Near-edge X-ray absorption fine-structure microscopy of organic and magnetic materials
Source abstract
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 microscopy to provide information that is otherwise inaccessible, and discuss a perspective on future developments.
Source: europepmc · Quality: candidate unverified · Source record ↗
Research context
OpenAlex topics: Advanced Electron Microscopy Techniques and Applications · Advanced X-ray Imaging Techniques · Force Microscopy Techniques and Applications
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
References (100+)
Show source-provided references
1. Stöhr, J. NEXAFS Spectroscopy (Springer, 1992).10.1007/978-3-662-02853-7 ↗
2. Stöhr, J. & Siegmann, H. C. Magnetism (Springer, 2006).
3. Ade, H. et al. Chemical contrast in X-ray microscopy and spatially resolved XANES spectroscopy of organic specimens. Science 258, 972–975 (1992).10.1126/science.1439809 ↗
4. Ade, H. & Hsiao, B. X-ray linear dichroism microscopy. Science 262, 1427–1429 (1993).10.1126/science.262.5138.1427 ↗
5. Stöhr, J. et al. Element-specific magnetic microscopy with circularly polarized X-rays. Science 259, 658–661 (1993).10.1126/science.259.5095.658 ↗
6. Stoll, H. et al. High-resolution imaging of fast magnetization dynamics in magnetic nanostructures. Appl. Phys. Lett. 84, 3328–3330 (2004).10.1063/1.1723698 ↗
7. Vogel, J. et al. Time-resolved magnetic domain imaging by X-ray photoemission electron microscopy. Appl. Phys. Lett. 82, 2299–2301 (2003).10.1063/1.1564876 ↗
8. Schmahl, G., Rudolph, D., Niemann, B. & Christ, O. Zone-plate X-ray microscopy. Q. Rev. Biophys. 13, 297–315 (1980).10.1017/S0033583500001700 ↗
9. Kirz, J., Jacobsen, C. & Howells, M. Soft X-ray microscopes and their biological applications. Q. Rev. Biophys. 28, 33–130 (1995).10.1017/S0033583500003139 ↗
10. Schneider, G. Cryo X-ray microscopy with high spatial resolution in amplitude and phase contrast. Ultramicroscopy 75, 85–104 (1998).10.1016/S0304-3991(98)00054-0 ↗
11. 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).10.1016/j.polymer.2007.10.030 ↗
12. 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).10.1016/j.elspec.2005.07.005 ↗
13. 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).10.1016/0304-3991(91)90153-W ↗
14. Griffith, O. H. & Rempfer, G. F. Photoelectron imaging in cell biology. Annu. Rev. Biophys. Biophys. Chem. 14, 113–130 (1985).10.1146/annurev.bb.14.060185.000553 ↗
15. Tonner, B. & Harp, G. R. Photoelectron microscopy with synchrotron radiation. Rev. Sci. Instrum. 59, 853–858 (1988).10.1063/1.1139792 ↗
16. 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).10.1021/jp9622748 ↗
17. Dhez, O., Ade, H. & Urquhart, S. Calibrated NEXAFS spectra of some common polymers. J. Electron Spectrosc. Relat. Phenom. 128, 85–96 (2003).10.1016/S0368-2048(02)00237-2 ↗
18. 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).10.1021/jp0255379 ↗
19. 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).10.1063/1.117120 ↗
20. 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).10.1107/S0909049502017739 ↗
21. 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).10.1046/j.1365-2818.2000.00640.x ↗
22. Ade, H. et al. X-ray spectromicroscopy with a zone plate generated microprobe. Appl. Phys. Lett. 56, 1841–1843 (1990).10.1063/1.103064 ↗
23. Gunther, S., Kaulich, B., Gregoratti, L. & Kiskinova, M. Photoelectron microscopy and applications in surface and materials science. Prog. Surf. Sci. 70, 187–260 (2002).10.1016/S0079-6816(02)00007-2 ↗
24. 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).10.1002/sia.2424 ↗
25. Tzvetkov, G. et al. In situ characterization of gas-filled microballoons using soft X-ray microspectroscopy. Soft Matter 4, 510–514 (2008).10.1039/b715392a ↗
26. Iwata, N. et al. Chemical component mapping of pulverized toner by scanning transmission X-ray microscopy. Micron 37, 290–295 (2006).10.1016/j.micron.2005.08.003 ↗
27. 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).10.1063/1.1400080 ↗
28. 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).10.1107/S0909049507029962 ↗
29. Weiss, D. et al. Computed tomography of cryogenic biological specimens based on X-ray microscopic images. Ultramicroscopy 84, 185–197 (2000).10.1016/S0304-3991(00)00034-6 ↗
30. Beetz, T. & Jacobsen, C. Soft X-ray radiation-damage studies in PMMA using a cryo-STXM. J. Synchrotron Radiat. 10, 280–283 (2003).10.1107/S0909049503003261 ↗
31. 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).10.1021/ja056589p ↗
32. Mitchell, G. E. et al. Quantitative characterization of microscopic variations in the cross-link density of gels. Macromolecules 35, 1336–1341 (2002).10.1021/ma010840d ↗
33. Köhler, K. et al. Soft X-ray Microscopy to characterize polyelectrolyte assemblies. J. Phys. Chem. B 111, 8388–8393 (2007).10.1021/jp070360+ ↗
34. Déjugnat, C. et al. Membrane densification of heated polyelectrolyte multilayer capsules characterized by soft X-ray microscopy. Adv. Mater. 19, 1331–1336 (2007).10.1002/adma.200602643 ↗
35. 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).10.1021/es0513638 ↗
36. Lawrence, J. R. et al. Mapping of metal species in biofilms using scanning transmission X-ray microscopy. Geochim. Cosmochim. Acta 69, A600 (2005).
