The concentration of small molecule biomarkers in human serum and saliva has been shown to be characteristic of viral disease and correlated with disease severity. Inexpensive point-of-care diagnostic methods to quantify and track these analytes would provide additional information beyond viral or antibody detection assays to guide diagnosis and therapy. Waveguide-enhanced Raman spectroscopy (WERS) enables the detection and identification of trace concentrations of dissolved analytes using a chip-scale photonic circuit based on long evanescent waveguides. Here, we describe WERS measurements of two biomarkers: glucose and urea. This proof-of-concept work will provide the basis for the development of handheld bio-marker detection systems based on packaged photonic circuits integrated with a laser source and detector.
Photodetectors harnessing hot carrier generation on surface plasmon resonant nanoantennas are a promising avenue to achieving sub-bandgap imaging at room temperature. However, efficient extraction of plasmonic hot carriers under low-energy infrared (IR) excitation predicates careful design of Schottky interfaces. This work reports on the simulation-guided fabrication of Au (i) planar diodes and (ii) embedded IR nanoantennas interfaced with both n-/p-type Si and GaAs semiconductors in order to elucidate the impact of their electronic properties on photocurrent generation.
The development of a foundry-scale waveguide-enhanced Raman spectroscopy (WERS) platform is a vital for the widespead implementation of this analytical technique. In this work we analyze the waveguide material and fabrication processes offered by AIM Photonics with regard to their effectiveness for WERS, and other sensing techniques. Optical characterization of these materials via white light spectroscopy and fluorescence spectroscopy points to the designation of an optimal wafer composition comprising a thermal bottom oxide and an LPCVD silicon nitride waveguide. This optimal composition has no measurable fluorescence and a propagation loss of 3.2 dB/m at 1064 nm in the TM00 mode. In the c/l band, the optimal wafer build has as thermal bottom oxide, a PECVD silicon nitride waveguide, and is annealed. This build has a propagation loss of 8.1 dB/m at 1550 nm in the TE00 mode.
Gas chromatography (GC) is a staple analytical technique used to separate chemical mixtures (analytes) prior to identification with a hyphenated technique, such as mass spectrometry or Fourier transform infrared (IR) spectroscopy. Traditionally, analytes elute through the GC separation column where they are detected when they exit. We have developed a technique to perform in situ IR spectroscopy during the process of separating the analytes along the GC column. This is achieved by spin coating the stationary phase onto a germanium prism and actively probing the stationary phase in an attenuated total reflectance configuration with a quantum cascade laser.. The GC column is formed by pressing a molded epoxy lid, with grooves that form the tubular column, onto the stationary phase coated prism.
The ability to rapidly detect hazardous airborne chemicals with high fidelity in a single point-detection system remains a significant challenge in a complex chemical background. Traditional Gas chromatography (GC) can significantly augment most detection technologies by separating complex mixtures for high fidelity detection, but with the disadvantage of requiring detection at the end of the GC column which adds a time disadvantage for any decision making process. Microfabrication of GC columns has reduced device footprint and power consumption, but the end-of-column detection paradigm remains. We present a rapid detection concept of in-column detection by probing the GC stationary phase which is coated on an IR transparent column substrate. The optical evanescent field interactions in the mid-infrared spectral region (US. Patent# 9,599,567) allows analyte detection along the column without having to wait for complete elution. These spectral signatures, collected at different points along the column, are analyzed by an algorithm to quickly identify components in a complex mixture. We present results with an ATR-based system that uses a focused tunable quantum cascade laser beam directed by galvo mirrors at points along a molded micro-GC column whose base comprises an optically transparent material coated with the stationary phase.
Waveguide-enhanced Raman spectroscopy (WERS) enables the detection and identification of trace concentrations of vapor-phase analytes using a functionalized chip-scale photonic circuit. Here, we show that WERS signal can be collected from part-per-billion levels of targeted analytes in a backscatter geometry, which, compared to forward-scatter, simplifies component integration and is more tolerant of waveguide loss and modal interference. In addition, we discuss our progress towards a compact Raman sensing system that incorporates a handheld spectrometer and chip-scale optical filters. We demonstrate that a handheld, thermo-electrically cooled spectrometer can be used for backscatter WERS with a comparable signal-to-noise to that of a liquid-nitrogen cooled benchtop spectrometer. Finally, we describe efforts to integrate the dichroic Raman filter on-chip using arrays of unbalanced Mach-Zehnder interferometers. Measurements show filter performance sufficient for integration with WERS: Transmission of >80% of the laser in the cross port and Stokes signal in the through port; and extinction of the laser by >20 dB in the though port and of Stokes signal by >8 dB in the cross port.
