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Virtual Journal for Biomedical Optics

Virtual Journal for Biomedical Optics

| EXPLORING THE INTERFACE OF LIGHT AND BIOMEDICINE

  • Editors: Andrew Dunn and Anthony Durkin
  • Vol. 7, Iss. 3 — Feb. 29, 2012
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Polarization-resolved two-photon luminescence microscopy of V-groove arrays

Jonas Beermann, Sergey M. Novikov, Tobias Holmgaard, René L. Eriksen, Ole Albrektsen, Kjeld Pedersen, and Sergey I. Bozhevolnyi  »View Author Affiliations


Optics Express, Vol. 20, Issue 1, pp. 654-662 (2012)
http://dx.doi.org/10.1364/OE.20.000654


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Abstract

Using two-photon luminescence (TPL) microscopy and local reflection spectroscopy we investigate electromagnetic field enhancement effects from a µm-sized composition of 450-nm-deep V-grooves milled by focused ion beam in a thick gold film and assembled to feature, within the same structure, individual V-grooves as well as one- and two-dimensional 300-nm-period arrays of, respectively, parallel and crossed V-grooves. We analyze TPL signal levels obtained at different spatial locations and with different combinations of excitation and detection polarizations, discovering that the TPL emitted from the V-grooves is polarized in the direction perpendicular to that of the V-grooves. This feature implies that the TPL occurs solely in the form of (p-polarized) surface plasmon modes and originates therefore from the very bottom of V-grooves, where no photonic modes exist. Implications of the results obtained to evaluation of local field enhancements using TPL microscopy, especially when investigating extended structures exhibiting different radiation channels, are discussed.

© 2011 OSA

1. Introduction

Large FE occurring due to SP resonances in one-dimensional (1D) V-groove metal gratings has very recently been treated theoretically [14

14. T. Søndergaard and S. I. Bozhevolnyi, “Surface-plasmon polariton resonances in triangular-groove metal gratings,” Phys. Rev. B 80(19), 195407 (2009). [CrossRef]

] and demonstrated experimentally with individual V-grooves milled in gold [15

15. T. Søndergaard, S. I. Bozhevolnyi, J. Beermann, S. M. Novikov, E. Devaux, and T. W. Ebbesen, “Resonant plasmon nanofocusing by closed tapered gaps,” Nano Lett. 10(1), 291–295 (2010). [CrossRef] [PubMed]

]. The achieved enhancements depend on the geometry of each individual V-groove (i.e., depth and opening angle) [15

15. T. Søndergaard, S. I. Bozhevolnyi, J. Beermann, S. M. Novikov, E. Devaux, and T. W. Ebbesen, “Resonant plasmon nanofocusing by closed tapered gaps,” Nano Lett. 10(1), 291–295 (2010). [CrossRef] [PubMed]

] as well as on the separation between V-grooves interacting in 1D gratings [14

14. T. Søndergaard and S. I. Bozhevolnyi, “Surface-plasmon polariton resonances in triangular-groove metal gratings,” Phys. Rev. B 80(19), 195407 (2009). [CrossRef]

]. By this means the FE can be tuned in the wavelength range from visible to infrared, making this configuration promising for a wide range of practical applications, e.g., within surface-enhanced spectroscopies. The periodic V-groove arrangement further increases the interaction and FE via SP polaritons (SPPs) reflected between the grooves, provided that the periodicity is optimized so that standing-wave SPP resonances would coincide with localized (shape-dependent) SP resonances of individual V-grooves [14

14. T. Søndergaard and S. I. Bozhevolnyi, “Surface-plasmon polariton resonances in triangular-groove metal gratings,” Phys. Rev. B 80(19), 195407 (2009). [CrossRef]

16

16. J. Beermann, S. M. Novikov, T. Søndergaard, J. Rafaelsen, K. Pedersen, and S. I. Bozhevolnyi, “Localized field enhancements in two-dimensional V-groove metal arrays,” J. Opt. Soc. Am. B 28(3), 372–378 (2011). [CrossRef]

].

