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Optics Express

Optics Express

  • Editor: C. Martijn de Sterke
  • Vol. 20, Iss. 12 — Jun. 4, 2012
  • pp: 13091–13099
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Fabrication of semiconductor-polymer compound nonlinear photonic crystal slab with highly uniform infiltration based on nano-imprint lithography technique

Fei Qin, Zi-Ming Meng, Xiao-Lan Zhong, Ye Liu, and Zhi-Yuan Li  »View Author Affiliations


Optics Express, Vol. 20, Issue 12, pp. 13091-13099 (2012)
http://dx.doi.org/10.1364/OE.20.013091


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Abstract

We present a versatile technique based on nano-imprint lithography to fabricate high-quality semiconductor-polymer compound nonlinear photonic crystal (NPC) slabs. The approach allows one to infiltrate uniformly polystyrene materials that possess large Kerr nonlinearity and ultrafast nonlinear response into the cylindrical air holes with diameter of hundred nanometers that are perforated in silicon membranes. Both the structural characterization via the cross-sectional scanning electron microscopy images and the optical characterization via the transmission spectrum measurement undoubtedly show that the fabricated compound NPC samples have uniform and dense polymer infiltration and are of high quality in optical properties. The compound NPC samples exhibit sharp transmission band edges and nondegraded high quality factor of microcavities compared with those in the bare silicon PC. The versatile method can be expanded to make general semiconductor-polymer hybrid optical nanostructures, and thus it may pave the way for reliable and efficient fabrication of ultrafast and ultralow power all-optical tunable integrated photonic devices and circuits

© 2012 OSA

1. Introduction

In the past decade, tremendous works have been devoted to making proper materials and structures for achieving ultrafast and ultra-low power integrated all-optical switches and modulators at the nanoscale [1

1. M. Scalora, J. P. Dowling, C. M. Bowden, and M. J. Bloemer, “Optical limiting and switching of ultrashort pulses in nonlinear photonic band gap materials,” Phys. Rev. Lett. 73(10), 1368–1371 (1994). [CrossRef] [PubMed]

5

5. Y. Liu, F. Qin, Z. Y. Wei, Q. B. Meng, D. Z. Zhang, and Z. Y. Li, “10 fs ultrafast all-optical switching in polystyrene nonlinear photonic crystals,” Appl. Phys. Lett. 95(13), 131116 (2009). [CrossRef]

]. Photonic crystal (PC) structures based on semiconductor materials are considered to be one of the most excellent candidates in fabricating nanoscale integrated all-optical circuits. However, the relatively weak and slow nonlinear optical properties of pure semiconductor materials have hindered the further progress in reducing the consumption power or pulse energy and the response time. So on one side sophisticated methods such as ion-implantation or placement of reverse bias are adopted to improve the nonlinear performance of semiconductor photonic devices [6

6. T. Tanabe, K. Nishiguchi, A. Shinya, E. Kuramochi, H. Inokawa, M. Notomi, K. Yamada, T. Tsuchizawa, T. Watanabe, H. Fukuda, H. Shinojima, and S. Itabashi, “Fast all-optical switching using ion-implanted silicon photonic crystal nanocavities,” Appl. Phys. Lett. 90(3), 031115 (2007). [CrossRef]

,7

7. H. S. Rong, S. B. Xu, Y. H. Kuo, V. Sih, O. Cohen, O. Raday, and M. Paniccia, “Low-threshold continuous-wave Raman silicon laser,” Nat. Photonics 1(4), 232–237 (2007). [CrossRef]

]. On the other side, people also resort to new kind of materials with large Kerr nonlinearity and fast relaxation time, such as pure polymers or nanocomposite doped polymer materials [4

4. X. Y. Hu, P. Jiang, C. Y. Ding, H. Yang, and Q. H. Gong, “Picosecond and low-power all-optical switching based on an organic photonic-bandgap microcavity,” Nat. Photonics 2(3), 185–189 (2008). [CrossRef]

,8

8. X. Y. Hu, Z. Q. Li, J. X. Zhang, H. Yang, Q. H. Gong, and X. P. Zhang, “Low-power and high-contrast nanoscale all-optical diodes via nanocomposite photonic crystal microcavities,” Adv. Funct. Mater. 21(10), 1803–1809 (2011). [CrossRef]

].

