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Sensors and Actuators B: Chemical

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A Lossy Mode Resonance optical sensor using silver nanoparticles-loaded lms for monitoring human breathing
Pedro J. Rivero , A. Urrutia, J. Goicoechea, I.R. Matias, F.J. Arregui
Electric and Electronic Engineering Department, Public University of Navarra, Campus Arrosada, 31006 Pamplona, Spain

a r t i c l e
Article history: Available online xxx

i n f o

a b s t r a c t
This work is focused on the fabrication of a human breathing sensor based on the in situ synthesis of silver nanoparticles (Ag-NPs) inside a polymeric coating previously deposited on an optical ber core by means of the Layer-by-Layer self-assembly. The Ag-NPs were created using a synthesis protocol consisting of a loading step of the Ag+ cations into the polymeric lm and a further reduction step using dimethylamine borane (DMAB). The morphology and distribution of the Ag-NPs inside the polymeric coating have been studied using atomic force microscopy (AFM). Furthermore, UVVIS spectroscopy and energy dispersive X-ray (EDX) were also used to conrm the synthesis of the Ag-NPs within the resultant coating. The amount of Ag-NPs increases when the number of loading/reduction cycles is higher. Therefore the incorporation of the Ag-NPs affects the refractive index of the overlay promoting the observation of a resonant attenuation band in the infrared region (NIR), known as Lossy Mode Resonance (LMR), which can be used as a sensing signal to monitor the human breathing. The quality of the device has been experimentally tested with good sensitivity (0.455 nm per RH%) and fast response time (692 ms and 839 ms for rise/fall). 2012 Elsevier B.V. All rights reserved.

Keywords: Silver nanoparticles (Ag-NPs) Lossy Mode Resonances (LMR) Humidity sensing

1. Introduction During the last two decades a growing attention has been paid to the Layer-by-Layer assembly (LbL) due to the potential applications in electronics and sensing devices. Some of the key points of this method are its simplicity, versatility and easiness for scaling-up with a precise control of the thickness [1,2]. Due to this, the LbL technique has been applied to a wide range of polymers and nanomaterials (polyelectrolytes, nanoparticles or nanocomposites) [35] for diverse applications (anti-reection, anti-fog, anti-corrosion, hydrophilic or hydrophobic coatings) [69]. These coatings can be used to fabricate optical ber sensors (small size, simple geometry or biocompatibility) which have been considered as a good choice for obtaining sensors based on LbL sensitive lms [10]. Moreover, the use of optical ber sensors has been increasing for humidity control due to provide several advantages such as sensitivity, fast response, dynamic range or remote sensing capability [11,12]. Very recently, a novel optical ber humidity sensor based on both lossy-mode resonance (LMR) and Localized Surface Plasmon Resonance (LSPR) has been explored [13] using LbL polymeric coating loaded with silver nanoparticles (Ag-NPs). The utilization of

Corresponding author. Tel.: +34 948 16 60 44; fax: +34 948 16 97 20. E-mail address: pedrojose.rivero@unavarra.es (P.J. Rivero). 0925-4005/$ see front matter 2012 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.snb.2012.09.022

metal nanoparticles (Ag-NPs) for optical sensors is well-known due to the phenomenon of LSPR as a sensing signal [1419] and the location of this resonant peak in the visible region depends on multiple factors such as nanoparticle size, shape or particles interaction. However, a new type of resonances (LMR) can be supported by thin-lm coated optical waveguides. These optical resonances occur when the real part of the thin lm permittivity is positive and higher in magnitude than both its own imaginary part and the real part of the material surrounding the thin lm [20,21]. LMRbased devices have been explored for the fabrication of optical ber refractometers [2224], humidity sensors [25,26] or pH sensors [27]. The devices based on LMR attenuation bands can be generated using diverse materials such as polymers or ceramics. Furthermore, LMR-based devices make possible the generation of multiple absorption bands without modifying the optical ber geometry and it is possible to obtain sensing signals as a function of the thickness and refractive index of optical ber overlay. In addition to this, very recently a new route of synthesis of in situ Ag-NPs has been developed for antibacterial applications [28]. It is important to remark that the use of Ag-NPs has an additional advantage when the sensors are placed in high humidity environments due to their antibacterial behavior preventing the bacteria growth [29,30]. In this work, a polymeric supporting layer was modied by in situ Ag-NPs synthesis. This synthetic route is based on a rst Ag+ loading step followed by a further reduction step. AgNPs make possible an increasing of the refractive index and permit

