18 - Rigaku MiniFlex + Diffractometer 17. Open the sliding cabinet door. Note that the intensity drops to zero. 18. Using the hex key, rotate the tube adjustment screw by a very small increment (10-15 o ) in one direction. 19. Open the shutter by closing the sliding cabinet door, and observe the count monitor. If the number of counts is less, you will need to slightly turn the adjustment screw in the opposite direction. If the number of counts increased, a greater increase may be achieved by turning the screw further in the same direction. 20. Repeat steps until you are able to locate the tube height position that yields the maximum intensity (counts). It is recommended that you record the counts in an instrument log. 21. Now the two locking screws must be carefully tightened without altering the tube height. Use the hex key again, tightening the locking screws a quarter turn at a time, alternating between the two screws. (Sometimes it helps to turn the height adjustment screw slightly clockwise, just before completing the tightening of the locking screws.) If you do not do this procedure carefully, the maximum intensity seen on the monitor will fall off. If the drop in intensity is greater than 2-5%, the adjustment procedure should be repeated. 22. When the locking screws are successfully tightened, click the Abort button, closing the Measurement Monitoring (Count monitor) window. Section 9 - Aligning the Optical Axis The procedures in this section ensure that the x-ray tube is aligned with the divergence slits, the theta axis, the scatter slits, and the receiving slits. Make sure no sample is in place before starting. 1. In the Manual measurement window, click the Goniometer button.

23 Installing the System Open the sliding door in the front of the MiniFlex In the Control drop-down list, select Setting if it is not already selected. The fields for the setting mode are displayed. 4. In the lower portion of the window labeled Setting, click the check box in front of both Initialize and Datum, so that a cross appears in each box. 5. Under Datum condition, select Not correct by clicking its button. 6. Click Execute. 7. Verify that the aluminum absorber is set onto the 2-theta soller slit box and close the door. Note: The absorber is used to prevent the direct beam from damaging the detector. Without the absorber in place, the direct beam will burn out the detector. 8. In the Manual measurement window, select Measurement in the Control drop-down list. The appearance of the Control frame changes, displaying the fields for the measurement mode. 9. Make the following selections in the Control frame: Msrment method: Select Continuous. Start angle: (minus 0.30) degrees. Stop angle: 0.30 degrees. Sampling: 0.01 degrees. Scan speed: 0.5 degrees per minute. 10. After making your selections, click Execute. The Measurement monitoring (Manual measurement) window appears, displaying the measurement results in real time. 11. When the measurement is complete, click any of the methods in the drop-down list in the Peak search field to the right; for example, FWHM midpoint method.

24 20 - Rigaku MiniFlex + Diffractometer 12. Click the Execute button under the scroll list. An X is displayed on the data profile, and the peak angle and intensity of the peak top are displayed in the Status Display frame. Record the peak angle for later use. 13. Click the End button. 14. In the Manual measurement window, select Setting in the Control drop-down list. The appearance of the Control frame changes, displaying the fields for the setting mode. 15. Make the following selections in the Control frame: Datum condition - Click the Correct option button on. 2theta correct. ang. - Enter the peak angle value obtained in step 12. The software rounds out the correction angle to the nearest 100 th. 16. Click Execute. The goniometer is repositioned. 17. If the peak position is greater than or equal to +/ degrees, adjust the x-ray tube height again. 18. If the peak position is within the proper range, the configuration is complete. Click the End button in the Manual measurement window. Section 10 - Confirming the HV and Correction Angle The setup procedure is complete. If you would like to confirm that the correct settings have been made, follow these steps: 1. Double-click the Condition Setting icon in the Rigaku window to access the Condition Setting window.

25 Installing the System Click the Counter condition button in the Condition Setting window to access the Counter condition dialog box. 3. In the SCHV field, confirm that the voltage to be applied to the detector is the voltage that you obtained earlier in step 12, Part 2, Section 7 - Optimizing the HV/PHA Value of the Scintillation Counter, starting on page Click OK. 5. Click the Gonio condition button in the Condition Setting window. The Gonio condition dialog box appears. 6. Click the Execute option button in the Gonio condition dialog box: 7. In the Correct. ang. field, verify that the angle to be used for the correction to the datum position is the angle that you obtained earlier in step 12 of Section 9 - Aligning the Optical Axis, starting on page Click OK in the Gonio condition dialog box. 9. Click the Save button and then the Exit button in the Condition Setting window.