A straightforward and efficient way for fabricating high-performance nonlinear photonic crystal (NPC) integrated optical devices is to combine planar semiconductor PC structures with these highly nonlinear polymer materials. The key point in fabricating this semiconductor-polymer compound NPC lies in how to uniformly and densely fill polymers into the small air holes with a diameter of only hundreds nanometer. Previously, several techniques have been employed for the infiltration of PC with organic composites [9

9. R. van der Heijden, C. F. Carlström, J. A. P. Snijders, R. W. van der Heijden, F. Karouta, R. Nötzel, H. W. M. Salemink, B. K. C. Kjellander, C. W. M. Bastiaansen, D. J. Broer, and E. van der Drift, “InP-based two-dimensional photonic crystals filled with polymers,” Appl. Phys. Lett. 88(16), 161112 (2006). [CrossRef]

16

16. K. Yoshino, Y. Shimoda, Y. Kawagishi, K. Nakayama, and M. Ozaki, “Temperature tuning of the stop band in transmission spectra of liquid-crystal infiltrated synthetic opal as tunable photonic crystal,” Appl. Phys. Lett. 75(7), 932–934 (1999). [CrossRef]

]. However, specific problems, such as delamination and shrinkage of the infiltrants, have to be addressed in these technical processes. For example, solution infiltration of PC with polymers results in shrinkage and trapped air bubbles after the removal of solvent [10

10. S. Cheylan, F. Y. Sychev, T. Murzina, T. Trifonov, A. Maydykovskiy, J. Puigdollers, R. Alcubilla, and G. Badenes, “Optical study of polymer infiltration into porous Si based structures,” Proc. SPIE 6593, 65931K, 65931K-11 (2007). [CrossRef]

,11

11. J. Martz, R. Ferrini, F. Nüesch, L. Zuppiroli, B. Wild, L. A. Dunbar, R. Houdré, M. Mulot, and S. Anand, “Liquid crystal infiltration of InP-based planar photonic crystals,” J. Appl. Phys. 99(10), 103105 (2006). [CrossRef]

]. Monomer infiltration and subsequent polymerization can lead to a good degree of infiltration, nevertheless, the materials suitable for this approach are limited and oftentimes they experience 10%–15% of shrinkage after the thermally initiated polymerization [9

9. R. van der Heijden, C. F. Carlström, J. A. P. Snijders, R. W. van der Heijden, F. Karouta, R. Nötzel, H. W. M. Salemink, B. K. C. Kjellander, C. W. M. Bastiaansen, D. J. Broer, and E. van der Drift, “InP-based two-dimensional photonic crystals filled with polymers,” Appl. Phys. Lett. 88(16), 161112 (2006). [CrossRef]

,12

12. S. Tay, J. Thomas, B. Momeni, M. Askari, A. Adibi, P. J. Hotchkiss, S. C. Jones, S. R. Marder, R. A. Norwood, and N. Peyghambarian, “Planar photonic crystals infiltrated with nanoparticle/polymer composites,” Appl. Phys. Lett. 91(22), 221109 (2007). [CrossRef]

]. Quite recently the vapor deposition method is chosen to completely fill the silicon slot waveguide with specific small organic molecule, where good homogeneity originates from the assembly of an amorphous phase without the formation of microcrystals or grains [17

17. B. Esembeson, M. L. Scimeca, T. Michinobu, F. Diederich, and I. Biaggio, Adv. Mater. 20(23), 4584–4587 (2008). [CrossRef]

]. So in order to homogeneously fill the hundred nanometer size holes or slots, the above infiltration methods are all limited to certain kind of organic molecules. A more general method, which can be applicable for most polymer materials, especially the nanocomposite polymer materials, is still lacking.

In this work, we present a general and practical technique for fabrication of NPCs by infiltrating polymer into semiconductor PC air hole arrays by utilizing the nano-imprint lithographic (NIL) technique, which is believed to be universal for all the thermoplastic materials. Not only complete compound NPC structures but also compound NPC microcavities have been successfully fabricated with high quality. The quality of the infiltration has been characterized by the cross-sectional scanning electron microscopy (SEM) analyses and optical transmission measurements, both of which confirm the success of this NIL based synthesis method.