Please cite this article in press as: P.J. Rivero, et al., A Lossy Mode Resonance optical sensor using silver nanoparticles-loaded lms for monitoring human breathing, Sens. Actuators B: Chem. (2012), http://dx.doi.org/10.1016/j.snb.2012.09.022

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the presence of a new optical resonant band (LMR) in the infrared region (9001600 nm) which it is used as a sensing signal. To our knowledge, this is the rst time that this new route of synthesis of in situ Ag-NPs has been described in literature to achieve optical ber Relative Humidity (RH) sensors. 2. Experimental process 2.1. Materials Poly(allylamine hydrochloride) (PAH) (Mw 56,000), poly(acrylic acid, sodium salt) 35 wt% solution in water (PAA) (Mw 15,000), silver nitrate (>99% titration) solution in water 0.1 N and borane dimethylamine complex (DMAB) were purchased from SigmaAldrich and used without any further purication. Aqueous solutions of 10 mM of PAH and PAA were prepared using ultrapure deionized water (18.2 M ) and adjusted to pH 7.0 by the addition of a few drops of NaOH or HCl with no additional salt concentration. Plastic-clad silica bers of 200/225 m core/cladding diameter (FT200EMT) were provided by Thorlabs Inc. 2.2. Device fabrication 2.2.1. Fabrication of the polymeric matrix A 4 cm long part of the optical ber cladding was chemically removed in order to expose part of the optical ber core prior to the coating fabrication. A polymeric matrix has been synthesized using the Layer-byLayer technique (LbL) by sequentially exposing the optical ber core to the cationic polyelectrolyte poly(allylamine hydrochloride) (PAH) and to the anionic polyelectrolyte poly(acrylic acid, sodium salt) (PAA) with an immersion time of 2 min in each solution. A rinsing step in deionized water was performed between the two polyelectrolytes baths in order to remove the excess of material adsorbed. After this sequence, it has been fabricated the [PAH/PAA] basic structure, known as bilayer. This process was carried out using a 3-axis robot (Nadetech Innovations) and was repeated until reaching a [PAH/PAA] structure of 40 bilayers. 2.2.2. In situ synthesis of silver nanoparticles into the polymeric coating Once the polymeric overlay was deposited on the optical ber a novel method for the in situ synthesis of Ag-NP was applied in order to incorporate these Ag-NPs in the polymeric matrix [28]. Basically, the Ag-NPs have been synthesized in the LbL coating by a two step synthesis process. Firstly, an Ag+ cation loading step using silver nitrate as a loading agent which formed electrostatic pairs with some of the carboxylate groups from PAA. Secondly, a further reduction of the silver loaded into the coating by immersing into a dimethylamine borane (DMAB) solution which acted as reducing agent. The carboxylate-bonded Ag+ cations have been reduced to produce zero-valent silver nanoparticles (Ag0 ). This loading/reduction cycle has been repeated up to 6 times. These Ag-NPs loaded LbL overlays onto the optical ber core will be the sensitive region, as it is schematically shown in Fig. 1. 2.3. Device characterization UV/Vis absorbance spectroscopy was used to monitor both the polymeric coating process and the in situ Ag-NPs fabrication process. The experimental set-up consisted of a white halogen lamp (ANDO Inc.) used as the excitation source which was connected to one end of the optical ber and a CCD-based NIR spectrometer (NIR512 from Oceanoptics Inc.) which was connected to the other end of the ber in order to obtain spectral information in the range between 900 and 1600 nm. Light passes through the sensitive

Fig. 1. Schematic representation of the device based on Ag-NPs loaded LbL overlays.

