Abstract
Many high-performance materials and novel devices consist of multiple components and are naturally or intentionally nano-structured for optimal properties and performance. To understand their structure–property relationships fully, quantitative compositional analysis at length scales below 100 nm is required, a need that is often uniquely addressed using soft X-ray microscopy. Similarly, the interaction of X-rays with magnetic materials provides unique element-specific contrast that allows the determination of magnetic properties in multi-element antiferromagnetic and ferromagnetic materials. Pump–probe-type experiments can even investigate magnetic domain dynamics. Here we review and exemplify the ability of soft X-ray micro-scopy to provide information that is otherwise inaccessible, and discuss a perspective on future developments.
This is a preview of subscription content, access via your institution
Access options
Subscribe to this journal
Receive 12 print issues and online access
$259.00 per year
only $21.58 per issue
Buy this article
- Purchase on Springer Link
- Instant access to full article PDF
Prices may be subject to local taxes which are calculated during checkout
Similar content being viewed by others
References
Stöhr, J. NEXAFS Spectroscopy (Springer, 1992).
Stöhr, J. & Siegmann, H. C. Magnetism (Springer, 2006).
Ade, H. et al. Chemical contrast in X-ray microscopy and spatially resolved XANES spectroscopy of organic specimens. Science 258, 972–975 (1992).
Ade, H. & Hsiao, B. X-ray linear dichroism microscopy. Science 262, 1427–1429 (1993).
Stöhr, J. et al. Element-specific magnetic microscopy with circularly polarized X-rays. Science 259, 658–661 (1993).
Stoll, H. et al. High-resolution imaging of fast magnetization dynamics in magnetic nanostructures. Appl. Phys. Lett. 84, 3328–3330 (2004).
Vogel, J. et al. Time-resolved magnetic domain imaging by X-ray photoemission electron microscopy. Appl. Phys. Lett. 82, 2299–2301 (2003).
Schmahl, G., Rudolph, D., Niemann, B. & Christ, O. Zone-plate X-ray microscopy. Q. Rev. Biophys. 13, 297–315 (1980).
Kirz, J., Jacobsen, C. & Howells, M. Soft X-ray microscopes and their biological applications. Q. Rev. Biophys. 28, 33–130 (1995).
Schneider, G. Cryo X-ray microscopy with high spatial resolution in amplitude and phase contrast. Ultramicroscopy 75, 85–104 (1998).
Ade, H. & Hitchcock, A. P. NEXAFS microscopy, resonant scattering and resonant reflectivity: composition and orientation probed in real and reciprocal space. Polymer 49, 643–675 (2008).
Bluhm, H. et al. Soft X-ray microscopy and spectroscopy at the molecular environmental science beamline at the Advanced Light Source. J. Electron Spectrosc. Relat. Phenom. 150, 86–104 (2006).
Birrell, G. B., Hedberg, K. K., Habliston, D. L. & Griffith, O. H. Biological applications of photoelectron imaging: A practical perspective. Ultramicroscopy 36, 235–251 (1991).
Griffith, O. H. & Rempfer, G. F. Photoelectron imaging in cell biology. Annu. Rev. Biophys. Biophys. Chem. 14, 113–130 (1985).
Tonner, B. & Harp, G. R. Photoelectron microscopy with synchrotron radiation. Rev. Sci. Instrum. 59, 853–858 (1988).
Rightor, E. G. et al. Spectromicroscopy of poly(ethylene terephthalate): Comparison of spectra and radiation damage rates in X-ray absorption and electron energy loss. J. Phys. Chem. B 101, 1950–1960 (1997).
Dhez, O., Ade, H. & Urquhart, S. Calibrated NEXAFS spectra of some common polymers. J. Electron Spectrosc. Relat. Phenom. 128, 85–96 (2003).
Urquhart, S. G. & Ade, H. Trends in the carbonyl core (C 1s, O 1s) → π*C=O transition in the near edge X-ray absorption fine structure spectra of organic molecules. J. Phys. Chem. B 106, 8531–8538 (2002).
Smith, A. P. & Ade, H. Quantitative orientational analysis of a polymeric material (Kevlar fiber) with X-ray microspectroscopy. Appl. Phys. Lett. 69, 3833–3835 (1996).
