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Optics Express

Optics Express

  • Editor: C. Martijn de Sterke
  • Vol. 19, Iss. 15 — Jul. 18, 2011
  • pp: 14726–14734
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Photothermal reshaping of gold nanoparticles in a plasmonic absorber

Jing Wang, Yiting Chen, Xi Chen, Jiaming Hao, Min Yan, and Min Qiu  »View Author Affiliations


Optics Express, Vol. 19, Issue 15, pp. 14726-14734 (2011)
http://dx.doi.org/10.1364/OE.19.014726


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Abstract

We experimentally demonstrate that a metamaterial nanostructure can have a localized heating response owing to plasmonic resonances in the near-infrared wavelength range (from 1.5 to 2µm). With a broadband nanosecond-pulse light, the temperature of composing gold particles in the nanostructure can be easily increased to over 900K within only several nanoseconds, resulting in re-shaping of the particles. The photothermal effect is elaborated with finite-element based numerical simulations. The absorption resonance can in principle be tailored with a great freedom by choosing appropriate metamaterial parameters. The light-induced heating in an artificial metamaterial can be potentially used for all-optical acute temperature tuning in a micro-environment, which may open new frontiers especially in nanotechnology and biotechnology.

© 2011 OSA

1. Introduction

2. Experiment

Figure 1
Fig. 1 Schematic diagrams for the experiment. (A) Fabricated metamaterial sample. Yellow regions correspond to gold, and green region is Al2O3. (B) Sample illuminated with a white light. (C) Sample after irradiation.
illustrates our experiment flow. First a gold nanostructure is fabricated by a standard nanofabrication procedure (Appendix A). A single unit of the structure consists of a layer of 40nm-thick gold particle and a 60nm-thick continuous gold film, separated by a 10nm-thick Al2O3 dielectric layer, shown in Fig. 1(A). A 150μm-thick SiO2 substrate is further beneath the structure (not shown). The gold nanoparticles have a rectangular shape of dimension 230 × 170nm2. A plasmonic resonance at NIR wavelength (λp) exists due to coupling between each gold particle and the bottom gold film [28

28. J. M. Hao, J. Wang, X. Liu, W. J. Padilla, L. Zhou, and M. Qiu, “High performance optical absorber based on a plasmonic metamaterial,” Appl. Phys. Lett. 96(25), 251104 (2010). [CrossRef]

]. Such a subwavelength resonator unit repeats in a square lattice with a period of 310nm, forming a metamaterial film which efficiently absorbs incoming light at λp with minimum reflection and transmission (refer to Fig. 2(A)
Fig. 2 Measured absorption spectra for (A) an unmelted sample region, and (B) a melted sample region at a 10° incidence angle. Plane of incidence: xz. Red-solid and blue-dashed curves are for TM and TE polarization respectively. (C,D) are simulated results for the situations described in (A,B) correspondingly. Insets: representative SEM images for a single sample unit.
for the absorption spectrum of our fabricated nanostructure sample). Such artificial structures formed with lossy EM resonators were reported also in [29

29. N. I. Landy, S. Sajuyigbe, J. J. Mock, D. R. Smith, and W. J. Padilla, “Perfect metamaterial absorber,” Phys. Rev. Lett. 100(20), 207402 (2008). [CrossRef] [PubMed]

32

32. V. A. Fedotov, P. L. Mladyonov, S. L. Prosvirnin, and N. I. Zheludev, “Planar electromagnetic metamaterial with a fish scale structure,” Phys. Rev. E Stat. Nonlin. Soft Matter Phys. 72(5), 056613 (2005). [CrossRef] [PubMed]

