Abstract

Synchrotron infrared nanospectroscopy is a recently developed technique that enables new possibilities in the broadband chemical analysis of materials in the nanoscale, far beyond the diffraction limit in this frequency domain. Synchrotron infrared ports have exploited mainly the high brightness advantage provided by electron storage rings across the whole infrared range. However, optical aberrations in the beam produced by the source depth of bending magnet emission at large angles prevent infrared nanospectroscopy to reach its maximum capability. In this work we present a low-aberration optical layout specially designed and constructed for a dedicated synchrotron infrared nanospectroscopy beamline. We report excellent agreement between simulated beam profiles (from standard wave propagation and raytracing optics simulations) with experimental measurements. We report an important improvement in the infrared nanospectroscopy experiment related to the improved beamline optics. Finally, we demonstrate the performance of the nanospectroscopy endstation by measuring a hyperspectral image of a polar material and we evaluate the setup sensitivity by measuring ultra-thin polymer films down to 6 nm thick.

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

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References

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2017 (4)

I. Amenabar, S. Poly, M. Goikoetxea, W. Nuansing, P. Lasch, and R. Hillenbrand, “Hyperspectral infrared nanoimaging of organic samples based on Fourier transform infrared nanospectroscopy,” Nature Communications 8, 14402 (2017).
[Crossref] [PubMed]

D. Grasseschi, D. Bahamon, F. C. B. Maia, A. H. C. Neto, R. O. Freitas, and C. J. S. de Matos, “Oxygen impact on the electronic and vibrational properties of black phosphorus probed by synchrotron infrared nanospectroscopy,” 2D Materials 4, aa8210 (2017).
[Crossref]

C. -Y. Wu, W. J. Wolf, Y. Levartovsky, H. A. Bechtel, M. C. Martin, F. D. Toste, and E. Gross, “High-spatial-resolution mapping of catalytic reactions on single particles,” Nature 541, 511–515 (2017).
[Crossref] [PubMed]

T. Moreno, “Compact IR synchrotron beamline design,” Journal of Synchrotron Radiation 24, 1–6 (2017).
[Crossref]

2016 (6)

P. Patoka, G. Ulrich, E. A. Nguyen, L. Bartels, P. A. Dowben, V. Turkowski, T. S. Rahman, P. Hermann, B. Kästner, A. Hoehl, G. Ulm, and E. Rühl, “Nanoscale plasmonic phenomena in CVD-grown MoS 2 monolayer revealed by ultra-broadband synchrotron radiation based nano-FTIR spectroscopy and near-field microscopy,” Optics Express 24, 1154–1164 (2016).
[Crossref]

C. M. Johnson and M. Böhmler, “Nano-FTIR microscopy and spectroscopy studies of atmospheric corrosion with a spatial resolution of 20nm,” Corrosion Science 108, 60–65 (2016).
[Crossref]

B. Pollard, F. C. B. Maia, M. B Raschke, and R. O. Freitas, “Infrared Vibrational Nanospectroscopy by Self-Referenced Interferometry,” Nano Letters 16, 55–61 (2016).
[Crossref]

S. Gamage, Z. Li, V. S. Yakovlev, C. Lewis, H. Wang, S. B. Cronin, and Y. Abate, “Nanoscopy of Black Phosphorus Degradation,” Advanced Materials Interfaces 3, 1–6 (2016).

H. Amrania, L. Drummond, R. C. Coombes, S. Shousha, K. Weir, W. Hart, I. Carter, and C. C. Phillips, “New IR imaging modalities for cancer detection and for intra-cell chemical mapping with a sub-diffraction mid-IR,” Faraday Discussions 187, 539–553 (2016).
[Crossref]

R. Wiens, C. R. Findlay, S. G. Baldwin, L. Kreplak, J. M. Lee, P. Veres, and K. M. Gough, “High spatial resolution (1.1 µ m and 20 nm) FTIR polarization contrast imaging reveals pre-rupture disorder in damaged tendon,” Faraday Discussions 187, 555–573 (2016).
[Crossref]

2015 (4)

E. Ritter, L. Puskar, F. J. Bartl, E. F. Aziz, P. Hegemann, and U. Schade, “Time-resolved infrared spectroscopic techniques as applied to channelrhodopsin,” Frontiers in Molecular Biosciences 2, 38 (2015).
[Crossref] [PubMed]

