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Optics Express

Optics Express

  • Editor: C. Martijn de Sterke
  • Vol. 19, Iss. 20 — Sep. 26, 2011
  • pp: 19061–19066
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Linear and nonlinear optical properties of gold nanoparticle-doped photonic crystal fiber

L. Bigot, H. El Hamzaoui, A. Le Rouge, G. Bouwmans, F. Chassagneux, B. Capoen, and M. Bouazaoui  »View Author Affiliations


Optics Express, Vol. 19, Issue 20, pp. 19061-19066 (2011)
http://dx.doi.org/10.1364/OE.19.019061


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Abstract

We report on the production of air/silica photonic crystal fiber doped with gold nanoparticles. The stack-and-draw technique was used to combine a gold nanoparticles-doped silica core rod synthesized by the sol-gel route with capillaries drawn from commercially available silica tubes. The presence of nanoparticles in the core region was confirmed at the different steps of the process down to the fiber geometry, even after multiple drawings at ∼2000°C. Optical properties of the fiber were investigated and put in evidence the impact of gold nanoparticles on both linear and nonlinear transmission.

© 2011 OSA

1. Introduction

The concept of photonic crystal fiber (PCF) has opened the route to a novel family of optical fibers available for a wide range of applications [1

1. P. S. J. Russell, “Photonic-crystal fibers,” J. Lightwave Technol. 24, 4729–4749 (2006). [CrossRef]

]. Among these fields, nonlinear optics took a large part of the benefits, making it possible to realize, for example, broad and powerful supercontinuum sources. The efficiency of these systems is based both on the easy chromatic dispersion management offered by PCFs and on the increased nonlinearity thanks to the small mode areas that are accessible with these fibers. The intrinsic nonlinear coefficients of the material generally plays a second role, as illustrated by the numerous realizations based on pure silica glass. However, various kinds of glasses are known to offer nonlinear coefficients larger than those of pure silica and could be useful to further improve the performances of systems based on highly nonlinear fibers. Roughly speaking, these glasses can be divided in two families: (1) nonlinear matrices, like chalcogenide glasses, multicomponent oxide glasses or tellurite glasses [2

2. G. Agrawal, Nonlinear Fiber Optics4th ed. (Academic Press, 2007).

] and, (2) conventional glasses containing dopants that present nonlinear properties, like nanometric inclusions (metal, semiconductor) [3

3. K. C. Rustagi and C. Flytzanis, “Optical nonlinearities in semiconductor-doped glasses,” Opt. Lett. 9, 344–346 (1984). [CrossRef] [PubMed]

, 4

4. D. Ricard, Ph. Roussignol, and Chr. Flytzanis, “Surface-mediated enhancement of optical phase conjugation in metal colloids,” Opt. Lett. 10, 511–513 (1985). [CrossRef] [PubMed]

]. Both kinds of materials have nonlinear coefficients significantly larger than those of pure silica and some of them have already been used to realize PCFs, like chalcogenide [5

5. J. Troles, Q Coulombier, G. Canat, M. Duhant, W. Renard, P. Toupin, L. Calvez, G. Renversez, F. Smektala, M. El Amraoui, J. L. Adam, T. Chartier, D. Mechin, and L. Brilland, “Low loss microstructured chalcogenide fibers for large non linear effects at 1995 nm,” Opt. Express 18, 26647–26654 (2010). [CrossRef] [PubMed]

] and tellurite [6

6. G. Qin, M. Liao, C. Chaudhari, X. Yan, C. Kito, T. Suzuki, and Y. Ohishi, “Second and third harmonics and flattened supercontinuum generation in tellurite microstructured fibers,” Opt. Lett. 35, 58–60 (2010). [CrossRef] [PubMed]

] for which the authors tried to exploit the high nonlinear-index coefficient. Besides this, realization of glasses doped by metal nanoparticles is mainly limited to films and bulk materials and there are only two reports of insertion of such systems in the core of a conventionnal optical fiber [7

7. A. Dhawan and J. F. Muth, “Plasmon resonances of gold nanoparticles incorporated inside an optical fibre matrix,” Nanotechnology 17, 2504–2511 (2006). [CrossRef] [PubMed]