37. Halls, J. J. M. et al. Efficient photodiodes from interpenetrating polymer networks. Nature 376, 498–500 (1995).10.1038/376498a0 ↗
38. 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).10.1126/science.270.5243.1789 ↗
39. McNeill, C. R. et al. Nanoscale quantitative chemical mapping of conjugated polymer blends. Nano Lett. 6, 1202–1206 (2006).10.1021/nl060583w ↗
40. Hoppe, H. & Sariciftci, N. S. Morphology of polymer/fullerene bulk heterojunction solar cells. J. Mater. Chem. 16, 45–61 (2006).10.1039/B510618B ↗
41. Arias, A. C. et al. Photovoltaic performance and morphology of polyfluorene blends: A combined microscopic and photovoltaic investigation. Macromolecules 34, 6005–6013 (2001).10.1021/ma010240e ↗
42. 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).10.1103/PhysRevLett.92.247402 ↗
43. McNeill, C. R. et al. X-ray microscopy of photovoltaic polyfluorene blends: Relating the nanomorphology to device performance. Macromolecules 40, 3263–3270 (2007).10.1021/ma070132d ↗
44. 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).10.1088/0957-4484/19/42/424015 ↗
45. 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).10.1021/ja067471r ↗
46. 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).
47. 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).10.1242/jeb.202.23.3295 ↗
48. Bader, S. D. Magnetism in low dimensionality. Surf. Sci. 500, 172–188 (2002).10.1016/S0039-6028(01)01625-9 ↗
49. Schütz, G. et al. Absorption of circularly polarized X-Rays in iron. Phys. Rev. Lett. 58, 737–740 (1987).10.1103/PhysRevLett.58.737 ↗
50. Fischer, P. et al. Imaging of magnetic domains by transmission X-ray microscopy. J. Phys. D 31, 649–655 (1998).10.1088/0022-3727/31/6/012 ↗
51. 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).10.1063/1.1149041 ↗
52. Eisebitt, S. et al. Lensless imaging of magnetic nanostructures by X-ray spectro-holography. Nature 432, 885–888 (2004).10.1038/nature03139 ↗
53. Hubert, A. & Schäfer, R. Magnetic Domains — The Analysis of Magnetic Microstructures (Springer, 1998).
54. Bode, M. Spin-polarized scanning tunnelling microscopy. Rep. Prog. Phys. 66, 523–582 (2003).10.1088/0034-4885/66/4/203 ↗
55. Wachowiak, A. et al. Direct observation of internal spin structure of magnetic vortex cores. Science 298, 577–580 (2002).10.1126/science.1075302 ↗
56. 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).10.1103/PhysRevLett.70.694 ↗
57. 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).10.1103/PhysRevLett.68.1943 ↗
58. Scholl, A. et al. Observation of antiferromagnetic domains in epitaxial thin films. Science 287, 1014–1016 (2000).10.1126/science.287.5455.1014 ↗
59. Nolting, F. et al. Direct observation of the alignment of ferromagnetic spins by antiferromagnetic spins. Nature 405, 767–769 (2000).10.1038/35015515 ↗
60. Ohldag, H. et al. Spectroscopic identification and direct imaging of interfacial magnetic spins. Phys. Rev. Lett. 87, 247201 (2001).10.1103/PhysRevLett.87.247201 ↗
61. Hillebrecht, F. U. et al. Magnetic moments at the surface of antiferromagnetic NiO(100). Phys. Rev. Lett. 86, 3419–3422 (2001).10.1103/PhysRevLett.86.3419 ↗
62. Eimüller, T. et al. Spin-reorientation transition in Co/Pt multilayers on nanospheres. Phys. Rev. B 77, 134415 (2008).10.1103/PhysRevB.77.134415 ↗
63. Ohldag, H. et al. pi-Electron ferromagnetism in metal-free carbon probed by soft X-ray dichroism. Phys. Rev. Lett. 98, 187204 (2007).10.1103/PhysRevLett.98.187204 ↗
64. Choe, S. B. et al. Vortex core-driven magnetization dynamics. Science 304, 420–422 (2004).10.1126/science.1095068 ↗
65. Puzic, A. et al. Spatially resolved ferromagnetic resonance: Imaging of ferromagnetic eigenmodes. J. Appl. Phys. 97, 10E704 (2005).10.1063/1.1860971 ↗
66. Chou, K. W. et al. Vortex dynamics in coupled ferromagnetic multilayer structures. J. Appl. Phys. 99, 08F305 (2006).10.1063/1.2173630 ↗
67. Slonczewski, J. C. Current-driven excitation of magnetic multilayers. J. Magn. Magn. Mater. 159, L1–L7 (1996).10.1016/0304-8853(96)00062-5 ↗