C. Pépin, P. Loubeyre, F. Occelli, and P. Dumas, “Synthesis of lithium polyhydrides above 130 GPa at 300 K,” Proceedings of the National Academy of Sciences 112, 7673–7676 (2015).
[Crossref]

I. D. Barcelos, A. R. Cadore, L. C. Campos, A. Malachias, K. Watanabe, T. Taniguchi, F. C. B. Maia, R. Freitas, and C. Deneke, “Graphene/h-BN plasmon-phonon coupling and plasmon delocalization observed by infrared nano-spectroscopy,” Nanoscale 7, 11620–11625 (2015).
[Crossref] [PubMed]

Z. Shi, H. A. Bechtel, S. Berweger, Y. Sun, B. Zeng, C. Jin, M. C. Martin, M. B. Raschke, H. Chang, and F. Wang, “Amplitude- and Phase-Resolved Nanospectral Imaging of Phonon Polaritons in Hexagonal Boron Nitride,” ACS Photonics 2, 790–796 (2015).
[Crossref]

2014 (7)

G. Dominguez, A. S. Mcleod, Z. Gainsforth, P. Kelly, H. A. Bechtel, F. Keilmann, A. Westphal, M. Thiemens, and D. N. Basov, “Nanoscale infrared spectroscopy as a non-destructive probe of extraterrestrial samples,” Nature Communications 5, 5445 (2014).
[Crossref] [PubMed]

P. Hermann, A. Hoehl, G. Ulrich, C. Fleischmann, A. Hermelink, B. Kästner, P. Patoka, A. Hornemann, B. Beckhoff, E. Rühl, and G. Ulm, “Characterization of semiconductor materials using synchrotron radiation-based near-field infrared microscopy and nano-FTIR spectroscopy,” Optics Express 22, 17948–17958 (2014).
[Crossref] [PubMed]

D. K. Spaulding, G. Weck, P. Loubeyre, F. Datchi, P. Dumas, and M. Hanfland, “Pressure-induced chemistry in a nitrogen-hydrogen host–guest structure,” Nature Communications 5, 5739 (2014).
[Crossref]

E. Giorgini, G. Gioacchini, S. Sabbatini, C. Conti, L. Vaccari, A. Borini, O. Carnevali, and G. Tosi, “Vibrational characterization of female gametes: a comparative study,” The Analyst 139, 5049–5060 (2014).
[Crossref] [PubMed]

D. A. Shapiro, Y. S. Yu, T. Tyliszczak, J. Cabana, R. Celestre, W. Chao, K. Kaznatcheev, A. L. D. Kilcoyne, F. Maia, S. Marchesini, Y. S. Meng, T. Warwick, L. L. Yang, and H. A. Padmore, “Chemical composition mapping with nanometre resolution by soft X-ray microscopy,” Nature Photonics 8, 765–769 (2014).
[Crossref]

U. Schade, E. Ritter, P. Hegemann, E. F. Aziz, and K. P. Hofmann, “Concept for a single-shot mid-infrared spectrometer using synchrotron radiation,” Vibrational Spectroscopy 75, 190–195 (2014).
[Crossref]

H. A. Bechtel, E. A. Muller, R. L. Olmon, M. C. Martin, and M. B. Raschke, “Ultrabroadband infrared nanospectroscopic imaging,” Proceedings of the National Academy of Sciences 111, 7191–7196 (2014).
[Crossref]

2013 (5)

P. Hermann, A. Hoehl, P. Patoka, F. Huth, E. Rühl, and G. Ulm, “Near-field imaging and nano-Fourier-transform infrared spectroscopy using broadband synchrotron radiation,” Optics Express 21, 2913–2919 (2013).
[Crossref] [PubMed]

A. A. Govyadinov, I. Amenabar, F. Huth, P. S. Carney, and R. Hillenbrand, “Quantitative measurement of local infrared absorption and dielectric function with tip-enhanced near-field microscopy,” Journal of Physical Chemistry Letters 4, 1526–1531 (2013).
[Crossref] [PubMed]

K. Goda and B. Jalali, “Dispersive Fourier transformation for fast continuous single-shot measurements,” Nature Photonics 7, 102–112 (2013).
[Crossref]

M. J. Hackett, F. Borondics, D. Brown, C. Hirschmugl, S. E. Smith, P. G. Paterson, H. Nichol, I. J. Pickering, and G. N. George, “Subcellular biochemical investigation of purkinje neurons using synchrotron radiation fourier transform infrared spectroscopic imaging with a focal plane array detector,” ACS Chemical Neuroscience 4, 1071–1080 (2013).
[Crossref] [PubMed]

T. Moreno, H. Westfahl, R. O. Freitas, Y. Petroff, and P. Dumas, “Optical layouts for large infrared beamline opening angles,” Journal of Physics: Conference Series 425, 142003 (2013).