, 8

8. S. Ju, V. L. Nguyen, P. R. Watekar, B. H. Kim, C. Jeong, S. Boo, C. J. Kim, and W. T. Han, “Fabrication and optical characteristics of a novel optical fiber doped with the Au nanoparticles,” J. Nanosci. Nanotechnol. 6, 3555–3558 (2006). [CrossRef]

]. However, it has been reported that these systems can also present high nonlinear-index coefficient and, in addition to this, high nonlinear-absorption coefficient that make them available for applications requiring saturable absorption or optical limiting [9

9. J. Matsuoka, R. Mizutani, S. Kaneko, H. Nasu, K. Kamiya, K. Kadono, T. Sakaguchi, and M. Miya, “Sol-Gel processing and optical nonlinearity of gold colloid-doped silica glass,” J. Ceram. Soc. Jpn. 101, 53–58 (1993). [CrossRef]

]. In the case of gold nanoparticles (Au-NPs), the difficulty there exists in maintaining them in the core of an optical fiber originates from the high temperatures associated to fiber drawing. Such temperatures (typically ∼2000°C for silica glasses) are much higher than the gold melting temperature (1064°C) and even higher than Au-NP melting temperature [10

10. Ph. Buffat and J. P. Borel, “Size effect on the melting temperature of gold particles,” Phys. Rev. A 13, 2287–2298 (1976). [CrossRef]

]. The first report of an optical fiber containing Au-NPs was based on the evaporation of gold on a fiber end and the splicing to a second fiber [7

7. A. Dhawan and J. F. Muth, “Plasmon resonances of gold nanoparticles incorporated inside an optical fibre matrix,” Nanotechnology 17, 2504–2511 (2006). [CrossRef] [PubMed]

]. The second work was based on conventional fiber fabrication technique (namely modified chemical vapor deposition) coupled to a solution doping technique using a gold precursor, similarly to what is done to realize rare-earth doped fibers [8

8. S. Ju, V. L. Nguyen, P. R. Watekar, B. H. Kim, C. Jeong, S. Boo, C. J. Kim, and W. T. Han, “Fabrication and optical characteristics of a novel optical fiber doped with the Au nanoparticles,” J. Nanosci. Nanotechnol. 6, 3555–3558 (2006). [CrossRef]

]. Looking in details, it appears that the first approach can only lead to short doped pieces of fibers, whereas the results obtained with the second technique led to surprising properties: the reported surface plasmon resonance (SPR) wavelength is blue-shifted as compared to what is commonly reported for Au-NPs in silica.

In the present work, we propose to combine the benefit of the PCF geometry and the increased nonlinearity induced by Au-NPs to realize nonlinear silica fibers. In order to reach this goal, an alternative approach has been developed, based on the synthesis of a glass rod by a soft technique (namely the sol-gel route) and its use as core material for the realization of a PCF by the stack-and-draw technique. The crucial question of conservation of Au-NPs at the different steps of the process up to the fiber geometry is studied as well as the optical properties of the final fiber.

2. Fiber synthesis

The first step of the fabrication consists in the synthesis of a cylindrical rod by the sol-gel route. This technique was chosen because it enables to achieve transparent glasses at temperature several hundreds degrees lower than the reaction temperature required in the conventional process used in the optical fiber industry. Porous silica monoliths, shaped as cylinders, were prepared from tetraethylorthosilicate (TEOS) as already described elsewhere [11

11. H. El Hamzaoui, L. Courtheoux, V. Nguyen, E. Berrier, A. Favre, L. Bigot, M. Bouazaoui, and B. Capoen, “From porous silica xerogels to bulk optical glasses: The control of densification,” Mater. Chem. Phys. 121, 83–88 (2010). [CrossRef]

]. Those porous monoliths, exhibiting interconnected nanometric pores, were doped by soaking with hydrogen tetrachloroaurate (HAuCl4) solution. Then, the samples were taken out and dried for several hours so as to to remove solvents. The resulting doped xerogels were then densified under air atmosphere at 1200°C and pink colored and cracks-free silica glass cylinders (few tens of millimeters in diameter and few centimeters in length - see inset of Fig. 1) were obtained. The absorbance is presented on Fig. 1.

