MXene-based kirigami designs: showcasing reconfigurable frequency selectivity in microwave regime.

Today's wireless environments, soft robotics, and space applications demand delicate design of devices with tunable performances and simple fabrication processes. Here we show strain-based adjustability of RF/microwave performance by applying frequency-selective patterns of conductive Ti3C2Tx MXene coatings on low-cost acetate substrates under ambient conditions. The tailored performances were achieved by applying frequency-selective patterns of thin Ti3C2Tx MXene coatings with high electrical conductivity as a replacement to metal on low-cost flexible acetate substrates under ambient conditions. Under quasi-axial stress, the Kirigami design enables displacements of individual resonant cells, changing the overall electromagnetic performance of a surface (i.e., array) within a simulated wireless channel. Two flexible Kirigami-inspired prototypes were implemented and tested within the S, C, and X (2-4 GHz, 4-8 GHz, and 8-12 GHz) microwave frequency bands. The resonant surface, having ~1/4 of the size of a standard A4 paper, was able to steer a beam of scattered waves from each resonator by ~25°. Under a strain of 22%, the resonant frequency of the wired co-planar resonator was shifted by 400 MHz, while the reflection coefficient changed by 158%. Deforming the geometry impacted the spectral response of the components across three arbitrary frequencies in the 4-10 GHz frequency range. With this proof of concept, we anticipate implementing thin films of MXenes on technologically relevant substrates, achieving multi-functionality through cost-effective and straightforward manufacturing.

Non-destructive erosive wear monitoring of multi-layer coatings using AI-enabled differential split ring resonator based system.

Unprotected surfaces where a coating has been removed due to erosive wear can catastrophically fail from corrosion, mechanical impingement, or chemical degradation, leading to major safety hazards, financial losses, and even fatalities. As a preventive measure, industries including aviation, marine and renewable energy are actively seeking solutions for the real-time and autonomous monitoring of coating health. This work presents a real-time, non-destructive inspection system for the erosive wear detection of coatings, by leveraging artificial intelligence enabled microwave differential split ring resonator sensors, integrated to a smart, embedded monitoring circuitry. The differential microwave system detects the erosion of coatings through the variations of resonant characteristics of the split ring resonators, located underneath the coating layer while compensating for the external noises. The system's response and performance are validated through erosive wear tests on single- and multi-layer polymeric coatings up to a thickness of 2.5 mm. The system is capable of distinguishing which layer is being eroded (for multi-layer coatings) and estimating the wear depth and rate through its integration with a recurrent neural network-based predictive analytics model. The synergistic combination of artificial intelligence enabled microwave resonators and a smart monitoring system further demonstrates its practicality for real-world coating erosion applications.

A Microwave Voyage into Swelling Phenomenon: Investigation of Polydimethylsiloxane and VOCs Interaction.

When exposed to specific gases, polymers undergo swelling, leading to physiochemical changes that can significantly affect their performance. Monitoring this swelling phenomenon requires innovative approaches. This study focuses on investigating the real-time resonant microwave behavior of two polydimethylsiloxane (PDMS) structures (solid and porous) in interaction with tetrahydrofuran (THF) and acetone, which are primary swelling agents. A microwave measurement method is proposed using an 8.63 GHz planar split ring resonator (SRR). The device's resonant frequency downshifts to 7.75 and 8.42 GHz when solid and porous PDMS blocks are placed on the split ring gap. Interaction of the solid PDMS and porous PDMS with target gases caused a change in PDMS structure resulting in alterations in the dielectric properties of the PDMS/gas system, as evidenced by the resonator's transmission amplitude and resonant frequency shifts. The magnitude of these shifts depends on the type and concentration of the solvent gas. The PDMS-integrated SRR exhibits a sensitivity of 25.3 MHz/1 ppt THF and 7 MHz/1 ppt acetone. Additionally, the solid block demonstrates response times of 6800 and 4200 s for swelling and deswelling, respectively, when in exposure to 25 ppt concentrations of THF and acetone. Overall, this study underscores the substantial potential of microwave resonators as versatile tools for investigating the physical changes in polymers during their interaction with gases, contributing to the understanding of polymer-gas interactions and opening avenues for further research and diverse applications.