In this work, using polarization-resolved TPL microscopy (i.e., recording TPL images with different combinations of excitation and detection polarizations) in combination with spatially-resolved linear reflection spectroscopy, we investigate a 7×7-µm2-sized structure composed of 450-nm-deep V-grooves milled by focused ion beam (FIB) in a thick gold film and assembled to feature, within the same configuration, individual V-grooves as well as one- and two-dimensional 300-nm-period arrays of parallel and crossed V-grooves (Fig. 1
Fig. 1 (a) Overview and (b) zoomed SEM images (taken at a tilt angle of 54° with respect to normal incidence) of the FIB fabricated structure of crossing V-grooves having a groove period Λ = 300 nm and depth d = 450 nm. Inset in (b) shows a similarly obtained SEM image of a cut through an individually V-groove milled under the same conditions.
). Differently oriented (individual and grouped) V-grooves allow us to directly compare TPL signals obtained for different polarization configurations and local environment by using the same TPL image, i.e., at the same illumination and detection conditions. In addition, linear reflection images, by revealing the radiation absorption at the illumination wavelength, elucidate interplay between FE effects and TPL generation.

In order to collect and send as much light as possible toward the bottom of the grooves we fabricate practically touching V-grooves with walls curving toward the groove tip and meeting with a vanishingly small angle [Fig. 1(b)], ending up with a configuration that is somewhat similar to the so-called kissing nanowires [30

30. A. Aubry, D. Y. Lei, A. I. Fernández-Domínguez, Y. Sonnefraud, S. A. Maier, and J. B. Pendry, “Plasmonic light-harvesting devices over the whole visible spectrum,” Nano Lett. 10(7), 2574–2579 (2010). [CrossRef] [PubMed]

]. However, here we implement the V-groove geometry with the purpose to investigate the FE effect when moving from individual V-grooves into a parallel 1D set and, finally, a 2D array of crossing V-grooves. Accordingly, we observed the effect of individual, 1D and 2D V-groove configurations in the same structure and with fixed parameters of depth and spacing between the V-grooves thereby rendering TPL measurements of different areas in the same scan to be directly comparable.

2. Sample and experimental setup

The sample consists of five V-grooves written by FIB (Zeiss 1540 XB) along the x-direction and five V-grooves written along the y-direction and crossing the others at the center as imaged by scanning electron microscopy (SEM) [Fig. 1(a)]. For both the vertical (along y) and horizontal (along x) V-grooves, the central one is 7 μm long, whereas the others are 4 μm long. The spacing between parallel V-grooves is 300 nm and each has a depth of ~450 nm. The grooves are fabricated using 20 pA milling current with initially 3 line runs along each groove for the horizontal and vertical directions all at the same dose, followed by additionally 1 line run at the same dose along the horizontal grooves and finally 1 line run with only 50% dose along the vertical grooves. This procedure was introduced after repeated testing in order to obtain the deepest V-grooves at relatively narrow spacing and with the best similarity and symmetry between the horizontal and vertical written grooves, which could be an issue due to material re-deposition at the initially written V-grooves. The zoomed SEM image reveals a good structure quality and with relatively deep V-grooves in both directions and forming pointy ellipsoids at the intersections, i.e., with no flat area between the grooves [Fig. 1(b)].

Scattering properties of the fabricated crossing V-grooves were studied using spatially-resolved linear reflection spectroscopy. The spectroscopic reflection analysis was performed on a BX51 microscope (Olympus) equipped with a halogen light source, polarizers and a fiber-coupled grating spectrometer QE65000 (Ocean Optics) with a wavelength resolution of 1.6 nm. The reflected light was collected in backscattering configuration using MPlanFL (Olympus) objective with magnification × 100 (NA = 0.9). The image area analyzed by the spectrometer is limited by a pinhole with a diameter of 150 μm resulting in a circular probing area with a diameter of 1.5 μm. The microscope images (1600 × 1200 pixels) were captured with a LC20 digital color camera (Olympus) [Fig. 2(a)
Fig. 2 Optical images of the crossing V-grooves with the groove period of 300 nm and depth of 450 nm obtained for (a) x- and (b) y-polarized detection as indicated by double arrows (Media 1). (c) Reflection spectra of the crossing V-grooves sample obtained for x- and y-polarization in the positions marked by letters A, B, C in (a) and (b). Optical image (b) is linked with the movie (3640KB) showing the image evolution with the rotation of analyzer.
-2(b)].