Fig. 1 Absorption spectrum of sol-gel Au-NPs -doped vitreous silica monolith. Inset: optical image of such a monolith.

It exhibits a broad resonance centered around 567 nm with a full width at half maximum (FWHM) of 117 nm, attributed to the SPR of Au-NPs. These Au-NPs were hence formed in the silica network during the drying and sintering of the sol-gel monolith. To obtain PCF, the sol-gel monolith presented in inset of Fig. 1 was jacketed with a pure silica tube and this set was then drawn down to millimeter-sized rods at around 2000°C. The resulting rods also present a pink color which suggests the presence of Au-NPs at this step. This is confirmed by high-resolution transmission electronic microscopy (HR-TEM) and absorption measurement. Indeed, Au-NP of around 5 nm in diameter is observed as shown in Fig. 2, the metallic nature of this crystallite being confirmed by the inter-planar distances, which are close to the distances between (−111), (1-11) and (002) lattice planes of cubic face centered gold.

Fig. 2 HR-TEM image realized on a rod directly drawn from a monolith.

Fig. 3 Optical attenuation of the Au-Nps -doped PCF measured by cutting back two different initial fiber lengths: 50 m (red line) and 2 m (black line). Inset: SEM image of the central part of the PCF. Au-NPs -doped region has been schematized by a yellow circle.

3. Optical properties

Fig. 4 Evolution of output intensity as a function of input intensity, at 532 nm, for two different optical fibers: undoped sol-gel -based pure silica core micro-structured fiber (open circles) and Au-Nps-doped fiber presented on Fig. 3 (open squares). In both cases, a linear fit of the first experimental data points is represented by a blue line. A fit of the experimental data points obtained for Au-NPs -doped PCF based on Eq. (2) is reported as a red line.

In order to further characterize the nonlinearity of the Au-NPs -doped PCF, the following law was used to describe the intensity dependence:
dIdz=(αI+βI2)
(1)

The solution of Eq. (1) for the transmitted intensity I(L) in a fiber of length L is given by:
I(L)=I(0)eαL1+I(0)βLeff
(2)
where I(0) stands for the injected intensity, α stands for the low-intensity absorption coefficient, β stands for the induced absorption coefficient (two-photon absorption coefficient for example) connected to the imaginary part of the third order susceptibility [15

15. R. Boyd, Nonlinear Optics2nd ed. (Academic Press, 2003).

] and Leff=1eαLα is the effective length. A fit by Eq. (2) leads to a value of the β coefficient of 0.84×10−12 cm/W for the Au-NPs -doped PCF. The relatively small apparent value obtained for β, as compared to reports on Au-NPs -doped films [14

14. N. Pinçon, B. Palpant, D. Prot, E. Charron, and S. Debrus, “Third-order nonlinear optical response of Au:SiO2 thin films : influence of gold nanoparticle concentration and morphologic parameters,” Eur. Phys. J. D 19, 395–402 (2002). [CrossRef]

], is attributed to the weak overlap between the guided mode and the doped region, together with the much smaller Au-NPs concentration when compared to what is commonly presented in the case of films. The resonant optical limiting behavior observed in the obtained fiber, can be correlated to the excited-state absorption of carriers in the Au-NPs and the generation of hot electrons.

4. Conclusion

In conclusion, we report on the production of PCFs with core realized by the sol-gel technique and doped with Au-NPs. Preservation of Au-NPs all along the fiber manufacturing process is demonstrated and SPR is clearly observed, even for the fiber geometry. The effect of this doping on the resonant nonlinear properties of the fiber is put in evidence and is characterized by an optical limiting effect. We hope that this optical limiting behavior could be extended to the non-resonant region, opening perspectives for clamping energy of lasers or amplifiers.

Acknowledgments

The authors would like to thank Karen Delplace for providing technical support. This work has been performed in the frame of the POMESCO ANR project. It has also been partly supported by the Conseil Régional Nord/Pas de Calais and the Fonds Européen de Développement Economique des Régions (FEDER).

