Silicon-Based Optoelectronic Integrated Circuit For Label-Free Bio/chemical Sensor
Silicon-Based Optoelectronic Integrated Circuit For Label-Free Bio/chemical Sensor
Silicon-Based Optoelectronic Integrated Circuit For Label-Free Bio/chemical Sensor
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17931
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1. Introduction
Label-free optical bio/chemical sensor is widely used to detect the refractive index change of
bio/chemical targets, which is with numerous advantages, such as non-physical contact, high
stability, high-speed detection, and high resolution etc. It is essential for the applications of
medical diagnosis, healthcare, and environmental monitoring [1–4]. Various kinds of optical
bio/chemical sensors are proposed and demonstrated, including surface-plasma resonance-
based devices, optical interferometers, optical fiber devices, grating-based devices, photonic
crystal structures, and micro-resonators devices [4–6]. Among all the approaches, silicon-on-
insulator (SOI) based bio/chemical sensors have been attracting great research interests due to
the advantage of large refractive index contrast, which enables the compact device footprint.
Furthermore, the fabrication of SOI-based devices is CMOS compatible, which enables large-
scale optoelectronic integrated circuits (OEIC). Plenty of SOI-based optical bio/chemical
sensors have been demonstrated with the detection limit as low as 10−5~10−7 [6–9]. A large
number multiple channel microring sensor integration system is also demonstrated recently
[10].
In general, there are two basic methods for optical sensing, namely, intensity scanning
method and wavelength scanning method [9]. As the sensitivity of the intensity scanning
method largely depends on the probe wavelength and the sensitivity of the photodetector in
order to achieve high signal-to-noise ratio to maximize the intensity change, most of the
demonstrated microresonator-based sensors adopt the wavelength-scanning method for
measuring the sharp resonance wavelength shift. However, the wavelength-scanning method
requires expensive high-resolution wavelength-tunable lasers, and thus the detection limit is
ultimately limited by the laser resolution. Therefore, the high-resolution wavelength-scanning
method might not be suitable for cost-effective point-of-care applications.
In order to overcome this aforementioned issue, we have proposed and demonstrated an
electrical tracing-assisted dual-microring label-free optical bio/chemical sensor [11]. We
integrated two cascade microrings on a single chip. One of microring is integrated with a
heater for thermal tuning, named as tracing microring. The other microring serves as the
sensing microring. The effective refractive index change of the detecting target is obtained by
scanning the voltage that is supplied to the tracing microring by monitoring the output
intensity from the sensing microring based on filter cascading effect. We demonstrated the
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17932
sensitivity of ~4.0 mW/ng·mm−2 and detection limit of ~5.35 pg/mm2. Following this work,
we integrated the one-dimensional grating coupler for the vertical light coupling between
optical fiber and on-chip waveguides, which is suitable for practical application with device
packaging [13]. However, such demonstrations still requires expensive off-the-shelf
photodetector. Furthermore, the power consumption of the tracing microring, about ~20 mW,
is relatively high.
In this paper, we demonstrate silicon-based OEIC for optical bio/chemical sensor by
integrating grating couplers, a tunable microring filter, a microring sensor, and a Ge
photodetector in a single chip. With the integrated Ge photodetector, we directly read out the
electrical signal and extract the effective refractive index change. Furthermore, we adopt the
undercut technique and remove the substrate Si, thus reduce tracing microring power
consumption to be less than 3 mW. The demonstrated sensing sensitivity is ~15 mW/RIU and
the detection limit is ~3.9 μ-RIU. For surface sensing, we obtain a surface mass sensitivity of
Sm = ~192 µW/ng·mm−2 and the detection limit of 0.3 pg/mm2. Such high-performance OEIC
sensing system is with low-cost and promising for the potential large-scale integration, hence
being suitable for point-of-care applications.
