Abstract

Phase transitions of solids and structural transformations of molecules are canonical examples of important photo-induced processes whose underlying mechanisms largely elude our comprehension due to our inability to correlate electronic excitation with atomic position in real time. Here, we present a decisive step towards such new methodology based on water-window covering (284–543 eV) attosecond soft x-ray pulses that can simultaneously access electronic and lattice parameters via dispersive x-ray absorption fine-structure (XAFS) spectroscopy. We validate this approach with an identification of the σ* and π* orbital contributions to the density of states in graphite simultaneously with its lattice’s four characteristic bonding distances. This work demonstrates the potential of dispersive XAFS, in combination with attosecond pulses, as a powerful investigative tool that is equally applicable to gas, liquid, and condensed phase.

© 2018 Optical Society of America under the terms of the OSA Open Access Publishing Agreement

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    [Crossref]
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    [Crossref]
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    [Crossref]
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    [Crossref]
  36. T. Tanaka, N. Matsubayashi, M. Imamura, and H. Shimada, “Synchronous scanning of undulator gap and monochromator for XAFS measurements in soft x-ray region,” J. Synchrotron Radiat. 8, 345–347 (2001).
    [Crossref]

2018 (1)

D. Popmintchev, B. R. Galloway, M.-C. Chen, F. Dollar, C. A. Mancuso, A. Hankla, L. Miaja-Avila, G. O’Neil, J. M. Shaw, G. Fan, S. Ališauskas, G. Andriukaitis, T. Balčiunas, O. D. Mücke, A. Pugzlys, A. Baltuška, H. C. Kapteyn, T. Popmintchev, and M. M. Murnane, “Near- and extended-edge x-ray-absorption fine-structure spectroscopy using ultrafast coherent high-order harmonic supercontinua,” Phys. Rev. Lett. 120, 93002 (2018).
[Crossref]

2017 (4)

Y. Pertot, C. Schmidt, M. Matthews, A. Chauvet, M. Huppert, V. Svoboda, A. Von Conta, A. Tehlar, D. Baykusheva, J. Wolf, and H. J. Wörner, “Time-resolved x-ray absorption spectroscopy with a water window high-harmonic source,” Science 355, 264–267 (2017).
[Crossref]

A. R. Attar, A. Bhattacherjee, C. D. Pemmaraju, K. Schnorr, K. D. Closser, D. Prendergast, and S. R. Leone, “Femtosecond x-ray spectroscopy of an electrocyclic ring-opening reaction,” Science 356, 54–59 (2017).
[Crossref]

M. Zürch, H. T. Chang, L. J. Borja, P. M. Kraus, S. K. Cushing, A. Gandman, C. J. Kaplan, M. H. Oh, J. S. Prell, D. Prendergast, C. D. Pemmaraju, D. M. Neumark, and S. R. Leone, “Direct and simultaneous observation of ultrafast electron and hole dynamics in germanium,” Nat. Commun. 8, 15734 (2017).
[Crossref]

S. L. Cousin, N. Di Palo, B. Buades, S. M. Teichmann, M. Reduzzi, M. Devetta, A. Kheifets, G. Sansone, and J. Biegert, “Attosecond streaking in the water window: a new regime of attosecond pulse characterization,” Phys. Rev. X 7, 41030 (2017).
[Crossref]

2016 (3)

H. Mashiko, K. Oguri, T. Yamaguchi, A. Suda, and H. Gotoh, “Petahertz optical drive with wide-bandgap semiconductor,” Nat. Phys. 12, 741–745 (2016).
[Crossref]

M. Lucchini, S. A. Sato, A. Ludwig, J. Herrmann, M. Volkov, L. Kasmi, Y. Shinohara, K. Yabana, L. Gallmann, and U. Keller, “Attosecond dynamical Franz-Keldysh effect in polycrystalline diamond,” Science 353, 916–919 (2016).
[Crossref]

S. M. Teichmann, F. Silva, S. L. Cousin, M. Hemmer, and J. Biegert, “0.5-keV Soft X-ray attosecond continua,” Nat. Commun. 7, 11493 (2016).
[Crossref]

