Towards efficient time-resolved X-ray absorption studies of electron dynamics at photocatalytic interfaces

Neppl, Stefan; Mahl, Johannes; Tremsin, Anton S; Rude, Bruce; Qiao, Ruimin; Yang, Wanli; Guo, Jinghua; Gessner, Oliver

doi:10.1039/c6fd00125d

Title: Towards efficient time-resolved X-ray absorption studies of electron dynamics at photocatalytic interfaces

Abstract

We present a picosecond time-resolved X-ray absorption spectroscopy (tr-XAS) setup designed for synchrotron-based studies of interfacial photochemical dynamics. The apparatus combines a high power, variable repetition rate picosecond laser system with a time-resolved X-ray fluorescence yield detection technique. Time-tagging of the detected fluorescence signals enables the parallel acquisition of X-ray absorption spectra at a variety of pump–probe delays employing the well-defined time structure of the X-ray pulse trains. The viability of the setup is demonstrated by resolving dynamic changes in the fine structure near the O1s X-ray absorption edge of cuprous oxide (Cu₂O) after photo-excitation with a 355 nm laser pulse. Two distinct responses are detected. A pronounced, quasi-static, reversible change of the Cu₂O O1s X-ray absorption spectrum by up to ~30% compared to its static line shape corresponds to a redshift of the absorption edge by ~1 eV. This value is small compared to the 2.2 eV band gap of Cu₂O but in agreement with previously published results. Here, the lifetime of this effect exceeds the laser pulse-to-pulse period of 8 μs, resulting in a quasi-static spectral change that persists as long as the sample is exposed to the laser light, and completely vanishes once the laser is blocked.more »« less

Authors:

Neppl, Stefan ^[1]; Mahl, Johannes ^[1]; Tremsin, Anton S ^[2]; Rude, Bruce ^[1]; Qiao, Ruimin ^[1]; Yang, Wanli ^[1]; Guo, Jinghua ^[1]; Gessner, Oliver ^[1]

Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Univ. of California, Berkeley, CA (United States)

Publication Date:: Wed May 18 00:00:00 EDT 2016

Research Org.:: Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

OSTI Identifier:: 1845090

Grant/Contract Number:: AC02-05CH11231

Resource Type:: Accepted Manuscript

Journal Name:: Faraday Discussions

Additional Journal Information:: Journal Volume: 194; Journal ID: ISSN 1359-6640

Publisher:: Royal Society of Chemistry

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats


                    Neppl, Stefan, Mahl, Johannes, Tremsin, Anton S, Rude, Bruce, Qiao, Ruimin, Yang, Wanli, Guo, Jinghua, and Gessner, Oliver. Towards efficient time-resolved X-ray absorption studies of electron dynamics at photocatalytic interfaces.  United States: N. p., 2016. 
Web.  doi:10.1039/c6fd00125d.

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                    Neppl, Stefan, Mahl, Johannes, Tremsin, Anton S, Rude, Bruce, Qiao, Ruimin, Yang, Wanli, Guo, Jinghua, & Gessner, Oliver. Towards efficient time-resolved X-ray absorption studies of electron dynamics at photocatalytic interfaces.  United States.  https://doi.org/10.1039/c6fd00125d

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                    Neppl, Stefan, Mahl, Johannes, Tremsin, Anton S, Rude, Bruce, Qiao, Ruimin, Yang, Wanli, Guo, Jinghua, and Gessner, Oliver. Wed .  
"Towards efficient time-resolved X-ray absorption studies of electron dynamics at photocatalytic interfaces".  United States.  https://doi.org/10.1039/c6fd00125d.  https://www.osti.gov/servlets/purl/1845090.