2. Working principle
Conventionally, the microresonator-based optical bio/chemical sensors use wavelength-
scanning method in order to obtain the resonance wavelength shift induced by the effective
refractive index change, as schematically shown in Fig. 1(a). A high-resolution wavelength
scanning laser is deployed as the light source. The off-the-shelve photodetector records the
transmission spectra. The refractive index change is extracted by the resonance wavelength
shift. In such a method, the detection limit is determined by the resolution of the wavelength-
tunable laser and the sensitivity of the photodetector. In order to resolve small changes of the
resonance wavelength shift to detect ultra-small refractive index change, very high-resolution
wavelength-tunable laser and highly sensitive photodetector are required, which would
increase the cost significantly.
Fig. 1. (a) Schematic of the conventional wavelength-scanning method. (b) Schematic of the
proposed silicon-based OEIC sensing system by using electrical-tracing-assisted sensing
method.
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17933
named as tracing microring, serves as the tunable filter [11]. Both tracing- and sensing-
microring are Add/Drop microring resonator structure. The dropped light from microring
resonator becomes a Lorentz-shaped narrow band. The centre wavelength is the microring
resonance wavelength, and the linewidth of such dropped light is determined by the microring
resonance quality factors (Q-factor). The higher the Q-factor is, the narrower the linewidth is.
If both resonance wavelengths of the tracing- and sensing- microrings are aligned with each
other, the output signal has the maximum intensity. By scanning the voltage supplied to the
tracing microring to shift the resonance wavelength, both wavelengths are always aligned and
the output intensity reaches maximum. By comparing the additional electrical power
difference supplied to the tracing microring in order to trace the sensing microring
wavelength change, the refractive index change is detected [11].
Fig. 2. Schematic of the proposed label-free optical bio/chemical sensing system. WB-LS:
wideband light source. WG: waveguide; TF: tunable filter (tracing microring); SS: sensing
microring; PD: photodetector.
3. Device fabrication
We fabricate the OEIC sensing system in silicon-on-insulator (SOI) platform by using
CMOS-compatible fabrication processes. The SOI wafer has a 220 nm silicon layer sitting on
a 2 μm buried oxide (BOX) layer. The device is patterned by using deep ultra-violet (DUV)
photolithography, followed by two steps of silicon reactive ion etching (RIE) to form the
vertical grating coupler and the slab waveguide with thickness of 150 nm, and the channel
waveguide. We design the slab waveguide for light propagating, while adopt channel
waveguides for the microring waveguides in order to minimize the optical transmission loss
and meanwhile keep high sensitivity of sensing microring. For the Ge photodetector, separate
masks are used for boron implantation to form the P type silicon under Ge, and P+ type silicon
Ohmic contacts. The implants are activated using rapid thermal anneal of 1050 °C for 5
seconds. After depositing a thin layer of field oxide, Ge epitaxial windows are opened by a
combination of dry and wet etching to expose the underlying Si. After growing a thin SiGe
buffer layer at 350 °C, Ge is selectively grown in an ultrahigh vacuum chemical vapor
deposition (UHVCVD) epitaxial reactor at 550 °C with a thickness of 500 nm. The N+ Ohmic
contact is formed by implanting phosphorus into Ge top surface, followed by an annealing at
500 °C for 5 min. A layer of SiO2 is deposited and the wafer goes through chemical-
mechanical polish (CMP) with1 μm-thick oxide insulating layer remained. The purpose of
CMP is reducing the surface step height. Following the deposition and patterning of TiN for
the thermal heater, another 500 nm insulating oxide deposition, separate contact holes to the
Si and Ge implantation regions and the thermal heater are opened by dry etching process,
followed with 0.75 μm Al metal deposition and patterning for the electrical pad. A
planarization step is carried out by depositing 1 μm oxide, reverse pattering/etching, and CMP
again for the microfluidic channel packaging. The sensing windows and bond pad windows
are opened afterwards via a combination of RIE dry etch and wet etch. Poly
(dimethysiloxane) (PDMS) microfluidic channels are separately fabricated using a standard
PDMS molding process [16]. A PDMS fluidic channel was bonded onto the diced silicon
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17934
sensor chip via activation of the silicon surface as well as the PDMS surface using the oxygen
plasma.