2. Compound NPC fabricated by NIL technique

The NIL technique was invented by Stephen Y. Chou in 1995 to replicate the nano structure conveniently with the advantage of cost-effective and high throughput [20

20. S. Y. Chou, P. R. Krauss, and P. J. Renstrom, “Imprint of sub-25nm vias and trenches in polymers,” Appl. Phys. Lett. 67(21), 3114–3116 (1995). [CrossRef]

,21

21. S. Y. Chou, P. R. Krauss, and P. J. Renstrom, “Nanoimprint lithography,” J. Vac. Sci. Technol. B 14(6), 4129–4133 (1996). [CrossRef]

]. For the common thermal NIL the principal procedure is as follows. A mold with nanostructures on its surface is pressed into a thin resist coated on a substrate. Keeping constant high pressure and the temperature beyond the glass transition temperature Tg of the resist, the resist becomes viscous and the flowing of it under high pressure will infiltrate the void region of the nanostructure completely after adequate time. After the removal of the mold the nanostructures are transferred into the resist film. So high-quality polymeric PC slab structures have been successfully fabricated by this technique [22

22. E. M. Arakcheeva, E. M. Tanklevskaya, S. I. Nesterov, M. V. Maksimov, S. A. Gurevich, J. Seekamp, and C. M. Sotomayor Torres, “Fabrication of semiconductor-and polymer-based photonic crystals using nanoimprint lithography,” Solid-State Electron. 50, 1043–1047 (2005).

,23

23. C. G. Choi, C. S. Kee, and H. Schift, “Fabrication of polymer photonic crystal slabs using nanoimprint lithography,” Curr. Appl Phys. 6s1, e8-e11 (2006).

]. By now the NIL is all treated only as a lithography technique for generating nano-pattern in the resist film. The great potential as an infiltration technique is largely neglected. So we envisage that if we remove the substrate instead of the mold after the imprint process, we would get perfectly mold-resist compound structures. This is our main idea for fabricating semiconductor-polymer compound NPC based on NIL. In our case, the corresponding mold and resist we used are SOI and polystyrene, respectively. As a matter of fact the NIL based method is expected to cover most of the polymer or nanocomposite polymer and semiconductor materials.

The fabrication procedure is illustrated in Fig. 1(b). Concisely it can be divided into two parts, i.e. the fabrication of the PC mold on SOI structure and the preparation of the PS film coated on the passivated silicon (Si) substrate. In our case silicon PC patterns were fabricated using Electron-Beam Lithography (Raith150, Germany) combined with HBr-based Inductively Coupled Plasma (System100, Oxford instruments, UK) etching. Then the NIL (Eitre-3, Obducat, Sweden) technique was adopted to fill the air holes array of silicon PC slab with polystyrene for the formation of compound NPC structure. The final fabricated silicon PCs, which serve as mold, consist of triangular lattice array of air holes etching through the top silicon layer of the SOI wafers with lattice constant as 400 nm and diameter as 252 nm, which is shown in Fig. 2
Fig. 2 SEM top view pictures of a triangular-lattice complete photonic crystal. Strip waveguides are visible at the left and right of the PC region. (a) Before infiltration; (b) After infiltration by utilizing NIL technique. The image contrast for the compound structure is low because of the poor conductivity of polystyrene covering the silicon membrane.
. The thickness of the top silicon layer is 235 nm. Before the preparation of the PS film, the surface of the Si substrate is treated with 1H,1H,2H,2H-Perfluorooctyltrichlorosilane, resulting in an anti-stick property between the polymer film and substrate surface so as to detach PS film from the substrate during the demold process. Here it must be emphasized that stable temperature and homogeneous large-area pressure during the imprint process are the crucial conditions for the success of NIL. In our NIL system the pressure applied to the mold and substrate are offered by the compressed air, which results in uniform pressure upon the whole area. Stable and program-controllable temperature is provided in the imprint chamber. Under an appropriate imprint condition of temperature, pressure, and contact time, a PS film with thickness of 1-2 μm is left on top of the silicon layer. The optimal imprint condition we found for our process as 160 °C for temperature and 50 barr for pressure with a contact time of 5 minutes beyond the Tg temperature. According to early theoretical work [18

18. F. Qin, Y. Liu, Z. M. Meng, and Z. Y. Li, “Design of Kerr-effect sensitive microcavity in nonlinear photonic crystal slabs for all-optical switching,” J. Appl. Phys. 108(5), 053108 (2010). [CrossRef]

], as the thickness of the PS layer above the semiconductor membrane is far larger than the lattice constant, the band location and band gap width of the fabricated compound NPC will reach a steady magnitude that is close to the values for the NPC with an infinitely thick PS overlayer. Furthermore, as the PS film is thick enough, the influence of the roughness of the top surface of the PS on the transmission spectrum can also be neglected.

