First, the coverage of reciprocal space is significantly reduced due to limited X-ray angular access through the body of the DAC and the backing plates. Place the DAC in the sample holder, and put it on the diffractometer's sample stage. Kolokathis, Evangelia Pantatosaki, and George K.
Increase the pressure inside the DAC sample chamber by tightening the compressing screws of the DAC, and monitor the pressure with ruby fluorescence Chemistry of Materials , 24 13 , After completing the detector calibration, remove the LaB6 standard from the diffractometer.
Find the sample chamber with the viewing camera at the minimum magnification first. Langmuir , 34 4 ,
ACS Catalysis , 7 4 ,
Single crystal diffraction using a diamond anvil cell differs from diffraction at ambient conditions in several important ways. Chemistry of Materials , 28 7 , Ensure that the height of the diamond, the diameter of the back side of the diamond, the opening angle of the backing plate and the opening angle of the DAC are compatible with each other, so as to maximize the angular access for diffraction 9, Use the RSV plugin to find the preliminary UB matrix of this crystal and to index the diffraction peaks. The sample was aligned with the rotation center of the diffraction goniometer Figures 3, 4. The Journal of Physical Chemistry C , 33 ,
Then, apply about 0. Kolokathis, Evangelia Pantatosaki, and George K. The offsets of the X-ray transmission profiles are used to calculate the positional correction along the incident X-ray direction.
Reconstruct the diffraction peaks' distribution in reciprocal space.
Using the RSV software, open the first peak table file. Sample Preparation NOTE: The sample preparation process includes three major steps: preparing the empty DAC, loading the sample and loading the inert gas pressure transmitting medium. Second, the angle-dependent absorption of X-rays by the diamonds and backing plates must be determined and used to correct the diffraction signal so that accurate structure factors can computed. Detailed procedures for conducting structure refinement with SHELX have been well described elsewhere 19,
After saving the calibrations for all detector positions, create these associations by checking the "Assign cal" checkbox in the ATREX software, so that the program will remember which calibrations to use. Journal of the American Chemical Society , 15 , Michael T.
Since chemical composition strongly influences electric and magnetic properties of these materials [ 1 — 3 ], detailed information on their stoichiometry is required. With the refined UB matrix of the crystal, more diffraction peaks were found using the "Predict" function of the software Figure 8. Chemistry of Materials , 26 1 , The Journal of Physical Chemistry C , 34 , NOTE: The diameter of the culet depends on the target maximum pressure of the experiment. Vogiatzis, A.
Apply a few kg of load to the diamond with compressing screws, so that it is in intimate contact with the backing plate. Clean the diamonds and backing plates in an acetone ultrasonic bath for min.