- Editors' Suggestion
- Letter
- Open Access
Nanofocused x-ray photon correlation spectroscopy
Phys. Rev. Research 4, L032012 – Published 25 July, 2022
DOI: https://doi.org/10.1103/PhysRevResearch.4.L032012
Abstract
Here, we demonstrate an experimental proof of concept for nanofocused x-ray photon correlation spectroscopy, a technique sensitive to nanoscale fluctuations present in a broad range of systems. The experiment, performed at the NanoMAX beamline at MAX IV, uses a novel event-based x-ray detector to capture nanoparticle structural dynamics with microsecond resolution. By varying the nanobeam size from nm to , we quantify the effect of the nanofocus on the small-angle scattering lineshape and on the diffusion coefficients obtained from nano-XPCS. We observe that the use of nanobeams leads to a multifold increase in speckle contrast, which greatly improves the experimental signal-to-noise ratio, quantified from the two-time intensity correlation functions. We conclude that it is possible to account for influence of the high beam divergence on the lineshape and measured dynamics by including a convolution with the nanobeam profile in the model.
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References (55)
- R. Hettel, DLSR design and plans: an international overview, J. Synchrotron Radiat. 21, 843 (2014).
- P. F. Tavares, S. C. Leemann, M. Sjöström, and Å. Andersson, The MAX IV storage ring project, J. Synchrotron Radiat. 21, 862 (2014).
- G. Grübel, A. Madsen, and A. Robert, X-ray photon correlation spectroscopy (XPCS), in Soft Matter Characterization (Springer Science+Business Media, LLC, New York, 2008), pp. 953–995.
- A. Madsen, A. Fluerasu, and B. Ruta, Structural dynamics of materials probed by X-ray photon correlation spectroscopy, in Synchrotron Light Sources and Free-Electron Lasers: Accelerator Physics, Instrumentation and Science Applications (Springer International Publishing, Switzerland, 2016), pp. 1617–1641.
- O. G. Shpyrko, X-ray photon correlation spectroscopy, J. Synchrotron Radiat. 21, 1057 (2014).
- A. R. Sandy, Q. Zhang, and L. B. Lurio, Hard X-ray photon correlation spectroscopy methods for materials studies, Annu. Rev. Mater. Res. 48, 167 (2018).
- S. K. Sinha, Z. Jiang, and L. B. Lurio, X-ray photon correlation spectroscopy studies of surfaces and thin films, Adv. Mater. 26, 7764 (2014).
- F. Perakis and C. Gutt, Towards molecular movies with X-ray photon correlation spectroscopy, Phys. Chem. Chem. Phys. 22, 19443 (2020).
- Q. Zhang, E. M. Dufresne, and A. R. Sandy, Dynamics in hard condensed matter probed by X-ray photon correlation spectroscopy: present and beyond, Curr. Opin. Solid State Mater. Sci. 22, 202 (2018).
- F. Lehmkühler, W. Roseker, and G. Grübel, From femtoseconds to hours—measuring dynamics over 18 orders of magnitude with coherent X-rays, Appl. Sci. 11, 6179 (2021).
- Q. Zhang, E. M. Dufresne, S. Narayanan, P. Maj, A. Koziol, R. Szczygiel, P. Grybos, M. Sutton, and A. R. Sandy, Sub-microsecond-resolved multi-speckle X-ray photon correlation spectroscopy with a pixel array detector, J. Synchrotron Radiat. 25, 1408 (2018).
- Q. Zhang, E. M. Dufresne, Y. Nakaye, P. R. Jemian, T. Sakumura, Y. Sakuma, J. D. Ferrara, P. Maj, A. Hassan, D. Bahadur, S. Ramakrishnan, F. Khan, S. Veseli, A. R. Sandy, N. Schwarz, and S. Narayanan, -resolved high-throughput X-ray photon correlation spectroscopy on a 500k pixel detector enabled by data-management workflow, J. Synchrotron Radiat. 28, 259 (2021).
- T. Poikela, J. Plosila, T. Westerlund, M. Campbell, M. De Gaspari, X. Llopart, V. Gromov, R. Kluit, M. van Beuzekom, F. Zappon, V. Zivkovic, C. Brezina, K. Desch, Y. Fu, and A. Kruth, Timepix3: A 65k channel hybrid pixel readout chip with simultaneous toa/tot and sparse readout, J. Instrum. 9, C05013 (2014).