The FE levels obtained with an individual V-groove, as well as with 1D and 2D configurations of V-grooves were characterized by TPL microscopy. Our experimental setup for TPL has been described in detail previously [15

15. T. Søndergaard, S. I. Bozhevolnyi, J. Beermann, S. M. Novikov, E. Devaux, and T. W. Ebbesen, “Resonant plasmon nanofocusing by closed tapered gaps,” Nano Lett. 10(1), 291–295 (2010). [CrossRef] [PubMed]

, 16

16. J. Beermann, S. M. Novikov, T. Søndergaard, J. Rafaelsen, K. Pedersen, and S. I. Bozhevolnyi, “Localized field enhancements in two-dimensional V-groove metal arrays,” J. Opt. Soc. Am. B 28(3), 372–378 (2011). [CrossRef]

, 29

29. J. Beermann, T. Søndergaard, S. M. Novikov, S. I. Bozhevolnyi, E. Devaux, and T. W. Ebbesen, “Field enhancement and extraordinary optical transmission by tapered periodic slits in gold films,” New J. Phys. 13(6), 063029 (2011). [CrossRef]

]. It consists of a scanning optical microscope in reflection geometry built on the base of a commercial microscope and a computer-controlled two-dimensional piezoelectric translation stage. The linearly polarized light beam from a mode-locked pulsed (pulse duration ~200 fs, repetition rate ~80 MHz) Ti-Sapphire laser (wavelength λ = 730 – 790 nm, δλ ~10 nm, average power ~300 mW) is used as a source of sample illumination at the fundamental harmonic (FH) frequency. After passing an optical isolator (to avoid back-reflection), half-wave plate, polarizer and wavelength selective beam splitter, the laser beam is focused on the sample surface at normal incidence with a Mitutoyo infinity-corrected × 100 objective (NA = 0.7). The TPL radiation generated in reflection and the reflected FH beam are collected with the same objective, separated by a beam splitter, directed through appropriate filters and polarizers and detected with two photomultiplier tubes, the tube for TPL photons (within the transmission band of 350-550 nm) being connected with a photon counter. The FH and TPL resolution at full-width-half-maximum were ~0.75 μm and ~0.35 μm, respectively. In this work, we used the following scan parameters: the integration time (at one point) of 100 ms, speed of scanning (between the measurement points) of 20 μm/s, scan area of 8 × 8 μm2, and scanning step size of 100 nm. We adjusted the incident power P within the range 0.7-2.5 mW in order to obtain significant TPL signals (typically, ~100 counts/s). It has also been checked that TPL signals depended quadratically on the incident power as expected for the two-photon induced up-conversion.

3. Results and discussion

The SPs modes in the V-groove can be excited only for p-polarized incident electric fields, i.e., here with the electric field being perpendicular (and the magnetic field parallel) to the V-grooves [15

15. T. Søndergaard, S. I. Bozhevolnyi, J. Beermann, S. M. Novikov, E. Devaux, and T. W. Ebbesen, “Resonant plasmon nanofocusing by closed tapered gaps,” Nano Lett. 10(1), 291–295 (2010). [CrossRef] [PubMed]

]. On the other hand, s-polarized light, with the electric field parallel to the V-grooves, is almost completely reflected because its penetration experiences cutoff with respect to the groove width, since no photonic modes can propagate down beyond the groove width that is less than half of the light wavelength and no SPs modes exist in the groove for s-polarization. Optical images of the crossing V-grooves obtained for different polarizations of the detected light clearly demonstrate this phenomenon [Fig. 2(a), 2(b))].