2015 (1)

M. Vacher, L. Steinberg, A. J. Jenkins, M. J. Bearpark, and M. A. Robb, “Electron dynamics following photoionization: decoherence due to the nuclear-wave-packet width,” Phys. Rev. A 92, 040502 (2015).
[Crossref]

2014 (3)

2011 (1)

B. J. Schultz, C. J. Patridge, V. Lee, C. Jaye, P. S. Lysaght, C. Smith, J. Barnett, D. A. Fischer, D. Prendergast, and S. Banerjee, “Imaging local electronic corrugations and doped regions in graphene,” Nat. Commun. 2, 372 (2011).
[Crossref]

2010 (1)

J. J. Rehr, J. J. Kas, F. D. Vila, M. P. Prange, and K. Jorissen, “Parameter-free calculations of X-ray spectra with FEFF9,” Phys. Chem. Chem. Phys. 12, 5503–5513 (2010).
[Crossref]

2009 (3)

M. Papagno, A. Fraile Rodríguez, Ç. Ö. Girit, J. C. Meyer, A. Zettl, and D. Pacilé, “Polarization-dependent C K near-edge X-ray absorption fine-structure of graphene,” Chem. Phys. Lett. 475, 269–271 (2009).
[Crossref]

F. Krausz and M. Ivanov, “Attosecond physics,” Rev. Mod. Phys. 81, 163–234 (2009).
[Crossref]

H. Ade and H. Stoll, “Near-edge X-ray absorption fine-structure microscopy of organic and magnetic materials,” Nat. Mater. 8, 281–290 (2009).
[Crossref]

2008 (2)

K. Sauer, J. Yano, and V. K. Yachandra, “X-ray spectroscopy of the photosynthetic oxygen-evolving complex,” Coord. Chem. Rev. 252, 318–335 (2008).
[Crossref]

J. A. Brandes, G. D. Cody, D. Rumble, P. Haberstroh, S. Wirick, and Y. Gelinas, “Carbon K-edge XANES spectromicroscopy of natural graphite,” Carbon 46, 1424–1434 (2008).
[Crossref]

2006 (4)

T. Hemraj-Benny, S. Banerjee, S. Sambasivan, M. Balasubramanian, D. A. Fischer, G. Eres, A. A. Puretzky, D. B. Geohegan, D. H. Lowndes, W. Han, J. A. Misewich, and S. S. Wong, “Near-edge X-ray absorption fine structure spectroscopy as a tool for investigating nanomaterials,” Small 2, 26–35 (2006).
[Crossref]

B. Watts, L. Thomsen, and P. C. Dastoor, “Methods in carbon K-edge NEXAFS: experiment and analysis,” J. Electron Spectrosc. Relat. Phenom. 151, 105–120 (2006).
[Crossref]

N. Ooi, A. Rairkar, and J. B. Adams, “Density functional study of graphite bulk and surface properties,” Carbon 44, 231–242 (2006).
[Crossref]

G. Hähner, “Near edge X-ray absorption fine structure spectroscopy as a tool to probe electronic and structural properties of thin organic films and liquids,” Chem. Soc. Rev. 35, 1244–1255 (2006).
[Crossref]

2005 (1)

B. Ravel and M. Newville, “ATHENA, ARTEMIS, HEPHAESTUS: data analysis for X-ray absorption spectroscopy using IFEFFIT,” J. Synchrotron Rad. 12, 537–541 (2005).
[Crossref]

2004 (1)

A. G. Marinopoulos, L. Reining, A. Rubio, and V. Olevano, “Ab initio study of the optical absorption and wave-vector-dependent dielectric response of graphite,” Phys. Rev. B 69, 245419 (2004).
[Crossref]

2001 (2)

G. te Velde, F. M. Bickelhaupt, E. J. Baerends, C. Fonseca Guerra, S. J. A. van Gisbergen, J. G. Snijders, and T. Ziegler, “Chemistry with ADF,” J. Comput. Chem. 22, 931–967 (2001).
[Crossref]