region which is located between the light source and the detector, and it is modied with the new boundary conditions created by the polymeric coating and the incorporation of the Ag-NPs. After fabrication of the sensor, the same setup was used to characterize the device when it is subjected to Relative Humidity (RH) changes. An environmental chamber (Angelantoni Inc.) was used to control both RH and temperature surrounding the sensor. 2.4. Characterization of the synthesized Ag-NPs Energy dispersive X-ray (EDX) and diffraction X-ray (XRD) were used to conrm the presence of the crystalline silver nanoparticles within the polymeric coating. The measurements were obtained from an INCA-X-ray microanalysis system from Oxford Instruments. Atomic force microscopy (AFM) was also used to characterize the distribution and the surface morphology of the resultant coating. The samples were scanned using a Veeco Innova AFM, in tapping mode. 3. Results and discussion As it has been reported in previous works [2027], different type of selective optical power absorption at certain wavelengths, can be supported by thin-lm coated optical ber core and the nature of these resonances depends on the optical properties of the outer thin-lm surrounding the optical waveguide. SPR occurs when the real part of the thin-lm permittivity is negative and higher in magnitude than both its own imaginary part and the permittivity of the material surrounding the thin-lm. LMR occurs when the real part of the thin-lm permittivity is positive and higher in magnitude than both its own imaginary part and the material surrounding the thin-lm. In fact, devices based on ITO, TiO2 or InO2 coatings have been already experimentally demonstrated [2224]. Here, the main goal of this work is to prove experimentally the generation of LMR by means of the in situ synthesis of Ag NPs into a polymeric overlay and its utilization for humidity sensing purposes. In the next paragraphs, different techniques of analysis have been used to corroborate the presence of AgNPs in the lm and also that this coating can produce LMR absorption bands in the infrared region with a high wavelength dependence to relative humidity changes. More details about the theoretical basis of LMR-based sensors can be found in the literature [3133]. It is well-known that the PAH/PAA structure fabricated onto the core of the optical ber presents a thickness dependence with the RH of the surrounding medium, known as swelling/deswelling, which it has been exploited before in the fabrication of humidity or pH sensors [26,27]. The use of Ag-NPs which were further in situ synthesized form silver nitrate (loading agent), and dimethyl borane complex (reducing agent) inside the previously polymeric PAH/PAA coating obtained by LbL assembly plays a key role in the modication of the refractive index. These Ag-NPs which were synthesized increase both the real and imaginary components, making possible to observe stronger LMR bands in the infrared region.

Please cite this article in press as: P.J. Rivero, et al., A Lossy Mode Resonance optical sensor using silver nanoparticles-loaded lms for monitoring human breathing, Sens. Actuators B: Chem. (2012), http://dx.doi.org/10.1016/j.snb.2012.09.022

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Fig. 2. AFM gure (20 m 20 m) in tapping mode of height (left) and phase (right) respectively.

A random distribution of the synthesized Ag-NPs inside the polymeric coating is conrmed by AFM analysis (see Fig. 2). The light spots observed in the topographic image (Fig. 2, top) correspond to the Ag-NPs. This is supported by the phase image (Fig. 2, bottom) that also conrms the presence of materials with different stiffness, such as the polymeric matrix and the metallic nanoparticles. In Fig. 3a, it is possible to appreciate an absorption band near 450 nm due to the LSPR phenomenon, typical of metallic silver nanoparticles. The visual aspect of the thin lm synthesized onto the optical ber core after the loading/reduction cycles showed a dramatic color change to golden-yellowish. This colored appearance is the result of the presence of a LSPR absorption band in the 410450 nm region, due to the presence of the silver nanoparticles within the polymeric overlay. The position and intensity of the LSPR absorption band depends on multiple factors such as shape, size or distribution of them in the polymeric lm. The size and amount of the Ag-NPs is increased when the number of load/reduction dips is increased. In Fig. 3b, it is shown the relation between the number of loading/reduction cycles and the increasing of the intensity of the LSPR absorption band, proportional to the amount of Ag-NPs trapped into the thin lm. An exponential-like growth of the intensity of the LSPR absorption band was observed with the increasing of the consecutive loading/reduction cycles. Additional techniques not shown here (EDX or XRD) were also used to conrm the presence of such Ag NPs in the nal coating. These Ag-NPs loaded LbL overlays on optical ber present several absorption bands in the spectral range from 400 to 1600 nm when their transmission spectra were monitored. The rst one appears at 450 nm (visible region) after the loading/reduction cycles which it is due to the SPR of the synthesized Ag-NPs. Furthermore, a new optical resonant band (LMR) is observed in the infrared region (NIR). The amount and size of the metal