2012 (3)

L. M. Zhang, G. O. Andreev, Z. Fei, A. S. McLeod, G. Dominguez, M. Thiemens, A. H. Castro-Neto, D. N. Basov, and M. M. Fogler, “Near-field spectroscopy of silicon dioxide thin films,” Physical Review B 85, 1–8 (2012).

Y. Ikemoto, M. Ishikawa, S. Nakashima, H. Okamura, Y. Haruyama, S. Matsui, T. Moriwaki, and T. Kinoshita, “Development of scattering near-field optical microspectroscopy apparatus using an infrared synchrotron radiation source,” Optics Communications 285, 2212–2217 (2012).
[Crossref]

F. Huth, A. Govyadinov, S. Amarie, W. Nuansing, F. Keilmann, and R. Hillenbrand, “Nano-FTIR absorption spectroscopy of molecular fingerprints at 20 nm spatial resolution,” Nano Letters 12, 3973–3978 (2012).
[Crossref] [PubMed]

2011 (2)

F. Huth, M. Schnell, J. Wittborn, N. Ocelic, and R. Hillenbrand, “Infrared-spectroscopic nanoimaging with a thermal source,” Nature Materials 10, 352–356 (2011).
[Crossref] [PubMed]

M. J. Nasse, M. J. Walsh, E. C. Mattson, R. Reininger, A. Kajdacsy-Balla, V. Macias, R. Bhargava, and C. J. Hirschmugl, “High-resolution Fourier-transform infrared chemical imaging with multiple synchrotron beams,” Nature Methods 8, 413–416 (2011).
[Crossref] [PubMed]

2009 (1)

G. Geloni, V. Kocharyan, E. Saldin, E. Schneidmiller, and M. Yurkov, “Theory of edge radiation. Part I: Foundations and basic applications,” Nuclear Instruments and Methods in Physics Research, Section A: Accelerators, Spectrometers, Detectors and Associated Equipment 605, 409–429 (2009).
[Crossref]

2006 (1)

E. Betzig, G. H. Patterson, R. Sougrat, O. W. Lindwasser, S. Olenych, J. S. Bonifacino, M. W. Davidson, J. Lippincott-Schwartz, and H. F. Hess, “Imaging intracellular fluorescent proteins at nanometer resolution,” Science 313, 1642–1645 (2006).
[Crossref] [PubMed]

2004 (1)

F. Keilmann and R. Hillenbrand, “Near-field microscopy by elastic light scattering from a tip,” Philosophical Transactions. Series A, Mathematical, Physical, and Engineering Sciences 362, 787–805 (2004).
[Crossref] [PubMed]

2003 (1)

C. B. Walsh and E. I. Franses, “Ultrathin PMMA films spin-coated from toluene solutions,” Thin Solid Films 429, 71–76 (2003).
[Crossref]

2001 (1)

T. Moreno and M. Idir, “SPOTX a ray tracing software for X-ray optics,” J. Phys. IV France 11, 527–531 (2001).
[Crossref]

2000 (1)

T. A. Klar, S. Jakobs, M. Dyba, A. Egner, and S. W. Hell, “Fluorescence microscopy with diffraction resolution barrier broken by stimulated emission,” Proceedings of the National Academy of Sciences 97, 8206–8210 (2000).
[Crossref]

1999 (1)

B. Knoll and F. Keilmann, “Near-field probing of vibrational absorption for chemical microscopy,” Nature 399, 7–10 (1999).
[Crossref]

1997 (1)

R. M. Dickson, A. B. Cubitt, R. Tsien, and W. E. Moerner, “On/off blinking and switching behaviour of single molecules of green fluorescent protein,” Nature 388, 355–358 (1997).
[Crossref] [PubMed]

1996 (1)

R. K. Agrawal, P. Penczek, R. A. Grassucci, Y. Li, A. Leith, K. H. Nierhaus, and J. Frank, “Direct visualization of A-, P-, and E-site transfer RNAs in the Escherichia coli ribosome,” Science 271, 1000–1002 (1996).
[Crossref] [PubMed]