References and links

1.

P. S. J. Russell, “Photonic-crystal fibers,” J. Lightwave Technol. 24, 4729–4749 (2006). [CrossRef]

2.

G. Agrawal, Nonlinear Fiber Optics4th ed. (Academic Press, 2007).

3.

K. C. Rustagi and C. Flytzanis, “Optical nonlinearities in semiconductor-doped glasses,” Opt. Lett. 9, 344–346 (1984). [CrossRef] [PubMed]

4.

D. Ricard, Ph. Roussignol, and Chr. Flytzanis, “Surface-mediated enhancement of optical phase conjugation in metal colloids,” Opt. Lett. 10, 511–513 (1985). [CrossRef] [PubMed]

5.

J. Troles, Q Coulombier, G. Canat, M. Duhant, W. Renard, P. Toupin, L. Calvez, G. Renversez, F. Smektala, M. El Amraoui, J. L. Adam, T. Chartier, D. Mechin, and L. Brilland, “Low loss microstructured chalcogenide fibers for large non linear effects at 1995 nm,” Opt. Express 18, 26647–26654 (2010). [CrossRef] [PubMed]

6.

G. Qin, M. Liao, C. Chaudhari, X. Yan, C. Kito, T. Suzuki, and Y. Ohishi, “Second and third harmonics and flattened supercontinuum generation in tellurite microstructured fibers,” Opt. Lett. 35, 58–60 (2010). [CrossRef] [PubMed]

7.

A. Dhawan and J. F. Muth, “Plasmon resonances of gold nanoparticles incorporated inside an optical fibre matrix,” Nanotechnology 17, 2504–2511 (2006). [CrossRef] [PubMed]

8.

S. Ju, V. L. Nguyen, P. R. Watekar, B. H. Kim, C. Jeong, S. Boo, C. J. Kim, and W. T. Han, “Fabrication and optical characteristics of a novel optical fiber doped with the Au nanoparticles,” J. Nanosci. Nanotechnol. 6, 3555–3558 (2006). [CrossRef]

9.

J. Matsuoka, R. Mizutani, S. Kaneko, H. Nasu, K. Kamiya, K. Kadono, T. Sakaguchi, and M. Miya, “Sol-Gel processing and optical nonlinearity of gold colloid-doped silica glass,” J. Ceram. Soc. Jpn. 101, 53–58 (1993). [CrossRef]

10.

Ph. Buffat and J. P. Borel, “Size effect on the melting temperature of gold particles,” Phys. Rev. A 13, 2287–2298 (1976). [CrossRef]

11.

H. El Hamzaoui, L. Courtheoux, V. Nguyen, E. Berrier, A. Favre, L. Bigot, M. Bouazaoui, and B. Capoen, “From porous silica xerogels to bulk optical glasses: The control of densification,” Mater. Chem. Phys. 121, 83–88 (2010). [CrossRef]

12.

S. J. Xia and V. I. Birss, “A multi-technique study of compact and hydrous Au oxide growth in 0.1M sulfuric acid solutions,” J. Electroanal. Chem. 500, 562–573 (2001). [CrossRef]

13.

S. Underwood and P. Mulvaney, “Effect of the solution refractive index on the color of gold colloids,” Langmuir 10, 3427–3430 (1994). [CrossRef]

14.

N. Pinçon, B. Palpant, D. Prot, E. Charron, and S. Debrus, “Third-order nonlinear optical response of Au:SiO2 thin films : influence of gold nanoparticle concentration and morphologic parameters,” Eur. Phys. J. D 19, 395–402 (2002). [CrossRef]

15.

R. Boyd, Nonlinear Optics2nd ed. (Academic Press, 2003).

16.