Fig. 3. (a) UVVIS absorption spectra of the coating with different number of loading/reduction cycles (top) and (b) maximum absorbance of the SPR of the synthesized Ag-NPs as a function of the number of loading/reduction cycles (bottom).

nanoparticles in the LbL coating modies the refractive index of the lm and consequently the wavelength of the LMR band maximum is shifted to longer wavelengths as more loading/reduction cycles were performed (Figs. 4 and 5). In previous work, it has been experimentally demonstrated the high wavelength shift of the LMR attenuation bands, compared to the low sensitivity of the SPR absorption band [13]. Due to this, it has been studied the

Fig. 4. Spectral response at NIR as a function of the number of the loading/reduction cycles on the optical ber core.

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Fig. 5. Evolution of the UVVIS absorption spectra with 4, 5 and 6 loading/reduction dips (L/R) at the LMR wavelength.

wavelength dependence of the LMR band in the infrared region with relative humidity changes (Fig. 6). It is important to remark that the in situ loading/reduction synthesis route makes possible the monitoring of the optical response of the optical ber during the whole synthesis process. This allows us to stop the Ag-NPs growth when the LMR band is located at the desired wavelength in the infrared region, 1150 nm in this case. Once the sensor was fabricated in order to position the working point of the sensor in the sensitivity region (NIR), the device was tested to cyclic variations from 20 to 80% Relative Humidity (RH) changes with a time of 3 h for rise/fall step respectively. In Fig. 6 the dynamical response of LMR to different RH values at constant temperature (25 C) for several cycles is shown. The dynamic range of the sensor in the studied range is 27.3 nm which corresponds to a sensitivity of 0.455 nm per RH%. In addition, the resonance wavelength shift follows perfectly the RH measurements from the electronic sensor located in the climatic chamber. Furthermore, the sensor has been tested several times to the same RH cycles without any signicant changes in the optical response. These tests have been performed in different periods of time with the same cyclic variations from 20 to 80% Relative Humidity (RH) and the results show a slight change of less than 3% in intensity and less than 1% in wavelength shift. Finally, the performance of the device has been tested experimentally for human breathing changes at the LMR wavelength to evaluate the response time. The results of this experiment to these quick changes of RH measurements are shown in Fig. 7a. The observed response time of the sensor was 692 and 839 ms for the

Fig. 7. Response of the sensor to several consecutive human breathing cycles (top) and (b) response time of the sensor for the rise and fall, respectively (bottom).

rise and fall, respectively (Fig. 7b). As the result, the combination of nanotechnology and biomedical science makes enable their use in practical RH monitoring applications or even, can lead to monitor high humidity changes such as human breathing (biomedical devices), due to the fast response in the maximum sensitivity region at 1150 nm (NIR). 4. Conclusions A lossy-mode resonance optical sensor based on wavelengthdisplacement in the infrared region (NIR) has been fabricated. Firstly, a polymeric matrix has been obtained using the Layerby-Layer technique (LbL) and then Ag-NPs have been synthesized in situ in the LbL coating by consecutive loading/reduction cycles. The synthesis of these Ag-NPs has been corroborated using several techniques such as UVVIS, EDX or XRD. Furthermore, AFM analysis was used to show a random distribution of synthesized Ag-NPs in the resultant polymeric coating. These Ag-NPs allow us to fabricate LbL lms with modied refractive index. In addition, Ag-NPs play a key role due to the generation of a new LMR band at 1150 nm in the NIR with a high wavelength shift as a function of the number of loading/reduction cycles. In addition, the device has been tested to RH changes with a sensitivity of 0.455 nm per RH% and a dynamic range of 27.3 nm. Finally, this LMR band could be used as a sensing signal with a very fast response time (692 ms and 839 ms for rise/fall respectively) and a good repeatability to several exhalation/inhalation cycles. To our knowledge, this is he rst time that this new route of synthesis of in situ Ag-NPs has been reported to monitor quick changes of humidity such as human breathing in the literature. The development of this LMR-sensing conguration could be designed for the measurement of physical, chemical or biological parameters.

