Energy Storage

Synchrotron techniques provide ways to see inside operating batteries and fuel cells, providing new insights into chemicals and physical changes within devices.

Many advanced electrochemical tools are available to battery and fuel cell manufacturers, but these techniques often don't provide information on the underlying mechanisms and material changes that occur inside the cell. Synchrotron techniques provide a way to observe changes in material properties such as oxidation state or crystalline phase. They also allow for the non-destructive, in situ analysis of complex electrochemical reactions in operating devices. Many synchrotron techniques are also element-specific, which is especially important for targeted analysis of alloy-based electrode materials.

Techniques:

POWDER X-RAY DIFFRACTION (PXRD) COMPUTED TOMOGRAPHY (CT) X-RAY ABSORPTION SPECTROSCOPY (XAS) X-RAY SPECTROMICROSCOPY X-RAY PHOTOELECTRON SPECTROSCOPY (XPS)

Pereira, T. L. E., Serrano-Sevillano, J., Moreno, B. D., Reid, J., Carlier, D., & Goward, G. (2024). A combined 7li NMR, density functional theory and operando synchrotron X-ray powder diffraction to investigate a structural evolution of cathode material lifev2O7. Faraday Discussions. https://doi.org/10.1039/d4fd00077c

Zhou, L., Bazak, J. D., Singh, B., Li, C., Assoud, A., Washton, N. M., Murugesan, V., & Nazar, L. F. (2023). A new sodium thioborate fast ion conductor: Na3B5s9. Angewandte Chemie International Edition, 62(30). https://doi.org/10.1002/anie.202300404

Zhang, N., Yu, H., Murphy, A., Garayt, M., Yu, S., Rathore, D., Leontowich, A., Bond, T., Kim, C.-Y., & Dahn, J. R. (2023). A liquid and waste-free method for preparing single crystal positive electrode materials for Li-Ion Batteries. Journal of The Electrochemical Society, 170(7), 070515. https://doi.org/10.1149/1945-7111/ace4f7

Xu, J., Pollard, T. P., Yang, C., Dandu, N. K., Tan, S., Zhou, J., Wang, J., He, X., Zhang, X., Li, A.-M., Hu, E., Yang, X.-Q., Ngo, A., Borodin, O., & Wang, C. (2023). Lithium halide cathodes for Li Metal batteries. Joule, 7(1), 83–94. https://doi.org/10.1016/j.joule.2022.11.002

Sun, G., Yu, F.-D., Lu, M., Zhu, Q., Jiang, Y., Mao, Y., McLeod, J. A., Maley, J., Wang, J., Zhou, J., & Wang, Z. (2022). Surface chemical heterogeneous distribution in over-lithiated li1+xcoo2 electrodes. Nature Communications, 13(1). https://doi.org/10.1038/s41467-022-34161-4

Composites

Uncovering the complex physical and chemical interactions between the components of composite materials is a unique advantage of synchrotron-based techniques.

Synchrotron-based x-ray imaging has proven extremely useful for imaging the microstructure of composite materials like carbon fiber, alloys, fiberglass, and laminar structures. Synchrotron-based imaging is also much faster than conventional techniques, allowing for in-situ imaging of defects, damage, stress, and manufacturing processes like resin curing. Other techniques allow us to probe the chemistry of material interfaces at the nanometer scale, which can provide invaluable information about how component materials interact with each other.

Techniques:

COMPUTED TOMOGRAPHY (CT) X-RAY ABSORPTION SPECTROSCOPY (XAS)

Xu, S., Hou, X., Wang, D., Zuin, L., Zhou, J., Hou, Y., & Mann, M. (2022). Insights into the effect of heat treatment and carbon coating on the electrochemical behaviors of SIO anodes for li‐ion batteries. Advanced Energy Materials, 12(18). https://doi.org/10.1002/aenm.202200127

Sun, Tianxiao; Sun, Gang; Yu, Fuda; Mao, Yongzhi; Tai, Renzhong; Zhang, Xiangzhi; Shao, Guangjie; Wang, Zhenbo; Wang, Jian and Zhou, Jigang. (2021). Soft x-ray ptychography chemical imaging of degradation in a composite surface-reconstructed Li-rich cathode. ACS Nano 15(1), 1475-1485. 10.1021/acsnano.0c08891

Catalysts

Catalysis is a well-established application of synchrotron spectroscopy, where experiments can be carried out in situ to monitor changes in metal chemistry and reaction intermediates.