In order to characterize the effect of the infiltration, we cut the structure using the Focused Ion Beam (FIB). In this process, the 1-2 μm polystyrene thin film has been largely polished out to a very thin and rough layer (tens nanometers thick) covering the silicon structure. Figure 3(a)
Fig. 3 (a) and (b) are the cross-section SEM image of the compound photonic crystal structure. The dark grey color corresponds to the polystyrene while the light grey color corresponds to the silicon owing to the difference between their conductivity. We can see that polystyrene fills the holes ideally and conformally without shrinkage and delamination from the side walls. (c) The cross-section SEM image of the compound photonic crystal structure after the deposition of Pt layer. We deposit a layer of Pt by FIB induced deposition on the surface of the compound structure after taking out the surface polymer by the O2 Reactive-Ion-Etching, and we can see that Pt cannot deposit into the holes array, indicating complete infiltration of polystyrene into the air holes. (d) The cross-section SEM image of the non-infiltrated photonic crystal structure after the deposition of Pt layer. In contrast with panel (c), we can see that the Pt can deposit into the air holes and reach their bottom. The bright rectangular bump on top of the slab is the deposited Pt layer.
and Fig. 3(b) show the cross-sectional SEM view of the compound NPC slabs. The residual polystyrene gums can be clearly seen here. We can see that complete filling for all holes is achieved using this technique. The polystyrene fills the holes ideally and conformally without shrinkage and delamination from the side walls. To further clarify that the holes are undoubtedly infiltrated with PS rather than imaging error arising from the poor conductivity of PS, we use a local deposition method to examine whether the holes are infiltrated or not, as is shown in the Fig. 3(c) and Fig. 3(d). Firstly we remove the covered PS layer of the compound structure totally by utilizing of O2 Reactive Ion Etching (RIE) until the silicon surface emerges exactly. Then we locally deposit a layer of platinum (Pt) by FIB induced deposition. After that we cut the deposited region by FIB, and we can see from the cross-sectional image [Fig. 3(c)] that Pt could not deposit into the holes array. For comparison, we deposit Pt layer on a PC structure without PS imprinted and we can see from Fig. 3(d) that Pt can fill air hole arrays completely. Based on the above SEM analysis results, it can be inferred that the silicon PCs are homogeneously and completely filled with PS.

3. Optical characterization of compound NPC

As we know, infiltration of silicon PCs with high index polymer, which leads to an increase of the effective refractive index, will result in the red-shift of the photonic band gap (PBG). To optically characterize the band shift effect of the PBG by infiltration of PS, the transmission spectrum is measured along the Γ-K direction of the NPC, as is represented in Fig. 2. Optical measurements are performed with the end-face fiber coupling system [24

24. L. Gan, C. Z. Zhou, C. Wang, R. J. Liu, D. Z. Zhang, and Z. Y. Li, “Two-dimensional air-bridged silicon photonic crystal slab devices,” Phys. Status Solidi A 207(12), 2715–2725 (2010). [CrossRef]

26

26. Y. Z. Liu, R. J. Liu, C. Z. Zhou, D. Z. Zhang, and Z. Y. Li, “Γ-Mu waveguides in two-dimensional triangular-lattice photonic crystal slabs,” Opt. Express 16(26), 21483–21491 (2008). [CrossRef] [PubMed]

]. The input optical signal with TE polarization comes from a continuous wave tunable diode laser with wavelength ranging from 1500 to 1640 nm, and launched into one facet of the silicon strip waveguide via a single-mode lensed fiber. The transmission signal is detected by a power meter via another lensed fiber collecting the emitted signal from the output side. The output strip waveguide was gradually tapered from 10 μm at the place adjacent the NPC structure to 1.5 μm at the end face of the whole sample that connects with tapered fiber lens, so that we can collect more signal light transmitting through the NPC structures.

