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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.

We are developing a new hard x-ray nanoprobe beamline with 30 nm resolution at the Advanced Photon Source (APS). Imaging and spectroscopy at this resolution level require staging of x-ray optics and specimens with a mechanical repeatability of better than 10 nm. We have developed a prototype instrument with a novel interferometrically controlled scanning stage system. The system consists of nine DC-motor-driven stages, four picomotor-driven stages, and two PZT-driven stages. An APS-designed custom-built laser Doppler displacement meter system provides two-dimensional differential displacement measurement with subnanometer resolution between the zone-plate x-ray optics and the sample holder. Also included is the alignment and stable positioning of two stacked zone plates for increasing the focusing efficiency. The entire scanning system was designed with high stiffness, high repeatability, low drift, flexible scanning schemes, and possibility of fast feedback for differential motion. Designs of the scanning stage system, as well as preliminary mechanical test results, are presented in this paper.

The Advanced Photon Source is currently developing a suite of new hard x-ray beamlines, aimed primarily at the study of materials and devices under real conditions. One of the flagship beamlines of the APS Upgrade is the In-Situ Nanoprobe beamline (ISN beamline), which will provide in-situ and operando characterization of advanced energy materials and devices under change of temperature and gases, under applied fields, in 3D. The ISN beamline is designed to deliver spatially coherent x-rays with photon energies between 4 keV and 30 keV to the ISN instrument. As an x-ray source, a revolver-type undulator with two interchangeable magnetic structures, optimized to provide high brilliance throughout the range of photon energies of 4 keV – 30 keV, will be used. The ISN instrument will provide a smallest hard x-ray spot of 20 nm using diffractive optics, with sensitivity to sub-10 nm sample structures using coherent diffraction. Using nanofocusing mirrors in Kirkpatrick-Baez geometry, the ISN will also provide a focus of 50 nm with a flux of 8·1011 Photons/s at a photon energy of 10 keV, several orders of magnitude larger than what is currently available. This will allow imaging of trace amounts of most elements in the periodic table, with a sensitivity to well below 100 atoms for most metals in thin samples. It will also enable nanospectroscopic studies of the chemical state of most materials relevant to energy science. The ISN beamline will be primarily used to study inorganic and organic photovoltaic systems, advanced batteries and fuel cells, nanoelectronics devices, and materials and systems diesigned to reduce the environmental impact of combustion.

The planned Center for Nanoscale Materials (CNM) at Argonne National Laboratory is aimed at the development and study of the properties of nanomaterials and nanodevices. As part of the characterization instruments at CNM, we are developing a new hard x‐ray nanoprobe beamline at the Advanced Photon Source. The beamline will provide microscopy and spectroscopy for photon energies from 3 keV to 30 keV. Hard x‐ray zone plates will be used to achieve a spatial resolution of 30 nm in the 3 – 10 keV region. Two operational modes will combine the speed of a transmission x‐ray microscope with the analytic capabilities of a hard x‐ray microprobe. The major operation mode will be a scanning probe mode, where spatially coherent radiation is focused into a diffraction‐limited spot to excite secondary signals in the specimen. This will allow elemental mapping and spectroscopy at high sensitivity using x‐ray fluorescence, or strain contrast imaging using x‐ray diffraction. A secondary mode will use partially coherent radiation to provide transmission imaging in absorption and phase contrast for photon energies between 3 – 10 keV.