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Preparation and Z-Scan nonlinear optical characterization of Au/SiO2- and Ag/SiO2-supported nanoparticles dispersed in silica sonogel films

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Abstract

Au/SiO2 and Ag/SiO2 supported metal-nanoparticles (MNPs) were implemented to fabricate SiO2-based inorganic–inorganic hybrid sonogel films. Prepared Au/SiO2- and Ag/SiO2-MNPs exhibited low 2D-HCP crystallinity with particle diameters below 10 nm and homogeneous size distribution. The catalyst-free (CF) sonogel route was successfully implemented to produce these optically active nanocomposite films by doping the liquid sol-phase with these MNP systems and its subsequent deposition onto glass substrates via standard spin-coating procedures. The easy MNP-loading within the mesoporous dielectric sonogel network evidenced a huge chemical affinity between the silica sonogel hosting system and the guest SiO2-supported MNPs. This fact allowed us to fabricate high quality hybrid films suitable for cubic nonlinear optical (NLO) characterizations via the Z-Scan technique. Indeed, the hosting sonogel network provided adequate thermal and mechanical stability protecting the active MNPs from environment conditions and diminished their tendency to aggregate; thus, preserving their pristine optical properties and morphology, giving rise to stable sol–gel hybrid films appropriate for photonic applications. Comprehensive morphological, structural, spectroscopic and nonlinear photophysical characterizations were optimally performed to the developed hybrid films. Our results have shown that the crystalline nature of the implemented MNPs, their small sizes and appropriate guest–host stabilizing interactions play a crucial role in the observation of improved cubic NLO-properties of these MNP structures embedded within the highly pure CF-sonogel confinement.

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Notes

  1. The TOES/H2O-mixture immediately obtained after sonication is a homogeneous opaque suspension containing both the sonochemically reacted and unreacted molecular species from the constituting reactants. Note that despite the fact that the cooling system is always on during sonication, the intermittent US-irradiation sequences of 5 s allow the system to cool down in order to avoid excessive reaction temperatures promoted by intense US-irradiation. These intermittent irradiation sequences also provide adequate silence periods for recombination of the formed molecular species, given rise to an increase of hydrolyzed Si-based molecular compounds, which form after condensation/polymerization a highly pure SiO2-glassy network [56–58].

  2. The slow drying process of the samples performed at room temperature into dissectors has proven to be efficient in order to produce fracture-free quality film structures with adequate morphology suitable for optical characterizations, as verified via AFM-microscopy. On the other hand, it has also been proven that negligible water residuals remain within the porous sonogel glassy film structure [57, 60].

  3. As reported in the literature [60], the thermal evolution of the sonogels XR-diffractograms show that the SiO2-sonogel network undergoes crystalline phase transformations at higher temperatures: between 800 and 1,200 °C broad bands corresponding to a mixture of trydimite and cristobalite; beyond 1,200 °C the highly crystalline β-cristobalite phase takes place (optimally observed for samples treated at ~1,400 °C).

  4. The bulk hybrid structures result from the remaining (not deposited) OH-TEOS:MNPs/SiO2 doped sol-mixtures (after drying).

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Acknowledgments

We are grateful to J. Guadalupe Bañuelos (CCADET-UNAM) for valuable support on AFM-imaging. Likewise, we wish to thank to Adriana Tejeda Cruz (IIM-UNAM) and Hugo Sanchez-Flores (CCADET-UNAM) for their valuable support on recording XRD- and FTIR-spectra, respectively. R. Z., V. M. R. and J. O. F. F. acknowledge PAPIIT-IN108310 and CONACYT-130407 projects and the Nanoscience and Nanotechnology CONACYT network for financial support. O. G. M. S. acknowledges financial support from the DAAD academic organization (Germany).

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Authors and Affiliations

  1. Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, CCADET-UNAM, Circuito Exterior S/N, Ciudad Universitaria, A.P. 70-186, Delegación Coyoacán, C.P. 04510, Mexico, DF, Mexico

    Omar G. Morales-Saavedra, Rodolfo Zanella, Viridiana Maturano-Rojas, Vicente Torres-Zúñiga, José O. Flores-Flores, Antonio A. Rodríguez-Rosales & Roberto Ortega-Martínez

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  1. Omar G. Morales-Saavedra
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  2. Rodolfo Zanella
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  3. Viridiana Maturano-Rojas
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Correspondence to Omar G. Morales-Saavedra.

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Morales-Saavedra, O.G., Zanella, R., Maturano-Rojas, V. et al. Preparation and Z-Scan nonlinear optical characterization of Au/SiO2- and Ag/SiO2-supported nanoparticles dispersed in silica sonogel films. J Sol-Gel Sci Technol 63, 340–355 (2012). https://doi.org/10.1007/s10971-012-2793-8

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