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X-ray Diffraction & Scattering
Wide Angle

Scintag XDS 2000 Diffractometer

Operating Instructions

Instrument Setup

  1. Put your TLD ring on.  If using a visitor ring, record the ring number in the logbook.
  2. Record your CUFS number, name, time on the hour log (on the goniometer) and the time of day in the computer.
  3. Diffractometer power:  3.0--4.0 mA and -9.0 kV.
  4. Slits, from left to right as you look at the instrument:  source:  0.05, 0.07, 0.5, 0.3 detector
  5. Datascan, Controller.
  6. Run the calibration option.  After the micrometer dials on top of the stop spinning, enter the omega and theta positions.  (Two-theta=theta*2, source=omega.)  Make sure you hit "enter" after entering each value.
  7. Drive both angles to zero.
  8. Load sample on sample stage.
  9. Close the hood, hit the red safety interlock button (lower right, just below the opening).
  10. In Datascan, open the shutter.
  11. Note reading on the rate meter (select 5 K--or whatever works).&nps; You will want the final reading to be 1/2 the reading when the sample stage is fully clear of the beam-sample holder cuts the beam in ½.
  12. If the reading on the rate meter is zero, the stage is completely blocking the beam the stage needs to be turned down.  If the reading on the rate meter is maximized, the stage needs to be raised.

Alignment of Reflection Sample Stage

  1. Record the micrometer position(s).
  2. To align, open the door (shutter closes automatically) and using the large micrometer, raise or lower the sample stage a small amount.  Close door, press interlock button, note detector reading.  When the reading is ½ that when the stage is fully clear of the beam, the vertical displacement is aligned.
  3. Align the tilt in an analogous manner.  Adjust tilt, note reading, repeat, until signal is maximized.  If the tilt had to be changed significantly, realign the vertical displacement.

Alignment of Temperature Stage

  1. Gently loosen the four allen screw (highlighted with blue marker) surrounding the sample stage.
  2. Move the holder up or down, using the micrometer, until the detector reading is one-half that when the stage is fully clear of the beam.  (When moving the stage down, gently tap on the top of the stage with a tool.)
  3. Tighten the screws and recheck the alignment.  Tightening the screws may cause the stage to move up slightly.

Instrument Set-up for Data Collection:

  1. Close the shutter.
  2. For reflection, use the same slits, drive the goniometer to the start angle, open the shutter, and adjust the power to just below the maximum of what the detector will allow.  Close the shutter and proceed to data collection.
  3. For diffraction, change the slits to:  source 1, 2, 0.5, 0.3 detector--and the power to 45 kV and 40 mA.

Data Collection

  1. Choose "Scan" on the toolbar.
  2. Choose the directory your file will be saved to (top bar).
  3. Enter the file name (less than 8 characters, no ".")
  4. Enter the file ID and comments if necessary
  5. Set up your scan by:
    1. Choose the "setup" window
    2. Enter a new scan setting name (or your existing one)
    3. Enter the scan settings (5.0 to 60.0, step of 0.04, dwell of 1.0, step scan)
    4. Save Setting
    5. Exit
  6. Click on "Go" to begin data collection.  (Clicking on the clock in the upper right corner will tell you how long the run will take.)
  7. To view the scan while in the data analysis program, highlight the "tack" on the toolbar.
  8. NOTE: You may analyze the scan while it is running.

Data Analysis

  1. Click on the "JADE" icon on the desktop.
  2. File, Open.
  3. Use the toolbar help for analysis-the left mouse key executes the command, the right mouse key provides the set-up menu.
  4. "Print setup" gives you the option of a color printout.
  5. Refer to the manual for specific information.

When Done

  1. Copy your files to a disk.
  2. Turn the power down to 3 ma and 9 kV.
  3. Clean up the sample preparation area.