1995 (4)

S. W. Hell and M. Kroug, “Ground-state-depletion fluorescence microscopy: a concept for breaking the diffracition resolution limit, Applied Physics B: Lasers and Optics,”  60, 495–497 (1995).
[Crossref]

E. Betzig, “Proposed method for molecular optical imaging,” Optics Letters 20, 237–239 (1995).
[Crossref] [PubMed]

S. Kawata and Y. Inouye, “Scanning probe optical microscopy using a metallic probe tip,” Ultramicroscopy 57, 313–317 (1995).
[Crossref]

F. Zenhausern, Y. Martin, and H. K. Wickramasinghe, “Scanning interferometric apertureless microscopy: optical imaging at 10 angstrom resolution,” Science 269, 1083–1085 (1995).
[Crossref]

1983 (1)

W. D. Duncan, G. P. Williams, B. Hill, and B. National, “Infrared synchrotron radiation from electron storage rings,” Applied Optics 22, 2914–2923 (1983).
[Crossref] [PubMed]

1981 (1)

J. Dubochet and A. W. McDowall, “Vitrification of Pure Water for Electron Microscopy,” Journal of Microscopy 124, 3–4 (1981).
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Nature Materials (1)

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Figures (7)

Fig. 1
Fig. 1 (a) Beamline primary optics for extraction, focusing and collimation of the BM radiation. (b) Scheme of the custom designed dipole vacuum chamber for IR extraction. The electrons trajectory in the sight of the port defines the source length. (c) Cartoon of the conical mirror M2 which is able to compensate for source depth aberrations. (d) SRW calculated spectral irradiance of the IR1 extraction port compared to blackbody emission from a 1000K globar simulated via XOP.
Fig. 2
Fig. 2 SRW (a–c) and spotX (d–f) simulations of the beam cross-section at M1 for λ=980 nm. Scale bars in (a,b) represent 20 mm.
Fig. 3
Fig. 3 Focal point intensity cross-sections (a) simulated by spotX and (b) measured at ∼7 m from the origin for λ=980 nm. (c,d) Intensity profiles along the white dashed lines in (a,b). Simulated (e) and measured (f) intensity cross-sections of the collimated beam right after M5. The yellow dashed rectangle in (f) indicates the portion of the beam used in the nano-FTIR experiment. Simulated (g,h) and measured (i,j) intensity profiles of the collimated beam taken along the white dashed lines in (e,f). White scale bars represent 500 µm (a,b) and 5 mm (e,f).
Fig. 4
Fig. 4 (a) Scheme of the nano-FTIR experiment at LNLS. (b) spotX simulation of the focal point at the AFM tip at 10 µm wavelength. (c–d) Intensity profiles along the horizontal and vertical dashed lines marked in (b). Black solid profiles in (c–d) indicate the spotX simulation using the proposed beamline optics (conical-cylindrical shapes for mirrors M2-M3) and red dashed profile in (d) indicate the focal point at the tip when using standard beamline optics (toroidal shape for M2-M3). In the actual experiment, a periscope is used in order to align the long axis of the focus with the tip shaft. Scale bar in (b) represents 20 µm.
Fig. 5
Fig. 5 Nano-FTIR (black curve), far-field FTIR (blue curve) standard reference spectra from a gold substrate in the IR1 setup. Scale bar in (b) represents 20 µm.
Fig. 6
Fig. 6 (a) Broadband IR image of a SiO2/Si AFM micro-standard. (b) Spectral linescan along the horizontal dashed line in (a). AFM topography indicated by the white line at the bottom of (b). (c) Point nano-FTIR spectrum taken at the center of the SiO2 step (red dot in the inset 3D cartoon of the sample). Energy-selective nano-FTIR maps for integrated frequency ranges (d) inside the SiO2 SPhP peak and for frequencies outside the SiO2 phonon resonance. Maps extracted from a full hyperspectral map of the sample.
Fig. 7
Fig. 7 (a) Nano-FTIR imaginary spectra of PMMA films with thicknesses from 312 nm to 3 nm. (b) Spectral comparison between far-field FTIR (blue curve) and nano-FTIR (black curve) measured from a 120 nm PMMA/Au film. Zoom on the spectral absorbance of the C=O functional group for several films thicknesses measured with (c) nano-FTIR and (d) ATR-FTIR. Bottom inset in (d) shows ATR-FTIR for thicknesses 3, 6 and 11 nm.

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