T. Tanaka, N. Matsubayashi, M. Imamura, and H. Shimada, “Synchronous scanning of undulator gap and monochromator for XAFS measurements in soft x-ray region,” J. Synchrotron Radiat. 8, 345–347 (2001).
[Crossref]

1998 (1)

C. F. Guerra, J. G. Snijders, G. te Velde, and E. J. Baerends, “Towards an order-N DFT method,” Theor. Chem. Acc. 99, 391–403 (1998).
[Crossref]

1996 (1)

R. Ahuja, P. Brühwiler, J. Wills, B. Johansson, N. Mårtensson, and O. Eriksson, “Theoretical and experimental study of the graphite 1s x-ray absorption edges,” Phys. Rev. B 54, 14396–14404 (1996).
[Crossref]

1995 (1)

P. A. Brühwiler, A. J. Maxwell, C. Puglia, A. Nilsson, S. Anderson, and N. Martensoon, “pi* and sigma* excitons in C- 1s absorption of graphite,” Phys. Rev. Lett. 74, 614–617 (1995).
[Crossref]

1994 (1)

B. R. Dobson, “Quick scanning EXAFS facilities at Daresbury SRS,” Synchrotron Radiat. News 7(1), 21–24 (1994).
[Crossref]

1988 (2)

R. Frahm, “Quick scanning EXAFS: first experiments,” Nucl. Instrum. Methods Phys. Res. Sect. A 270, 578–581 (1988).
[Crossref]

G. Comelli, J. Stöhr, W. Jark, and B. B. Pate, “Extended x-ray-absorption fine-structure studies of diamond and graphite,” Phys. Rev. B 37, 4383–4389 (1988).
[Crossref]

1986 (1)

R. A. Rosenberg, P. J. Love, and V. Rehn, “Polarization-dependent C(K) near-edge x-ray-absorption fine structure of graphite,” Phys. Rev. B 33, 4034–4037 (1986).
[Crossref]

1971 (1)

D. E. Sayers, E. A. Stern, and F. W. Lytle, “New technique for investigating noncrystalline structures: Fourier analysis of the extended x-ray—absorption fine structure,” Phys. Rev. Lett. 27, 1204–1207 (1971).
[Crossref]

Adams, J. B.

N. Ooi, A. Rairkar, and J. B. Adams, “Density functional study of graphite bulk and surface properties,” Carbon 44, 231–242 (2006).
[Crossref]

Ade, H.

H. Ade and H. Stoll, “Near-edge X-ray absorption fine-structure microscopy of organic and magnetic materials,” Nat. Mater. 8, 281–290 (2009).
[Crossref]

Ahuja, R.

R. Ahuja, P. Brühwiler, J. Wills, B. Johansson, N. Mårtensson, and O. Eriksson, “Theoretical and experimental study of the graphite 1s x-ray absorption edges,” Phys. Rev. B 54, 14396–14404 (1996).
[Crossref]

Ališauskas, S.

D. Popmintchev, B. R. Galloway, M.-C. Chen, F. Dollar, C. A. Mancuso, A. Hankla, L. Miaja-Avila, G. O’Neil, J. M. Shaw, G. Fan, S. Ališauskas, G. Andriukaitis, T. Balčiunas, O. D. Mücke, A. Pugzlys, A. Baltuška, H. C. Kapteyn, T. Popmintchev, and M. M. Murnane, “Near- and extended-edge x-ray-absorption fine-structure spectroscopy using ultrafast coherent high-order harmonic supercontinua,” Phys. Rev. Lett. 120, 93002 (2018).
[Crossref]

Anderson, S.

P. A. Brühwiler, A. J. Maxwell, C. Puglia, A. Nilsson, S. Anderson, and N. Martensoon, “pi* and sigma* excitons in C- 1s absorption of graphite,” Phys. Rev. Lett. 74, 614–617 (1995).
[Crossref]

Andriukaitis, G.

D. Popmintchev, B. R. Galloway, M.-C. Chen, F. Dollar, C. A. Mancuso, A. Hankla, L. Miaja-Avila, G. O’Neil, J. M. Shaw, G. Fan, S. Ališauskas, G. Andriukaitis, T. Balčiunas, O. D. Mücke, A. Pugzlys, A. Baltuška, H. C. Kapteyn, T. Popmintchev, and M. M. Murnane, “Near- and extended-edge x-ray-absorption fine-structure spectroscopy using ultrafast coherent high-order harmonic supercontinua,” Phys. Rev. Lett. 120, 93002 (2018).
[Crossref]

Attar, A. R.