]. We irradiate (Fig. 1(B)) the fabricated gold nanostructure by a focused broadband white light. The setup is illustrated in Fig. 3
Fig. 3 Schematic setup for the photothermal experiment.
. A super-continuum white light source (NKT SuperK Compact) with a spectral range of 0.5-2.4µm, a repetition rate of 27 kHz, and an average output power of 101mW is utilized. The output fiber of the source is connected to a reflective collimator (Thorlabs RC08FC), generating a collimated beam with a diameter of 8.5 mm. The collimated beam is then attenuated by two circular variable BK7 neutral-density filters (Melles Griot CND-1-100.0M) and then focused by an aspherized achromatic lens (Edmund NT49-665, EFL = 5cm) onto the nanostructure. The time-averaged light power reaching the sample is about 2.3mW, with a beam diameter of 20μm. The exposure time is fixed at about 0.2 second. Behind the sample there are a 20 × long-working-distance objective (Mitutoyo 378-804-2, NA = 0.42, WD = 20mm) and a CCD camera (Micro Ocular MD300) connected to a computer, working as a microscope to keep track of the nanostructure position. Figure 1(C) shows the schematic picture of the sample after irradiation. The top gold particles are converted to spherical domes due to excessive heating and reshaping owing to surface tension in liquid phase.

Figure 4(A)
Fig. 4 (A) SEM image of a region of the irradiated sample with both unmelted and melted gold nanoparticles. (B,C) Enlarged oblique views.
shows a top-view scanning electron microscopy (SEM) image of the illuminated sample. One sees clearly the reshaped particles (only the lower half of the melted pattern is shown). Outside the half-circular melted domain, the particles remain intact. The circular boundary separating the reshaped and original particles is caused by the Gaussian beam profile. Further increasing the incident power we observe, of less technological interest, fragmented gold particles in the beam center and even severely burnt sample (not shown). Fragmentation of gold particles due to laser pulse irradiation was previously thoroughly studied in [9

9. H. Kurita, A. Takami, and S. Koda, “Size reduction of gold particles in aqueous solution by pulsed laser irradiation,” Appl. Phys. Lett. 72(7), 789 (1998). [CrossRef]

]. Figures 4(B) and 4(C) compare the detailed oblique SEM views of the particles before and after irradiation. The particles in thin blocks in Fig. 4(A) have grainy top surfaces and rough side edges due to, respectively, the electron beam evaporation method used for metal deposition and the lift-off patterning process. In contrast, the gold particles after irradiation have a much higher surface quality. The quality of gold domes can be further elucidated by examining the 3D atomic force microscopy images of the nanoparticles before and after irradiation, as shown in Fig. 5(A)
Fig. 5 Atomic-force microscope images of the gold nanoparticles before (A) and after (B) melting. (C) A histogram illustrating the diameter distribution of 80 semi-spherical nanoparticles from an SEM image. The red line is a Gaussian fit. The mean diameter of spherical nanoparticles is 160nm with a derivation of ~4%.
and Fig. 5(B), respectively. The spherical particles have an average radius of 80nm (refer to Fig. 5(C)) and a height around 90nm; their contacting surface to the Al2O3 layer has a radius about 70nm.

The shape transformation and possibly some improvement in the inner structure of the gold nanoparticles should substantially influence the absorption characteristics of the metamaterial absorber. By using a homemade setup, we measure the absorbance (Appendix B) of the sample at both melted and un-melted regions with a 10° incidence angle. We point out that the absorber in such a configuration in general has an absorption spectrum insensitive to the incidence angle [33

33. J. Wang, Y. Chen, J. Hao, M. Yan, and M. Qiu, “Shape-dependent absorption characteristics of three-layered metamaterial absorbers at near-infrared,” J. Appl. Phys. 109(7), 074510 (2011). [CrossRef]

]. The plane of incidence intersects with the metamaterial in the direction along which the particles have a smaller size. Two measurement results are given in Figs. 2(A) and 2(B) for both the transverse-magnetic (TM) and the transverse-electric (TE) polarizations. For the sample region with rectangular nanoparticles (Fig. 2(A)), the absorption peak differs for the two polarizations, at 1.58μm for TM and ~2µm for TE [28

28. J. M. Hao, J. Wang, X. Liu, W. J. Padilla, L. Zhou, and M. Qiu, “High performance optical absorber based on a plasmonic metamaterial,” Appl. Phys. Lett. 96(25), 251104 (2010). [CrossRef]

]. For the region with dome-shaped nanoparticles (Fig. 2(B)), due to the higher symmetry of the unit cell, the absorption peaks for two polarizations almost overlap at 1.1μm. We carried out EM scattering simulations with structural parameters extracted from the experimental sample (Appendix C). The simulated absorption spectra for two sample regions are shown in Figs. 2(C) and 2(D). Overall, the experimental results agree well with simulated results. This study suggests that an absorption spectrum can serve as a second signature for such a photothermal fusion experiment. Here for the simulation of absorption by an unmelted sample region we used a constant much larger than its bulk value [34

