1 Grazing angle diffraction and reflectivity step by step 11/16/2015 1) Log into the computer Login: XpertPro MRD user Pssw: XpertPro 2) Double-Click on the Data collector software short cut icon 3) log into the program using your login and password (if you do not have on contact Emmanuel Soignard; the account is generated during training) 4) go to menu : Instrument / connect and select the detector needed for your experiment: click no to reset the sample offsets The computer is now connected to the diffractometer
Transcript
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Grazing angle diffraction and reflectivity step by step 11/16/2015
1) Log into the computer Login: XpertPro MRD user Pssw: XpertPro 2) Double-Click on the Data collector software short cut icon
3) log into the program using your login and password (if you do not have on contact Emmanuel Soignard; the account is generated during training)
4) go to menu : Instrument / connect and select the detector needed for your experiment:
click no to reset the sample offsets The computer is now connected to the diffractometer
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5) Check that the selected optical components are correct Incident beam optics (make sure your anti-scatter slit is in place)
Click ok
Diffracted beam optics
Click ok 6) User settings: - Sample offset / clear all - Fine calibration offset / clear all 7) in Instrument settings (left hand side left most menu)
- Place all angles (2theta, offset, Omega, Phi, chi) and coordinates (X, Y) at zero and
Z = 7 mm if using a regular quartz plate Z = 8 mm if using thinner quartz plate Z = 9.5 for standard wafers
- Set the X-ray power to 45 kV and 40mA
8) MAKE SURE THE Cu attenuator is in place ( ) 9) - if doing XRR make sure the slit is in the PPC
- if doing grazing angle make sure the slit is removed from the PPC
11) go to User settings / fine calibration offsets and type 0 for the new position of 2 theta
12) make sure the sample is in the beam and parallel to the beam d) scan Z set half way point in intensity using move mode (release the mouse at the half way point)
e) scan ω set maximum as new ω (move mode)
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f) If the stage was moved at step e Repeat step d. 13) Close the manual scan windows
THE SURFACE OF THE SAMPLE IS NOW ALIGNED!!!
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14) You now want to measure you powder diffraction: a ) - for grazing angleRemove the Cu attenuator. - for reflectivity either keep attenuator or use a less strong attenuator c )File / Open Program / select your program
d) File / Save
e) Measure / Program - In the list find your program in the list. - click OK - Select the folder and data file name - click OK The program is now collecting your powder pattern. If you have another sample to run
- place the Cu filter back. - set 2 theta and omega to 0° - go back to step 12
When done with your cession: Click on Instrument settings Set 2θ at 10° and ω at 5°. X-ray tab: change power to 45 kV and 20 mA Place stronger Cu filter back in
You can now remove your sample and log out of the software.
Adjust to match the needed start and end angles of your scan
0.0125 for sharp peaks 0.025 for typical scans 0.05 or 0.1 when the peaks are very broad
The longer the time per step the better the signal to noise and the longer the scan