Fig. 6. Dynamic response of the device (LMR maximum sensitivity) to RH changes from 20 to 80% at 25 C.

Please cite this article in press as: P.J. Rivero, et al., A Lossy Mode Resonance optical sensor using silver nanoparticles-loaded lms for monitoring human breathing, Sens. Actuators B: Chem. (2012), http://dx.doi.org/10.1016/j.snb.2012.09.022

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Acknowledgments This work was funded in part by the Spanish Ministry of Education and Science-FEDER Research Grant TEC2010-17805 and Public University of Navarra (UPNA) Research Grants. The authors express their gratitude to Carlos Ruiz for his help with the EDX analysis. References
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Biographies
Pedro J. Rivero obtained his MS degree in Chemistry and Biochemistry in 2006 and 2007 respectively from the Catholic University of Navarra, Pamplona, Spain. He graduated in Materials Engineering Postgraduate Master from the Public University of Navarra (UPNA) and Science and Polymer Technology Postgraduate Master from the National Distance Education University (UNED) in 2010 and 2011, respectively. Nowadays, he is working toward his PhD degree in the Electrical and Electronic Engineering Department at the Public University of Navarra. His main areas of interest are the research and development of nanostructured functional thin lms, optical ber devices and their engineering applications. Aitor Urrutia received the MS degree in telecommunications engineering and the MS degree in communications from the Public University of Navarra (UPNA), in 2009 and 2011, respectively. Currently, he is working toward the PhD degree in the Communications Doctoral Program, Department of Electrical and Electronic Engineering, UPNA. His research interests include optical ber sensors and nanostructured materials. Javier Goicoechea received his MS degree in electrical engineering and the PhD degree in 2003 and 2008 respectively from the Public University of Navarra (UPNA), Pamplona, Spain. In 2004 he obtained a predoctoral scholarship from the Spanish Ministry of Culture and Science. In 2010 he became reader at the Public University of Navarra. His research interest includes organic light emitting diodes, organic photovoltaic cells and ber optic sensors. He has authored more than 21 scientic international publications and 4 book chapters (international edition). Ignacio R. Matas received the MS degree in electrical and electronic engineering and the PhD degree in optical ber sensors from the Polytechnic University of Madrid, Madrid, Spain, in 1992 and 1996, respectively. He became a Lecturer at the Public University of Navarra in 1996, where presently he is a Permanent Professor. He has co-authored more than 200 chapter books, journal and conference papers related to optical ber sensors and passive optical devices and systems. He is an Associate Editor of IEEE Sensors Journal. Francisco J. Arregui is a Full Professor at the Public University of Navarre, Pamplona, Spain. He was part of the team that fabricated the rst optical ber sensor by means of the Layer-by-Layer self-assembly method at Virginia Tech, Blacksburg, VA, USA, in 1998. He is the author of around 300 scientic journal and conference publications, most of them related to optical ber sensors based on nanostructured coatings. Prof. Arregui has been an Associate Editor of the Journals IEEE Sensors Journal, International Journal on Smart Sensing and Intelligent Systems and Journal of Sensors. He is also the Editor of the books Sensors Based on Nanostructured Materials and Optochemical nanosensors. Journal of Sensors was founded in 2007 by Prof. Arregui who served as the Editor-in-Chief of the journal between 2007 and 2011.

Please cite this article in press as: P.J. Rivero, et al., A Lossy Mode Resonance optical sensor using silver nanoparticles-loaded lms for monitoring human breathing, Sens. Actuators B: Chem. (2012), http://dx.doi.org/10.1016/j.snb.2012.09.022