Dual-Mode Comb Plasmonic Optical Fiber Sensing.

Surface plasmon (SP) excitation in metal-coated tilted fiber Bragg gratings (TFBGs) has been a focal point for highly sensitive surface biosensing. Previous efforts focused on uniform metal layer deposition around the TFBG cross section and temperature self-compensation with the Bragg mode, requiring both careful control of the core-guided light polarization and interrogation over most of the C + L bands. To circumvent these two important practical limitations, we studied and developed an original platform based on partially coated TFBGs. The partial metal layer enables the generation of dual-comb resonances, encompassing highly sensitive (TM/EH mode families) and highly insensitive (TE/HE mode families) components in unpolarized transmission spectra. The interleaved comb of insensitive modes acts as wavelength and power references within the same spectral region as the SP-active modes. Despite reduced fabrication and measurement complexity, refractometric accuracy is not compromised through statistical averaging over seven individual resonances within a narrowband window of 10 nm. Consequently, measuring spectra over 60 nm is no longer needed to compensate for small temperature or power fluctuations. This sensing platform brings the following important practical assets: (1) a simpler fabrication process, (2) no need for polarization control, (3) limited bandwidth interrogation, and (4) maintained refractometric accuracy, which makes it a true game changer in the ever-growing plasmonic sensing domain.

In-situ monitoring of refractive index change during water-ice phase transition with a multiresonant fiber grating.

In-situ monitoring of refractive index changes during a liquid-solid phase transition is achieved by measurement of the transmission spectrum from a single tilted fiber Bragg grating immersed in water. Differential wavelength shifts of multiple mode resonances are used to eliminate cross-talk from temperature, throughout the phase transition, and from strains occurring after solidification. The measured sudden shift of refractive index at the phase transition is shown to be consistent with the expected difference from water to ice, in spite of the observed onset of compressive strain on the fiber by the frozen water. Beyond the obvious application to research on the dynamics of liquid-solid phase transitions, this work demonstrates the multiparameter measurement capabilities of multiresonant gratings.

Operando monitoring of thermal runaway in commercial lithium-ion cells via advanced lab-on-fiber technologies.

Operando monitoring of complex physical and chemical activities inside rechargeable lithium-ion batteries during thermal runaway is critical to understanding thermal runaway mechanisms and giving early warning of safety-related failure. However, most existing sensors cannot survive during such extremely hazardous thermal runaway processes (temperature up to 500 °C accompanied by fire and explosion). To address this, we develop a compact and multifunctional optical fiber sensor (12 mm in length and 125 µm in diameter) capable of insertion into commercial 18650 cells to continuously monitor internal temperature and pressure effects during cell thermal runaway. We observe a stable and reproducible correlation between the cell thermal runaway and the optical response. The sensor's signal shows two internal pressure peaks corresponding to safety venting and initiation of thermal runaway. Further analysis reveals that a scalable solution for predicting imminent thermal runaway is the detection of the abrupt turning range of the differential curves of cell temperature and pressure, which corresponds to an internal transformation between the cell reversible and irreversible reactions. By raising an alert even before safety venting, this new operando measurement tool can provide crucial capabilities in cell safety assessment and warning of thermal runaway.

Strong cladding mode excitation in ultrathin fiber inscribed Bragg grating with ultraviolet photosensitivity.

Strong UV-written Bragg gratings written in 50 µm-diameter cladding single mode fibers compatible with conventional fiber couple core guided light to dozens of cladding modes distributed across 140 nm in the 1400-1600 nm region, without the need for complex symmetry breaking mechanisms such as tilted, laterally offset, or localized gratings. The extent of the coupling to high order modes and the smaller cladding diameter both contribute to increasing the sensitivity to surrounding refractive index changes by more than one order of magnitude, and to an increased spacing between mode resonances to facilitate unambiguous measurements of larger index changes between 1.3 and 1.44. These improvements are confirmed by theoretical and experimental studies that also cover the temperature and strain differential sensitivities of the cladding mode resonances for complete multiparameter sensing capability.

