DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Modular soft x-ray spectrometer for applications in energy sciences and quantum materials

Journal Article · · Review of Scientific Instruments
DOI: https://doi.org/10.1063/1.4974356 · OSTI ID:1361744
 [1];  [2];  [1];  [1];  [1];  [3];  [1];  [1];  [1];  [4];  [5];  [6];  [7];  [6]; ORCiD logo [8];  [2];  [1];  [1]; ORCiD logo [9]; ORCiD logo [1] more »; ORCiD logo [1];  [1];  [1] « less
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
  2. Tamkang Univ., New Taipei City (Taiwan)
  3. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Univ. of California, Berkeley, CA (United States)
  4. Lund Univ., Lund (Sweden)
  5. New York Univ. (NYU), New York, NY (United States)
  6. SLAC National Accelerator Lab., Menlo Park, CA (United States)
  7. SLAC National Accelerator Lab., Menlo Park, CA (United States); Stanford Univ., Stanford, CA (United States)
  8. National Univ. of Kaohsiung, Kaohsiung (Taiwan)
  9. Argonne National Lab. (ANL), Argonne, IL (United States)

Over the past decade, the advances in grating-based soft X-ray spectrometers have revolutionized the soft X-ray spectroscopies in materials research. However, these novel spectrometers are mostly dedicated designs, which cannot be easily adopted for applications with diverging demands. Here we present a versatile spectrometer design concept based on the Hettrick-Underwood optical scheme that uses modular mechanical components. The spectrometer’s optics chamber can be used with gratings operated in either inside or outside orders, and the detector assembly can be reconfigured accordingly. The spectrometer can be designed to have high spectral resolution, exceeding 10 000 resolving power when using small source (~1μm) and detector pixels (~5μm) with high line density gratings (~3000 lines/mm), or high throughput at moderate resolution. We report two such spectrometers with slightly different design goals and optical parameters in this paper. We show that the spectrometer with high throughput and large energy window is particularly useful for studying the sustainable energy materials. We demonstrate that the extensive resonant inelastic X-ray scattering (RIXS) map of battery cathode material LiNi1/3Co1/3Mn1/3O2 can be produced in few hours using such a spectrometer. Unlike analyzing only a handful of RIXS spectra taken at selected excitation photon energies across the elemental absorption edges to determine various spectral features like the localized dd excitations and non-resonant fluorescence emissions, these features can be easily identified in the RIXS maps. Studying such RIXS maps could reveal novel transition metal redox in battery compounds that are sometimes hard to be unambiguously identified in X-ray absorption and emission spectra. As a result, we propose that this modular spectrometer design can serve as the platform for further customization to meet specific scientific demands.

Research Organization:
Argonne National Laboratory (ANL), Argonne, IL (United States); SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States); Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE
Grant/Contract Number:
AC02-06CH11357; AC02-76SF00515; AC02-05CH11231
OSTI ID:
1361744
Alternate ID(s):
OSTI ID: 1353087; OSTI ID: 1365830; OSTI ID: 1420488; OSTI ID: 1530269
Journal Information:
Review of Scientific Instruments, Vol. 88, Issue 1; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)Copyright Statement
Country of Publication:
United States
Language:
English

References (46)

Plane-grating flat-field soft x-ray spectrometer journal February 2005
High resolution X-ray spectroscopy with silicon drift detectors and integrated electronics
  • Bertuccio, G.; Sampietro, M.; Fazzi, A.
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 322, Issue 3 https://doi.org/10.1016/0168-9002(92)91228-2
journal November 1992
Linac Coherent Light Source: The first five years journal March 2016
Optimization of high count rate event counting detector with Microchannel Plates and quad Timepix readout
  • Tremsin, A. S.; Vallerga, J. V.; McPhate, J. B.
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 787 https://doi.org/10.1016/j.nima.2014.10.047
journal July 2015
Novel high-resolution silicon drift detectors journal July 2004
Review of superconducting transition-edge sensors for x-ray and gamma-ray spectroscopy journal July 2015
Centroid position measurements and subpixel sensitivity variations with the MAMA detector journal January 1989
A new compact soft x-ray spectrometer for resonant inelastic x-ray scattering studies at PETRA III journal September 2015
Lithium Batteries and Cathode Materials journal October 2004
Design of a novel transmission-grating spectrometer for soft X-ray emission studies journal June 2005
Issues and challenges facing rechargeable lithium batteries journal November 2001
Charge-compensation in 3d-transition-metal-oxide intercalation cathodes through the generation of localized electron holes on oxygen journal March 2016
Numerical optimization of spherical variable-line-spacing grating X-ray spectrometers journal January 2011
Design and performance of AERHA, a high acceptance high resolution soft x-ray spectrometer journal April 2014
Resonant X-Ray Raman Spectra of Cu dd Excitations in Sr 2 CuO 2 Cl 2 journal June 1998
Soft x‐ray emission spectroscopy using monochromatized synchrotron radiation (invited) journal July 1989
SAXES, a high resolution spectrometer for resonant x-ray emission in the 400–1600eV energy range journal November 2006
Resonant inelastic x-ray scattering studies of elementary excitations journal June 2011
Prospects of high-resolution resonant X-ray inelastic scattering studies on solid materials, liquids and gases at diffraction-limited storage rings journal August 2014
Recent Progress on Synchrotron-Based In-Situ Soft X-ray Spectroscopy for Energy Materials journal May 2014
Resonant inelastic x-ray scattering of MnO : L 2 , 3 edge measurements and assessment of their interpretation journal January 2006
Ultrahigh resolution soft x-ray emission spectrometer at BL07LSU in SPring-8 journal January 2012
Superconducting Tunnel Junction Array Development for High-Resolution Energy-Dispersive X-ray Spectroscopy journal December 1998
New Developments in Superconducting Tunnel Junction X-Ray Spectrometers for Synchrotron Science journal January 2012
High-resolution soft X-ray beamline ADRESS at the Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies journal July 2010
Design of a Holographically Recorded Plane Grating with a Varied Line Spacing for a Soft X-ray Grazing-Incidence Monochromator journal November 1996
X-Ray Wavelengths journal January 1967
Novel instruments for ultra-soft X-ray emission spectroscopy
  • Agåker, M.; Andersson, J.; Englund, C. -J.
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 601, Issue 1-2 https://doi.org/10.1016/j.nima.2008.12.227
journal March 2009
Transmission-grating spectrometer for highly efficient and high-resolution soft X-ray emission studies journal June 2013
Core Level Spectroscopy of Solids book January 2008
High-resolution, high-transmission soft x-ray spectrometer for the study of biological samples journal June 2009
SHADOW3 : a new version of the synchrotron X-ray optics modelling package journal July 2011
Progress in resonant inelastic X-ray scattering journal June 2013
Design of a variable-included-angle Monk–Gillieson monochromator with varied-line-spacing gratings journal February 2004
Distinct charge dynamics in battery electrodes revealed by in situ and operando soft X-ray spectroscopy journal October 2013
High-efficiency in situ resonant inelastic x-ray scattering (iRIXS) endstation at the Advanced Light Source journal March 2017
Perspectives of in situ/operando resonant inelastic X-ray scattering in catalytic energy materials science journal April 2015
Towards 10 meV resolution: The design of an ultrahigh resolution soft X-ray RIXS spectrometer journal November 2016
Stigmatic high throughput monochromator for soft x rays journal January 1986
Quantitative probe of the transition metal redox in battery electrodes through soft x-ray absorption spectroscopy journal September 2016
Key electronic states in lithium battery materials probed by soft X-ray spectroscopy journal October 2013
The development of in situ photon-in/photon-out soft X-ray spectroscopy on beamline 7.0.1 at the ALS journal June 2013
Layered Lithium Insertion Material of LiCo 1/3 Ni 1/3 Mn 1/3 O 2 for Lithium-Ion Batteries journal July 2001
High-resolution soft X-ray emission spectrograph at advanced light source journal December 2005
Issues and challenges facing rechargeable lithium batteries book October 2010
Lithium Batteries and Cathode Materials journal December 2004