The need for ever-growing communications bandwidths has led to an interest in mode-division-multiplexed communications to increase the information carrying capacity of fiber-optic networks. More recently, mode-division multiplexed chip-scale photonic devices have been investigated as a means towards highly integrated photonic components and systems. To date, however, most chip-scale demonstrations have focused on fixed coupling and routing of individual waveguide modes on a chip. In this work we propose and investigate a new technique to dynamically couple and convert between different propagating waveguide modes via symmetry-breaking optomechanical near-field interactions. Silicon nitride waveguides (tSi3N4=175 nm) with air top cladding are fabricated and enable propagation of weakly-confined modes with substantial evanescent field near the waveguide surface. Suspended silicon nitride (tSiNx=200 nm) micro-electro-mechanical structures (MEMS) interact with the propagating mode’s evanescent field. However, the slight offset of the MEMS perturber with respect to the waveguide’s center axis leads to a symmetry breaking mode perturbation. This perturbation converts even propagating modes (e.g. TE0) to higher-order odd modes (e.g. TE1). We present various experimental techniques for characterizing the mode conversion including direct imaging, mode beating, and FFT spectrogram analysis. Simulation and experimental results demonstrate this new concept of using symmetry-breaking optomechanical near field interactions for mode coupling and conversion towards future mode-division multiplexing on a chip.
Waveguide-enhanced Raman spectroscopy (WERS) enables the detection and identification of trace concentrations of vapor-phase analytes using a chip-scale photonic circuit coated with a sorbent material. Previous demonstrations of WERS utilized a hydrogen-bond acidic hyperbranched carbosilane fluoroalcohol-based sorbent polymer and focused on detection limits for different nerve agent simulants. In this work, we examine the Raman spectra of a number of new sorbent materials obtained using WERS. By comparing the spectra pre-exposure to the modified spectra measured during analyte exposure, the effects of hydrogen-bonding on the sorbent and analyte molecules are observed. Changes to the Raman transition strength or frequency of individual lines due to analyte binding shed light on the partitioning of vapor-phase molecular agents into the sorbent, and can be used to design sorbent materials with even higher sensitivity. We examine two new types of sorbents: Fluorinated bisphenol-based materials that increase the steric bulk of the substituents ortho- to the hydroxyl group, designed to reduce self-binding; and carbosilane fluoroalcohol polymers synthesized with a novel hydrosilylation reaction. The WERS detection limits for these new sorbents are measured for nerve-agent simulants and compared to previous generation materials.
We report the design, fabrication, and measurement of waveguide lattice filters for use in integrated Raman- or fluorescence-based spectroscopy and sensing systems. The filters consist of a series of broadband directional couplers and optical delay sections that create an n-stage unbalanced Mach–Zehnder interferometer specifically designed to segregate pump light and redshifted signal light in the two output ports. We first report the design criteria for optimal filter performance. Then, we use these criteria with numerical beam propagation methods to design specific broadband couplers. The filters were fabricated by a photonic integrated circuit foundry and measured using white-light spectroscopy. We report both four-stage and eight-stage filters, with the eight-stage filter demonstrating a 190-nm-wide signal passband (1100 cm − 1) on the “through” port with <1.5 dB of ripple and a 17-nm-wide, 20-dB extinction band at the filter resonance.
A significant remaining challenge in chemical detection is the ability to rapidly detect with high fidelity a full suite of CWAs and TICs in a single point-detection system. Gas chromatography (GC) is a proven laboratory technique that can achieve the stated detection goal, but not at the required speed and not in a wearable (or even portable) form factor. Efforts in miniaturizing GCs yielded small devices, but they remain slow as they retain the end-of-column detection paradigm which results in long elution times of CWAs and TICs. We describe a novel concept of in-column detection by probing the sorbent coating (stationary phase) of a micro-GC column through optical evanescent field interactions in the long-wave infrared (“chemical fingerprint”) spectral region (U.S. Patent US9599567B2). Detection closer to the injection port ensures a rapid response for slow-eluting analytes. Although this results in poor separation (i.e. poor ability to identify chemicals), this is more than compensated by having full IR absorbance spectra at each location. This orthogonal spectral signature (along with GC retention times) is used in a powerful algorithm to quickly identify components in a complex mixture under conditions of incomplete separation. We present results with an ATR-based system that uses a focused tunable quantum cascade laser beam directed by galvo mirrors at points along a molded micro-GC column whose bottom wall is the sorbent coated ATR prism. Efforts are under way to further miniaturize this device by employing novel long-wave-IR photonic waveguides for a truly portable integrated photonic chromatographic detector of CBRNE threats.