MXene Free Standing Films: Unlocking the Impact of Flake Sizes in Microwave Resonant Structures in Humid Environments.

Microwave communication devices necessitate elements with high electrical conductivity, a property which was traditionally found in metals (e.g., copper). However, in applications such as satellite communications, metals prevent the payload from achieving lightweight and flexible characteristics. Here, we demonstrate the development of MXene film microwave resonators, leveraging MXene's high electrical conductivity and unique mechanical properties. To investigate resonant performance in humid conditions and study the effects of MXene's processing and treatment, MXene films with different flake sizes are prepared and exposed to cyclic humidity. For the large- and small-flake Ti3 C2 MXene films in cyclic humidity, the large-flake film demonstrates higher electrical conductivity, higher resonance quality factor (150 and 35 as unloaded, and loaded), and less fluctuation of performance (≈1.7% total shift in resonance frequency). Further, by implementing MXene films of two different diameters, the correlation between film size and resonant frequency is demonstrated. By introducing an active resonant configuration, the effect of MXene degradation and microwave losses can be compensated. This active feedback loop demonstrates a ≈300 times increase in the quality factor of MXene resonators. As a building block for terrestrial and satellite communication modules, MXene resonators potentiate the replacement of metals in achieving unique electrical and mechanical properties.

Gigahertz-Based Visible Light Detection Enabled via CdS-Coated TiO2 Nanotube Layers.

Detection of visible light is a key component in material characterization techniques and often a key component of quality or purity control analyses for health and safety applications. Here in this work, to enable visible light detection at gigahertz frequencies, a planar microwave resonator is integrated with high aspect ratio TiO2 nanotube (TNT) layer-sensitized CdS coating using the atomic layer deposition (ALD) technique. This unique method of visible light detection with microwave-based sensing improves integration of the light detection devices with digital technology. The designed planar microwave resonator sensor was implemented and tested with resonant frequency between 8.2 and 8.4 GHz and a resonant amplitude between -15 and -25 dB, depending on the wavelength of the illuminated light illumination on the nanotubes. The ALD CdS coating sensitized the nanotubes in visible light up to ∼650 nm wavelengths, as characterized by visible spectroscopy. Furthermore, CdS-coated TNT layer integration with the planar resonator sensor allowed for development of a robust microwave sensing platform with improved sensitivity to green and red light (60 and 1300%, respectively) compared to the blank TNT layers. Moreover, the CdS coating of the TNT layer enhanced the sensor's response to light exposure and resulted in shorter recovery times once the light source was removed. Despite having a CdS coating, the sensor was capable of detecting blue and UV light; however, refining the sensitizing layer could potentially enhance its sensitivity to specific wavelengths of light in certain applications.

Smart low interfacial toughness coatings for on-demand de-icing without melting.

Ice accretion causes problems in vital industries and has been addressed over the past decades with either passive or active de-icing systems. This work presents a smart, hybrid (passive and active) de-icing system through the combination of a low interfacial toughness coating, printed circuit board heaters, and an ice-detecting microwave sensor. The coating's interfacial toughness with ice is found to be temperature dependent and can be modulated using the embedded heaters. Accordingly, de-icing is realized without melting the interface. The synergistic combination of the low interfacial toughness coating and periodic heaters results in a greater de-icing power density than a full-coverage heater system. The hybrid de-icing system also shows durability towards repeated icing/de-icing, mechanical abrasion, outdoor exposure, and chemical contamination. A non-contact planar microwave resonator sensor is additionally designed and implemented to precisely detect the presence or absence of water or ice on the surface while operating beneath the coating, further enhancing the system's energy efficiency. Scalability of the smart coating is demonstrated using large (up to 1 m) iced interfaces. Overall, the smart hybrid system designed here offers a paradigm shift in de-icing that can efficiently render a surface ice-free without the need for energetically expensive interface melting.