34. P. B. Johnson and R. W. Christy, “Optical constants of the noble metals,” Phys. Rev. B 6(12), 4370–4379 (1972). [CrossRef]

] to take into account the extra scattering caused by its rough surface, as a common practice in such EM simulations [31

31. N. Liu, M. Mesch, T. Weiss, M. Hentschel, and H. Giessen, “Infrared perfect absorber and its application as plasmonic sensor,” Nano Lett. 10(7), 2342–2348 (2010). [CrossRef] [PubMed]

]. However, for the simulation of absorption by a melted sample region we used a damping constant equal to its bulk value, owing to the higher-quality gold nanoparticles.

3. Numerical Confirmation

To unfold the mechanism behind the reshaping of the nanoparticles, we numerically simulate the photothermal heating process with the help of a finite-element numerical tool offered by the commercial COMSOL Multiphysics software [35

35. The detailed implementation of the numerical model will be submitted for publication separately.

]. All input parameters are in accordance to those used in the experiment. In laser heating experiment, the plasmonic absorber is irradiated with a super-continuum light source with an average power of 2.3mW, a beam diameter of 20μm, and a repetition rate of27 kHz. Our simulation results are summarized in Fig. 6
Fig. 6 (A) Radial distribution of the temperature in top-layer gold particles at various timings. r = 0 refers to the center of the incident light beam. (B) The transient heating of the top-layer gold nanoparticle and the gold film subject to a pulsed heat source. The traces are for the particle at r = 5μm. The yellow-shaded region in (A) and (B) is for temperature>682K, e.g. the reshaping threshold temperature. (C) The temperature distribution in the unit cell studied in (B) at t = t0 + 1.5ns when the particle reaches its highest temperature.
. Figure 6(A) presents the spatial distribution of the top-layer nanoparticle temperature at various timings. The distribution in general inherits the Gaussian profile of the light beam. Notice that at time t = t0 + 1ns, where t0 is pulse delay for the heat source, gold nanoparticles at the beam centre exceeds 682K in temperature and are therefore experiencing melting. This portion of particles becomes at first larger, up to a circular region enclosed by r ≈ 5μm where r is the distance from the beam centre, and then smaller due to the dominance of heat diffusion. Notice that here the particle melting temperature, i.e. 682K, is interpreted according to the pattern of the melted sample as in Fig. 4(A), which roughly is a circle with a radius of 5μm. Outside the circle, the sample retains its structure after irradiation; just within the circle, the top-layer nanoparticles are expected to experience partial melting or surface melting; further to the centre of the circle, where temperature of gold particles reach 928K, complete melting and damage to the sample can happen. Figure 6(B) presents the transient temperature variations in both the top gold nanoparticle and the bottom gold film at r = 5µm, just within the reshaped region, subject to a time-dependent Gaussian heat source. It is seen that temperature in the gold particle reaches to its maximum at t0 + 1.5ns, i.e. 1.5ns after the peak heat source power occurs. The temperature drops slowly through heat diffusion, and back to 358K. A difference of ~50K between the particle and the film in their maximum achievable temperatures is clearly visible. The temperature distribution in a single unit of the sample at t = t0 + 1.5ns (as highlighted in Fig. 6(B)) is plotted in Fig. 6(C). One important observation is that the temperature has a huge spatial gradient of ~400K/200nm in z direction, due to the fact that the generated heat around the nanoparticle cannot be dissipated in a few nanoseconds. Although not shown explicitly, our calculation also reveals that the photothermal reshapings of the top nanoparticles can be induced with just one-pulse irradiance.