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@article{osti_1845090,

  title        = {Towards efficient time-resolved X-ray absorption studies of electron dynamics at photocatalytic interfaces},

  author       = {Neppl, Stefan and Mahl, Johannes and Tremsin, Anton S and Rude, Bruce and Qiao, Ruimin and Yang, Wanli and Guo, Jinghua and Gessner, Oliver},

  abstractNote = {We present a picosecond time-resolved X-ray absorption spectroscopy (tr-XAS) setup designed for synchrotron-based studies of interfacial photochemical dynamics. The apparatus combines a high power, variable repetition rate picosecond laser system with a time-resolved X-ray fluorescence yield detection technique. Time-tagging of the detected fluorescence signals enables the parallel acquisition of X-ray absorption spectra at a variety of pump–probe delays employing the well-defined time structure of the X-ray pulse trains. The viability of the setup is demonstrated by resolving dynamic changes in the fine structure near the O1s X-ray absorption edge of cuprous oxide (Cu2O) after photo-excitation with a 355 nm laser pulse. Two distinct responses are detected. A pronounced, quasi-static, reversible change of the Cu2O O1s X-ray absorption spectrum by up to ~30% compared to its static line shape corresponds to a redshift of the absorption edge by ~1 eV. This value is small compared to the 2.2 eV band gap of Cu2O but in agreement with previously published results. Here, the lifetime of this effect exceeds the laser pulse-to-pulse period of 8 μs, resulting in a quasi-static spectral change that persists as long as the sample is exposed to the laser light, and completely vanishes once the laser is blocked. Additionally, a short-lived response corresponding to a laser-induced shift of the main absorption line by ~2 eV to lower energies appears within <200 ps and decays with a characteristic timescale of 43 ± 5 ns. Both the picosecond rise and nanosecond decay of this X-ray response are simultaneously captured by making use of a time-tagging approach – highlighting the prospects of the experimental setup for efficient probing of the electronic and structural dynamics in photocatalytic systems on multiple timescales.},

  doi          = {10.1039/c6fd00125d},

  journal      = {Faraday Discussions},

  number       = ,

  volume       = 194,

  place        = {United States},

  year         = {Wed May 18 00:00:00 EDT 2016},

  month        = {Wed May 18 00:00:00 EDT 2016}

}

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Works referencing / citing this record:

Femtosecond time-resolved two-photon photoemission studies of ultrafast carrier relaxation in Cu2O photoelectrodes
journal, May 2019

Borgwardt, Mario; Omelchenko, Stefan T.; Favaro, Marco
Nature Communications, Vol. 10, Issue 1
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Decomposing electronic and lattice contributions in optical pump – X-ray probe transient inner-shell absorption spectroscopy of CuO
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Mahl, Johannes; Neppl, Stefan; Roth, Friedrich
Deutsches Elektronen-Synchrotron, DESY, Hamburg
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Chergui, Majed
Faraday Discussions, Vol. 216
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Decomposing electronic and lattice contributions in optical pump – X-ray probe transient inner-shell absorption spectroscopy of CuO
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Mahl, Johannes; Neppl, Stefan; Roth, Friedrich
Faraday Discussions, Vol. 216
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The Influence of Low-temperature Plasma Treatment on Some Wool Properties

Journal Article Radetic, Maja - AIP Conference Proceedings

If swift heavy ions (5 MeV/u) hit solid targets energy is transferred to the electrons of the solid. Caused by the high electronic energy deposition along the flight path of the ion a cylindrical shaped chemical or structural defect cluster is formed. This kind of defect cluster together with its electronic and atomic precursors is called ion track. Ion-track formation is mainly described by two different mechanisms: At the beginning of the ion-track formation, within a timescale of 10-17 s, the energy is transferred into the electronic system and the electrons move away from the center of the track wheremore »« less
https://doi.org/10.1063/1.1843509

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Title: Towards efficient time-resolved X-ray absorption studies of electron dynamics at photocatalytic interfaces

Abstract

Citation Formats

A liquid flow cell to study the electronic structure of liquids with soft X-rays journal, February 2008

Time-resolved X-ray photoelectron spectroscopy techniques for the study of interfacial charge dynamics journal, April 2015

Probing the Electronic Structure of a Photoexcited Solar Cell Dye with Transient X-ray Absorption Spectroscopy journal, June 2012

Unoccupied electronic structure and core-hole effects in the x-ray-absorption spectra of Cu 2 O journal, February 1992