26

27 Chapter 2 Performing Measurements This chapter contains a recipe for collecting data on silicon powder. The recommended measuring conditions for silicon lead you through typical entries for each of the fields available in the Standard measuring conditions window, the Scan condition edit frame and the File condition list. 23

28 24 - Rigaku MiniFlex + Diffractometer Measuring Full Charts This section describes the configuration of a measurement to collect diffraction data from silicon (Si). It assumes the use of a Cu tube. 1. Insert the silicon standard in the sample holder. 2. Double-click the Rigaku group icon in the Program Manager window, and then double-click the Standard measurement icon in the Rigaku window to open the Standard measurement window. 3. Click the Msment cond. button in the Standard measurement window to open the Measurement conditions window. Scan condition list Using the Measurement Conditions Window 4. Make the following entries in the Measurement conditions window. Msrment cond. - Type a number for this measurement conditions, or select one from the scroll list. The maximum number of measurement conditions is 50. Memo - This is an optional field. Type Silicon scan here. Operator - This is an optional field. Type Laboratory here. Scan axis - Theta/2Theta, the only selection available. Msment method - Select Continuous (see the glossary for an explanation of this and Fixed time measurement). Counting unit - Select cps by clicking its option button.

29 Performing Measurements - 25 Divergence - Variable, the only selection available. Scattering - 4.2deg, the only selection available, since the scattering slit is fixed. Receiving - 0.3mm, the only selection available, since the receiving slit is fixed. Repeat - Leave this at its default setting, 1 measurement time. BG msment - Select No by clicking the option button, for no background measurement. Auto scale - Leave this at its default setting, toggled on (cross) to automatically adjust the vertical axis scale of the Measurement Monitoring window to accommodate the maximum peak intensity in the window. Initial scale - Leave this at its default setting, 1000 cps. 2theta/theta initialization - Leave this at its default setting, toggled on (cross) to initialize the 2theta/theta axis after the measurement is completed, moving the 2theta/theta position to 10 o /5 o. Using the Scan Condition List 5. Make the following selections in the Scan condition list in the bottom half of the Measurement conditions window: Use - Toggle this to Yes by clicking it, instructing the program to use this scan condition for the measurement. Print column - Toggle this to No by clicking it, instructing the program not to print the results, unless you have a printer connected and want to print them. Comment (Optional) - Type Full Range Scan. Start Angle - Type 5 as the angle for starting the measurement. Stop Angle - Type 140 as the angle for ending the measurement. Sampling - Type 0.02 as the sampling width (the size of the angle for each data point). Scan speed - Type 2.00 as the number of degrees per minute for the speed of measurement. Material (Optional) - If you wish to input anything, click the detail... field. 6. Click the Close button, or select File > Close from the Measurement condition window menu bar. The Standard measurement window reappears.

30 26 - Rigaku MiniFlex + Diffractometer File condition list Using the File Condition List 7. Make the following selections in the File condition list at the bottom of the Standard conditions window: Use - Toggle this to Yes by clicking it, instructing the program to use this file condition for the measurement. Directory name (Optional) - The default setting is \RW\DATA. File name - Use the format; name.raw (or >asc. If the ASCII package is supplied). Sample name Enter a sample name, lot number, and identifier. Cond. No. - This is the condition number specified in step Click the Msrment start button to start the measurement. Measuring a Series of Selected Peaks/Saving the Results in a Single File This section describes the configuration of a run to collect data from the measurement of eleven silicon (Si) peaks, and saving the results in a single file. 1. Double-click the Rigaku group icon in the Program Manager window, and then double-click the Standard measurement icon in the Rigaku window to open the Standard measurement window. 2. Click the Msment cond. button in the Standard measurement window to open the Measurement conditions window.

