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LSPR-based Fiber Optic Sensing With Chemically Deposited Au Nanoparticles

Alexandre R. Camara1, Paula M. P. Gouva2, Alexandre G. Brolo3, Meikun Fan3, Ryan Abel3, Michael Fokine4, Arthur M. B. Braga2, Isabel C. S. Carvalho1
2 1 Department of Physics, Pontifcia Universidade Catlica do Rio de Janeiro, Rio de Janeiro, Brazil Department of Mechanical Engineering, Pontifcia Universidade Catlica do Rio de Janeiro, Rio de Janeiro, Brazil 3 Department of Chemistry, University of Victoria, Victoria, Canada 4 Department of Applied Physics, Royal Institute of Technology, Stockholm, Sweden isabel.carvalho@ puc-rio.br

Abstract: A refractive index fiber optic sensor based on Localized Surface Plasmon Resonance (LSPR) and specular reflection from chemically deposited gold nanoparticles has been characterized, presenting a sensitivity of 38 nm/RIU. @2010 Optical Society of America OCIS codes: (060.2370) Fiber optic sensors; (250.5403) Plasmonics

1. Introduction Light incident on metal nanoparticles surrounded by dielectric material experiences Localized Surface Plasmon Resonance (LSPR). The wavelengths in the plasmon band of the nanoparticle-dielectric system will be partially extinct (absorbed + scattered). This phenomenon can be used in sensing of liquids and gases or in biosensing applications, since changes in the refractive index of the surrounding medium cause the plasmon band to shift [1-4]. Previously, we demonstrated a novel reflection LSPR-based optical fiber sensor with Au nanoparticles obtained by depositing and annealing a thin film on one endface of the optical fiber [5-6]. These devices are somewhat straightforward to fabricate, but with a drawback that it is not possible to control the size, shape nor distribution of the deposited gold nanoparticles. Seeking for improving the control of the fabricated nanoparticles, we have tested our reflection LSPR-based optical fiber sensor with Au nanoparticles prepared by other methods. In this paper, we report results obtained with nanoparticles deposited on the endface of the fiber by immersing a previously functionalized optical fiber tip in gold nanoparticle solutions. 2. Experimental details Prior to the deposition of nanoparticles, it is necessary to perform a rigorous cleanning of the tip of the fiber and a subsequent immersion in an ethanolic solution containing 10% (V:V) 3-mercaptotrimethoxysilane (MPTMS) to allow functionalization with thiol groups. The thiol-modified fiber is then immersed for several hours in a solution of sherically-shaped 13 nm-gold nanoparticles to achieve a layer of self-assembled gold nanoparticles on the endface of the fiber (Figure 1) [7]. The process can be repeated to allow multiple nanoparticle depositions; in this paper, the sensing results shown are for fibers with 4 layers of nanoparticles. A Scanning Electron Microscope (SEM) image of a fiber endface is shown in Figure 2. As can be seen, in Figure 2a, the nanoparticles cover uniformly the whole surface of the fiber endface. The nanoparticle distribution, however, presents clusters of ~15 nm particles that are linked by the sylane during the deposition procedure (Figure 2b).

Fig. 1. Schematic diagram of Au nanoparticles deposited on the endface of an optical fiber where MPTMS is the 3-mercaptotrimethoxysilane.

(a)

(b)

Fig. 2. (a) SEM image of Au nanoparticles on fiber endface and a (b) zoomed view of figure (a).

After the nanoparticles were deposited on the fiber, the device was ready to be used as a reflection LSPR-based optical fiber sensor. The sensor (Figure 3) consists of a white light source (OceanOpticsLS-1), a 2 x 2 optical fiber coupler (OptoLink Ltda) and a spectrum analyzer (OceanOpticsUSB 4000). As can be seen in the Figure 3, the fiber with the nanoparticles is spliced to Fiber 3, one of the output fibers of the coupler. Light from the OceanOpticsLS-1, coupled into Fiber 1, propagates through the coupler and into Fiber 2 and Fiber 3. Fiber 2 is immersed in an index matching solution to avoid light from reflecting back from that endface. Light reflected from the endface of Fiber 3, where the nanoparticles were located, containned the LSPR signal and was measured at the output of coupler (Fiber 4), using the OceanOpticsUSB 4000.