Flexible, robust, and high-performance gas sensors based on lignocellulosic nanofibrils.

Gas detection in flexible electronics demands novel materials with superior sensing performance that have high mechanically strength, are flexible, low-cost, and sustainable. We explore a composite sensing nanopaper based on lignocellulosic cellulose nanofibrils (LCNF) as a renewable and mechanically strong substrate that enables the fabrication of flexible, and highly sensitive gas sensors. In the system the hydrophobic lignin covalently bonds to cellulose in the nanofibrils, increasing the nanopaper water-resistance and limiting sensing materials response to humidity. The sensor is composed of polyaniline (PANI) grown on flexible LCNF and reduced graphene oxide (rGO) nanosheets. The proposed structure, at 10 wt% rGO, demonstrated a 10-fold improvement in sensitivity to volatile amines (i.e. ammonia detection down to 1 ppm) while maintaining an acceptable selectivity. Furthermore, we demonstrated the application of the sensing nanopaper in a microwave sensor that paves the path toward flexible, wireless, and high-performance sensing devices.

High-Frequency TiO2 Nanotube-Adapted Microwave Coplanar Waveguide Resonator for High-Sensitivity Ultraviolet Detection.

Ultraviolet (UV) sensors are a key component in growing applications such as water quality treatment and environmental monitoring, with considerable interest in their miniaturization and enhanced operation. This work presents a passive gold coplanar waveguide split ring resonator integrated with anodic self-organized TiO2 nanotube (TNT) membranes with a thickness of 20 µm to provide real-time UV detection. The resonator operated as a one-port device to capture the reflection coefficient (S11) signal, with a center frequency of 16 GHz and a notch amplitude of -88 dB. It was experimentally analyzed for its UV sensing capability in the range of 36.5-463 µW/cm2. The high-frequency resonator was improved through design choices including the addition of a tapered input transmission line, wire bonding for practical device design, and an interdigitated capacitive ring gap. The high frequency also helped mitigate noise due to water vapor or environmental contaminants. S11 amplitude variation was found through both experiments and modeling to follow a linear trend with UV illumination intensity. The resonator exhibited over 45 ± 2 dB shift in the resonant amplitude under the highest UV illumination conditions, with a sensitivity of 0.084 dB/µW cm-2 and the potential to sense UV intensity as low as 2.7 µW/cm2. The presented device enabled a repeatable and accurate microwave response under UV illumination with very high sensitivity, entirely through the use of passive circuit elements.

Patch antenna sensor for wireless ice and frost detection.

A patch antenna sensor with T-shaped slots operating at 2.378 GHz was developed and investigated for wireless ice and frost detection applications. Detection was performed by monitoring the resonant amplitude and resonant frequency of the transmission coefficient between the antenna sensor and a wide band receiver. This sensor was capable of distinguishing between frost, ice, and water with total shifts in resonant frequency of 32 MHz and 36 MHz in the presence of frost and ice, respectively, when compared to the bare sensor. Additionally, the antenna was sensitive to both ice thickness and the surface area covered in ice displaying resonant frequency shifts of 2 MHz and 8 MHz respectively between 80 and 160 µL of ice. By fitting an exponential function to the recorded data, the freezing rate was also extracted. The analysis within this work distinguishes the antenna sensor as a highly accurate and robust method for wireless ice accretion detection and monitoring. This technology has applications in a variety of industries including the energy sector for detection of ice on wind turbines and power lines.

Smart Superhydrophobic Textiles Utilizing a Long-Range Antenna Sensor for Hazardous Aqueous Droplet Detection plus Prevention.