31 Performing Measurements - 27 Using the Measurement Conditions Window 3. Make the following entries in the Measurement conditions window. Msrment cond. - Type a number for this measurement conditions, or select one from the scroll list. Memo - This is an optional field. Type Silicon scan here. Operator - This is an optional field. Type Laboratory here. Scan axis - Theta/2Theta, the only selection available. Msment method - Select Continuous. Counting unit - Select cps by clicking its option button. Divergence - Variable, the only selection available. Scattering - 4.2deg, the only selection available, since the scattering slit is fixed. Receiving - 0.3mm, the only selection available, since the receiving slit is fixed. Repeat - Leave this at its default setting, 1 measurement time. BG msment - Select No by clicking the option button, for no background measurement. Auto scale - Leave this at its default setting, toggled on (cross) to automatically adjust the vertical axis scale of the Measurement Monitoring window to accommodate the maximum peak intensity in the window. Initial scale - Leave this at its default setting, 1000 cps. 2theta/theta initialization - Leave this at its default setting, toggled on (cross) to initialize the 2theta/theta axis after the measurement is completed, moving the 2theta/theta position to 10 o /5 o.

32 28 - Rigaku MiniFlex + Diffractometer 4. Select View > Show the window for editing the scan condition from the Measurement conditions window menu bar to open the Scan condition edit frame at the bottom of the Measurement conditions window. Scan condition list Scan condition edit frame Using the Scan Condition Edit Frame 5. Make the following selections in the Scan condition edit frame: Edit mode:dupli/delete - Select Dupli to duplicate a scan condition. No. (in Scan condition list) - Click and highlight this column of a scan condition to be duplicated. Execute - Click this button to create a duplicate of the selected scan condition. Repeat this procedure 9 more times to register a total of 11 scan conditions. Not in use/all in use - Click this button so that the Use column of all the scan conditions contains Yes. Not in print/all print - Click this button so that the Print column of all the scan conditions contains No. 6. Select Edit < Unify scan condition from the Measurement condition window menu bar to open the Unify scan condition dialog box.

33 Performing Measurements Unify the silicon scan by clicking Comment, Scan speed and Sampling width on (check mark). 8. Click OK. The Measurement conditions window reappears. 9. Enter the following start and stop angles in the Scan condition list (use the scroll bar on the right as needed): Start Angle Stop Angle Click the Close button to return to the Standard measurement window. Using the File Condition List 11. Make the following selections in the File condition list at the bottom of the Standard conditions window: Use - Toggle this to Yes by clicking it, instructing the program to use this file condition for the measurement. Directory name (Optional) - The default setting is \RW\DATA. File name - If you enter a name, use the format; name.raw. Sample name - Enter a sample name, lot number, and identifier. Cond. No. - This is the condition number specified in step 3.

34 30 - Rigaku MiniFlex + Diffractometer 12. Click the Msrment start button to start the measurement.

35 Appendix A Troubleshooting This appendix is divided into two sections: Section 1 lists the error messages that result when errors occur while operating the Manual measurement program. Section 2 lists the error messages that result when errors occur while operating the Standard measurement program. See page 37. Section 1 - Manual Measurement Errors at Screen Startup Failed to connect the measurement server. Screen start-up aborted. Cannot connect with the measurement server used for communication between the software and hardware. Close all programs and reboot the computer. Failed to get the measurement information. Screen start-up aborted. An attempt was made to open the Manual measurement program while the Standard measurement program was already open. Close the Standard measurement program, and then open the Manual measurement program. 31

36 32 - Rigaku MiniFlex + Diffractometer Errors During Manual Operation Execution Failed to execute initialize. Initialize aborted. Initialize was executed before Reset was performed. Execute Reset. Failed to set the mode for correction value(s). Datum aborted. Datum was executed before Initialize was performed. Execute Reset and then Initialize. Failed to set the correction value(s). Datum aborted. Failed to execute datum. Datum was executed before Initialize was performed. Execute Reset and then Initialize. Datum aborted. Failed to execute set-up. Datum was executed before Initialize was performed. Execute Reset and then Initialize. Setting aborted. Setting was executed before Reset was performed. Execute Reset. Failed to execute positioning or oscillation. Independent mode aborted. Independent mode was executed before Datum was performed. Execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window, and then execute Initialize and Datum. Failed to start the monitor screen. Measurement is aborted. The Measurement Monitoring (Manual Measurement) window could not be opened because of memory shortage. Close other running programs, and then start measurement. If the Measurement Monitoring (Manual Measurement) window still will not