Using the x-polarized light one can see only the vertical 1D part of the crossing V-grooves and for y-polarized light only the horizontal 1D parts, whereas for both cases the 2D center of the sample is visible and actually appears slightly darker. Turning to the spatially-resolved linear reflection spectroscopy described above, we were able to obtain local spectra [Fig. 2(c)] for both x- and y-polarized detection from within a 1.5-µm-diameter spot at the center [letter A in Fig. 2(a), 2(b)], where V-grooves intersect - forming a 2D configuration, as well as at the horizontal (letter B) and vertical (letter C) positions with 1D V-grooves. The experimental data in Fig. 2(c) represent the reflection ratio Rstr/Rref, where Rstr is the reflection measured from the structure and Rref is the reference spectrum recorded from the smooth gold surface. The x-polarized incident light experiences almost full reflection from area B, whereas the reflection dramatically decreases in areas A and C [Fig. 2(c)]. On the other hand, the y-polarized light gives the reverse situation - with almost full reflection in area C and low reflection in area B, whereas the reflection level from the center (area A) remains very low as for the x-polarized light [Fig. 2(c)]. It should be noted, that the reflection from the central part of the sample for both polarizations is even less than from areas C for x-polarization and B for y-polarization. We think that the phenomena of broadband reflection suppression observed for 1D and 2D arrays of V-grooves (indicating substantial light absorption) might be similar in underlying physics to that described theoretically for touching nanowires [30

30. A. Aubry, D. Y. Lei, A. I. Fernández-Domínguez, Y. Sonnefraud, S. A. Maier, and J. B. Pendry, “Plasmonic light-harvesting devices over the whole visible spectrum,” Nano Lett. 10(7), 2574–2579 (2010). [CrossRef] [PubMed]

]. Here it should be emphasized that the V-groove array period of 300 nm was specifically chosen to be sufficiently small so as to exclude the influence grating diffraction effects, e.g., Rayleigh anomalies [14

14. T. Søndergaard and S. I. Bozhevolnyi, “Surface-plasmon polariton resonances in triangular-groove metal gratings,” Phys. Rev. B 80(19), 195407 (2009). [CrossRef]

], on the reflection spectra.

In order to characterize the local FE of the crossing V-grooves we used the TPL microscopy described above to obtain both FH [Fig. 3(a)
Fig. 3 (a), (b) FH and (c), (d) TPL images of the crossing V-grooves with groove period 300 nm and depth 450 nm obtained at λ = 740 nm for (a), (c) x- and (b), (d) y-polarized excitation and detection as indicated by double arrows. (e) SEM image of a test area with only a 1D structure exhibiting slightly wider grooves at one end caused by less re-deposition during the last part of each FIB-written line along the groove. (f) Averaged and normalized TPL signal cross sections taken at the positions indicated by white lines numbered in (c) and corresponding to the cross section number labeled in (f). Insets in (a), (b) show optical images obtained for the same polarization as indicated in (a), (b) by double arrows.
, 3(b)] and TPL images [Fig. 3(c), 3(d)] of the cross structure. As expected the FH images exhibit good correlation with the results obtained in white light illumination [Fig. 2(a), 2(b)) and insets in Fig. 3(a, b)]. Likewise, the polarized TPL images exhibit bright areas (highest TPL signals) at the locations corresponding to V-grooves being excited in a p-polarized configuration, but with an improved contrast and larger differences observed between the individual, 1D and 2D locations. One fine detail is that, for each of the TPL bright V-groove directions, the TPL images are actually slightly asymmetric along the V-groove with respect to the 2D center of the structure, i.e., the top part of Fig. 3(c) and right side of Fig. 3(d). This can be explained by a slight variation in the groove width and depth at the end of the FIB writing of each V-groove as demonstrated by a detailed normal incidence SEM image of a test structure with 5 parallel V-grooves fabricated in only one direction [Fig. 3(e)]. For this test structure the FIB fabrication along each groove was starting from the left and ending to the right, where it is clear that the grooves are both wider and deeper than to the left [Fig. 3(e)]. This is probably caused by ongoing re-deposition at the bottom and sides of the V-groove, which is then not the case at the very end of each FIB written line. A more open V-groove is likely to facilitate both increased excitation of SP groove modes and emission of TPL generated at the narrow bottom. Accordingly, we obtain slightly higher TPL signals at those ends of the V-grooves where each line in the FIB writing was terminated and thereby causing more open V-grooves due to less re-deposition. In hindsight, one could most likely have reduced these effects of less re-deposition at one end by systematical changing the writing direction between each FIB line, a procedure that one should definitely try out in future investigations.