Kilcoyne, A. L. D. et al. Interferometer-controlled scanning transmission X-ray microscopes at the Advanced Light Source. J. Synchrotron Radiat. 10, 125–136 (2003).
Jacobsen, C., Wirick, S., Flynn, G. & Zimba, C. Soft X-ray spectroscopy from image sequences with sub-100 nm spatial resolution. J. Microsc. 197, 173–184 (2000).
Ade, H. et al. X-ray spectromicroscopy with a zone plate generated microprobe. Appl. Phys. Lett. 56, 1841–1843 (1990).
Gunther, S., Kaulich, B., Gregoratti, L. & Kiskinova, M. Photoelectron microscopy and applications in surface and materials science. Prog. Surf. Sci. 70, 187–260 (2002).
Locatelli, A., Aballe, L., Mentes, T. O., Kiskinova, M. & Bauer, E. Photoemission electron microscopy with chemical sensitivity: SPELEEM methods and applications. Surf. Interface Anal. 38, 1554–1557 (2006).
Tzvetkov, G. et al. In situ characterization of gas-filled microballoons using soft X-ray microspectroscopy. Soft Matter 4, 510–514 (2008).
Iwata, N. et al. Chemical component mapping of pulverized toner by scanning transmission X-ray microscopy. Micron 37, 290–295 (2006).
Mobus, G. & Inkson, B. J. Three-dimensional reconstruction of buried nanoparticles by element-sensitive tomography based on inelastically scattered electrons. Appl. Phys. Lett. 79, 1369–1371 (2001).
Johansson, G. A., Tyliszczak, T., Mitchell, G. E., Keefe, M. H. & Hitchcock, A. P. Three-dimensional chemical mapping by scanning transmission X-ray spectromicroscopy. J. Synchrotron Radiat. 14, 395–402 (2007).
Weiss, D. et al. Computed tomography of cryogenic biological specimens based on X-ray microscopic images. Ultramicroscopy 84, 185–197 (2000).
Beetz, T. & Jacobsen, C. Soft X-ray radiation-damage studies in PMMA using a cryo-STXM. J. Synchrotron Radiat. 10, 280–283 (2003).
Fujii, S., Armes, S. P., Araki, T. & Ade, H. Direct imaging and spectroscopic characterization of stimulus-responsive microgels. J. Am. Chem. Soc. 127, 16808–16809 (2005).
Mitchell, G. E. et al. Quantitative characterization of microscopic variations in the cross-link density of gels. Macromolecules 35, 1336–1341 (2002).
Köhler, K. et al. Soft X-ray Microscopy to characterize polyelectrolyte assemblies. J. Phys. Chem. B 111, 8388–8393 (2007).
Déjugnat, C. et al. Membrane densification of heated polyelectrolyte multilayer capsules characterized by soft X-ray microscopy. Adv. Mater. 19, 1331–1336 (2007).
Dynes, J. J. et al. Speciation and quantitative mapping of metal species in microbial biofilms using scanning transmission X-ray microscopy. Environ. Sci. Technol. 40, 1556–1565 (2006).
Lawrence, J. R. et al. Mapping of metal species in biofilms using scanning transmission X-ray microscopy. Geochim. Cosmochim. Acta 69, A600 (2005).
Halls, J. J. M. et al. Efficient photodiodes from interpenetrating polymer networks. Nature 376, 498–500 (1995).
Yu, G., Gao, J., Hummelen, J. C., Wudl, F. & Heeger, A. J. Polymer photovoltaic cells - Enhanced efficiencies via a network of internal donor-acceptor heterojunctions. Science 270, 1789–1791 (1995).
McNeill, C. R. et al. Nanoscale quantitative chemical mapping of conjugated polymer blends. Nano Lett. 6, 1202–1206 (2006).
Hoppe, H. & Sariciftci, N. S. Morphology of polymer/fullerene bulk heterojunction solar cells. J. Mater. Chem. 16, 45–61 (2006).
Arias, A. C. et al. Photovoltaic performance and morphology of polyfluorene blends: A combined microscopic and photovoltaic investigation. Macromolecules 34, 6005–6013 (2001).
