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In-situ/Operando X-ray Powder Diffraction


Real time monitoring of the formation of kinetic and thermodynamic products in a reaction is extremely important for the synthesis, isolation, and growth of new materials. Powder X-ray diffraction methods are proven to be an excellent probe for such in-situ/operando experiments . X-ray radiation of an appropriate wavelength can penetrate through the reaction vessel or device and provide diffraction information about solid-to-solid reactions, transformations, gas-to-solid interactions, liquid-to-solid crystal growth processes, and decomposition or intermediate products. Please check out some selected publications resulted by IMSERC users along with the list of other crystallographic services available in IMSERC.

User's Success Story

crystallography-success-story-mcclain-photo The in-situ PXRD capabilities at IMSERC have provided essential data for my doctoral work
Becca McClain
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Example of an in-situ diffraction pattern of a mixture of solid starting materials (left plot) showing two transformations and a melting event during heating. Thermal analysis (right plot) is a poweful complementary technique for probing thermal events in unexplored reaction systems


  • Monitor reactions in real time as a function of time, temperature, pressure, and gas flow/pressure
  • In-situ monitoring of crystallization processes with increasing temperature
  • Operando measurements
  • Accelarated aging measurements and stability tests
  • Phase identification in small size samples (<1mm)
  • Probe catalytic changes to substrates

Please visit our expanded list of application per research area for more details about this technique.

If you are interested in utilizing any of these applications for your research Start a project

Selected Publications

  • In-situ crystal growth using X-ray diffraction
    Phase Transitions in Metal–Organic Frameworks Directly Monitored through In Situ Variable Temperature Liquid-Cell Transmission Electron Microscopy and In Situ X-ray Diffraction
    Lyu, Jiafei; Gong, Xinyi; Lee, Seung-Joon; Gnanasekaran, Karthikeyan; Zhang, Xuan; Wasson, Megan C.; Wang, Xingjie; Bai, Peng; Guo, Xianghai; Gianneschi, Nathan C.; Farha, Omar K. [10.1021/jacs.0c00542]

  • Time-Resolved in Situ Polymorphic Transformation
    Time-Resolved in Situ Polymorphic Transformation from One 12-Connected Zr-MOF to Another
    Lee, S. J.; Mancuso, J. L.; Le, K. N.; Malliakas, C. D.; Bae, Y. S.; Hendon, C. H.; Islamoglu, T.; Farha, O. K. [10.1021/acsmaterialslett.0c00012]