First we note that the TPL intensity measured in the cross-sections at the ends of the individual (black curve) and 1D grooves (green curves) is slightly higher compared to the intermediate positions (red and blue), a feature that is in accordance with the end-effects and visual inspection of the TPL images mentioned above. The fact that the central 2D part of the cross exhibits higher TPL signals compared with the 1D parallel grooves is believed to be due to the main TPL origin being the narrow bottom of the V-grooves which is only accessible via SP modes. At the intersections there is, however, an increased possibility of also photonic modes actually accessing the bottom of the structure, as well as some additional signal caused by pointy ellipsoids formed at these intersections [Fig. 1(b)]. Images obtained in white light illumination [Fig. 4(a)
Fig. 4 (a) White light and (b) TPL images of the crossing V-grooves with period 300 nm and depth 450 nm obtained at λ = 740 nm in cross-polarized configuration, i.e., with the y-polarized excitation and x-polarized detection as indicated by double arrows, along with (c) averaged TPL signal in the cross section taken across the sample as indicated by a white line in (b).
] and TPL [Fig. 4(b)] when using the cross-polarized configuration of FH excitation and detection demonstrate these phenomena more clearly.

4. Conclusion

Acknowledgments

The authors gratefully acknowledge financial support from the Danish Council for Independent Research (FTP contract no. 09-072949) and the Lundbeck Foundation (contract no. R49-A5871). The authors thank P. K. Kristensen and J. Rafaelsen (Aalborg University) for assistance in the sample fabrication.

References and links

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J. A. Schuller, E. S. Barnard, W. Cai, Y. C. Jun, J. S. White, and M. L. Brongersma, “Plasmonics for extreme light concentration and manipulation,” Nat. Mater. 9(3), 193–204 (2010). [CrossRef] [PubMed]

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3.

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4.

G. T. Boyd, Th. Rasing, J. R. R. Leite, and Y. R. Shen, “Local-field enhancement on rough surfaces of metals, semimetals, and semiconductors with the use of optical second-harmonic generation,” Phys. Rev. B 30(2), 519–526 (1984). [CrossRef]

5.

E. J. Sánchez, L. Novotny, and X. S. Xie, “Near-field fluorescence microscopy based on two-photon excitation with metal tips,” Phys. Rev. Lett. 82(20), 4014–4017 (1999). [CrossRef]

6.

K. Kneipp, H. Kneipp, I. Itzkan, R. R. Dasari, and M. S. Feld, “Surface-enhanced Raman scattering and biophysics,” J. Phys. Condens. Matter 14(18), R597–R624 (2002). [CrossRef]

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P. J. Schuck, D. P. Fromm, A. Sundaramurthy, G. S. Kino, and W. E. Moerner, “Improving the mismatch between light and nanoscale objects with gold bowtie nanoantennas,” Phys. Rev. Lett. 94(1), 017402 (2005). [CrossRef] [PubMed]

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P. Ghenuche, S. Cherukulappurath, T. H. Taminiau, N. F. van Hulst, and R. Quidant, “Spectroscopic mode mapping of resonant plasmon nanoantennas,” Phys. Rev. Lett. 101(11), 116805 (2008). [CrossRef] [PubMed]

10.

A. Hohenau, J. Krenn, F. Garcia-Vidal, S. Rodrigo, L. Martin-Moreno, J. Beermann, and S. Bozhevolnyi, “Spectroscopy and nonlinear microscopy of gold nanoparticle arrays on gold films,” Phys. Rev. B 75(8), 085104 (2007). [CrossRef]

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S. I. Bozhevolnyi, J. Beermann, and V. Coello, “Direct observation of localized second-harmonic enhancement in random metal nanostructures,” Phys. Rev. Lett. 90(19), 197403 (2003). [CrossRef] [PubMed]

13.

J. Beermann, I. P. Radko, A. Boltasseva, and S. I. Bozhevolnyi, “Localized field enhancements in fractal shaped periodic metal nanostructures,” Opt. Express 15(23), 15234–15241 (2007). [CrossRef] [PubMed]

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T. Søndergaard and S. I. Bozhevolnyi, “Surface-plasmon polariton resonances in triangular-groove metal gratings,” Phys. Rev. B 80(19), 195407 (2009). [CrossRef]

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T. Søndergaard, S. I. Bozhevolnyi, J. Beermann, S. M. Novikov, E. Devaux, and T. W. Ebbesen, “Resonant plasmon nanofocusing by closed tapered gaps,” Nano Lett. 10(1), 291–295 (2010). [CrossRef] [PubMed]

16.