Multiresonant analysis improves the limit of detection of tilted fiber Bragg grating refractometers.

A multiresonant approach based on tracking 27 cladding mode resonances of tilted fiber Bragg grating refractometers is shown to improve the limit of detection by a factor of 3 to 4 relative to the conventional approach of tracking the single-most sensitive resonance. Limits of detection below 2 × 10-5 in index change are achieved for dilutions of ethanol in water in repeated experiments. In all cases, wavelengths are referenced to the core mode resonance which eliminates the effect of small temperature changes during and between experiments.

Operando optical fiber monitoring of nanoscale and fast temperature changes during photo-electrocatalytic reactions.

In situ and continuous monitoring of thermal effects is essential for understanding photo-induced catalytic processes at catalyst's surfaces. However, existing techniques are largely unable to capture the rapidly changing temperatures occurring in sub-µm layers at liquid-solid interfaces exposed to light. To address this, a sensing system based on a gold-coated conventional single-mode optical fiber with a tilted fiber Bragg grating inscribed in the fiber core is proposed and demonstrated. The spectral transmission from these devices is made up of a dense comb of narrowband resonances that can differentiate between localized temperatures rapid changes at the catalyst's surface and those of the environment. By using the gold coating of the fiber as an electrode in an electrochemical reactor and exposing it to light, thermal effects in photo-induced catalysis at the interface can be decoded with a temperature resolution of 0.1 °C and a temporal resolution of 0.1 sec, without perturbing the catalytic operation that is measured simultaneously. As a demonstration, stable and reproducible correlations between the light-to-heat conversion and catalytic activities over time were measured for two different catalysis processes (linear and nonlinear). These kinds of sensing applications are ideally suited to the fundamental qualities of optical fiber sensors, such as their compact size, flexible shape, and remote measurement capability, thereby opening the way for various thermal monitoring in hard-to-reach spaces and rapid catalytic reaction processes.

Operando monitoring of ion activities in aqueous batteries with plasmonic fiber-optic sensors.

Understanding ion transport kinetics and electrolyte-electrode interactions at electrode surfaces of batteries in operation is essential to determine their performance and state of health. However, it remains a challenging task to capture in real time the details of surface-localized and rapid ion transport at the microscale. To address this, a promising approach based on an optical fiber plasmonic sensor capable of being inserted near the electrode surface of a working battery to monitor its electrochemical kinetics without disturbing its operation is demonstrated using aqueous Zn-ion batteries as an example. The miniature and chemically inert sensor detects perturbations of surface plasmon waves propagating on its surface to rapidly screen localized electrochemical events on a sub-µm-scale thickness adjacent to the electrode interface. A stable and reproducible correlation between the real-time ion insertions over charge-discharge cycles and the optical plasmon response has been observed and quantified. This new operando measurement tool will provide crucial additional capabilities to battery monitoring methods and help guide the design of better batteries with improved electro-chemistries.

Discrimination of Bulk and Surface Refractive Index Change in Plasmonic Sensors with Narrow Bandwidth Resonance Combs.

A method to enable surface plasmon resonance (SPR) sensors to discriminate between bulk and surface-localized refractive index changes is demonstrated with modified gold-coated tilted fiber Bragg grating SPR sensors (TFBG-SPR). Without this capability, all high-resolution SPR sensors should be using reference channels and strict temperature control to prevent the contamination of the desired detection of surface-localized chemical or binding events by drift of the refractive index of the medium, in which the experiment is carried out. The very fine comb of high-quality-factor resonances of a TFBG-SPR device coupled to the large differential sensitivity of some of the resonances to various perturbations is used to measure unambiguously the refractive index changes within a surface layer thinner than 25 nm from those of the bulk surrounding. The enabling modification of the conventional TFBG-SPR is a reduction of the gold coating from its optimum value near 50-30 nm: at this lower thickness, a surface plasmon wave can still be excited by a limited number of cladding mode resonances, but at the same time, the metal is thin enough to allow modes away from the SPR to tunnel across the metal and probe the bulk RI value. Measurements and simulations of the deposition of a self-assembled monolayer of 1-dodecanethiol in ethanol show that the bulk refractive index changes as small as 0.0004 can be distinguished from the formation of a 1 nm thick coating on the surface of the fiber.