Figures 3(a)-3(d) show the scanning electrode microscopes (SEMs) of the building blocks
of the sensing system, including the vertical grating coupler in Fig. 3(a), the thermal tunable
tracing microring in Fig. 3(b), the sensing microring in Fig. 3(c), and the Ge photodetector in
Fig. 3(d). The grating period is designed as 630 nm with a filing factor 50%. The etch depth
of the grating coupler is 70 nm. We adopt a low power consumption thermal tunable tracing
microring by using isolation trenches. The silicon substrate of the microring resonator is
etched away in order to efficiently confine the generated thermal heating, thus lower down
the electrical power consumption significantly [14]. Both tracing microring and sensing
microring are designed identically with 10 μm radius and 20 μm interaction lengths with a
gap of 300 nm between waveguide and microring. The on-chip Ge photodetector is designed
with 6 μm width and 100 μm length, which is sufficient for the light absorption.
Fig. 3. The SEMs of the building blocks. (a) Optical one dimensional grating coupler. (b)
Thermal-optical tunable ring filter. (c) Sensing microring. (d) Ge photodetector.
Fig. 4. (a) Schematic of the testing setup. (b) The optical image of the biochip on the test setup.
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17935
4.2 Characterization of the tracing microring with isolation trench
The resonance wavelength λr of the microring resonator (both tracing- and sensing-
microrings) depends on the waveguide effective refractive index neff, which is determined by
the environment situations, including the temperature T for the tracing microring, and optical
index nc of the cladding material (sensing target) on the sensing microring. The relationship
among them can be expressed as:
λr ∂neff ∂n
Δλr = ΔT + eff Δnc (1)
ng ∂T ∂nc
where, ng is the group index of waveguide, ΔT and Δnc are temperature change and the index
change of the target objective (sensing microring cladding index change).
Firstly, we characterized a stand-alone tracing microring (the tunable filter), which is
fabricated in the same chip with identical designs of the sensing microring. In the tracing
microring, Δnc = 0, while the temperature change ΔT linearly relates to the heater power
variation of ΔW. In such case, we link the resonance wavelength shift to the electrical power
change as:
Δλr = AΔW (2)
where, coefficient A is the sensitivity of the tracing microring to electrical power. Figure 5(a)
shows the measured transmission spectra of the tracing microring upon different voltages.
The voltage increases from 0 V to 1.2 V with a step of 0.2 V. As the supplied voltage
increases, the microring effective refractive index increases due to the increase of the
temperature. The measured resistivity of the thermal heater R is ~940 Ω. Thus, the relation
between the resonance wavelength to the electrical power is calculated with W = V2/R and is
shown in Fig. 5(b). The extracted thermal coefficient is ~3.4 nm/mW. However, for the
identically designed tunable microring without isolation trench, the thermal coefficient is only
~0.155 nm/mW, suggesting a 20 times enhancement. As the FSR of the microring is ~5.5 nm,
the resonance shift of an FSR requires 1.62 mW electrical powers, which corresponds to the
voltage supply of ~1.23 V.
Fig. 5. (a) The measured transmission spectra of the tracing microring upon different electrical
voltages. Voltage increases from 0 V to 1.2 V with step of 0.2V. (b) The resonance wavelength
as function of the electrical power supplying to the tracing microring. Blue circles are
experimental data from (a) and red line is linear fitting curve.
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17936
Δλr = S Δnc (3)
Where, S is the sensitivity of the sensing microring to the target objective. Furthermore, the
sensing sensitivity can be expressed as:
λr δ neff
S= (4)
n g δ nc
Where, δneff/δnc is determined by light distribution in the waveguide and in the cladding. The
weaker the light confinement inside the waveguide is, the stronger the light interaction with
the cladding material, the larger the value of δneff/δnc. ng is the group index and is dependent
on the dispersion of waveguide materials and waveguide dimension. In our design, ng is ~4.2.
In order to experimentally investigate the sensing sensitivity, we employ NaCl solution as
the detecting target. The concentrations of the NaCl solution used are 1%, 3%, 5%, 7% and
10%. The relation between concentration and the index is as n = 0.17151C + 1.3119, where C
is the concentration. Figure 6 shows the measured resonance wavelength as function of the
refractive index of the NaCl solution. The extracted sensing sensitivity is ~58.3 nm/RIU.