Synchrotron-based spectroscopy is uniquely suited for the chemical analysis of catalytic systems. Many synchrotron techniques are surface-sensitive and element-specific, allowing for targeted analysis of complex catalytic reactions. Several facilities within the CLS are outfitted with gas- and fluid-flow cells so that processes like degradation and catalyst poisoning can be monitored in situ. Synchrotron techniques provide direct information on important catalytic properties like oxidation state, crystalline phase, and coordination chemistry.

Techniques:

POWDER X-RAY DIFFRACTION (PXRD) SMALL ANGLE X-RAY SCATTERING (SAXS) X-RAY ABSORPTION SPECTROSCOPY (XAS) X-RAY SPECTROMICROSCOPY

Gusev, Dmitry G. and Spasyuk, Denis M. (2018). Revised mechanisms for aldehyde disproportionation and the related reactions of the Shvo catalyst. ACS Catalysis 8, 6851-6861. 10.1021/acscatal.8b01153

Materials Chemistry

Designing new materials with novel functional properties requires understanding the interplay of structure and composition across different length and time scales, a major strength of synchrotron techniques.

Understanding the function of new materials requires capabilities that bridge length scales, from atomic to macroscopic, for both bulk materials and surfaces. Synchrotrons provide a wealth of techniques to aid a complete understanding of the chemistry and function of new materials, from determining crystal structure or the functional role of a trace element, to imaging surfaces or mapping three-dimensional microstructure. Many of these techniques can be applied in situ or operando, to gain insight into material performance under real operating conditions.

Techniques:

POWDER X-RAY DIFFRACTION (PXRD) COMPUTED TOMOGRAPHY (CT) X-RAY ABSORPTION SPECTROSCOPY (XAS) X-RAY SPECTROMICROSCOPY

Vázquez, M. C., Reid, J. W., Avila, Y., González, M., Sánchez, L., Martínez-dlCruz, L., Rodríguez-Hernández, J., Moreno, B. D., & Reguera, E. (2024). Fe(L)2[M(CN)4] with L = 4-ethyl isonicotinate and M = ni, pd, pt.─a series of Hofmann-type frameworks with spin crossover: The dominant role of the fe–NC coordination bond. The Journal of Physical Chemistry C, 128(22), 9353–9363. https://doi.org/10.1021/acs.jpcc.4c01838

Lin, L., Tresp, D. S., Spasyuk, D. M., Lalancette, R. A., & Prokopchuk, D. E. (2024). Accessing ni(0) to ni(iv) via nickel–carbon–phosphorus bond reorganization. Chemical Communications, 60(6), 674–677. https://doi.org/10.1039/d3cc04687g

Bai, Y., Nasr, P., King, G., Reid, J. W., Leontowich, A. F., Corradini, M. G., Weiss, R. G., Auzanneau, F.-I., & Rogers, M. A. (2023). Halogen- and hydrogen-bonded self-assembled fibrillar networks of substituted 1,3:2,4-dibenzylidene-d-sorbitols (DBS). Nanoscale, 15(42), 16933–16946. https://doi.org/10.1039/d3nr03988a

Huynh, R. P., Evans, D. R., Lian, J. X., Spasyuk, D., Siahrostrami, S., & Shimizu, G. K. (2023). Creating order in ultrastable phosphonate metal–organic frameworks via isolable hydrogen-bonded intermediates. Journal of the American Chemical Society, 145(39), 21263–21272. https://doi.org/10.1021/jacs.3c05279

Beh, D. W., Cuellar De Lucio, A. J., del Rosal, I., Maron, L., Spasyuk, D., Gelfand, B. S., Li, J.-B., & Piers, W. E. (2023). Organotitanium complexes supported by a dianionic pentadentate ligand. Organometallics, 42(11), 1149–1157. https://doi.org/10.1021/acs.organomet.2c00609

Energy Materials

Bringing the power of synchrotron-based tools to advanced materials science and research.

Energy Storage

Synchrotron techniques provide ways to see inside operating batteries and fuel cells, providing new insights into chemicals and physical changes within devices.

Composites

Uncovering the complex physical and chemical interactions between the components of composite materials is a unique advantage of synchrotron-based techniques.

Catalysts

Catalysis is a well-established application of synchrotron spectroscopy, where experiments can be carried out in situ to monitor changes in metal chemistry and reaction intermediates.

Materials Chemistry

Designing new materials with novel functional properties requires understanding the interplay of structure and composition across different length and time scales, a major strength of synchrotron techniques.

Case Studies