Cited By (29)

In‐Situ/Operando X‐ray Characterization of Metal Hydrides journal March 2019
X-ray Microscopy book January 2019
Coupling between oxygen redox and cation migration explains unusual electrochemistry in lithium-rich layered oxides journal December 2017
Monovalent manganese based anodes and co-solvent electrolyte for stable low-cost high-rate sodium-ion batteries journal February 2018
Elucidating anionic oxygen activity in lithium-rich layered oxides journal March 2018
Ultrahigh power and energy density in partially ordered lithium-ion cathode materials journal March 2020
Metal–oxygen decoordination stabilizes anion redox in Li-rich oxides journal February 2019
High-efficiency in situ resonant inelastic x-ray scattering (iRIXS) endstation at the Advanced Light Source journal March 2017
Soft X-ray spectroscopy with transition-edge sensors at Stanford Synchrotron Radiation Lightsource beamline 10-1 journal November 2019
Evolution of superconductivity in K 2−x Fe 4+y Se 5 : Spectroscopic studies of X-ray absorption and emission journal October 2019
Ultrafast magnetodynamics with free-electron lasers journal January 2018
Ultrafast dynamics of spin and orbital correlations in quantum materials: an energy- and momentum-resolved perspective
  • Cao, Y.; Mazzone, D. G.; Meyers, D.
  • Philosophical Transactions of the Royal Society A: Mathematical, Physical and Engineering Sciences, Vol. 377, Issue 2145 https://doi.org/10.1098/rsta.2017.0480
journal April 2019
Towards an extremely high resolution broad-band flat-field spectrometer in the `water window' journal June 2019
Characterization of the soft X-ray spectrometer PEAXIS at BESSY II journal January 2020
Dissociate lattice oxygen redox reactions from capacity and voltage drops of battery electrodes journal February 2020
Ultrafast time-resolved x-ray scattering reveals diffusive charge order dynamics in La 2– x Ba x CuO 4 journal August 2019
X-ray spectroscopy with variable line spacing based on reflection zone plate optics journal January 2018
Resonant Inelastic X-Ray Scattering Reveals Hidden Local Transitions of the Aqueous OH Radical text January 2020
Resonant Inelastic X-Ray Scattering Reveals Hidden Local Transitions of the Aqueous OH Radical journal June 2020
X-ray spectroscopy with variable line spacing based on reflection zone plate optics text January 2018
Characterization of the soft X-ray spectrometer PEAXIS at BESSY II text January 2019
X-ray microscopy journal July 1965
Ultrafast dynamics of spin and orbital correlations in quantum materials: an energy- and momentum-resolved perspective text January 2018
Coupling between oxygen redox and cation migration explains unusual electrochemistry in lithium-rich layered oxides journal December 2017
Monovalent manganese based anodes and co-solvent electrolyte for stable low-cost high-rate sodium-ion batteries journal February 2018
Elucidating anionic oxygen activity in lithium-rich layered oxides journal March 2018
Transmission zone plates as analyzers for efficient parallel 2D RIXS-mapping journal August 2017
Dissociate lattice oxygen redox reactions from capacity and voltage drops of battery electrodes journal February 2020
Ultrafast dynamics of spin and orbital correlations in quantum materials: an energy- and momentum-resolved perspective text January 2018