A Next-Generation Hard X-Ray Nanoprobe Beamline for In Situ Studies of Energy Materials and Devices


The Advanced Photon Source is developing a suite of new X-ray beamlines to study materials and devices across many length scales and under real conditions. One of the flagship beamlines of the APS upgrade is the In Situ Nanoprobe (ISN) beamline, which will provide in situ and operando characterization of advanced energy materials and devices under varying temperatures, gas ambients, and applied fields, at previously unavailable spatial resolution and throughput. Examples of materials systems include inorganic and organic photovoltaic systems, advanced battery systems, fuel cell components, nanoelectronic devices, advanced building materials and other scientifically and technologically relevant systems. To characterize these systems at very high spatial resolution and trace sensitivity, the ISN will use both nanofocusing mirrors and diffractive optics to achieve spots sizes as small as 20 nm. Nanofocusing mirrors in Kirkpatrick–Baez geometry will provide several orders of magnitude increase in photon flux at a spatial resolution of 50 nm. Diffractive optics such as zone plates and/or multilayer Laue lenses will provide a highest spatial resolution of 20 nm. Coherent diffraction methods will be used to study even small specimen features with sub-10 nm relevant length scale. A high-throughput data acquisition system will be employed to significantly increase operations efficiency and usability of the instrument. The ISN will provide full spectroscopy capabilities to study the chemical state of most materials in the periodic table, and enable X-ray fluorescence tomography. In situ electrical characterization will enable operando studies of energy and electronic devices such as photovoltaic systems and batteries. We describe the optical concept for the ISN beamline, the technical design, and the approach for enabling a broad variety of in situ studies. We furthermore discuss the application of hard X-ray microscopy to study defects in multi-crystalline solar cells, one of the lines of inquiries for which the ISN is being developed.

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We thank Wenjun Liu for continued productive discussions on nanofocusing mirrors and nanopositioning. We thank Oliver Schmidt for his help in beamline design work, Roger Dejus for preparing tuning curves for the ISN undulator, and Lahsen Assoufid for his suggestions on X-ray mirrors. We furthermore thank our colleagues Seth Darling, Conal Murray, Tijana Rajh, Wilson Chiu, Ken Kemner, Paolo Monteiro, Ellery Ingall, Yong Chu, and Hanfei Yan for their valuable scientific and technical discussions, and their continued engagement in the ISN facility. T.B. acknowledges funding from U.S. Department of Energy SunShot Initiative under Contracts No. DE-EE0005314, DE-EE0005329, and DE-EE0005948. Use of the Advanced Photon Source (APS) at Argonne National Laboratory was supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

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Maser, J., Lai, B., Buonassisi, T. et al. A Next-Generation Hard X-Ray Nanoprobe Beamline for In Situ Studies of Energy Materials and Devices. Metall Mater Trans A 45, 85–97 (2014). https://doi.org/10.1007/s11661-013-1901-x

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  • Mirror System
  • Diffractive Optic
  • Advance Photon Source
  • Insertion Device
  • Double Crystal Monochromator