37 Troubleshooting - 33 your open, exit from all programs and reboot your computer. Restart measurement again. Failed to communicate with the monitor screen. Measurement is aborted. The measurement server program could not process all data because another program occupying a majority of CPU time was executed during manual processing. Failed to set the HV value. Close other programs, and then restart the measurement. If the Measurement Monitoring (Manual Measurement) window still will not start, reboot your computer, and then restart your measurement. Setting aborted. An attempt was made to set an HV value before Reset was performed. Execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window. Failed to set the PHA values. Setting aborted. An attempt was made to set an HV value before Reset was performed. Execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window. Errors During Measurement An Error occurred in the measurement server program. Execution of manual processing aborted. Loss of communication between MiniFlex + and control software. Check power to the MiniFlex + or reseat the communication cable. Exit the Manual measurement program. Turn off the power to the MiniFlex +, and then turn it back on. Restart the Manual measurement processing. Measurement server failed in a communication. Execution of manual processing aborted. Loss of communication between MiniFlex + and control software. Check power to the MiniFlex + or reseat the communication cable. Exit the Manual measurement program. Turn off the power to the MiniFlex +, and then turn it back on. Restart the Manual measurement processing.

38 34 - Rigaku MiniFlex + Diffractometer No connection on the lines yet. Measurement is aborted. Failure in communication cable. Hardware Related Errors Check that the communication cable is properly connected, and then execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window. An Error occured? Double issue error of a command in the RCD. RCD received an unregistered command. An I/O busy error occurred in RCD. A sub-command error occurred in RCD. The RCD received an invalid execution command parameter. A time over error of the relay process in the RCD. A memory check error occurred in RCD. A CPU in RCD detected a bus error. An abnormality occurred on the dual-port RAM in RCD. An abnormality occurred on the scaler or timer in RCD. An abnormality has been found in checking of RS232C port in RCD. An abnormality has been found in the memories of RCD. An abnormality has been found in the pulse controller of RCD. A parity error occurred on the RS232C communication in RCD. A framing error occurred on the RS232C communication in RCD. An over-run error occurred on the RS232C communication in RCD. An Abnormal interruption occurred in the CPU-G of RCD. An abnormality occurred in checking a stepping motor driver in the RCD. An abnormality occurred in checking a AC/DC motor driver in the RCD.

39 Troubleshooting - 35 A link command has been executed for the axes other than the normal linking-axis in RCD. An improper command for a linking motion has been executed to RCD. An error occurred in the RCD. Execution of manual processing aborted. Controller error. Exit the Manual measurement program. Turn off the power to the MiniFlex +, and then turn it back on. Restart the Manual measurement processing. RCD received an invalid measurement stop command. Execution of manual processing aborted. Unspecified goniometer attachment. Open the Condition Setting window and correctly identify the attachment installed on the goniometer. RCD received an invalid measurement restart command. Execution of manual processing aborted. Unspecified goniometer attachment. Open the Condition Setting window and correctly identify the attachment installed on the goniometer. RCD received an invalid command during processing of measurement stop. Execution of manual processing aborted. Unspecified goniometer attachment. Open the Condition Setting window and correctly identify the attachment installed on the goniometer. A pulse motor stopped at the limit. Reset for a system will be done. Execution of manual processing aborted. A goniometer or an attachment s drive axis has tripped a limiting switch. Execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window. Then execute Initialize and Datum. A AC/DC motor stopped at the limit. Reset for a system will be done. Execution of manual processing aborted. A goniometer or an attachment s drive axis has tripped a limiting switch.