Band-Selective Measurements of Electron Dynamics in VO 2 Using Femtosecond Near-Edge X-Ray Absorption journal, August 2005

Development of high-repetition-rate laser pump/x-ray probe methodologies for synchrotron facilities journal, July 2011

Capturing Ultrafast Quantum Dynamics with Femtosecond and Attosecond X-ray Core-Level Absorption Spectroscopy journal, January 2013

Tracking excited-state charge and spin dynamics in iron coordination complexes journal, May 2014

A high-repetition rate scheme for synchrotron-based picosecond laser pump/x-ray probe experiments on chemical and biological systems in solution journal, June 2011

Electrochemical Studies for CO 2 Reduction Using Synthesized Co 3 O 4 (Anode) and Cu 2 O (Cathode) as Electrocatalysts journal, October 2015

Visualizing the non-equilibrium dynamics of photoinduced intramolecular electron transfer with femtosecond X-ray pulses journal, March 2015

Atomic resolution mapping of the excited-state electronic structure of Cu 2 O with time-resolved x-ray absorption spectroscopy journal, September 2009

Electron-yield saturation effects in L -edge x-ray magnetic circular dichroism spectra of Fe, Co, and Ni journal, March 1999

Optical Absorption of Cuprous Oxide journal, January 1961

Photoelectrochemistry of Electrodeposited Cu[sub 2]O journal, January 2000

Capturing interfacial photoelectrochemical dynamics with picosecond time-resolved X-ray photoelectron spectroscopy journal, January 2014

On the band structure and the absorption spectrum of Cu2O journal, July 1966

Femtosecond M 2,3 -Edge Spectroscopy of Transition-Metal Oxides: Photoinduced Oxidation State Change in α-Fe 2 O 3 journal, October 2013

Nanostructured copper oxide semiconductors: a perspective on materials, synthesis methods and applications journal, January 2014

X-ray spectroscopy of energy materials under in situ/operando conditions journal, April 2015

Enhanced high rate properties of ordered porous Cu2O film as anode for lithium ion batteries journal, July 2010

Femtosecond Soft X-ray Spectroscopy of Solvated Transition-Metal Complexes: Deciphering the Interplay of Electronic and Structural Dynamics journal, March 2011

Probing the transition state region in catalytic CO oxidation on Ru journal, February 2015

Electronic structure and binding mechanism of Cu2O journal, June 1986

Real-Time Observation of Surface Bond Breaking with an X-ray Laser journal, March 2013

Time-resolved soft x-ray absorption setup using multi-bunch operation modes at synchrotrons journal, December 2011

Oxygen 1 s x-ray-absorption edges of transition-metal oxides journal, September 1989

Coexistence of ionic and metallic bonding in noble-metal oxides journal, July 2005

Bonding in Liquid Carbon Studied by Time-Resolved X-Ray Absorption Spectroscopy journal, February 2005

Long Exciton Lifetime in Cu 2 O journal, October 1979

A setup for ultrafast time-resolved x-ray absorption spectroscopy journal, January 2004

Electronic and Molecular Structure of Photoexcited [Ru II (bpy) 3 ] 2+ Probed by Picosecond X-ray Absorption Spectroscopy journal, April 2006

Mapping of the Photoinduced Electron Traps in TiO 2 by Picosecond X-ray Absorption Spectroscopy journal, May 2014

Determination of the optical band gap for amorphous and nanocrystalline copper oxide thin films prepared by SILAR technique journal, December 2008

On-site interband excitations in resonant inelastic x-ray scattering from Cu 2 O journal, April 2008

Direct Observation of Two Electron Holes in a Hematite Photoanode during Photoelectrochemical Water Splitting journal, August 2012

Molecular Structural Dynamics Probed by Ultrafast X-Ray Absorption Spectroscopy journal, March 2010

Observing Photochemical Transients by Ultrafast X-Ray Absorption Spectroscopy journal, January 2003

Bulk and surface properties of Cu2O: A first-principles investigation journal, June 2009