Fig. 3. Reflection LSPR-based optical fiber sensor: a white light source (OceanOpticsLS-1), a 2 x 2 optical fiber coupler (OptoLink Ltda) and a spectrum analyzer (OceanOpticsUSB 4000).

3. Results and discussion To evaluate the performance of the sensor with Au nanoparticles prepared by the method described above, the LSPR response to refractive index changes was measured. For this purpose, the tip of the fiber was immersed in several liquids with various refractive indices.
1.4 1.3 1.2 1.1 1.0 n increases 0.9 420 440 460 480 500 520

Normalized reflected signal (a.u.)

Air (n=1.00) Water (n=1.33)

Wavelength (nm)

Fig. 4. Normalized reflected signal in air (n=1.00) and in water (n=1.33).

Figure 4 shows the normalized reflected signal obtained when the fiber tip was in air (n=1.00) and in water (n=1.33). Note that, in a reflection geometry, the LSPR band is measured as a minimum, as opposed to the more usual maximum obtained in a transmission geometry. As expected, the LSPR band exibits a red-shift when the refractive index of the surrounding medium increases. Furthermore, the device response for aqueous glucose solutions with various refractive indices (n=1.351, n=1.373, n=1.391 and n=1.403) was obtained. The center of the LSPR signal was measured at 3db (50% height) for all mediums tested, presenting a linear wavelength shift as a function of refractive index with sensitivity of approximately 38 nm/RIU (Figure 5). This sensitivity can be improved by increasing the number of layers of nanoparticles.
480

Center plasmon band (nm)

475

470

Center plasmon band y = 38x + 429


1.0 1.1 1.2 1.3 1.4

465

Refractive index
Fig. 5. Center of plasmon band at 3 db (50% height) as a function of refractive index for n=1, n=1.33, n=1.351, n=1.373, n=1.391 and n=1.403.

4. Conclusion A technique for chemically depositing Au nanoparticles on the endface of an optical fiber was used in LSPR-based refractive index sensor. As expected, the response of the device is such that the LSPR peak shifts linearly to longer wavelengths as the refractive index increases, showing a sensitivity of 38 nm/RIU. The refractive index sensor sensitivity is comparable with the previous device based on the fabrication of the nanoparticles by Au film deposition and subsequent annealing [6]. However, in the present case, it is possible to control the size, shape or the distribution of the deposited gold nanoparticles on the glassy substrate and, potentially, change the NPs structure to obtain LSPR in other wavelengths and/or with higher sensitivity. 5. Acknowledgements The authors wish to thank CNPq for financial support under MCT/CNPq NanoFoton (Rede de Nanofotnica), and NSERC (Canada) under the CIAM program. Alexandre R. Camara thanks Capes for financial support. 6. References
1. 2. 3. 4. 5. Amanda J. Haes and Richard Van Duyne, A unified view of propagating and localized surface plasmon resonance biosensors, Analytical and Bioanalytical Chemistry, 379, 920-930 (2004). F. Meriaudeau, A. Wig, A. Passian, T. Downey, M. Buncick and T. L. Ferrell, Gold island fiber optic sensor for refractive index sensing, Sensors and Actuators B: Chemical, 69, 51-57 (2000). F. Meriaudeau, A. Wig, A. Passian, J. P. Lauret and T. L. Ferrell, Multiple gold island layers on a fiber core: a promising sensing device, Opt. Eng., 40, 658-660 (2001). Lai-Kwan Chau, Yi-Fang Lin, Shu-Fang Cheng and Tsao-Jen Lin, Fiber-optic chemical and biochemical probes based on localized surface plasmon resonance, Sensors and Actuators B: Chemical, 113, 100-105 (2006). Paula M. P. Gouva, Michael Fokine, Isabel C. S. Carvalho, Marco Cremona and Arthur M. B. Braga, Reflection-based Au surface plasmon resonance fiber optic sensor in 11th International Conference on Advanced Materials ICAM 2009 (International Union of Materials Research Societies). Paula M. P. Gouva, Isabel C. S. Carvalho, Hoon Jang, Marco Cremona, Arthur M. B. Braga and Michael Fokine, Characterization of a fiber optic sensor based on LSPR and specular reflection in Optical Sensors (Sensors), Optical Society of America (OSA), 2010. Christopher J. Addison, Alexandre G. Brolo, Nanoparticle-Containing Structures as a Substrate of Surface-Enhanced Surface Scattering, Langmuir 2006, 22, 8696-8702.

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