- H. Yousef, G. Crevatin, E. N. Gimenez, I. Horswell, D. Omar, and N. Tartoni, Timepix3 as x-ray detector for time resolved synchrotron experiments, Nucl. Instrum. Methods Phys. Res., Sect. A 845, 639 (2017).
- A. S. Tremsin, J. V. Vallerga, O. H. W. Siegmund, J. Woods, L. E. De Long, J. T. Hastings, R. J. Koch, S. A. Morley, Y.-D. Chuang, and S. Roy, Photon-counting MCP/Timepix detectors for soft X-ray imaging and spectroscopic applications, J. Synchrotron Radiat. 28, 1069 (2021).
- F. Perakis, K. Amann-Winkel, F. Lehmkühler, M. Sprung, D. Mariedahl, J. A. Sellberg, H. Pathak, A. Späh, F. Cavalca, D. Schlesinger, A. Ricci, A. Jain, B. Massani, F. Aubree, C. J. Benmore, T. Loerting, G. Gröbel, L. G. Pettersson, and A. Nilsson, Diffusive dynamics during the high-to-low density transition in amorphous ice, Proc. Natl. Acad. Sci. USA 114, 8193 (2017).
- K.-I. Oh and C. R. Baiz, Molecular heterogeneity in aqueous cosolvent systems, J. Chem. Phys. 152, 190901 (2020).
- D. Sheyfer, Q. Zhang, J. Lal, T. Loeffler, E. Dufresne, A. Sandy, S. Narayanan, S. Sankaranarayanan, R. Szczygiel, P. Maj, L. Soderholm, M. Antonio, and G. Stephenson, Nanoscale Critical Phenomena in a Complex Fluid Studied by X-Ray Photon Correlation Spectroscopy, Phys. Rev. Lett. 125, 125504 (2020).
- Y. Shin and C. P. Brangwynne, Liquid phase condensation in cell physiology and disease, Science 357, eaaf4382 (2017).
- N. Begam, A. Ragulskaya, A. Girelli, H. Rahmann, S. Chandran, F. Westermeier, M. Reiser, M. Sprung, F. Zhang, C. Gutt, and F. Schreiber, Kinetics of Network Formation and Heterogeneous Dynamics of an Egg White Gel Revealed by Coherent X-Ray Scattering, Phys. Rev. Lett. 126, 098001 (2021).
- A. Girelli, H. Rahmann, N. Begam, A. Ragulskaya, M. Reiser, S. Chandran, F. Westermeier, M. Sprung, F. Zhang, C. Gutt, and F. Schreiber, Microscopic Dynamics of Liquid-Liquid Phase Separation and Domain Coarsening in a Protein Solution Revealed by X-Ray Photon Correlation Spectroscopy, Phys. Rev. Lett. 126, 138004 (2021).
- B. Ruta, Y. Chushkin, G. Monaco, L. Cipelletti, E. Pineda, P. Bruna, V. M. Giordano, and M. Gonzalez-Silveira, Atomic-Scale Relaxation Dynamics and Aging in a Metallic Glass Probed by X-Ray Photon Correlation Spectroscopy, Phys. Rev. Lett. 109, 165701 (2012).
- B. Ruta, S. Hechler, N. Neuber, D. Orsi, L. Cristofolini, O. Gross, B. Bochtler, M. Frey, A. Kuball, S. Riegler, M. Stolpe, Z. Evenson, C. Gutt, F. Westermeier, R. Busch, and I. Gallino, Wave-Vector Dependence of the Dynamics in Supercooled Metallic Liquids, Phys. Rev. Lett. 125, 055701 (2020).
- P. Myint, K. F. Ludwig, L. Wiegart, Y. Zhang, A. Fluerasu, X. Zhang, and R. L. Headrick, de Gennes Narrowing and Relationship between Structure and Dynamics in Self-Organized Ion-Beam Nanopatterning, Phys. Rev. Lett. 126, 016101 (2021).