Quasiparticle Self-Consistent G W Theory journal, June 2006

Probing Transient Molecular Structures in Photochemical Processes Using Laser-Initiated Time-Resolved X-Ray Absorption Spectroscopy journal, May 2005

Concentration and chemical-state profiles at heterogeneous interfaces with sub-nm accuracy from standing-wave ambient-pressure photoemission journal, November 2014

Atomic-Scale Perspective of Ultrafast Charge Transfer at a Dye–Semiconductor Interface journal, July 2014

Ambient-Pressure XPS Study of a Ni–Fe Electrocatalyst for the Oxygen Evolution Reaction journal, January 2016

Ground-state and optical properties of Cu 2 O and CuO crystals journal, October 1989

Redox activity of surface oxygen anions in oxygen-deficient perovskite oxides during electrochemical reactions journal, January 2015

Electronic Relaxation Effects in Core Level Spectra of Solids journal, July 1982

Synthesis and Characterization of High-Photoactivity Electrodeposited Cu 2 O Solar Absorber by Photoelectrochemistry and Ultrafast Spectroscopy journal, March 2012

Exciton lifetime, Auger recombination, and exciton transport by calibrated differential absorption spectroscopy in Cu 2 O journal, June 2002

In Situ IR and X-ray High Spatial-Resolution Microspectroscopy Measurements of Multistep Organic Transformation in Flow Microreactor Catalyzed by Au Nanoclusters journal, February 2014

Photocatalytic production of hydrogen from electrodeposited p-Cu2Op-Cu2O film and sacrificial electron donors journal, December 2007

Etude spectrophotometrique de la serie jaune de Cu2O aux basses temperatures journal, January 1961

Photoluminescence at high exciton densities in cuprous oxide journal, May 1976

Resonant inelastic x-ray scattering study of the electronic structure of Cu 2 O journal, May 2010

Characterization of Photo-Induced Charge Transfer and Hot Carrier Relaxation Pathways in Spinel Cobalt Oxide (Co 3 O 4 ) journal, September 2014

Femtochemistry: Atomic-Scale Dynamics of the Chemical Bond † journal, June 2000

Carrier thermalization in Cu 2 O: Phonon emission by excitons journal, August 1991

Orbital-specific mapping of the ligand exchange dynamics of Fe(CO)5 in solution journal, April 2015

Probing the valence band structure of Cu 2 O using high-energy angle-resolved photoelectron spectroscopy journal, September 2007

Binary copper oxide semiconductors: From materials towards devices journal, June 2012

Atomic Structure of Pt 3 Ni Nanoframe Electrocatalysts by in Situ X-ray Absorption Spectroscopy journal, December 2015

Electronic structure of Cu 2 O and CuO journal, December 1988

Experimental and theoretical investigation of the electronic structure of Cu 2 O and CuO thin films on Cu(110) using x-ray photoelectron and absorption spectroscopy journal, January 2013

The p-type conduction mechanism in Cu2O: a first principles study journal, January 2006

Electronic Band Structure of Solids by X-Ray Spectroscopy journal, July 1959

Direct Observation of the Transition-State Region in the Photodissociation of CH 3 I by Femtosecond Extreme Ultraviolet Transient Absorption Spectroscopy journal, December 2015

Femtosecond time-resolved two-photon photoemission studies of ultrafast carrier relaxation in Cu2O photoelectrodes journal, May 2019

Decomposing electronic and lattice contributions in optical pump – X-ray probe transient inner-shell absorption spectroscopy of CuO text, January 2019

Ultrafast photoinduced energy and charge transfer journal, January 2019

Decomposing electronic and lattice contributions in optical pump – X-ray probe transient inner-shell absorption spectroscopy of CuO journal, January 2019

A liquid flow cell to study the electronic structure of liquids with soft X-rays
journal, February 2008

Time-resolved X-ray photoelectron spectroscopy techniques for the study of interfacial charge dynamics
journal, April 2015

Probing the Electronic Structure of a Photoexcited Solar Cell Dye with Transient X-ray Absorption Spectroscopy
journal, June 2012

Unoccupied electronic structure and core-hole effects in the x-ray-absorption spectra of ${Cu}_{2}$ O
journal, February 1992