J. Beermann, S. M. Novikov, T. Søndergaard, J. Rafaelsen, K. Pedersen, and S. I. Bozhevolnyi, “Localized field enhancements in two-dimensional V-groove metal arrays,” J. Opt. Soc. Am. B 28(3), 372–378 (2011). [CrossRef]

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T. Søndergaard, S. I. Bozhevolnyi, S. M. Novikov, J. Beermann, E. Devaux, and T. W. Ebbesen, “Extraordinary optical transmission enhanced by nanofocusing,” Nano Lett. 10(8), 3123–3128 (2010). [CrossRef] [PubMed]

29.

J. Beermann, T. Søndergaard, S. M. Novikov, S. I. Bozhevolnyi, E. Devaux, and T. W. Ebbesen, “Field enhancement and extraordinary optical transmission by tapered periodic slits in gold films,” New J. Phys. 13(6), 063029 (2011). [CrossRef]

30.

A. Aubry, D. Y. Lei, A. I. Fernández-Domínguez, Y. Sonnefraud, S. A. Maier, and J. B. Pendry, “Plasmonic light-harvesting devices over the whole visible spectrum,” Nano Lett. 10(7), 2574–2579 (2010). [CrossRef] [PubMed]

31.

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OCIS Codes
(180.5810) Microscopy : Scanning microscopy
(240.4350) Optics at surfaces : Nonlinear optics at surfaces
(240.6680) Optics at surfaces : Surface plasmons
(250.5403) Optoelectronics : Plasmonics

ToC Category:
Microscopy

History
Original Manuscript: November 22, 2011
Revised Manuscript: December 17, 2011
Manuscript Accepted: December 17, 2011
Published: December 23, 2011

Virtual Issues
Vol. 7, Iss. 3 Virtual Journal for Biomedical Optics

Citation
Jonas Beermann, Sergey M. Novikov, Tobias Holmgaard, René L. Eriksen, Ole Albrektsen, Kjeld Pedersen, and Sergey I. Bozhevolnyi, "Polarization-resolved two-photon luminescence microscopy of V-groove arrays," Opt. Express 20, 654-662 (2012)
http://www.opticsinfobase.org/vjbo/abstract.cfm?URI=oe-20-1-654


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References

  1. J. A. Schuller, E. S. Barnard, W. Cai, Y. C. Jun, J. S. White, and M. L. Brongersma, “Plasmonics for extreme light concentration and manipulation,” Nat. Mater.9(3), 193–204 (2010). [CrossRef] [PubMed]
  2. Y. Liu, C. Yu, and S. Sheu, “Low concentration rhodamine 6G observed by surface-enhanced Raman scattering on optimally electrochemically roughened silver substrates,” J. Mater. Chem.16(35), 3546–3551 (2006). [CrossRef]
  3. K. Kneipp, Y. Wang, H. Kneipp, L. T. Perelman, I. Itzkan, R. R. Dasari, and M. S. Feld, “Single molecule detection using surfaceenhanced Raman scattering (SERS),” Phys. Rev. Lett.78(9), 1667–1670 (1997). [CrossRef]
  4. G. T. Boyd, Th. Rasing, J. R. R. Leite, and Y. R. Shen, “Local-field enhancement on rough surfaces of metals, semimetals, and semiconductors with the use of optical second-harmonic generation,” Phys. Rev. B30(2), 519–526 (1984). [CrossRef]
  5. E. J. Sánchez, L. Novotny, and X. S. Xie, “Near-field fluorescence microscopy based on two-photon excitation with metal tips,” Phys. Rev. Lett.82(20), 4014–4017 (1999). [CrossRef]
  6. K. Kneipp, H. Kneipp, I. Itzkan, R. R. Dasari, and M. S. Feld, “Surface-enhanced Raman scattering and biophysics,” J. Phys. Condens. Matter14(18), R597–R624 (2002). [CrossRef]
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