4. Conclusion

Appendix A: Sample Preparation

The silica substrate is first covered with a 60nm-thick gold film and then a 10nm-thick alumina film using electron-beam (E-beam) evaporation. A very low deposition rate of 0.5Å/s is used during the deposition of the layers in order to obtain smooth films. The substrate is then covered by a positive resist (ZEP 520A, R&D center, Special Materials Division, Japan) and rectangular nanoparticle structures are defined in the resist by E-beam lithography (Raith 150, Raith GmbH). Usually, E-beam lithography of such a high-density structure is challenging due to scattering of electrons within the resist, which can destroy the designed structure and cause the resist to collapse. In our fabrication, the best structures are obtained with a 25kV acceleration voltage and a very low beam current of 25pA. Using these settings, the scattering of electrons during E-beam writing is reduced. A 4nm-thick titanium layer and a 40nm-thick gold layer are then deposited by E-beam evaporation on the sample. The deposition rate for both the Titanium and gold layers is again at 0.5Å/s. A lift-off process is used to produce rectangular gold nanoparticles from the gold film. The Titanium layer functions as an adhesion layer so that the gold nanoparticles do not easily fall off. The fabricated metamaterial absorber sample has an area of 100×100μm2.

Appendix B: Transmission and Reflection Spectra Measurement

The transmission and reflection spectra in the case of oblique incidence are obtained by a homemade setup. Refer to Fig. 7
Fig. 7 Transmission/reflection measurement setup for oblique incidence angle.
for the measurement setup. The light source (same as that in the photothermal experiment) first passes through a pinhole with a diameter of 600μm (Edmund NT56-288), which acts as an attenuator, then a linear polarizer (Thorlabs LPNIR100-NP), and finally is focused by an aspherized achromatic doublet. When reaching the nanostructure, the light beam has a diameter less than 50µm. The average beam power is kept less than 30µW to avoid melting of the gold particles. A 20× objective and a CCD are placed behind the sample, which play the same roles as they do in the photothermal experiment. The reflected light from the metamaterial absorber, after being focused by an achromatic doublet (Thorlabs AC254-045-C-ML, EFL=4.5cm) is collected by a multimode fiber (Thorlabs M31L03), which is connected to an optical spectrum analyzer (OSA, Agilent 86142B). The reflectance spectrum is normalized by the reflectance of a gold film. To measure the transmission spectrum, the objective as well as the CCD, which were placed behind the sample, is then replaced with the doublet and multi-mode fiber receiver. The transmission spectra are recorded by OSA connected to the fiber receiver.

Appendix C: EM Scattering Simulations

Numerical simulations are performed with the commercial COMSOL Multiphysics (Version 3.5a) using a 3D finite-element method. The permittivity of gold is given by the Drude model εAu(ω)=9ωp2/(ω2+iωγ) with the plasma frequency ωp= 2π×2.175×1015s1 and the collision frequency γ=2π×1.5958×1013s1. This Drude model agrees well with the experimental values [31

31. N. Liu, M. Mesch, T. Weiss, M. Hentschel, and H. Giessen, “Infrared perfect absorber and its application as plasmonic sensor,” Nano Lett. 10(7), 2342–2348 (2010). [CrossRef] [PubMed]

] in the concerned wavelength range of 0.5~2.4µm. The refractive index of Al2O3 is chosen as a fixed value of 1.75 over the wavelength range. All materials are assumed to be non-magnetic (µ=µ 0). Fine mesh is imposed on spatial regions where strong inhomogeneity exists.

Acknowledgments

This work is supported by the Swedish Foundation for Strategic Research (SSF) and the Swedish Research Council (VR).

References and links

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P. Zijlstra, J. W. M. Chon, and M. Gu, “Five-dimensional optical recording mediated by surface plasmons in gold nanorods,” Nature 459(7245), 410–413 (2009). [CrossRef] [PubMed]

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D. Boyer, P. Tamarat, A. Maali, B. Lounis, and M. Orrit, “Photothermal imaging of nanometer-sized metal particles among scatterers,” Science 297(5584), 1160–1163 (2002). [CrossRef] [PubMed]

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W. S. Chang, J. W. Ha, L. S. Slaughter, and S. Link, “Plasmonic nanorod absorbers as orientation sensors,” Proc. Natl. Acad. Sci. U.S.A. 107(7), 2781–2786 (2010). [CrossRef] [PubMed]

