SAXS Batch Data Analysis Reveals Particle Size Temporal Evolution

Time-resolved Small Angle X-Ray Scattering (SAXS) measurements, performed during synthesis procedures or other physical or chemical reactions, can reveal valuable information,¹ which can be employed to optimize the process or design materials with specific properties. 

These experiments tend to result in a large data set that follows the system's progression as a function of varying parameters (temperature, concentration, time, etc.).

All data files must be analyzed in a consistent manner to extract the evolution of a particular parameter, such as size, polydispersity, or shape. This application note exemplifies the use of batch mode analysis of XSACT software.

The high surface areas and inherent microporosity of zeolitic imidazolate frameworks have generated significant scientific attention. This is because these properties make them promising candidates for various applications, including gas separation and storage, chromatography, drug delivery, and catalysis.

It has been demonstrated that particle shape and size can be modified by controlling the chemistry during the initial stages of synthesis.²

At the Brazilian Synchrotron Light Laboratory, SAXS experiments have been used to study the synthesis of ZIF-8 (LNLS).³ The time-dependent size evolution has subsequently been extracted and is detailed in this article in combination with the methods used. 

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Acknowledgments

The data set was provided by Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas (INIFTA).

References

1. Xenocs application highlight: In-situ Small Angle X-ray Scattering for nanoparticle characterization. [Online]. Available: https://www.xenocs.com/in-situ-small-angle-x-ray-scattering-for-nanoparticle-characterization/
2. Sindoro, Melinda, Nobuhiro Yanai, Ah-Young Jee, and Steve Granick. “Colloidal-sized metal-organic frameworks: synthesis and applications.” Accounts of chemical research 47, no. 2 (2014): 459-469
3. Segovia, Gustavo M., Juan A. Allegretto, Jimena S. Tuninetti, Lucía B. Pizarro, Agustín S. Picco, Marcelo Ceolín, Tanja Ursula Lüdtke et al. “Post-synthetic modification and chemical modulation of the ZIF-8 MOF using 3-mercaptopropionic acid (MPA): a multi-technique study on thermodynamic and kinetic aspects.” Molecular Systems Design & Engineering (2022)

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