Morteani, A. C., Sreearunothai, P., Herz, L. M., Friend, R. H. & Silva, C. Exciton regeneration at polymeric semiconductor heterojunctions. Phys. Rev. Lett. 92, 247402 (2004).
McNeill, C. R. et al. X-ray microscopy of photovoltaic polyfluorene blends: Relating the nanomorphology to device performance. Macromolecules 40, 3263–3270 (2007).
McNeill, C. R. et al. Evolution of the nanomorphology of photovoltaic polyfluorene blends: Sub-100 nm resolution with X-ray spectromicroscopy. Nanotechnology 19, 424015 (2008).
Rousseau, M. E., Hernández Cruz, D., West, M. M., Hitchcock, A. P. & Pezolet, M. Nephila clavipes spider dragline silk microstructure studied by scanning transmission X-ray microscopy. J. Am. Chem. Soc. 129, 3897–3905 (2007).
Pézolet, M. et al. Mapping Protein Orientation in Spider Silk by STXM — The Effect of Water. 2007 Activity Report, 118–119 (Canadian Light Source, 2007).
Gosline, J. M., Guerette, P. A., Ortlepp, C. S. & Savage, K. N. The mechanical design of spider silks: From fibroin sequence to mechanical function. J. Exp. Biol. 202, 3295–3303 (1999).
Bader, S. D. Magnetism in low dimensionality. Surf. Sci. 500, 172–188 (2002).
Schütz, G. et al. Absorption of circularly polarized X-Rays in iron. Phys. Rev. Lett. 58, 737–740 (1987).
Fischer, P. et al. Imaging of magnetic domains by transmission X-ray microscopy. J. Phys. D 31, 649–655 (1998).
Warwick, T. et al. A scanning transmission X-ray microscope for materials science spectromicroscopy at the Advanced Light Source. Rev. Sci. Instrum. 69, 2964–2973 (1998).
Eisebitt, S. et al. Lensless imaging of magnetic nanostructures by X-ray spectro-holography. Nature 432, 885–888 (2004).
Hubert, A. & Schäfer, R. Magnetic Domains — The Analysis of Magnetic Microstructures (Springer, 1998).
Bode, M. Spin-polarized scanning tunnelling microscopy. Rep. Prog. Phys. 66, 523–582 (2003).
Wachowiak, A. et al. Direct observation of internal spin structure of magnetic vortex cores. Science 298, 577–580 (2002).
Carra, P., Thole, B. T., Altarelli, M. & Wang, X. D. X-ray circular-dichroism and local magnetic-fields. Phys. Rev. Lett. 70, 694–697 (1993).
Thole, B. T., Carra, P., Sette, F. & Van der Laan, G. X-ray circular-dichroism as a probe of orbital magnetization. Phys. Rev. Lett. 68, 1943–1946 (1992).
Scholl, A. et al. Observation of antiferromagnetic domains in epitaxial thin films. Science 287, 1014–1016 (2000).
Nolting, F. et al. Direct observation of the alignment of ferromagnetic spins by antiferromagnetic spins. Nature 405, 767–769 (2000).
Ohldag, H. et al. Spectroscopic identification and direct imaging of interfacial magnetic spins. Phys. Rev. Lett. 87, 247201 (2001).
Hillebrecht, F. U. et al. Magnetic moments at the surface of antiferromagnetic NiO(100). Phys. Rev. Lett. 86, 3419–3422 (2001).
Eimüller, T. et al. Spin-reorientation transition in Co/Pt multilayers on nanospheres. Phys. Rev. B 77, 134415 (2008).
Ohldag, H. et al. pi-Electron ferromagnetism in metal-free carbon probed by soft X-ray dichroism. Phys. Rev. Lett. 98, 187204 (2007).
Choe, S. B. et al. Vortex core-driven magnetization dynamics. Science 304, 420–422 (2004).
Puzic, A. et al. Spatially resolved ferromagnetic resonance: Imaging of ferromagnetic eigenmodes. J. Appl. Phys. 97, 10E704 (2005).
Chou, K. W. et al. Vortex dynamics in coupled ferromagnetic multilayer structures. J. Appl. Phys. 99, 08F305 (2006).