40 36 - Rigaku MiniFlex + Diffractometer Execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window. Then execute Initialize and Datum. An error occurred in the RCD. Reset is not executed. Execution of manual processing aborted. The controller has not been reset. Execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window. An error occurred in the RCD. Datum is not executed. yet. Execution of manual processing aborted. Datum for goniometer/driving axis of attachment has not been performed Execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window. Then execute Initialize and Datum. An error occurred in the RCD. Initialize is not executed! Execution of manual processing aborted. Goniometer/driving axis of attachment has not been initialized yet. Execute Reset while Setting is selected in the Setting control frame - Goniometer status, of the Manual measurement window. Then execute Initialize and Datum. System Failure Manual processing cannot be executed properly if communication between the MiniFlex + controller and the computer is disabled. Following are potential sources of the problem: The power to either the MiniFlex + or the computer has been turned off. The communication cable has broken down or has been unplugged. The measurement server program is not receiving adequate CPU time. Hardware errors have occurred. In such cases, exit the Manual measurement program. Turn off the MiniFlex + and turn it back on. Then start manual processing over again.

41 Troubleshooting - 37 Section 2 - Standard Measurement This section lists the error messages that result when errors occur while operating the Standard measurement program. For errors messages while operating the Manual measurement program, see Section 1 - Manual Measurement on page 31. Errors at Screen Start-up Restart After built-in of the standard Gothic font. Starting up of the screen aborted. No standard gothic font has been built into Windows. Open the Control panel from the Main group of Windows. At the fontsetting window, build a standard gothic font. Failed to connect the measurement server. Screen start-up aborted. Cannot connect with the measurement server used for communication between the software and hardware. Close all open programs and reboot your computer. Then restart Windows. Failed to get the measurement information. Screen start-up aborted. An attempt was made to open the Standard measurement program while the Manual measurement program was already open. Close the Manual measurement program, and then open the Standard measurement program. The driving-axis of goniometer could not be found. The Condition Setting file is destroyed or does not exist. Screen start-up aborted. The HV information does not exist. Open the Condition Setting window and register current system structure. Screen start-up aborted. The Condition Setting file is destroyed or does not exist. Open the Condition Setting window and register current system structure.

42 38 - Rigaku MiniFlex + Diffractometer The HV informations exist more than one. Screen start-up aborted. The Condition Setting file is destroyed or does not exist. Open the Condition Setting window and register current system structure. The PHA information does not exist. Screen start-up aborted. The Condition Setting file is destroyed or does not exist. Open the Condition Setting window and register current system structure. The PHA informations exist more than one. Screen start-up aborted. The slit information does not exist. The Condition Setting file is destroyed or does not exist. Open the Condition Setting window and register current system structure. Screen start-up aborted. The Condition Setting file is destroyed or does not exist. Open the Condition Setting window and register current system structure. The counter informations exist more than one. Screen start-up aborted. The Condition Setting file is destroyed or does not exist. Open the Condition Setting window and register current system structure. The monochromator informations exist more than one. Screen start-up aborted. The Condition Setting file is destroyed or does not exist. Open the Condition Setting window and register current system structure. Errors at Starting Measurement The drives specified the following file condition don t exit. Measurement is aborted.

43 Troubleshooting - 39 A drive name which does not exist at the directory column in the File condition list has been specified. Refer to the File manager etc., to check the specified drive name. Standard setting for drives is as follows: a: is for a floppy disk drive, c: is for a hard disk drive if your machine is DOS/V (AT convertibles), and a: is for a hard disk drive and b: is for a floppy disk drive if your machine is PC98 (including convertibles). The disk is write-protected or full. Measurement is aborted. The specified disk in which measurement data are going to be written is write-protected or full. Check whether the disk is write-protected or not, and if it has enough capacity. The following files already exist. Are you ready for overwriting? If you click on the Yes button in the confirmation dialog box, the system starts measurement and the data overwrites the existing file. If you click on the No button, the system aborts the measurement. A file which has the same name as the one specified at the File column in the File condition list already exists. Refer to above. All of the file conditions are not in use. Measurement is aborted. All at the Use column in the file condition list are No. In the file condition list, change No to Yes in the Use column of measurement conditions which are going to be used. Entire of the scan conditions are not in use. Measurement is aborted. Failed to start the monitor screen. All at the Use column in the scan condition list are No. In the scan condition list, change No to Yes in the Use column of measurement conditions which are going to be used. Measurement is aborted. The Monitoring Measurement window could not be started for lack of memory. Terminate other running programs, and then start the measurement. If the Monitoring Measurement window still cannot be started after you have exited all other running programs, close all the open programs and reboot your computer, and then start the measurement again.