Fig. 6. The resonance wavelength shift of the sensing microring with different concentration of
the cladding NaCl solutions. Five different concentrations are adopted as 1%, 3%, 5%, 7% and
10%, respectively.
Fig. 7. (a) The measured I-V curve of the Ge-Photodetector with (red) and without (blue) light
illumination. (b) The enhancement of the photocurrent with and without light illumination.
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17937
4.5 Demonstration of optical sensing using OEIC sensing system
We then demonstrate the optical bio/chemical sensing using such OEIC sensing system
including the detection of the bulky refractive index change and the surface sensing of
specific protein.
For bulk refractive index sensing, we characterize the detection limit of the sensing
system by using NaCl solution as the detection target. For the sensing microring upon
different concentrations of the NaCl solution, we scan the applied voltage to the tracing
microring and record the photocurrent generated from the on-chip photodetector. Figure 8(a)
shows the measured photocurrent spectra upon the scanning of the electrical power to the
tracing microring. By using Lorentz fitting [11], we obtain the required electrical power at
which the peak current achieved, and subsequently relate that to the index change of the NaCl
solution upon different concentrations. Figure 8(b) shows the extracted relationship between
the optical refractive index of the NaCl solution and the electrical power supplied to the
tracing microring. The sensing sensitivity according to linear fitting is ~15 mW/ RIU.
Fig. 8. (a) The measured photocurrent spectra upon the scanning of the electrical power to the
tracing microring with different NaCl concentrations. The blue circle lines are the
experimental measurements while the red lines are the fitting results. (b) The relationship
between the extracted electrical power and the optical index of the NaCl solutions.
Fig. 9. (a) The measured photocurrent spectra upon the supplied electrical power to the tracing
microring. There are 20 times repeat measurements. (b) Zoom in of (a) around spectra peeks.
(c) The electrical power deviation for 20 measurements. σ: standard deviation, 3σ: the
extracted electrical power resolution.
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17938
From Eqs. (2) and (3), the detection limit relates to the electrical power resolution, which
can be determined by measuring the standard deviation of the supplied electrical power. This
is obtained by repeating the measurement for multiple times. Figure 9(a) shows as an example
the photocurrent spectra as function of the electrical power with 20 times measurement. The
voltage is scanned at a step of 0.5 mV and sensing microring is exposed to the air. The zoom-
in views of the intensity distributions around peak intensity are shown in Fig. 9(b). The peak
positions of every measurement can be extracted by Lorentz fitting to the optical response
[11]. The obtained electrical powers corresponding to the peak current are shown in Fig. 9(c).
The extracted standard deviation σ is ~19.6 nW, suggesting the electrical power resolution 3σ
of 58.8 nW. Such high resolution can be attributed to the following reasons: 1) the electrical
tracing assisted sensing method is intrinsically with high resolution comparing to the
wavelength-scanning method due to the achievable smaller equipment resolution [11]. For
instance, the equivalent wavelength resolution is calculated to be ~0.2 pm in current
demonstration. 2) the data fitting adopted here smooth the measurement results, thus
enhancing the signal-to-noise ratio, and 3) the measurement for achieving the standard
deviation is with air cladding in order to make sure the stable testing system. This may
introduce slight difference comparing to the sensing microring that cladded with detection
objective. Based on the extracted detection resolution, the detection limit is ~3.9 μ-RIU.
For surface sensing of specific protein interaction, a well-characterized biotin-streptavidin
interaction is used as a model system. The interaction between biotin and streptavidin is one
of the highest non-covalent affinities (KD = 10−13 M) and is therefore stable and specific. The
silicon microring device is first treated with oxygen plasma during a PDMS bonding process.