The measured transmission spectra of the complete silicon PC structure before and after infiltration are presented in Fig. 4(a)
Fig. 4 Transmission spectra of the TE-like mode along the Γ-K direction of the empty and infiltrated triangular-lattice PCs. (a) Experimental data, where both of the samples before and after infiltration are measured twice to clarify the validity of measurement data. The two lines with solid cubic symbol are the transmission curves before infiltration, and the two lines with hollow circle symbol are the transmission curves after infiltration; (b) 3D-FDTD simulation data.
. In both cases, the transmission contrast between the pass-band and the forbidden-band of the PC is around 15-20 dB, and moreover, the span of wavelength from PBG to pass band takes only 5 nm. It can be observed that the long wavelength band-edge of the PCs exhibits a 20 nm red-shift after infiltration. Furthermore, the transmission contrast of the infiltrated samples is about 5 dB larger than that of the sample before infiltration. This is caused by the increase of the effective refractive index of the structure region after PS infiltration, which leads to the reduction of the out-of plane loss [6

6. T. Tanabe, K. Nishiguchi, A. Shinya, E. Kuramochi, H. Inokawa, M. Notomi, K. Yamada, T. Tsuchizawa, T. Watanabe, H. Fukuda, H. Shinojima, and S. Itabashi, “Fast all-optical switching using ion-implanted silicon photonic crystal nanocavities,” Appl. Phys. Lett. 90(3), 031115 (2007). [CrossRef]

]. Figure 4(b) is the calculated transmission spectrum for the empty and the filled PCs simulated by three-dimensional finite-difference time-domain (3D-FDTD) method [27]. Compared with Fig. 4(a) we can see that the experiment curves are 20 dB lower than the simulation results, and this is due to the coupling loss at the two interfaces between the lensed fiber and the input and output Si strip waveguides. The simulation data show an average 20 nm red-shift of the band edge after infiltration of polystyrene, which is close to the value found in experiments. The significant shift of band-edge and large transmission contrast indicate that the filling of the PC holes is complete and uniform. On the other hand, the absolute position and the line shape (e.g., the steepness) of the band edge show a slight deviation between experiment and theory, and this can be attributed to the nanofabrication imprecision as well as the departure of the models used in the numerical simulation from the practical samples under experimental studies. For instance, the input and output ridge waveguides have been neglected in the numerical simulations for the sake of simplicity.

4. Summary

In summary, we have presented a general method for making semiconductor-polymer compound NPC slab by utilizing nano-imprint lithography technique, which can help to realize perfect infiltration of thermoplastic polymer during the nano-imprint process. We have demonstrated that silicon-polystyrene compound complete NPC and NPC microcavity can be fabricated with highly uniform infiltration of polystyrene. Both the cross-sectional SEM analysis and optical transmission measurement confirm the high-quality infiltration. The transmission contrast between pass band and forbidden band of the complete photonic crystal slab is more than 15 dB and the quality factor of the compound photonic crystal microcavity is about 227, and both results are in good agreement with the simulation values. This filling method can be applied to most of semiconductors and thermo-plastic nanocomposite polymer materials in bringing together the optical property advantages of each compound material. In addition, this NIL technique is applicable to fabrication of all silicon photonic crystal structures and devices. Therefore, we expect that this technology will open up a novel route for achieving nano-photonic components with ultrafast tunable and switchable optical properties and pave the way towards building all-optical integrated devices and circuits.

Acknowledgments

This work was supported by the National Basic Research Foundation of China under Grant Nos. 2011CB922002 and 2007CB613205, and the Knowledge Innovation Program of the Chinese Academy of Sciences (No. Y1V2013L11).

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M. Notomi and S. Mitsugi, “Wavelength conversion via dynamic refractive index tuning of a cavity,” Phys. Rev. A 73(5), 051803 (2006). [CrossRef]

35.

Y. Liu, F. Qin, Z. M. Meng, F. Zhou, Q. H. Mao, and Z. Y. Li, “All-optical logic gates based on two-dimensional low-refractive-index nonlinear photonic crystal slabs,” Opt. Express 19(3), 1945–1953 (2011). [CrossRef] [PubMed]

OCIS Codes
(190.4390) Nonlinear optics : Nonlinear optics, integrated optics
(230.1150) Optical devices : All-optical devices
(110.4235) Imaging systems : Nanolithography
(230.5298) Optical devices : Photonic crystals

ToC Category:
Photonic Crystals

History
Original Manuscript: February 27, 2012
Revised Manuscript: April 21, 2012
Manuscript Accepted: April 23, 2012
Published: May 25, 2012

Citation
Fei Qin, Zi-Ming Meng, Xiao-Lan Zhong, Ye Liu, and Zhi-Yuan Li, "Fabrication of semiconductor-polymer compound nonlinear photonic crystal slab with highly uniform infiltration based on nano-imprint lithography technique," Opt. Express 20, 13091-13099 (2012)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-20-12-13091


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