- G. Ju, D. Xu, M. J. Highland, C. Thompson, H. Zhou, J. A. Eastman, P. H. Fuoss, P. Zapol, H. Kim, and G. B. Stephenson, Coherent x-ray spectroscopy reveals the persistence of island arrangements during layer-by-layer growth, Nat. Phys. 15, 589 (2019).
- F. Dallari, A. Martinelli, F. Caporaletti, M. Sprung, G. Grübel, and G. Monaco, Microscopic pathways for stress relaxation in repulsive colloidal glasses, Sci. Adv. 6, eaaz2982 (2020).
- S. Gorfman, A. A. Bokov, A. Davtyan, M. Reiser, Y. Xie, Z.-G. Ye, A. V. Zozulya, M. Sprung, U. Pietsch, and C. Gutt, Ferroelectric domain wall dynamics characterized with x-ray photon correlation spectroscopy, Proc. Natl. Acad. Sci. USA 115, E6680 (2018).
- O. G. Shpyrko, E. D. Isaacs, J. M. Logan, Y. Feng, G. Aeppli, R. Jaramillo, H. C. Kim, T. F. Rosenbaum, P. Zschack, M. Sprung, S. Narayanan, and A. R. Sandy, Direct measurement of antiferromagnetic domain fluctuations, Nature (London) 447, 68 (2007).
- X. M. Chen, B. Farmer, J. S. Woods, S. Dhuey, W. Hu, C. Mazzoli, S. B. Wilkins, R. V. Chopdekar, A. Scholl, I. K. Robinson, L. E. De Long, S. Roy, and J. T. Hastings, Spontaneous Magnetic Superdomain Wall Fluctuations in an Artificial Antiferromagnet, Phys. Rev. Lett. 123, 197202 (2019).
- A. Ghazal, J. P. Lafleur, K. Mortensen, J. P. Kutter, L. Arleth, and G. V. Jensen, Recent advances in x-ray compatible microfluidics for applications in soft materials and life sciences, Lab Chip 16, 4263 (2016).
- A. Björling, L. A. B. Marçal, J. Solla-Gullón, J. Wallentin, D. Carbone, and F. R. N. C. Maia, Three-Dimensional Coherent Bragg Imaging of Rotating Nanoparticles, Phys. Rev. Lett. 125, 246101 (2020).
- L. Chayanun, L. Hrachowina, A. Björling, M. T. Borgström, and J. Wallentin, Direct three-dimensional imaging of an x-ray nanofocus using a single 60 nm diameter nanowire device, Nano Lett. 20, 8326 (2020).
- K. Kawahara, K. Gohara, Y. Maehara, T. Dobashi, and O. Kamimura, Beam-divergence deconvolution for diffractive imaging, Phys. Rev. B 81, 081404(R) (2010).
- O. Bikondoa and D. Carbone, X-ray photon correlation spectroscopy with coherent nanobeams: A numerical study, Crystals 10, 766 (2020).
- U. Johansson, D. Carbone, S. Kalbfleisch, A. Björling, M. Kahnt, S. Sala, T. Stankevic, M. Liebi, A. Rodriguez Fernandez, B. Bring, D. Paterson, K. Thånell, P. Bell, D. Erb, C. Weninger, Z. Matej, L. Roslund, K. Åhnberg, B. Norsk Jensen, H. Tarawneh et al., Nanomax: the hard x-ray nanoprobe beamline at the MAX IV Laboratory, J. Synchrotron Radiat. 28, 1935 (2021).
- A. Björling, S. Kalbfleisch, M. Kahnt, S. Sala, K. Parfeniukas, U. Vogt, D. Carbone, and U. Johansson, Ptychographic characterization of a coherent nanofocused x-ray beam, Opt. Express 28, 5069 (2020).
- Y. Sasanuma, R. V. Law, Y. Kobayashi, and K. Sasaki, Small-angle x-ray scattering measurements and image reconstruction by the maximum entropy method, Anal. Chem. 69, 794 (1997).
- See Supplemental Material at http://link.aps.org/supplemental/10.1103/PhysRevResearch.4.L032012 for details on data analysis, analytical estimations and simulations, as well as for additional data and data representations.