We describe the detection of trace concentrations of chemical agents using waveguide-enhanced Raman spectroscopy in a photonic integrated circuit fabricated by AIM Photonics. The photonic integrated circuit is based on a five-centimeter long silicon nitride waveguide with a trench etched in the top cladding to allow access to the evanescent field of the propagating mode by analyte molecules. This waveguide transducer is coated with a sorbent polymer to enhance detection sensitivity and placed between low-loss edge couplers. The photonic integrated circuit is laid-out using the AIM Photonics Process Design Kit and fabricated on a Multi-Project Wafer. We detect chemical warfare agent simulants at sub parts-per-million levels in times of less than a minute. We also discuss anticipated improvements in the level of integration for photonic chemical sensors, as well as existing challenges.
We will review the state of the art for on-chip, Raman-based sensing using waveguides including our recent work with sorbent-coated waveguides for trace gas sensing showing parts-per-billion limits of detection. We will show that signal enhancements due to scattering that takes place in the evanescent field coupled with a thin hypersorbent polymer coating can yield Raman efficiencies which are nine orders of magnitude larger than traditional micro-Raman techniques. We will also discuss challenges with gas component discrimination and in moving toward a fully integrated photonic circuit architecture for handheld Raman-based trace gas sensors.
Silicon photonics enables the development of optical components on a chip with the potential for large-scale optical integrated circuits that can be fabricated at the wafer-scale using foundries similar to those used in the electronics industry. Although silicon is a passive optical material with an indirect bandgap, reconfigurable devices have been demonstrated using thermo-optic effects (large phase shifts, but relatively slow with large power consumption) and carrier plasma dispersion effects (high-speed, but small phase shifts). We recently demonstrated a low-power approach for inducing large phase shifts (>2π) using a technique that we call micro-opto-electro-mechanical index perturbation (MOEM-IP). In this initial work we characterized silicon nitride waveguides in which the propagating optical mode’s evanescent field is vertically coupled to silicon nitride microbridges. This interaction leads to an effective index tuning that is a strong function of the waveguide-microbridge separation. We now extend our MOEM-IP approach to different configurations (i.e. in-plane coupling) and material systems (i.e. silicon-oninsulator). Mode perturbation simulations indicate that the MOEM-IP approach is widely applicable to many configurations and material systems enabling large effective index tuning (Δneffective>0.1) requiring microbridge displacements of only a few hundred nanometers. We also examine several device applications that take advantage of MOEM-IP. These include tunable optical filters using high-Q microring cavities and optical phased arrays that enable chip-scale beam steering in two-dimensions using low-power phase shifting enabled by MOEM-IP.
Highly evanescent nanophotonic waveguides enable extremely efficient Raman spectroscopy in chip-scale photonic integrated circuits due to the continuous excitation and collection of Raman scattering along the entire waveguide length. Such waveguides can be used for detection and identification of condensed-phase analytes, or, if functionalized by a sorbent as a top-cladding, can be used to detect trace concentrations of chemical species. The scattering efficiency is modified in guided-mode structures compared to unconfined, micro-Raman geometries. Here, we describe the theoretical framework for understanding the Raman scattering efficiency in nanophotonic waveguides, and compare these calculations to our measurements of trace gases in hypersorbent-clad silicon nitride waveguides.
Components for free space optical communication terminals such as lasers, amplifiers, and receivers have all seen substantial reduction in both size and power consumption over the past several decades. However, pointing systems, such as fast steering mirrors and gimbals, have remained large, slow and power-hungry. Optical phased arrays provide a possible solution for non-mechanical beam steering devices that can be compact and lower in power. Silicon photonics is a promising technology for phased arrays because it has the potential to scale to many elements and may be compatible with CMOS technology thereby enabling batch fabrication. For most free space optical communication applications, two-dimensional beam steering is needed. To date, silicon photonic phased arrays have achieved two-dimensional steering by combining thermo-optic steering, in-plane, with wavelength tuning by means of an output grating to give angular tuning, out-of-plane. While this architecture might work for certain static communication links, it would be difficult to implement for moving platforms. Other approaches have required N2 controls for an NxN element phased array, which leads to complexity. Hence, in this work we demonstrate steering using the thermo-optic effect for both dimensions with a simplified steering mechanism requiring only two control signals, one for each steering dimension.