JCPDS, file 00–004–0784

OCIS Codes
(060.4370) Fiber optics and optical communications : Nonlinear optics, fibers
(160.4236) Materials : Nanomaterials
(060.5295) Fiber optics and optical communications : Photonic crystal fibers

ToC Category:
Fiber Optics and Optical Communications

History
Original Manuscript: June 27, 2011
Revised Manuscript: August 25, 2011
Manuscript Accepted: August 26, 2011
Published: September 15, 2011

Citation
L. Bigot, H. El Hamzaoui, A. Le Rouge, G. Bouwmans, F. Chassagneux, B. Capoen, and M. Bouazaoui, "Linear and nonlinear optical properties of gold nanoparticle-doped photonic crystal fiber," Opt. Express 19, 19061-19066 (2011)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-19-20-19061


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References

  1. P. S. J. Russell, “Photonic-crystal fibers,” J. Lightwave Technol.24, 4729–4749 (2006). [CrossRef]
  2. G. Agrawal, Nonlinear Fiber Optics4th ed. (Academic Press, 2007).
  3. K. C. Rustagi and C. Flytzanis, “Optical nonlinearities in semiconductor-doped glasses,” Opt. Lett.9, 344–346 (1984). [CrossRef] [PubMed]
  4. D. Ricard, Ph. Roussignol, and Chr. Flytzanis, “Surface-mediated enhancement of optical phase conjugation in metal colloids,” Opt. Lett.10, 511–513 (1985). [CrossRef] [PubMed]
  5. J. Troles, Q Coulombier, G. Canat, M. Duhant, W. Renard, P. Toupin, L. Calvez, G. Renversez, F. Smektala, M. El Amraoui, J. L. Adam, T. Chartier, D. Mechin, and L. Brilland, “Low loss microstructured chalcogenide fibers for large non linear effects at 1995 nm,” Opt. Express18, 26647–26654 (2010). [CrossRef] [PubMed]
  6. G. Qin, M. Liao, C. Chaudhari, X. Yan, C. Kito, T. Suzuki, and Y. Ohishi, “Second and third harmonics and flattened supercontinuum generation in tellurite microstructured fibers,” Opt. Lett.35, 58–60 (2010). [CrossRef] [PubMed]
  7. A. Dhawan and J. F. Muth, “Plasmon resonances of gold nanoparticles incorporated inside an optical fibre matrix,” Nanotechnology17, 2504–2511 (2006). [CrossRef] [PubMed]
  8. S. Ju, V. L. Nguyen, P. R. Watekar, B. H. Kim, C. Jeong, S. Boo, C. J. Kim, and W. T. Han, “Fabrication and optical characteristics of a novel optical fiber doped with the Au nanoparticles,” J. Nanosci. Nanotechnol.6, 3555–3558 (2006). [CrossRef]
  9. J. Matsuoka, R. Mizutani, S. Kaneko, H. Nasu, K. Kamiya, K. Kadono, T. Sakaguchi, and M. Miya, “Sol-Gel processing and optical nonlinearity of gold colloid-doped silica glass,” J. Ceram. Soc. Jpn.101, 53–58 (1993). [CrossRef]
  10. Ph. Buffat and J. P. Borel, “Size effect on the melting temperature of gold particles,” Phys. Rev. A13, 2287–2298 (1976). [CrossRef]
  11. H. El Hamzaoui, L. Courtheoux, V. Nguyen, E. Berrier, A. Favre, L. Bigot, M. Bouazaoui, and B. Capoen, “From porous silica xerogels to bulk optical glasses: The control of densification,” Mater. Chem. Phys.121, 83–88 (2010). [CrossRef]
  12. S. J. Xia and V. I. Birss, “A multi-technique study of compact and hydrous Au oxide growth in 0.1M sulfuric acid solutions,” J. Electroanal. Chem.500, 562–573 (2001). [CrossRef]
  13. S. Underwood and P. Mulvaney, “Effect of the solution refractive index on the color of gold colloids,” Langmuir10, 3427–3430 (1994). [CrossRef]
  14. N. Pinçon, B. Palpant, D. Prot, E. Charron, and S. Debrus, “Third-order nonlinear optical response of Au:SiO2 thin films : influence of gold nanoparticle concentration and morphologic parameters,” Eur. Phys. J. D19, 395–402 (2002). [CrossRef]
  15. R. Boyd, Nonlinear Optics2nd ed. (Academic Press, 2003).
  16. JCPDS, file 00–004–0784

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