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S. Link, C. Burda, B. Nikoobakht, and M. A. El-Sayed, “Laser-induced shape changes of colloidal gold nanorods using femtosecond and nanosecond laser pulses,” J. Phys. Chem. B 104(26), 6152–6163 (2000). [CrossRef]

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C. M. Aguirre, C. E. Moran, J. F. Young, and N. J. Halas, “Laser-induced reshaping of metallodielectric nanoshells under femtosecond and nanosecond plasmon resonant illumination,” J. Phys. Chem. B 108(22), 7040–7045 (2004). [CrossRef]

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J. Bosbach, D. Martin, F. Stietz, T. Wenzel, and F. Träger, “Laser-based method for fabricating monodisperse metallic nanoparticles,” Appl. Phys. Lett. 74(18), 2605 (1999). [CrossRef]

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A. Plech, V. Kotaidis, M. Lorenc, and J. Boneberg, “Femtosecond laser near-field ablation from gold nanoparticles,” Nat. Phys. 2(1), 44–47 (2006). [CrossRef]

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A. O. Govorov and H. H. Richardson, “Generating heat with metal nanoparticles,” Nano Today 2(1), 30–38 (2007). [CrossRef]

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H. H. Richardson, M. T. Carlson, P. J. Tandler, P. Hernandez, and A. O. Govorov, “Experimental and theoretical studies of light-to-heat conversion and collective heating effects in metal nanoparticle solutions,” Nano Lett. 9(3), 1139–1146 (2009). [CrossRef] [PubMed]

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F. Xiao, T.-H. Wu, and P. Y. Chiou, “Near field photothermal printing of gold microsctructures and nanostuctures,” Appl. Phys. Lett. 97(3), 031112 (2010). [CrossRef]

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G. Baffou, R. Quidant, and F. J. García de Abajo, “Nanoscale control of optical heating in complex plasmonic systems,” ACS Nano 4(2), 709–716 (2010). [CrossRef] [PubMed]

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29.

N. I. Landy, S. Sajuyigbe, J. J. Mock, D. R. Smith, and W. J. Padilla, “Perfect metamaterial absorber,” Phys. Rev. Lett. 100(20), 207402 (2008). [CrossRef] [PubMed]

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31.

N. Liu, M. Mesch, T. Weiss, M. Hentschel, and H. Giessen, “Infrared perfect absorber and its application as plasmonic sensor,” Nano Lett. 10(7), 2342–2348 (2010). [CrossRef] [PubMed]

32.

V. A. Fedotov, P. L. Mladyonov, S. L. Prosvirnin, and N. I. Zheludev, “Planar electromagnetic metamaterial with a fish scale structure,” Phys. Rev. E Stat. Nonlin. Soft Matter Phys. 72(5), 056613 (2005). [CrossRef] [PubMed]

33.

J. Wang, Y. Chen, J. Hao, M. Yan, and M. Qiu, “Shape-dependent absorption characteristics of three-layered metamaterial absorbers at near-infrared,” J. Appl. Phys. 109(7), 074510 (2011). [CrossRef]

34.

P. B. Johnson and R. W. Christy, “Optical constants of the noble metals,” Phys. Rev. B 6(12), 4370–4379 (1972). [CrossRef]

35.

The detailed implementation of the numerical model will be submitted for publication separately.

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OCIS Codes
(160.3918) Materials : Metamaterials
(220.4241) Optical design and fabrication : Nanostructure fabrication
(250.5403) Optoelectronics : Plasmonics

ToC Category:
Metamaterials

History
Original Manuscript: May 19, 2011
Revised Manuscript: July 8, 2011
Manuscript Accepted: July 8, 2011
Published: July 15, 2011

Citation
Jing Wang, Yiting Chen, Xi Chen, Jiaming Hao, Min Yan, and Min Qiu, "Photothermal reshaping of gold nanoparticles in a plasmonic absorber," Opt. Express 19, 14726-14734 (2011)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-19-15-14726