Band-Selective Measurements of Electron Dynamics in ${VO}_{2}$ Using Femtosecond Near-Edge X-Ray Absorption
journal, August 2005

Development of high-repetition-rate laser pump/x-ray probe methodologies for synchrotron facilities
journal, July 2011

Capturing Ultrafast Quantum Dynamics with Femtosecond and Attosecond X-ray Core-Level Absorption Spectroscopy
journal, January 2013

Tracking excited-state charge and spin dynamics in iron coordination complexes
journal, May 2014

A high-repetition rate scheme for synchrotron-based picosecond laser pump/x-ray probe experiments on chemical and biological systems in solution
journal, June 2011

Electrochemical Studies for CO ₂ Reduction Using Synthesized Co ₃ O ₄ (Anode) and Cu ₂ O (Cathode) as Electrocatalysts
journal, October 2015

Visualizing the non-equilibrium dynamics of photoinduced intramolecular electron transfer with femtosecond X-ray pulses
journal, March 2015

Atomic resolution mapping of the excited-state electronic structure of ${Cu}_{2} O$ with time-resolved x-ray absorption spectroscopy
journal, September 2009

Electron-yield saturation effects in L -edge x-ray magnetic circular dichroism spectra of Fe, Co, and Ni
journal, March 1999

Optical Absorption of Cuprous Oxide
journal, January 1961

Photoelectrochemistry of Electrodeposited Cu[sub 2]O
journal, January 2000

Capturing interfacial photoelectrochemical dynamics with picosecond time-resolved X-ray photoelectron spectroscopy
journal, January 2014

On the band structure and the absorption spectrum of Cu2O
journal, July 1966

Femtosecond M _2,3 -Edge Spectroscopy of Transition-Metal Oxides: Photoinduced Oxidation State Change in α-Fe ₂ O ₃
journal, October 2013

Nanostructured copper oxide semiconductors: a perspective on materials, synthesis methods and applications
journal, January 2014

X-ray spectroscopy of energy materials under in situ/operando conditions
journal, April 2015

Enhanced high rate properties of ordered porous Cu2O film as anode for lithium ion batteries
journal, July 2010

Femtosecond Soft X-ray Spectroscopy of Solvated Transition-Metal Complexes: Deciphering the Interplay of Electronic and Structural Dynamics
journal, March 2011

Probing the transition state region in catalytic CO oxidation on Ru
journal, February 2015

Electronic structure and binding mechanism of Cu2O
journal, June 1986

Real-Time Observation of Surface Bond Breaking with an X-ray Laser
journal, March 2013

Time-resolved soft x-ray absorption setup using multi-bunch operation modes at synchrotrons
journal, December 2011

Oxygen 1 s x-ray-absorption edges of transition-metal oxides
journal, September 1989

Coexistence of ionic and metallic bonding in noble-metal oxides
journal, July 2005

Bonding in Liquid Carbon Studied by Time-Resolved X-Ray Absorption Spectroscopy
journal, February 2005

Long Exciton Lifetime in ${Cu}_{2}$ O
journal, October 1979

A setup for ultrafast time-resolved x-ray absorption spectroscopy
journal, January 2004

Electronic and Molecular Structure of Photoexcited [Ru ^II (bpy) ₃ ] ²⁺ Probed by Picosecond X-ray Absorption Spectroscopy
journal, April 2006

Mapping of the Photoinduced Electron Traps in TiO ₂ by Picosecond X-ray Absorption Spectroscopy
journal, May 2014

Determination of the optical band gap for amorphous and nanocrystalline copper oxide thin films prepared by SILAR technique
journal, December 2008

On-site interband excitations in resonant inelastic x-ray scattering from ${Cu}_{2} O$
journal, April 2008

Direct Observation of Two Electron Holes in a Hematite Photoanode during Photoelectrochemical Water Splitting
journal, August 2012

Molecular Structural Dynamics Probed by Ultrafast X-Ray Absorption Spectroscopy
journal, March 2010