This paper demonstrates the feasibility of a long-range antenna sensor embedded underneath a liquid repellent fabric to be employed as a wearable sensor in personal protective fabrics. The sensor detects and monitors hazardous aqueous liquids on the outer layer of fabrics, to add an additional layer of safety for professionals working in hazardous environments. A modified patch antenna was designed to include a meandering-shaped resonant structure, which was embedded underneath the fabric. Superhydrophobic fabrics were prepared using silica nanoparticles and a low-surface-energy fluorosilane. 4 to 20 µL droplets representing hazardous aqueous solutions were drop-cast on the fabrics to investigate the performance of the embedded antenna sensor. Long-range (S21) measurements at a distance of 2-3 m were performed using the antenna sensor with treated and untreated fabrics. The antenna sensor successfully detected the liquid for both types of fabrics. The resonant frequency sensitivity of the antenna sensor underneath the treated fabric exhibiting superhydrophobicity was measured as 370 kHz/µL, and 1 MHz/µL for the untreated fabric. The results demonstrate that the antenna sensor is a good candidate for wearable hazardous aqueous droplet detection on fabrics.

Graphene oxide/polyaniline-based microwave split-ring resonator: A versatile platform towards ammonia sensing.

Ammonia gas sensors have always received significant attention as robust platforms for emission control, food safety, and monitoring human exhaled breath for the early diagnosis of diseases such as dysfunction of the kidney and liver. This study explores the development of a microwave-based split-ring resonator (SRR) sensor with enhanced sensitivity to detect ammonia gas at low concentrations. The sensor is based on a nanocomposite fabricated by incorporating 10 wt% of graphene oxide (GO) into polyaniline (PANI) via the in-situ polymerization of aniline monomers over the surface of the GO sheets. The addition of GO to PANI results in a high sensitivity of 0.038 dB ppm-1 for low concentrations (1-25 ppm) and 0.0045 dB ppm-1 for high concentrations (> 25 ppm) of ammonia gas, in a 150-400 s time interval at room temperature. The prepared sensor can selectively sense ammonia gas in the presence of other higher concentrations of hazardous gases and a wide range of relative humidity levels (15-90%). The response signal is repeatable after 30 days with less than 0.32% deviation. The developed low-cost and robust sensor has the potential to monitor ammonia gas in various applications, including medical, environmental, food, and agricultural sectors.

Microwave resonator array with liquid metal selection for narrow band material sensing.

A microwave resonator array is integrated with liquid metal to select an individual resonator response within a resonator array, enabling simple and accurate analysis for dielectric sensing. Galinstan, a liquid metal, acts as a multiplexer by inducing a capacitive load to the nearby resonator, lowering its resonant frequency, and thereby isolating its resonant response from other resonators in the array. The liquid metal could be positioned within a fluidic channel to be above any of the resonators, which tuned the resonant frequency from 3.9 to 3.3 GHz where it can be analyzed individually. The resonators showed a consistent response to liquid metal tuning, with tuning error measured below 30 MHz (5%). The sensor also exhibited stable sensitivity to test materials placed on the selected resonator, with a maximum resonant frequency shift of 300 MHz for a dielectric test material (ε = 10.2) and almost no variation in resonant amplitude. The selected resonant response was only sensitive to materials on the selected resonator, and was unaffected by test materials, even when placed on other resonators. The presented design enabled robust and accurate detection of materials using planar microwave resonators that can be controlled at a user's convenience, specifically for use in systems where multiple parameters or system settings may need to be individually determined.

Modified Microwave Sensor with a Patterned Ground Heater for Detection and Prevention of Ice Accumulation.