A. R. Attar, A. Bhattacherjee, C. D. Pemmaraju, K. Schnorr, K. D. Closser, D. Prendergast, and S. R. Leone, “Femtosecond x-ray spectroscopy of an electrocyclic ring-opening reaction,” Science 356, 54–59 (2017).
[Crossref]

Baerends, E. J.

G. te Velde, F. M. Bickelhaupt, E. J. Baerends, C. Fonseca Guerra, S. J. A. van Gisbergen, J. G. Snijders, and T. Ziegler, “Chemistry with ADF,” J. Comput. Chem. 22, 931–967 (2001).
[Crossref]

C. F. Guerra, J. G. Snijders, G. te Velde, and E. J. Baerends, “Towards an order-N DFT method,” Theor. Chem. Acc. 99, 391–403 (1998).
[Crossref]

Balasubramanian, M.

T. Hemraj-Benny, S. Banerjee, S. Sambasivan, M. Balasubramanian, D. A. Fischer, G. Eres, A. A. Puretzky, D. B. Geohegan, D. H. Lowndes, W. Han, J. A. Misewich, and S. S. Wong, “Near-edge X-ray absorption fine structure spectroscopy as a tool for investigating nanomaterials,” Small 2, 26–35 (2006).
[Crossref]

Balciunas, T.

D. Popmintchev, B. R. Galloway, M.-C. Chen, F. Dollar, C. A. Mancuso, A. Hankla, L. Miaja-Avila, G. O’Neil, J. M. Shaw, G. Fan, S. Ališauskas, G. Andriukaitis, T. Balčiunas, O. D. Mücke, A. Pugzlys, A. Baltuška, H. C. Kapteyn, T. Popmintchev, and M. M. Murnane, “Near- and extended-edge x-ray-absorption fine-structure spectroscopy using ultrafast coherent high-order harmonic supercontinua,” Phys. Rev. Lett. 120, 93002 (2018).
[Crossref]

Baltuška, A.

D. Popmintchev, B. R. Galloway, M.-C. Chen, F. Dollar, C. A. Mancuso, A. Hankla, L. Miaja-Avila, G. O’Neil, J. M. Shaw, G. Fan, S. Ališauskas, G. Andriukaitis, T. Balčiunas, O. D. Mücke, A. Pugzlys, A. Baltuška, H. C. Kapteyn, T. Popmintchev, and M. M. Murnane, “Near- and extended-edge x-ray-absorption fine-structure spectroscopy using ultrafast coherent high-order harmonic supercontinua,” Phys. Rev. Lett. 120, 93002 (2018).
[Crossref]

Banerjee, S.

B. J. Schultz, C. J. Patridge, V. Lee, C. Jaye, P. S. Lysaght, C. Smith, J. Barnett, D. A. Fischer, D. Prendergast, and S. Banerjee, “Imaging local electronic corrugations and doped regions in graphene,” Nat. Commun. 2, 372 (2011).
[Crossref]

T. Hemraj-Benny, S. Banerjee, S. Sambasivan, M. Balasubramanian, D. A. Fischer, G. Eres, A. A. Puretzky, D. B. Geohegan, D. H. Lowndes, W. Han, J. A. Misewich, and S. S. Wong, “Near-edge X-ray absorption fine structure spectroscopy as a tool for investigating nanomaterials,” Small 2, 26–35 (2006).
[Crossref]

Barnett, J.

B. J. Schultz, C. J. Patridge, V. Lee, C. Jaye, P. S. Lysaght, C. Smith, J. Barnett, D. A. Fischer, D. Prendergast, and S. Banerjee, “Imaging local electronic corrugations and doped regions in graphene,” Nat. Commun. 2, 372 (2011).
[Crossref]

Baykusheva, D.