68. Berger, L. Emission of spin waves by a magnetic multilayer traversed by a current. Phys. Rev. B 54, 9353–9358 (1996).10.1103/PhysRevB.54.9353 ↗
69. Acremann, Y. et al. Time-resolved imaging of spin transfer switching: Beyond the macrospin concept. Phys. Rev. Lett. 96, 217202 (2006).10.1103/PhysRevLett.96.217202 ↗
70. Strachan, J. P. et al. Direct observation of spin-torque driven magnetization reversal through nonuniform modes. Phys. Rev. Lett. 100, 247201 (2008).10.1103/PhysRevLett.100.247201 ↗
71. 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).10.1063/1.2832656 ↗
72. Meier, G. et al. Direct imaging of stochastic domain-wall motion driven by nanosecond current pulses. Phys. Rev. Lett. 98, 187202 (2007).10.1103/PhysRevLett.98.187202 ↗
73. Argyle, B. E., Terrenzio, E. & Slonczewski, J. C. Magnetic vortex dynamics using the optical Cotton-Mouton effect. Phys. Rev. Lett. 53, 190–193 (1984).10.1103/PhysRevLett.53.190 ↗
74. Thiele, A. A. Steady-state motion of magnetic domains. Phys. Rev. Lett. 30, 230–233 (1973).10.1103/PhysRevLett.30.230 ↗
75. Huber, D. L. Equation of motion of a spin vortex in a two-dimensional planar magnet. J. Appl. Phys. 53, 1899–1900 (1982).10.1063/1.330661 ↗
76. 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).10.1016/S0304-8853(01)00708-9 ↗
77. 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).10.1103/PhysRevB.67.094410 ↗
78. Van Waeyenberge, B. et al. Magnetic vortex core reversal by excitation with short bursts of an alternating field. Nature 444, 461–464 (2006).10.1038/nature05240 ↗
79. 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).10.1063/1.2424673 ↗
80. Hertel, R., Gliga, S., Fähnle, M. & Schneider, C. M. Ultrafast nanomagnetic toggle switching of vortex cores. Phys. Rev. Lett. 98, 117201 (2007).10.1103/PhysRevLett.98.117201 ↗
81. 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).10.1103/PhysRevB.76.174410 ↗
82. Yamada, K. et al. Electrical switching of the vortex core in a magnetic disk. Nature Mater. 6, 269–273 (2007).10.1038/nmat1867 ↗
83. 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).10.1063/1.2773748 ↗
84. Curcic, M. et al. Polarisation selective magnetic vortex dynamics and core reversal in rotating magnetic fields. Phys. Rev. Lett. 101, 197204 (2008).10.1103/PhysRevLett.101.197204 ↗
85. 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).10.1140/epjb/e2003-00057-y ↗
86. 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).10.1063/1.2770819 ↗
87. 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).10.1063/1.2807274 ↗
88. Bolte, M. et al. Time-resolved X-ray microscopy of spin-torque-induced magnetic vortex gyration. Phys. Rev. Lett. 100, 176601 (2008).10.1103/PhysRevLett.100.176601 ↗
89. Sandford, S. A. et al. Organics captured from comet 81P/Wild 2 by the Stardust spacecraft. Science 314, 1720–1724 (2006).10.1126/science.1135841 ↗
90. 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).10.1126/science.1103491 ↗
91. 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).10.1021/jp076583h ↗
92. Si, M. et al. Compatibilizing bulk polymer blends by using organoclays. Macromolecules 39, 4793–4801 (2006).10.1021/ma060125+ ↗
93. 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).10.1021/ma020725i ↗
94. 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).10.1038/nature03719 ↗
95. Jefimovs, K. et al. Zone-doubling technique to produce ultrahigh-resolution x-ray optics. Phys. Rev. Lett. 99, 264801 (2007).10.1103/PhysRevLett.99.264801 ↗
96. 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).10.1038/22498 ↗
97. McNulty, I., Kirz, J. & Jacobsen, C. High resolution imaging by Fourier transform X-ray holography. Science 256, 1009–1012 (1992).10.1126/science.256.5059.1009 ↗
98. 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).10.1038/35021099 ↗
99. Chapman, H. N. et al. Femtosecond diffractive imaging with a soft-X-ray free-electron laser. Nature Phys. 2, 839–843 (2006).10.1038/nphys461 ↗
100. Feldhaus, J., Arthur, J. & Hastings, J. B. X-ray free-electron lasers. J. Phys. B 38, S799–S819 (2005).10.1088/0953-4075/38/9/023 ↗