Observing Photochemical Transients by Ultrafast X-Ray Absorption Spectroscopy
journal, January 2003

Bulk and surface properties of Cu2O: A first-principles investigation
journal, June 2009

Quasiparticle Self-Consistent $G W$ Theory
journal, June 2006

Probing Transient Molecular Structures in Photochemical Processes Using Laser-Initiated Time-Resolved X-Ray Absorption Spectroscopy
journal, May 2005

Concentration and chemical-state profiles at heterogeneous interfaces with sub-nm accuracy from standing-wave ambient-pressure photoemission
journal, November 2014

Atomic-Scale Perspective of Ultrafast Charge Transfer at a Dye–Semiconductor Interface
journal, July 2014

Ambient-Pressure XPS Study of a Ni–Fe Electrocatalyst for the Oxygen Evolution Reaction
journal, January 2016

Ground-state and optical properties of ${Cu}_{2}$ O and CuO crystals
journal, October 1989

Redox activity of surface oxygen anions in oxygen-deficient perovskite oxides during electrochemical reactions
journal, January 2015

Electronic Relaxation Effects in Core Level Spectra of Solids
journal, July 1982

Synthesis and Characterization of High-Photoactivity Electrodeposited Cu ₂ O Solar Absorber by Photoelectrochemistry and Ultrafast Spectroscopy
journal, March 2012

Exciton lifetime, Auger recombination, and exciton transport by calibrated differential absorption spectroscopy in ${Cu}_{2} O$
journal, June 2002

In Situ IR and X-ray High Spatial-Resolution Microspectroscopy Measurements of Multistep Organic Transformation in Flow Microreactor Catalyzed by Au Nanoclusters
journal, February 2014

Photocatalytic production of hydrogen from electrodeposited p-Cu2Op-Cu2O film and sacrificial electron donors
journal, December 2007

Etude spectrophotometrique de la serie jaune de Cu2O aux basses temperatures
journal, January 1961

Photoluminescence at high exciton densities in cuprous oxide
journal, May 1976

Resonant inelastic x-ray scattering study of the electronic structure of ${Cu}_{2} O$
journal, May 2010

Characterization of Photo-Induced Charge Transfer and Hot Carrier Relaxation Pathways in Spinel Cobalt Oxide (Co ₃ O ₄ )
journal, September 2014

Femtochemistry: Atomic-Scale Dynamics of the Chemical Bond ^†
journal, June 2000

Carrier thermalization in ${Cu}_{2}$ O: Phonon emission by excitons
journal, August 1991

Orbital-specific mapping of the ligand exchange dynamics of Fe(CO)5 in solution
journal, April 2015

Probing the valence band structure of ${Cu}_{2} O$ using high-energy angle-resolved photoelectron spectroscopy
journal, September 2007

Binary copper oxide semiconductors: From materials towards devices
journal, June 2012

Atomic Structure of Pt ₃ Ni Nanoframe Electrocatalysts by in Situ X-ray Absorption Spectroscopy
journal, December 2015

Electronic structure of ${Cu}_{2}$ O and CuO
journal, December 1988

Experimental and theoretical investigation of the electronic structure of Cu ₂ O and CuO thin films on Cu(110) using x-ray photoelectron and absorption spectroscopy
journal, January 2013

The p-type conduction mechanism in Cu2O: a first principles study
journal, January 2006

Electronic Band Structure of Solids by X-Ray Spectroscopy
journal, July 1959

Direct Observation of the Transition-State Region in the Photodissociation of CH ₃ I by Femtosecond Extreme Ultraviolet Transient Absorption Spectroscopy
journal, December 2015

Femtosecond time-resolved two-photon photoemission studies of ultrafast carrier relaxation in Cu2O photoelectrodes
journal, May 2019

Decomposing electronic and lattice contributions in optical pump – X-ray probe transient inner-shell absorption spectroscopy of CuO
text, January 2019

Ultrafast photoinduced energy and charge transfer
journal, January 2019

Decomposing electronic and lattice contributions in optical pump – X-ray probe transient inner-shell absorption spectroscopy of CuO
journal, January 2019