Y. Pertot, C. Schmidt, M. Matthews, A. Chauvet, M. Huppert, V. Svoboda, A. Von Conta, A. Tehlar, D. Baykusheva, J. Wolf, and H. J. Wörner, “Time-resolved x-ray absorption spectroscopy with a water window high-harmonic source,” Science 355, 264–267 (2017).
[Crossref]

Bearpark, M. J.

M. Vacher, L. Steinberg, A. J. Jenkins, M. J. Bearpark, and M. A. Robb, “Electron dynamics following photoionization: decoherence due to the nuclear-wave-packet width,” Phys. Rev. A 92, 040502 (2015).
[Crossref]

Bhattacherjee, A.

A. R. Attar, A. Bhattacherjee, C. D. Pemmaraju, K. Schnorr, K. D. Closser, D. Prendergast, and S. R. Leone, “Femtosecond x-ray spectroscopy of an electrocyclic ring-opening reaction,” Science 356, 54–59 (2017).
[Crossref]

Bickelhaupt, F. M.

G. te Velde, F. M. Bickelhaupt, E. J. Baerends, C. Fonseca Guerra, S. J. A. van Gisbergen, J. G. Snijders, and T. Ziegler, “Chemistry with ADF,” J. Comput. Chem. 22, 931–967 (2001).
[Crossref]

Biegert, J.

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M. Schultze, K. Ramasesha, C. D. Pemmaraju, S. A. Sato, D. Whitmore, A. Gandman, J. S. Prell, L. J. Borja, D. Prendergast, K. Yabana, D. M. Neumark, and S. R. Leone, “Attosecond band-gap dynamics in silicon,” Science 346, 1348–1352 (2014).
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Supplementary Material (1)

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Figures (3)

Fig. 1.
Fig. 1. XAFS–Simultaneous XANES and EXAFS with an isolated attosecond SXR pulse. (a) Shown is the spectrum of the isolated attosecond pulse spanning the entire SXR water window (284–543 eV) at once. Overlaid as vertical lines are the positions of accessible K- (orange), L- (green), and M-shell (blue) absorption edges. Note that the depletion at the C-edge is due to the ubiquitous hydrocarbon contamination originating from turbo pumps in the beamline. (b) shows the XAFS measurement in graphite in which the XANES is highlighted in red and the EXAFS in blue. The shading around the absorbance indicates the confidence band of the measurement. (c) indicates that spectral components with photon energy above 284 eV access 1s carbon K-shell core-level electrons. Transitions to bound states close to the Fermi edge are known as XANES, and transition into the continuum, giving rise to the EXAFS. XANES provides orbital sensitivity depending on the angle of the impinging x-ray pulse field vector relative to the basal plane normal of the sample, while EXAFS predominantly provides local structural information as it is related to the scattered electron wave from the absorber atom on the neighboring atoms. Note that no hard boundary exists between XANES and EXAFS, and that the color separation is solely chosen to indicate the predominant contribution to the measurement.
Fig. 2.
Fig. 2. XAFS identifies different electronic orbitals. (a) shows the XANES region for three measurements in which the angle of incidence of the impinging attosecond SXR pulse is varied with respect to the basal plane normal of the sample. Normal incidence [shown also in (b) and (c)] probes states in the basal plane, while any deviation from normal incidence also probes components out of the basal plane. (b) and (c) show results from DFT calculations using BAND [2224]. The DOSs correspond to the lowest unoccupied states π* (b) and σ* (c) in the conduction band. Two main features can be identified from (a) at 285.5 eV and 292.5 eV, corresponding to 1sπ* and 1sσ* transitions, respectively.
Fig. 3.
Fig. 3. Bond distances from EXAFS. (a) shows two layers of graphite together with the identified bond distances. The experimental EXAFS is shown by the blue circles in (b) together with the back-transformed fit (solid red line) and the fit’s uncertainty (red shaded area). (c) shows the Fourier amplitude of the experimental data together with the individual contributions from the first four scattering paths (dashed lines). The summed scattering contribution is shown by the solid red line and, considering the scattering phases, results in a 2% fit accuracy. Note that the experimental spectra correspond to k values of 1.18 to 6.90  Å1.

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