Slonczewski, J. C. Current-driven excitation of magnetic multilayers. J. Magn. Magn. Mater. 159, L1–L7 (1996).
Berger, L. Emission of spin waves by a magnetic multilayer traversed by a current. Phys. Rev. B 54, 9353–9358 (1996).
Acremann, Y. et al. Time-resolved imaging of spin transfer switching: Beyond the macrospin concept. Phys. Rev. Lett. 96, 217202 (2006).
Strachan, J. P. et al. Direct observation of spin-torque driven magnetization reversal through nonuniform modes. Phys. Rev. Lett. 100, 247201 (2008).
Bryan, M. T., Fry, P. W., Fischer, P. J. & Allwood, D. A. Observation of field-induced domain wall propagation in magnetic nanowires by magnetic transmission X-ray microscopy. J. Appl. Phys. 103, 07D909 (2008).
Meier, G. et al. Direct imaging of stochastic domain-wall motion driven by nanosecond current pulses. Phys. Rev. Lett. 98, 187202 (2007).
Argyle, B. E., Terrenzio, E. & Slonczewski, J. C. Magnetic vortex dynamics using the optical Cotton-Mouton effect. Phys. Rev. Lett. 53, 190–193 (1984).
Thiele, A. A. Steady-state motion of magnetic domains. Phys. Rev. Lett. 30, 230–233 (1973).
Huber, D. L. Equation of motion of a spin vortex in a two-dimensional planar magnet. J. Appl. Phys. 53, 1899–1900 (1982).
Okuno, T., Shigeto, K., Ono, T., Mibu, K. & Shinjo, T. MFM study of magnetic vortex cores in circular permalloy dots: behavior in external field. J. Magn. Magn. Mater. 240, 1–6 (2002).
Thiaville, A., Garcia, J. M., Dittrich, R., Miltat, J. & Schrefl, T. Micromagnetic study of Bloch-point-mediated vortex core reversal. Phys. Rev. B 67, 094410 (2003).
Van Waeyenberge, B. et al. Magnetic vortex core reversal by excitation with short bursts of an alternating field. Nature 444, 461–464 (2006).
Xiao, Q. F., Rudge, J., Choi, B. C., Hong, Y. K. & Donohoe, G. Dynamics of vortex core switching in ferromagnetic nanodisks. Appl. Phys. Lett. 89, 262507 (2006).
Hertel, R., Gliga, S., Fähnle, M. & Schneider, C. M. Ultrafast nanomagnetic toggle switching of vortex cores. Phys. Rev. Lett. 98, 117201 (2007).
Lee, K. S., Guslienko, K. Y., Lee, J. Y. & Kim, S. K. Ultrafast vortex-core reversal dynamics in ferromagnetic nanodots. Phys. Rev. B 76, 174410 (2007).
Yamada, K. et al. Electrical switching of the vortex core in a magnetic disk. Nature Mater. 6, 269–273 (2007).
Kim, S. K., Choi, Y. S., Lee, K. S., Guslienko, K. Y. & Jeong, D. E. Electric-current-driven vortex-core reversal in soft magnetic nanodots. Appl. Phys. Lett. 91, 082506 (2007).
Curcic, M. et al. Polarisation selective magnetic vortex dynamics and core reversal in rotating magnetic fields. Phys. Rev. Lett. 101, 197204 (2008).
Zagorodny, J. P., Gaididei, Y., Mertens, F. G. & Bishop, A. R. Switching of vortex polarization in 2D easy-plane magnets by magnetic fields. Eur. Phys. J. B 31, 471–487 (2003).
Kravchuk, V. P., Sheka, D. D., Gaididei, Y. & Mertens, F. G. Controlled vortex core switching in a magnetic nanodisk by a rotating field. J. Appl. Phys. 102, 043908 (2007).
Kim, S. K., Lee, K. S., Yu, Y. S. & Choi, Y. S. Reliable low-power control of ultrafast vortex-core switching with the selectivity in an array of vortex states by in-plane circular-rotational magnetic fields and spin-polarized currents. Appl. Phys. Lett. 92, 022509 (2008).
Bolte, M. et al. Time-resolved X-ray microscopy of spin-torque-induced magnetic vortex gyration. Phys. Rev. Lett. 100, 176601 (2008).
