The development of sensitive graphene-based surface acoustic wave sensors for NO2 detection at room temperature.

Bilayer graphene (Bl-Gr) and sulphur-doped graphene (S-Gr) have been integrated with LiTaO3 surface acustic wave (SAW) sensors to enhance the performance of NO2 detection at room temperature. The sensitivity of the Bl-Gr SAW sensors toward NO2, measured at room temperature, was 0.29º/ppm, with a limit of detection of 0.068 ppm. The S-Gr SAW sensors showed 0.19º/ppm sensitivity and a limit of detection of 0.140 ppm. The origin of these high sensitivities was attributed to the mass loading and elastic effects of the graphene-based sensing materials, with surface changes caused by the absorption of the NO2 molecules on the sensing films. Although there are no significant differences regarding the sensitivity and detection limit of the two types of sensors, the measurements in the presence of interferent gases and various humidity conditions outlined much better selectivity and sensing performances towards NO2 gas for the Bl-Gr SAW sensors.

Hybrid nanomaterial-based indirect electrochemical sensing of glyphosate in surface water: a promising approach for environmental monitoring.

Glyphosate (GLY), a widely utilized pesticide, poses a significant threat to human health even at minute concentrations. In this study, we propose an innovative electrochemical sensor for the indirect detection of GLY in surface water samples. The sensor incorporates a nanohybrid material composed of multi-layer graphene decorated with gold nanoparticles (AuNPs), synthesized in a single-step electrochemical process. To ensure portability and on-site measurements, the sensor is developed on a screen-printed electrode, chosen for its integration and miniaturization capabilities. The proposed sensor demonstrates remarkable sensitivity and selectivity for GLY detection in surface water samples, with an exceptional limit of detection (LOD) of 0.03 parts per billion (ppb) in both buffer and surface water matrices. Moreover, it exhibits a remarkably high sensitivity of 0.15 µA ppb-1. This electrochemical sensor offers a promising approach for accurate GLY monitoring, addressing the urgent need for reliable pesticide detection in environmental samples. The proposed sensor showed high selectivity towards GLY, when analysed in the presence of other pesticides such as phosmet, chlorpyrifos and glufosinate-ammonium. The recovery percentages of GLY from spiked surface water samples were between 93.8 and 98.9%. The study's broader implications extend to revolutionizing the way environmental chemistry addresses pesticide contamination, water quality assessment, and sustainable management of environmental pollutants. By pushing the boundaries of detection capabilities and offering practical solutions, this research contributes to the advancement of knowledge and practices that are essential for preserving and protecting our environment.

Tuning the infrared resonance of thermal emission from metasurfaces working in near-infrared.

We simulated numerically and demonstrated experimentally that the thermal emittance of a metasurface consisting of an array of rectangular metallic meta-atoms patterned on a layered periodic dielectric structure grown on top of a metallic layer can be tuned by changing several parameters. The resonance frequency, designed to be in the near-infrared spectral region, can be tuned by modifying the number of dielectric periods, and the polarization and incidence angle of the incoming radiation. In addition, the absorbance/emittance value at the resonant wavelength can be tuned by modifying the orientation of meta-atoms with respect to the illumination direction.

UV-Nanoimprint and Deep Reactive Ion Etching of High Efficiency Silicon Metalenses: High Throughput at Low Cost with Excellent Resolution and Repeatability.

As metasurfaces begin to find industrial applications there is a need to develop scalable and cost-effective fabrication techniques which offer sub-100 nm resolution while providing high throughput and large area patterning. Here we demonstrate the use of UV-Nanoimprint Lithography and Deep Reactive Ion Etching (Bosch and Cryogenic) towards this goal. Robust processes are described for the fabrication of silicon rectangular pillars of high pattern fidelity. To demonstrate the quality of the structures, metasurface lenses, which demonstrate diffraction limited focusing and close to theoretical efficiency for NIR wavelengths λ ∈ (1.3 µm, 1.6 µm), are fabricated. We demonstrate a process which removes the characteristic sidewall surface roughness of the Bosch process, allowing for smooth 90-degree vertical sidewalls. We also demonstrate that the optical performance of the metasurface lenses is not affected adversely in the case of Bosch sidewall surface roughness with 45 nm indentations (or scallops). Next steps of development are defined for achieving full wafer coverage.

