Effect of synchrotron X-ray radiation damage on phase transitions in coordination polymers at high pressure

Abstract

The high-pressure phase-transition behaviour of metal–organic frameworks and coordination polymers upon varying degrees of X-ray irradiation are highlighted with four example studies. These show that, in certain cases, the radiation damage, while not extreme in changing unit-cell values, can impact the existence of a phase transition. In particular, pressure-induced phase transitions are suppressed after a certain absorbed dose threshold is reached for the sample. This is thought to be due to partial amorphization and/or defect formation in the sample, hindering the co-operative structural distortions needed for a phase transition. The high-pressure experiments were conducted with several crystals within the sample chamber in order to measure crystals with minimal X-ray irradiation at the highest pressures, which are compared with the crystals measured continuously upon pressure increase. Ways to minimize radiation damage are also discussed within the frame of high-pressure experiments.

Tracking structural phase transitions via single crystal x-ray diffraction at extreme conditions: advantages of extremely brilliant source

“…Synchrotrons benefit from the tuneable x-ray wavelength, but usually the data collection strategy is limited to a simple ω-scan, due to geometrical constraints of the heavy-duty goniometers. High-energy photons at the synchrotron source may additionally cause radiation damage, which should be checked before loading the sample in DAC [27,28].…”

Beam Effects in Synchrotron Radiation Operando Characterization of Battery Materials: X-Ray Diffraction and Absorption Study of LiNi0.33Mn0.33Co0.33O2 and LiFePO4 Electrodes

“…Beam effects range from reversible to permanent alterations, such as loss of resolution in irradiated protein crystals, beam-induced phase transitions in coordination polymers, , changes in crystal nucleation and metal oxidation states, , metal ion reduction and water radiolysis in aqueous solutions, , and even total sample obliteration in extreme cases, such as with X-ray free-electron lasers (FELs). , These effects span a wide range of energies (5–50 keV), techniques, and material types.…”