Sandford, S. A. et al. Organics captured from comet 81P/Wild 2 by the Stardust spacecraft. Science 314, 1720–1724 (2006).
Maria, S. F., Russell, L. M., Gilles, M. K. & Myneni, S. C. B. Organic aerosol growth mechanisms and their climate-forcing implications. Science 306, 1921–1924 (2004).
Li, L. et al. X-ray microscopy studies of protein adsorption on a phase segregated polystyrene/polymethylmethacrylate surface. 2. Effect of pH on site preference. J. Phys. Chem. B 112, 2150–2158 (2008).
Si, M. et al. Compatibilizing bulk polymer blends by using organoclays. Macromolecules 39, 4793–4801 (2006).
Zhang, W. H. et al. Effect of methyl methacrylate/polyhedral oligomeric silsesquioxane random copolymers in compatibilization of polystyrene and poly(methyl methacrylate) blends. Macromolecules 35, 8029–8038 (2002).
Chao, W. L., Harteneck, B. D., Liddle, J. A., Anderson, E. H. & Attwood, D. T. Soft X-ray microscopy at a spatial resolution better than 15 nm. Nature 435, 1210–1213 (2005).
Jefimovs, K. et al. Zone-doubling technique to produce ultrahigh-resolution x-ray optics. Phys. Rev. Lett. 99, 264801 (2007).
Miao, J. W., Charalambous, P., Kirz, J. & Sayre, D. Extending the methodology of X-ray crystallography to allow imaging of micrometre-sized non-crystalline specimens. Nature 400, 342–344 (1999).
McNulty, I., Kirz, J. & Jacobsen, C. High resolution imaging by Fourier transform X-ray holography. Science 256, 1009–1012 (1992).
Neutze, R., Wouts, R., van der Spoel, D., Weckert, E. & Hajdu, J. Potential for biomolecular imaging with femtosecond X-ray pulses. Nature 406, 752–757 (2000).
Chapman, H. N. et al. Femtosecond diffractive imaging with a soft-X-ray free-electron laser. Nature Phys. 2, 839–843 (2006).
Feldhaus, J., Arthur, J. & Hastings, J. B. X-ray free-electron lasers. J. Phys. B 38, S799–S819 (2005).
Thibault, P. et al. High-resolution scanning X-ray diffraction microscopy. Science 321, 379–382 (2008).
Chapman, H. N. Focus on X-ray diffraction. Science 321, 352–353 (2008).
Araki, T. et al. Soft X-ray resonant scattering of structured polymer nanoparticles. Appl. Phys. Lett. 89, 124106 (2006).
Wang, C., Araki, T. & Ade, H. Soft X-ray resonant reflectivity of low Z material thin films. Appl. Phys. Lett. 87, 214109 (2005).
Wang, C. et al. Resonant soft X-ray reflectivity of organic thin films: Capabilities and limitations. J. Vac. Sci. Technol. A 25, 575–586 (2007).
Acknowledgements
We are grateful to J. Stöhr, R. Fink, A. P. Hitchcock, M. Pézolet, C. McNeill, Y. Acremann and H. Chapman for providing us with figures and A. P. Hitchcock for commenting on a draft document. H.A. is supported by the US Department of Energy under contract DE-FG02-98ER45737.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Ade, H., Stoll, H. Near-edge X-ray absorption fine-structure microscopy of organic and magnetic materials. Nature Mater 8, 281–290 (2009). https://doi.org/10.1038/nmat2399
Issue Date:
DOI: https://doi.org/10.1038/nmat2399
This article is cited by
-
A polymeric hydrogel electrocatalyst for direct water oxidation
Nature Communications (2023)
-
Nanoparticle-mediated cancer cell therapy: basic science to clinical applications
Cancer and Metastasis Reviews (2023)
-
Electron energy loss spectroscopy database synthesis and automation of core-loss edge recognition by deep-learning neural networks
Scientific Reports (2022)
-
Design and fabrication of Fe–Si–Al soft magnetic composites by controlling orientation of particles in a magnetic field: anisotropy of structures, electrical and magnetic properties
Journal of Materials Science (2019)
-
Classical topological order in the kinetics of artificial spin ice
Nature Physics (2018)