Co-located angularly offset fiber Bragg grating pair for temperature-compensated unambiguous 3D shape sensing.

A 10 mm-long three-dimensional shape sensor in a single-mode fiber is described and demonstrated experimentally. The sensor is based on a pair of fiber Bragg gratings inscribed at the same location along the fiber axis but offset along different radial directions away from the fiber center. Each offset grating generates cladding mode resonances over a ${\sim}{20}\;{\rm{nm}}$-wide spectral bandwidth, and the two gratings are also offset in period so that their transmission spectra are separated by 40 nm, and thus non-overlapping and fully distinguishable. Directional bending sensitivity results from the differential amplitude response of the cladding mode resonances from the two gratings, depending on the relative orientation of the bend with the azimuthal direction of the grating offsets. It is further demonstrated that both axial deformation and temperature have no influence on the shape measurement as they both only cause a global wavelength shift of the spectra without amplitude change. The experimental results demonstrate that the shape orientation of an object can be unambiguously determined for bend directions covering the full 360° range around the fiber axis with sensitivities of the order of ${{1}}\;{\rm{dB/}}{{\rm{m}}^{- 1}}$ and small curvatures between 0 and ${{1}}\;{{\rm{m}}^{- 1}}$.

Self-monitored and optically powered fiber-optic device for localized hyperthermia and controlled cell death in vitro.

Localized hyperthermia therapy involves heating a small volume of tissue in order to kill cancerous cells selectively and with limited damage to healthy cells and surrounding tissue. However, these features are only achievable through real-time control of the tissue temperature and heated volume, both of which are difficult to obtain with current heating systems and techniques. This work introduces an optical fiber-based active heater that acts both as a miniature heat source and as a thermometer. The heat-induced damage in the tissue is caused by the conductive heat transfer from the surface of the device, while the heat is generated in an absorptive coating on the fiber by near-infrared light redirected from the fiber core to the surface by a tilted fiber Bragg grating inscribed in the fiber core. Simultaneous monitoring of the reflection spectrum of the grating provides a measure of the local temperature. Localized temperature increases between 0°C and 100°C in 10 mm-long/5 mm-diameter cylindrical volumes are obtained with continuous-wave pump power levels up to 1.8 W. Computational and experimental results further indicate that the temperature rise and dimensions of the heated volume can be maintained at a nearly stable level determined by the input optical power.

Microfluidic flow direction and rate vector sensor based on a partially gold-coated TFBG.

In microfluidic chips applications, the monitoring of the rate and the direction of a microfluidic flow is very important. Here, we demonstrate a liquid flow rate and a direction sensor using a partially gold-coated tilted fiber Bragg grating (TFBG) as the sensing element. Wavelength shifts and amplitude changes of the TFBG transmission resonances in the near infrared reveal the direction of the liquid flowing along the fiber axis in the vicinity of the TFBG due to a nanoscale gold layer over part of the TFBG. For a device length of 10 mm (and a diameter of 125 µm for easy insertion into microfluidic channels), the flow rates and the direction can be detectable unequivocally. The TFBG waveguiding properties allow such devices to function in liquids with refractive indices ranging from 1.33 to about 1.40. In addition, the proposed sensor can be made inherently temperature-insensitive by referencing all wavelengths to the wavelength of the core mode resonance of the grating, which is isolated from the fiber surroundings.

High-resolution interrogation of tilted fiber Bragg gratings using an extended range dual wavelength differential detection.