- J. Als-Nielsen and D. McMorrow, Kinematical scattering I: Non-crystalline materials, in Elements of Modern X-ray Physics, 1st ed. (John Wiley & Sons, United Kingdom, 2011), pp. 113–146.
- S. R. Aragón, Theory of dynamic light scattering from polydisperse systems, J. Chem. Phys. 64, 2395 (1976).
- B. J. Berne and R. Pecora, Dynamic Light Scattering: With Applications to Chemistry, Biology, and Physics, 2nd ed. (Dover Publications, Mineola, New York, 2000).
- S. O. Hruszkewycz, M. Sutton, P. H. Fuoss, B. Adams, S. Rosenkranz, K. F. Ludwig, W. Roseker, D. Fritz, M. Cammarata, D. Zhu, S. Lee, H. Lemke, C. Gutt, A. Robert, G. Grübel, and G. B. Stephenson, High Contrast X-ray Speckle from Atomic-Scale Order in Liquids and Glasses, Phys. Rev. Lett. 109, 185502 (2012).
- A. Einstein, Über die von der molekularkinetischen theorie der wärme geforderte bewegung von in ruhenden flüssigkeiten suspendierten teilchen, Ann. Phys. (Berlin, Ger.) 322, 549 (1905).
- J. Möller, M. Sprung, A. Madsen, and C. Gutt, X-ray photon correlation spectroscopy of protein dynamics at nearly diffraction-limited storage rings, IUCrJ 6, 794 (2019).
- A. R. Sandy, L. B. Lurio, S. G. J. Mochrie, A. Malik, G. B. Stephenson, J. F. Pelletier, and M. Sutton, Design and characterization of an undulator beamline optimized for small-angle coherent x-ray scattering at the advanced photon source, J. Synchrotron Radiat. 6, 1174 (1999).
- J. Als-Nielsen and D. McMorrow, X-rays and their interaction with matter, in Elements of Modern X-ray Physics, 1st ed. (John Wiley & Sons, Ltd, Chichester, West Sussex, UK, 2011), pp. 1–28.
- G. Ju, M. J. Highland, C. Thompson, J. A. Eastman, P. H. Fuoss, H. Zhou, R. Dejus, and G. B. Stephenson, Characterization of the x-ray coherence properties of an undulator beamline at the advanced photon source, J. Synchrotron Radiat. 25, 1036 (2018).
- S. A. Schichman and R. L. Amey, Viscosity and local liquid structure in dimethyl sulfoxide-water mixtures, J. Phys. Chem. 75, 98 (1971).
- H. Voigt and S. Hess, Comparison of the intensity correlation function and the intermediate scattering function of fluids: A molecular dynamics study of the Siegert relation, Phys. A (Amsterdam, Neth.) 202, 145 (1994).
- S. R. Aragón and R. Pecora, Fluorescence correlation spectroscopy as a probe of molecular dynamics, J. Chem. Phys. 64, 1791 (1976).
- Evelien J. Nijman, Henk G. Merkus, Jan C. M. Marijnissen, and Brian Scarlett, Simulations and experiments on number fluctuations in photon-correlation spectroscopy at low particle concentrations, Appl. Opt. 40, 4058 (2001).
- F. Lehmkühler, F. Dallari, A. Jain, M. Sikorski, J. Möller, L. Frenzel, I. Lokteva, G. Mills, M. Walther, H. Sinn, F. Schulz, M. Dartsch, V. Markmann, R. Bean, Y. Kim, P. Vagovic, A. Madsen, A. P. Mancuso, and G. Grübel, Emergence of anomalous dynamics in soft matter probed at the European XFEL, Proc. Natl. Acad. Sci. USA 117, 24110 (2020).
- B. Ruta, F. Zontone, Y. Chushkin, G. Baldi, G. Pintori, G. Monaco, B. Rufflé, and W. Kob, Hard x-rays as pump and probe of atomic motion in oxide glasses, Sci. Rep. 7, 3962 (2017).
- A. Madsen, R. L. Leheny, H. Guo, M. Sprung, and O. Czakkel, Beyond simple exponential correlation functions and equilibrium dynamics in x-ray photon correlation spectroscopy, New J. Phys. 12, 055001 (2010).
- DOI: 10.17045/sthlmuni.20198975.