44 40 - Rigaku MiniFlex + Diffractometer Errors During Measurement An error occurred in the measurement server program. Finish a program, then restart the program. Measurement is aborted. Communication has been disabled during measurement because the power to the MiniFlex + was turned off or the communication cable was unplugged. Exit the Standard measurement program. Turn off and then turn on the power to the MiniFlex +. Restart Manual measurement and reset the system and set the initial conditions. Then restart the Standard measurement program and start the measurement. No connection on the lines yet. Finish a program and connect the line(s), then restart the program. Measurement is aborted. The communication cable is broken down or unplugged. Check if the communication cable is connected properly and then restart the measurement. Measurement server failed in a communication. Finish a program, then restart the program. Measurement is aborted. The disk is write-protected or full. Communication has been disabled during measurement because the power to the MiniFlex + was turned off or the communication cable was unplugged. Exit the Standard measurement program. Turn off and then turn on the MiniFlex +. Restart the Standard measurement program and start the measurement. If the Retry button on the confirmation dialog box is clicked, the system saves measurement data again. If the Cancel button is clicked, the system terminates measurement without saving measurement data. The specified disk on which data are to be written is write-protected or full. Release write-protection on the disk, or create space in the disk, and then click the Retry button to save the data. Failed to write-in the measurement condition on the memory. Finish the other applications(s) and then execute again. Measurement is terminated without saving measurement data.

45 Troubleshooting - 41 Out of memory. Close other running programs, and then start measurement. If the measurement data still cannot be saved, reboot the computer, and then restart the measurement. Failed to execute print. Measurement is terminated without producing a data output. The printer is turned off or not connected, or the system is out of memory. Turn the printer on or connect the cable. If this is not the problem, close other running programs, and then start measurement. If the measurement data still cannot be printed, reboot the computer, and then restart the measurement. Hardware Related Errors An error occurred! Double issue error of a command in the RCD. RCD received an unregistered command. An I/O busy error occurred in RCD. A sub-command error occurred in RCD. The RCD received an invalid execution command parameter. A time over error of the relay process in the RCD. A memory check error occurred in RCD. A CPU in RCD detected a bus error. An abnormality occurred on the dual-port RAM in RCD. An abnormality occurred on the scaler or timer in RCD. An abnormality has been found in checking of RS232C port in RCD. An abnormality as been found in the memories of RCD. An abnormality has been found in the pulse controller of RCD. A parity error occurred on the RS232C communication in RCD. A framing error occurred on the RS232C communication in RCD.

46 42 - Rigaku MiniFlex + Diffractometer An over-run error occurred on the RS232C communication in RCD. An Abnormal interruption occurred in the CPU-G of RCD. An abnormality occurred in checking a stepping motor driver in the RCD. An abnormality occurred in checking a AC/DC motor driver in the RCD. A link command has been executed for the axes other than the normal linking-axes in RCD. An improper command for a linking motion has been executed to RCD. An error occurred in the RCD. Measurement is aborted. An electrical error occurred. Exit the Standard measurement program. Turn the MiniFlex + power off and then turn it on. Restart Manual measurement and reset the system and set the initial conditions. Open the Standard measurement program and restart the measurement. RCD received an invalid measurement stop command. Measurement is aborted. An unrecognized attachment is installed on the goniometer. Open the Condition Setting window and register the attachment appropriately. RCD received an invalid measurement restart command. Measurement is aborted. An unrecognized attachment is installed on the goniometer. Open the Condition Setting window and register the attachment appropriately. RCD received an invalid command during processing of measurement stop. Measurement is aborted. An unrecognized attachment is installed on the goniometer. Open the Condition Setting window and register the attachment appropriately. A pulse motor stopped at the limit. Reset for a system will be done. Measurement is aborted. A limit switch has been tripped.