An extended range dual wavelength differential detection technique for interrogating fiber Bragg grating sensors is implemented for the measurement of tilted fiber Bragg gratings. The dynamic chirp of a single DFB laser diode modulated with a square wave is used to generate two pairs of wavelengths, in the high and low modulation states, with a separation approximately equal to the bandwidth of the TFBG, resulting in a doubling of the range of the DWDD measurement. A spectral resolution of 0.08 pm and a refractive index resolution of 9.9 × 10-6 are obtained over a range of refractive index of 3.7 × 10-2, corresponding to 11.9 bits of resolution.

Rapid Detection of Circulating Breast Cancer Cells Using a Multiresonant Optical Fiber Aptasensor with Plasmonic Amplification.

The detection of circulating tumor cells (CTCs), which are responsible for metastasis in several forms of cancer, represents an important goal in oncological diagnosis and treatment. These cells remain extremely challenging to detect, despite numerous previous studies, due to their low concentration (1-10 cells/mL of blood). In this work, an all-fiber plasmonic aptasensor featuring multiple narrowband resonances in the near-infrared wavelength range was developed to detect metastatic breast cancer cells. To this aim, specific aptamers against mammaglobin-A were selected and immobilized as receptors on the sensor surface. In vitro assays confirm that the label-free and real-time detection of cancer cells [limit of detection (LOD) of 49 cells/mL] occurs within 5 min, while the additional use of functionalized gold nanoparticles allows a 2-fold amplification of the biosensor response. Differential measurements on selected optical resonances were used to process the sensor response, and results were confirmed by microscopy. The detection of only 10 cancer cells/mL was achieved with relevant specificity against control cells and with quick response time.

Self-heating tilted fiber Bragg grating device for melt curve analysis of solid-phase DNA hybridization and thermal cycling.

We demonstrate a DNA-based optical fiber device that uses an in-fiber grating, a light absorbing coating with surface anchored DNA, and a built-in optical thermometer. This device is used for precisely thermal cycling surface DNA spots bound by a simple UV cross-linking technique. Near-infrared light of wavelengths near 1550 nm and guided power near 300 mW is coupled out of the fiber core by a tilted fiber Bragg grating inscribed in the fiber and absorbed by the coating to increase its temperature to more than 95 °C. A co-propagating broadband light signal (also in the near-infrared region) is used to measure the reflection spectrum of the grating and thus the temperature from the wavelength shifts of the reflection peaks. The device is capable of sensitive DNA melt analysis and can be used for DNA amplification. Graphical abstract.

Symmetry selective cladding modes coupling in ultrafast-written fiber Bragg gratings in two-mode fiber.

The lower order cladding mode resonances of a fiber Bragg grating (FBG) are sensitive to fiber bending but their spectral density makes their response to bending very complex. In this work we present a simple method to reduce and control the number of low order cladding mode resonances via FBGs written in a two-mode fiber (TMF) with an ultrafast laser. Owing to the larger core size of the TMF, a slight break of the cylindrical asymmetry of the grating patterns can be induced when using femtosecond side-irradiation with a small change in the writing condition. This allows us to control the mode families coupled by the grating, and in particular to those modes that have positive or negative bending responses along certain bend directions. Experimental results demonstrate that several lower-order neighboring-cladding mode pairs coupled by the asymmetric TMFBG have antagonistic loss responses (by several dB) for different bending directions, thus allowing full 2D bending measurements with many applications in shape sensing. Finally, this device has similar advantages as tilted FBGs, i.e. temperature de-correlation and the possibility of increasing the signal to noise ratio by averaging simultaneous measurements on several pairs of resonances.

Sample orientation in corona-poled multilayer silica structures.

The impact of sample orientation on the poling of single-sided multilayer silica structures is studied. The results show that the presence of a multilayer stack near the cathode creates a nonlinear region where it otherwise would not have formed. It is shown that field orientation impacts the location and magnitude of the induced nonlinearity. A nonlinearity is always present in the stack independent of whether the stack is on the anode or cathode side of the sample unlike the nonlinearity in bulk silica, which is always located on the anode side.

Cytokeratins Biosensing Using Tilted Fiber Gratings.

