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Infrared Spectroscopy and Spectro-Microscopy with Synchrotron Radiation

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Infrared Spectroscopy and Spectro-Microscopy with Synchrotron Radiation BNL-213673-2020-BOOK Infrared Spectroscopy and spectro-microscopy with synchrotron radiation P. Dumas, G. L. Carr To be published in "Synchrotron Light Sources and Free-Electron Lasers" January 2020 Photon Sciences Brookhaven National Laboratory U.S. Department of Energy USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22) Notice: This manuscript has been authored by employees of Brookhaven Science Associates, LLC under Contract No. DE-SC0012704 with the U.S. Department of Energy. The publisher by accepting the manuscript for publication acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce the published form of this manuscript, or allow others to do so, for United States Government purposes. DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, nor any of their contractors, subcontractors, or their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or any third party’s use or the results of such use of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof or its contractors or subcontractors. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. From Synchrotron Light Sources and Free-Electron Lasers (Springer, 2020) INFRARED SPECTROSCOPY AND SPECTRO-MICROSCOPY WITH SYNCHROTRON RADIATION Paul Dumas*a, Michael C. Martinb and G. Lawrence Carrc a SOLEIL Synchrotron, L’Orme des Merisiers, Saint Aubin, BP48- 91192- Gif Sur Yvette Cedex (France) b Advanced Light Source, 1 Cyclotron Road, Lawrence Berkeley National Laboratory, Berkeley CA 94720-8229 (USA) c National Synchrotron Light Source II, Bldg. 741, Brookhaven National Laboratory, Upton NY 11973-5000 (USA) Contents Introduction Source Types and Characteristics Dipole Bend Radiation (conventional Synchrotron Radiation) Approximate Expressions Gaussian Beam Parameters Edge, Transition and Diffraction radiation Long Wavelength Cutoff Electron Bunching and Coherence Time-resolved Spectroscopy Coherent Emission Light Hazards, Optics and Instrumentation Light Hazards Optics First Mirror Beam Propagation Aberration-free Optical Designs Instrumentation Spectrometers Spectral Resolution Microscopes Detectors Beyond the Diffraction Limit: Towards Sub-Wavelength and Nanospectroscopy Array Detector Imaging and Oversampling Scanning Probe Systems Applications 1 From Synchrotron Light Sources and Free-Electron Lasers (Springer, 2020) Spectroscopy using non-coherent far-IR synchrotron radiation Solid State Physics Gas Phase Surface Science Microscopy at diffraction-limited spot size Material Science Extreme Conditions Earth and Planetary Science Archaeology Biology Spectroscopy using Coherent Radiation Nanospectroscopy and Nanoimaging References Abstract This chapter addresses the general properties of infrared radiation as produced at synchrotron light source facilities as well as the optical systems for extracting the light and matching it to various infrared instruments. As such, it can serve as a guide for understanding basic radiation properties as well as for the successful design of a beamline to perform infrared microspectroscopy. The bending magnets that steer the synchrotron electron beam into a circular orbit serve as the essential source of infrared emission, and simplified formulas are provided to allow calculating flux and brilliance for a particular beamline design. Various optical designs for collecting the infrared and efficiently propagating it to the measurement instruments are also presented, including a novel optical design for managing the large source depth. A wide range of measurement techniques and associated instrumentation have been reported over the last twenty-five years, and some of the more recently developed techniques are described here with examples. Spectroscopy and microscopy (especially in combination) are among the most prevalent techniques and continue to evolve via new instruments for near-field nanospectroscopy and tomography. Infrared detectors are a mostly well- developed technology so only a basic overview is provided here as guidance for the types commonly used with the synchrotron infrared source. An exception is the need for detectors to enable near-field nanospectroscopy across the entire far-infrared and 2D detector arrays for complete spectroscopic imaging. Glossary • AFM Atomic Force Microscope • ALS Advanced Light Source (Berkeley, CA, USA) • BESSY Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung (Berlin, Germany) • CGS centimeter, grams, seconds and Gaussian unit system • CLS Canadian Light Source (Saskatoon, Canada) • CVD Chemical Vapor Deposition (for diamond) • ER Edge Radiation • ETH Eidgenössische Technische Hochschule (Swiss Federal Institute of Technology) 2 From Synchrotron Light Sources and Free-Electron Lasers (Springer, 2020) • FPA Focal Plane Array (2D detector array) • FTIR Fourier Transform InfraRed • FWHM Full Width at Half Maximum • IR Infrared • IRENI Infrared imaging beamline at the former SRC • LURE Laboratory for the Utilization of Radiation Electromagnetic at Univ. of Paris – Sud • MAX-Lab Accelerator and light source facility in Lund, Sweden • MCT Mercury Cadmium Telluride • NA Numerical Aperture ( = n sin for a focus half angle in a medium of refractive index n) • Nd:YAG Neodymium Yttrium Aluminum Garnet (laser) • NSLS National Synchrotron Light Source (Upton, NY, USA) • NSLS-II National Synchrotron Light Source II (Upton, NY, USA) • rad Radian (angular unit of measure) • RF Radio Frequency • RMS Root Mean Square • SI Système International (Int’l System of Units) • SLS Swiss Light Source (Paul Scherrer Inst., Switzerland) • sr Steradian (solid angle unit of measure) • SRC Synchrotron Radiation Center (Stoughton, WI, USA) • SOLEIL Synchrotron Soleil (Saint Aubin, France) • SOR Synchrotron Orbital Radiation (Okazaki, Japan) • SRW Synchrotron Radiation Workshop (software) • s-SNOM scattering-type Scanning Near-field Optical Microscopy • THz Terahertz • Ti:S Titanium Sapphire (laser) • UHV Ultra-High Vacuum Introduction Interest in infrared synchrotron radiation began in the late 1970’s (Lagarde 1978; Stevenson and Cathcart 1980; Williams 1982; Duncan and Williams 1983), with the characteristics of the infrared synchrotron source being well-described. These include being highly polarized, pulsed, and having a spectrally broad emission. Most significantly, it is typically more than 1 thousand times more brilliant than the standard thermal source used for most infrared spectroscopy. Two of the earliest reports on infrared synchrotron radiation came from the original BESSY in Berlin, Germany (Schweizer 1985) and SOR facility in Okazaki, Japan (Nanba 1986). It has since developed into an important source for a variety of throughput-limited measurement techniques that have impacted many different scientific disciplines (e.g. biology & medicine, materials science, earth & space sciences, and catalysis). While spectro-microscopy has been the dominant measurement technique, the source has proved important for grazing incidence reflection/absorption spectroscopy (for surface studies), ellipsometry (for directly extracting optical response functions), and very high-resolution spectroscopy. The pulsed nature of the source has also been exploited for time-resolved spectroscopy. New techniques under development include near-field nano-spectroscopy and tomography. Though there are 3 From Synchrotron Light Sources and Free-Electron Lasers (Springer, 2020) many types of infrared sources based on electron accelerators (e.g. free electron lasers), the scope of this chapter is limited to high-energy electron synchrotron / storage ring type sources. Therefore, only the source types that produce a continuum of photon energies (frequencies) from millimeter waves through visible light — such as dipole bending magnet radiation — are considered here. The design of an optimized facility for infrared synchrotron radiation science must manage several constraints associated with the environment of a high energy electron accelerator and storage ring. As will be shown below, the requirements for large vertical and horizontal collection angles can be difficult to fulfill and tend to limit performance in the far-infrared to millimeter spectral ranges. The variety of measurement techniques have expanded in concert with improvements in beamline optical designs for matching the source to the instrumentation. These designs require a detailed knowledge of all characteristics of emitted radiation such as the intensity distribution, polarization and phase distribution. In the analysis to follow, it is assumed that the synchrotron source of interest is a storage ring employing high energy (>500 MeV) electrons such that all photon energies of interest — from a few eV down to below 1 meV — are far below the critical frequency for dipole bend sources defined as 3 c 3 C = {1} 4 where
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