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References

  1. X. Huang, I. H. El-Sayed, W. Qian, and M. A. El-Sayed, “Cancer cell imaging and photothermal therapy in the near-infrared region by using gold nanorods,” J. Am. Chem. Soc. 128(6), 2115–2120 (2006). [CrossRef] [PubMed]
  2. W. Zhao and J. M. Karp, “Tumour targeting: Nanoantennas heat up,” Nat. Mater. 8(6), 453–454 (2009). [CrossRef] [PubMed]
  3. G. L. Liu, J. Kim, Y. Lu, and L. P. Lee, “Optofluidic control using photothermal nanoparticles,” Nat. Mater. 5(1), 27–32 (2006). [CrossRef] [PubMed]
  4. J. X. Huang and R. B. Kaner, “Flash welding of conducting polymer nanofibres,” Nat. Mater. 3(11), 783–786 (2004). [CrossRef] [PubMed]
  5. Y. Lu, J. Y. Huang, C. Wang, S. Sun, and J. Lou, “Cold welding of ultrathin gold nanowires,” Nat. Nanotechnol. 5(3), 218–224 (2010). [CrossRef] [PubMed]
  6. P. Zijlstra, J. W. M. Chon, and M. Gu, “Five-dimensional optical recording mediated by surface plasmons in gold nanorods,” Nature 459(7245), 410–413 (2009). [CrossRef] [PubMed]
  7. D. Boyer, P. Tamarat, A. Maali, B. Lounis, and M. Orrit, “Photothermal imaging of nanometer-sized metal particles among scatterers,” Science 297(5584), 1160–1163 (2002). [CrossRef] [PubMed]
  8. W. S. Chang, J. W. Ha, L. S. Slaughter, and S. Link, “Plasmonic nanorod absorbers as orientation sensors,” Proc. Natl. Acad. Sci. U.S.A. 107(7), 2781–2786 (2010). [CrossRef] [PubMed]
  9. H. Kurita, A. Takami, and S. Koda, “Size reduction of gold particles in aqueous solution by pulsed laser irradiation,” Appl. Phys. Lett. 72(7), 789 (1998). [CrossRef]
  10. S. Link, C. Burda, B. Nikoobakht, and M. A. El-Sayed, “Laser-induced shape changes of colloidal gold nanorods using femtosecond and nanosecond laser pulses,” J. Phys. Chem. B 104(26), 6152–6163 (2000). [CrossRef]
  11. C. M. Aguirre, C. E. Moran, J. F. Young, and N. J. Halas, “Laser-induced reshaping of metallodielectric nanoshells under femtosecond and nanosecond plasmon resonant illumination,” J. Phys. Chem. B 108(22), 7040–7045 (2004). [CrossRef]
  12. J. Bosbach, D. Martin, F. Stietz, T. Wenzel, and F. Träger, “Laser-based method for fabricating monodisperse metallic nanoparticles,” Appl. Phys. Lett. 74(18), 2605 (1999). [CrossRef]
  13. A. Plech, V. Kotaidis, M. Lorenc, and J. Boneberg, “Femtosecond laser near-field ablation from gold nanoparticles,” Nat. Phys. 2(1), 44–47 (2006). [CrossRef]
  14. A. O. Govorov and H. H. Richardson, “Generating heat with metal nanoparticles,” Nano Today 2(1), 30–38 (2007). [CrossRef]
  15. H. H. Richardson, M. T. Carlson, P. J. Tandler, P. Hernandez, and A. O. Govorov, “Experimental and theoretical studies of light-to-heat conversion and collective heating effects in metal nanoparticle solutions,” Nano Lett. 9(3), 1139–1146 (2009). [CrossRef] [PubMed]
  16. F. Xiao, T.-H. Wu, and P. Y. Chiou, “Near field photothermal printing of gold microsctructures and nanostuctures,” Appl. Phys. Lett. 97(3), 031112 (2010). [CrossRef]
  17. G. Baffou, R. Quidant, and F. J. García de Abajo, “Nanoscale control of optical heating in complex plasmonic systems,” ACS Nano 4(2), 709–716 (2010). [CrossRef] [PubMed]
  18. G. Baffou, C. Girard, and R. Quidant, “Mapping heat origin in plasmonic structures,” Phys. Rev. Lett. 104(13), 136805 (2010). [CrossRef] [PubMed]
  19. R. D. Averitt, S. L. Westcott, and N. J. Halas, “Linear optical properties of gold nanoshells,” J. Opt. Soc. Am. B 16(10), 1824 (1999). [CrossRef]
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