Optical fiber gratings have widely proven their applicability in biosensing, especially when they are coupled with antibodies for specific antigen recognition. While this is customarily done with fibers coated by a thin metal film to benefit from plasmonic enhancement, in this paper, we propose to study their intrinsic properties, developing a label-free sensor for the detection of biomarkers in real-time without metal coatings for surface plasmon resonances. We focus on the inner properties of our modal sensor by immobilizing receptors directly on the silica surface, and reporting the sensitivity of bare tilted fiber Bragg gratings (TFBGs) used at near infrared wavelengths. We test different strategies to build our sensing surface against cytokeratins and show that the most reliable functionalization method is the electrostatic adsorption of antibodies on the fiber, allowing a limit of detection reaching 14 pM by following the guided cladding modes near the cut-off area. These results present the biodetection performance that TFBGs bring through their modal properties for different functionalizations and data processing strategies.

Hypersensitivity and Applications of Cladding Modes of Optical Fibers Coated with Nanoscale Metal Layers.

Theoretical and experimental results are presented to show that the complex effective index of the modes of optical fibers coated with non-uniform metal coatings of gold, silver, copper, or palladium, with thicknesses between 0 and 20 nm, acquire a greatly enhanced sensitivity to various forms of perturbations. Thickness changes of less than 1 nm can be measured as well as the binding of record low concentrations of chemical and biochemical species.

Hydrogen peroxide and glucose concentration measurement using optical fiber grating sensors with corrodible plasmonic nanocoatings.

We propose and demonstrate hydrogen peroxide (H2O2) and glucose concentration measurements using a plasmonic optical fiber sensor. The sensor utilizes a tilted fiber Bragg grating (TFBG) written in standard single mode communication fiber. The fiber is over coated with an nm-scale film of silver that supports surface plasmon resonances (SPRs). Such a tilted grating SPR structure provides a high density of narrow spectral resonances (Q-factor about 105) that overlap with the broader absorption band of the surface plasmon waves in the silver film, thereby providing an accurate tool to measure small shifts of the plasmon resonance frequencies. The H2O2 to be detected acts as an oxidant to etch the silver film, which has the effect of gradually decreasing the SPR attenuation. The etching rate of the silver film shows a clear relationship with the H2O2 concentration so that monitoring the progressively increasing attenuation of a selected surface plasmon resonance over a few minutes enables us to measure the H2O2 concentration with a limit of detection of 0.2 µM. Furthermore, the proposed method can be applied to the determination of glucose in human serum for a concentration range from 0 to 12 mM (within the physiological range of 3-8 mM) by monitoring the H2O2 produced by an enzymatic oxidation process. The sensor does not require accurate temperature control because of the inherent temperature insensitivity of TFBG devices referenced to the core mode resonance. A gold mirror coated on the fiber allows the sensor to work in reflection, which will facilitate the integration of the sensor with a hypodermic needle for in vitro measurements. The present study shows that Ag-coated TFBG-SPR can be applied as a promising type of sensing probe for optical detection of H2O2 and glucose detection in human serum.

Optical spectral sweep comb liquid flow rate sensor.

In microfluidic chip applications, the flow rate plays an important role. Here we propose a simple liquid flow rate sensor by using a tilted fiber Bragg grating (TFBG) as the sensing element. As the water flows in the vicinity of the TFBG along the fiber axis direction, the TFBG's spectrum changes due to its contact with water. By comparing the time-swept spectra of the TFBG in water to that of the TFBG with water flowing over it, a spectral sweep comb was formed, and the flow rate can be detected by selecting a suitable sweeping frequency. The proposed sensor has a high Q-value of over 17,000 for the lower rate and a large detectable range from 0.0058 mm/s to 3.2 mm/s. And the calculated corresponding lower detectable flow rate of 0.03 nL/s is 3 orders magnitude better than that of the current fiber flowmeter. Meanwhile, the proposed sensor has the temperature self-compensation function for the variation of the external temperature. We believe that this simple configuration will open a research direction of the TFBG-deriving theory and configuration for lower flow rate measurements for microfluidic chip applications.