It is then treated by injecting a solution of 2% 3-aminopropyltriethoxysilane (APTES, Sigma-
Aldrich) in a mixture of ethanol/H2O (95%/5%, v/v) using a syringe pump for 2 h, followed
by thorough rinsing with ethanol. It is then treated through injection of a solution of 0.25
mg/ml NHS-PEG4-biotin (Thermo Scientific Pierce) in DI water for 1 h and rinsed with DI
water in the same method. In addition, 1% bovine serum albumin (BSA, Sigma-Aldrich) in
phosphate buffered saline (PBS) is injected into microchannel for 30 min to prevent non-
specific binding at the surface of a silicon microring device and rinsed with PBS. The binding
assay between biotin and streptavidin is performed by applying streptavidin solution in PBS.
Fig. 10. Real time detection of biotin-streptavidin interaction. Blue triangles and circles are the
experimental data of 10 µg/ml and 1 µg/ml, respectively. Red dashed line and solid line are the
fitting results.
Figure 10 shows the supplied electrical power of the tracing microring with biotin-
streptavidin interaction time. The blue triangle and circle markers are the supplied electrical
power supplied in order to trace the effective index change of the sensing microring upon 10
µg/ml and 1 µg/ml solutions, respectively. Upon the exposure of the sensing microring to
streptavidin solution, the electrical power rapidly increased, which indicates an increase in the
effective index on the sensor surface resulting from the binding of streptavidin molecules to
immobilized biotin on the sensor surface. The electrical power reached saturation after 5 min
of binding. The electrical power increments from biotin/streptavidin interaction at the
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17939
saturation are ~38 µW and ~441 µW for 1 µg/ml and 10 µg/ml, respectively. Red-dashed line
and solid line are the fitting results by using following equation:
t − t0
W ( t ) = W0 + (W∞ − W0 ) 1 − exp − (5)
τ
where, W(t) is the instantaneous electrical power, W0 is the initial power, W∞ is the final
steady state power, t0 is the start time of interaction, τ is the interaction time. For 10 µg/ml
and 1 µg/ml, the interaction times τ are 32 seconds and 22 seconds, respectively. Considering
the strong affinity between biotin and streptavidin, we assume that the sensor surface is
saturated with streptavidin molecules at 10 µg/ml, resulting in ~441 µW increase in electrical
power.
The sensitivity for surface binding detection is given by Sm = ΔW/σp, where σp the surface
density of streptavidin monolayer and ΔW is is the electrical power increase. With known
surface coverage of streptavidin monolayer of 2.5 × 1010 molecules/mm2 [16], the surface
density is calculated to be ~2.3 ng/mm2. Using the values of the electrical power increase
from this experiment, we obtain a surface mass sensitivity of Sm = ~192 µW/ng·mm−2. The
detection limit of a sensor is defined by Lm = R/Sm, where R is the sensor resolution (3σ) and
Sm is the mass sensitivity. If we consider 3σ of ~58.8 nW, we estimate the surface detection
limit to be ~0.3 pg/mm2.
5. Conclusion
We have fabricated a silicon-based OEIC for label-free optical bio/chemical sensor using
CMOS-compatible fabrication process. Such OEIC sensing system integrates grating
couplers, a tracing microring, a sensing microring, and a Ge photodetector on a single SOI
chip, which features the advantage of large-scale integration and significantly reduced cost.
By using electrical-tracing assisted sensing method, we have demonstrated the sensitivity of
~15 mW/RIU and the detection limit of 3.9 μ-RIU for bulky index sensing, and obtained a
surface mass sensitivity of Sm = ~192 µW/ng·mm−2 and the detection limit of 0.3 pg/mm2 for
surface biotin-streptavidin sensing. Such OEIC sensing system is favored for point-of-care
application with low electrical power consumption.
Acknowledgments
This work was supported by the Agency for Science, Technology and Research (A*STAR)
Joint Council Office (JCO) Development Programme Grant (1234e00018), Singapore, and
National Natural Science Foundation of China (NSFC, Grant No. 61177090).
#186886 - $15.00 USD Received 12 Mar 2013; revised 25 Apr 2013; accepted 29 Apr 2013; published 19 Jul 2013
(C) 2013 OSA 29 July 2013 | Vol. 21, No. 15 | DOI:10.1364/OE.21.017931 | OPTICS EXPRESS 17940