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.
Adair, Keegan R.; Banis, Mohammad N.; Zhao, Yang; Bond, Toby; Li, Ruying and Sun, Xueliang. (2020). Temperature-dependent chemical and physical microstructure of Li metal anodes revealed through synchrotron-based imaging techniques. Advanced Materials 32, 2002550. 10.1002/adma.202002550
Lu, Mi; Yu, Fuda; Hu, Yongfeng; Zaghib, Karim; Schougaard, Steen B.; Wang, Zhenbo; Zhou, Jigang; Wang, Jian; Goodenough, John and Sham, T.K. (2020). Correlative imaging of ionic transport and electronic structure in nano Li0.5FePO4 electrodes. Chemical Communications 56(6), 984-987. 10.1039/c9cc09116e
Rasool, Majid; Chiu, Hsien-Chieh; Gauvin, Raynald; Jiang, De-Tong; Zhou, Jigang; Ryan, Dominic; Zaghib, Karim and Demopoulos, George P. (2020). Unusual Li-ion intercalation activation with progressive capacity increase in orthosilicate nanocomposite cathode. The Journal of Physical Chemistry 124(11), 5966-5977. 10.1021/acs.jpcc.9b11896
Rasool, Majid; Chiu, Hsien-Chieh; Zank, Benjamin; Zeng, Yan; Zhou, Jigang; Zaghib, Karim; Perepichka, Dmitrii F. and Demopoulos, George P. (2020). PEDOT encapsulated and mechanochemically engineered silicate nanocrystals for high energy density cathodes. Advanced Materials Interfaces 7(13), 200-226. 10.1002/admi.202000226
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.
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
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.
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
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.
Reid, Joel W. and Kaduk, James A. (2021). Crystal structure of donepezil hydrochloride form III, C24H29NO3-HCl. Powder Diffraction, 1-8. 10.1017/S0885715621000415
Reid, Joel W. (2021). Powder x-ray diffraction data for dimethylarsenic acid, (CH3)2AsO(OH). Powder Diffraction, 1-6. 10.1017/S0885715621000270
Leontowich, Adam F.G.; Gomez, Ariel; Moreno, Beatriz D.; Muir, David; Spasyuk, Denis; King, Graham; Reid, Joel W.; Kim, Chang-Yong and Kycia, Stefan. (2021). The lower energy diffraction and scattering side-bounce beamline for materials science at the Canadian Light Source. Journal of Synchrotron Radiation 28(3), 961-969. 10.1107/S1600577521002496
Zurakowski, Joseph A.; Bhattacharyya, Moulika; Spasyuk, Denis M. and Drover, Marcus W. (2021). Octaboraneyl [Ni(H)(diphosphine)2]+ complexes: Exploiting phosphine ligand lability for hydride transfer to an [NAD]+ model. Inorganic Chemistry 60(1), 37-41. 10.1021/acs.inorgchem.0c03409
Thiessen, Alyxandra N.; Zhang, Lijuan; Oliynyk, Anton O.; Yu, Haoyang; O'Connor, Kevin M.; Meldrum, Alkiviathes and Veinot, Jonathan G.C. (2020). A tale of seemingly "identical" silicon quantum dot families: Structural insight into silicon quantum dot photoluminescence. Chemistry of Materials 32(16), 6838-6846. 10.1021/acs.chemmater.0c00650
Nguyen, Minh Tho; Gusev, Dmitry; Dmitrienko, Anton; Gabidullin, Bulat M.; Spasyuk, Denis; Pilkington, Melanie and Nikonov, Georgii I. (2020). Ge(0) compound stabilized by a diimino-carbene ligand: Synthesis and ambiphilic reactivity. Journal of the American Chemical Society 142(12), 5852-5861. 10.1021/jacs.0c01283