We report long-wave infrared (LWIR, 5-15 μm) and mid-wave infrared (MWIR, 2.5 – 5 μm) differential absorption spectra of different nerve agent simulants and common solutes sorbed to poly(methyldi(1,1,1-trifluoro-2-trifluoromethyl- 2-hydroxypent-4-enyl)silane, HCSFA2, an NRL developed hypersorbent polymer. HCSFA2 is a strong hydrogen-bond acidic polymer which exhibits large gas-polymer partitions for a variety of hazardous chemicals with hydrogen-bond basic properties such as the phosphonate ester G-nerve agents or their simulants. The measured ATR-FTIR differential absorption spectra show complex fingerprint signal changes in the resonances for the sorbent material itself, as well as new resonances arising from chemical bonding between the solute or analyte and the sorbent or the solute itself being present in the sorbent.
The unique optical properties of porous silicon show it to be a promising material for imaging and spectroscopy in the
mid-infrared and long-infrared wavelength ranges. A tunable MEMS filter using porous silicon as a high-reflectivity
layer is proposed. Measurements on fabricated porous silicon-based distributed Bragg reflectors and Fabry-Perot etalons
are presented.
Hyperspectral infrared imagers are of great interest in applications requiring remote identification of complex chemical agents. The combination of mercury cadmium telluride detectors and Fabry–Perot filters (FPFs) is highly desirable for hyperspectral detection over a broad wavelength range. The geometries of distributed Bragg reflector (DBR)-based tunable FPFs are modeled to achieve a desired spectral resolution and wavelength range. Additionally, acceptable fabrication tolerances are determined by modeling the spectral performance of the FPFs as a function of DBR surface roughness and membrane curvature. These fabrication nonidealities are then mitigated by developing an optimized DBR process flow yielding high-performance FPF cavities suitable for integration with hyperspectral imagers.
The Mid-wave infrared (MWIR) spectrum has applications to many fields, from night vision to chemical and biological
sensors. Existing broadband detector technology based on HgCdTe allows for high sensitivity and wide range, but lacks
the spectral decomposition necessary for many applications. Combining this detector technology with a tunable optical
filter has been sought after, but few commercial realizations have been developed. MEMS-based optical filters have
been identified as promising for their small size, light-weight, scalability and robustness of operation. In particular,
Fabry-Perot interferometers with dielectric Bragg stacks used as reflective surfaces have been investigated. The
integration of a detector and a filter in a device that would be compact, light-weight, inexpensive to produce and scaled
for the entire range of applications could provide spectrally resolved detection in the MWIR for multiple instruments.
We present a fabrication method for the optical components of such a filter. The emphasis was placed on wafer-scale
fabrication with IC-compatible methods. Single, double and triple Bragg stacks composed of germanium and silicon
oxide quarter-wavelength layers were designed for MWIR devices centered around 4 microns and have been fabricated
on Silicon-On-Insulator (SOI) wafers, with and without anti-reflective half-wavelength silicon nitride layers. Optical
testing in the MWIR and comparison of these measurements to theory and simulations are presented. The effect of film
stress induced by deposition of these dielectric layers on the mechanical performance of the device is investigated. An
optimal SOI substrate for the mechanical performance is determined. The fabrication flow for the optical MEMS
component is also determined. Part of this work investigates device geometry and fabrication methods for scalable
integration with HgCdTe detector and IC circuitry.
In the past decades, there have been several attempts to create a tunable optical detector with operation in the infrared.
The drive for creating such a filter is its wide range of applications, from passive night vision to biological and chemical
sensors. Such a device would combine a tunable optical filter with a wide-range detector. In this work, we propose
using a Fabry-Perot interferometer centered in the mid-wave infrared (MWIR) spectrum with an HgCdTe detector.
Using a MEMS-based interferometer with an integrated Bragg stack will allow in-plane operation over a wide range.
Because such devices have a tendency to warp, creating less-than-perfect optical surfaces, the Fabry-Perot interferometer
is prototyped using the SOI-MUMPS process to ensure desirable operation. The mechanical design is aimed at optimal
optical flatness of the moving membranes and a low operating voltage. The prototype is tested for these requirements.
An HgCdTe detector provides greater performance than a pyroelectic detector used in some previous work, allowing for
lower noise, greater detection speed and higher sensitivity. Both a custom HgCdTe detector and commercially available
pyroelectric detector are tested with commercial optical filter. In previous work, monolithic integration of HgCdTe
detectors with optical filters proved to be problematic. Part of this work investigates the best approach to combining
these two components, either monolithically in HgCdTe or using a hybrid packaging approach where a silicon MEMS
Fabry-Perot filter is bonded at low temperature to a HgCdTe detector.
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