Recent Progress on Nanomaterials for NO2 Surface Acoustic Wave Sensors.

NO2 gas surface acoustic wave (SAW)sensors are under continuous development due to their high sensitivity, reliability, low cost and room temperature operation. Their integration ability with different receptor nanomaterials assures a boost in the performance of the sensors. Among the most exploited nano-materials for sensitive detection of NO2 gas molecules are carbon-based nanomaterials, metal oxide semiconductors, quantum dots, and conducting polymers. All these nanomaterials aim to create pores for NO2 gas adsorption or to enlarge the specific surface area with ultra-small nanoparticles that increase the active sites where NO2 gas molecules can diffuse. This review provides a general overview of NO2 gas SAW sensors, with a focus on the different sensors' configurations and their fabrication technology, on the nanomaterials used as sensitive NO2 layers and on the test methods for gas detection. The synthesis methods of sensing nanomaterials, their functionalization techniques, the mechanism of interaction between NO2 molecules and the sensing nanomaterials are presented and discussed.

Silicon Metalens Fabrication from Electron Beam to UV-Nanoimprint Lithography.

This study presents the design and manufacture of metasurface lenses optimized for focusing light with 1.55 µm wavelength. The lenses are fabricated on silicon substrates using electron beam lithography, ultraviolet-nanoimprint lithography and cryogenic deep reactive-ion etching techniques. The designed metasurface makes use of the geometrical phase principle and consists of rectangular pillars with target dimensions of height h = 1200 nm, width w = 230 nm, length l = 354 nm and periodicity p = 835 nm. The simulated efficiency of the lens is 60%, while the master lenses obtained by using electron beam lithography are found to have an efficiency of 45%. The lenses subsequently fabricated via nanoimprint are characterized by an efficiency of 6%; the low efficiency is mainly attributed to the rounding of the rectangular nanostructures during the pattern transfer processes from the resist to silicon due to the presence of a thicker residual layer.

Metasurface Fabrication by Cryogenic and Bosch Deep Reactive Ion Etching.

The research field of metasurfaces has attracted considerable attention in recent years due to its high potential to achieve flat, ultrathin optical devices of high performance. Metasurfaces, consisting of artificial patterns of subwavelength dimensions, often require fabrication techniques with high aspect ratios (HARs). Bosch and Cryogenic methods are the best etching candidates of industrial relevance towards the fabrication of these nanostructures. In this paper, we present the fabrication of Silicon (Si) metalenses by the UV-Nanoimprint Lithography method and cryogenic Deep Reactive Ion Etching (DRIE) process and compare the results with the same structures manufactured by Bosch DRIE both in terms of technological achievements and lens efficiencies. The Cryo- and Bosch-etched lenses attain efficiencies of around 39% at wavelength λ = 1.50 µm and λ = 1.45 µm against a theoretical level of around 61% (for Si pillars on a Si substrate), respectively, and process modifications are suggested towards raising the efficiencies further. Our results indicate that some sidewall surface roughness of the Bosch DRIE is acceptable in metalense fabrication, as even significant sidewall surface roughness in a non-optimized Bosch process yields reasonable efficiency levels.

Significance Testing and Multivariate Analysis of Datasets from Surface Plasmon Resonance and Surface Acoustic Wave Biosensors: Prediction and Assay Validation for Surface Binding of Large Analytes.

In this study, we performed uni- and multivariate data analysis on the extended binding curves of several affinity pairs: immobilized acetylcholinesterase (AChE)/bioconjugates of aflatoxin B1(AFB1) and immobilized anti-AFB1 monoclonal antibody/AFB1-protein carriers. The binding curves were recorded on three mass sensitive cells operating in batch configurations: one commercial surface plasmon resonance (SPR) sensor and two custom-made Love wave surface-acoustic wave (LW-SAW) sensors. We obtained 3D plots depicting the time-evolution of the sensor response as a function of analyte concentration using real-time SPR binding sensograms. These "calibration" surfaces exploited the transient periods of the extended kinetic curves, prior to equilibrium, creating a "fingerprint" for each analyte, in considerably shortened time frames compared to the conventional 2D calibration plots. The custom-made SAW sensors operating in different experimental conditions allowed the detection of AFB1-protein carrier in the nanomolar range. Subsequent statistical significance tests were performed on unpaired data sets to validate the custom-made LW-SAW sensors.