Ice accumulation on aircraft is known to negatively impact the aerodynamic and mechanical operation, sometimes resulting in catastrophic failure. Recently, microwave resonators have gained interest as durable and reliable frost and ice detectors. Here, a microwave resonator sensor with built-in heating capability patterned into the ground plane was designed, fabricated, and tested to investigate real-time ice and frost growth. Sensing was performed on surfaces with anti-icing coatings to quantitatively analyze the effectiveness of these materials. The sensor was also tested to determine its ability to evaluate different deicing methods. The sensor itself was a split-ring resonator (SRR) operating at 5.82 GHz, which could effectively distinguish between water and ice by detecting changes in the dielectric properties on or around its surface. This application was particularly suited for an SRR due to the extreme difference between the relative permittivity of water (ε = 90) and ice (ε = 3.2) at 5 GHz and 0 °C. The results from this sensor can be used to determine the holdover time of various coatings to resist ice formation. This study validates the use of SRRs as ice detection sensors for applications where ice and frost are of great interest, such as on aircraft, roads, or walkways.

Kirigami-Enabled Microwave Resonator Arrays for Wireless, Flexible, Passive Strain Sensing.

Wireless and highly sensitive flexible strain sensors would have widespread application across a number of different fields. Here, the novel combination of two different metamaterials, one mechanical and one electronic, is demonstrated for its potential as such a sensor. An array of split-ring resonators (SRRs) were mounted on a bespoke kirigami sheet. The hybrid kirigami structure was designed specifically for the resonator array, in terms of both its physical dimensions and elastic response. Mechanical tests in concert with finite element modeling confirmed that the hybrid kirigami structure, containing two disparate kirigami motifs, exhibited a high range of strain and out-of-plane rotation without plastic deformation. The microwave sensing was designed to monitor variations in the S11 response of the resonators as a function of out-of-plane kirigami hinge rotation. The mounted array of SRRs on the hybrid kirigami sheet could wirelessly detect changes in strain with high sensitivity (>30 MHz shift in resonant frequency; >30 dB shift in resonant amplitude) over a large range of strain, from 0.6 to 21.3%.

Highly Sensitive and Contactless Ammonia Detection Based on Nanocomposites of Phosphate-Functionalized Reduced Graphene Oxide/Polyaniline Immobilized on Microstrip Resonators.

Ammonia is a key compound in a variety of industrial sectors, including automotive, chemical, and food. Its hazardous effects on the environment and human health require the implementation of proper safety guidelines and monitoring techniques. An attractive approach is to add sensing functionality to low-cost wireless communication devices to allow for the monitoring/mapping of the chemical environment across a large area. This study outlines a highly sensitive contactless ammonia gas sensor with the potential for continuous and wireless mapping of ammonia emissions by integrating an antenna on the device. The devices were fabricated by casting a novel advanced sensing nanocomposite, polyaniline (PANI), and phosphate-functionalized reduced graphene oxide (P-rGO) on split-ring resonators (SRRs). P-rGO incorporation in PANI produced a positive-sensing synergistic effect to multiply the sensing response severalfold to ammonia and dimethylamine gases. Furthermore, we identified that the modification of the semiconductive behavior of the nanosheets, achieved via phosphate functionalization, is the key factor to the positive-sensing synergy observed in the nanocomposites because of the formation of localized heterojunctions. The prepared SRRs exhibited remarkably a low detection limit, ∼1 ppm, to ammonia gas, as well as good stability and selectivity, which paves the path for a novel generation of wireless, chipless, potentially fully printable, and passive sensor platforms.

Distinguishing between Deep Trapping Transients of Electrons and Holes in TiO2 Nanotube Arrays Using Planar Microwave Resonator Sensor.

A large signal direct current (DC) bias and a small signal microwave bias were simultaneously applied to TiO2 nanotube membranes mounted on a planar microwave resonator. The DC bias modulated the electron concentration in the TiO2 nanotubes and was varied between 0 and 120 V in this study. Transients immediately following the application and removal of DC bias were measured by monitoring the S-parameters of the resonator as a function of time. The DC bias stimulated Poole-Frenkel-type trap-mediated electrical injection of excess carriers into TiO2 nanotubes, which resulted in a near-constant resonant frequency but a pronounced decrease in the microwave amplitude due to free electron absorption. When ultraviolet illumination and DC bias were both present and then stepwise removed, the resonant frequency shifted due to trapping-mediated change in the dielectric constant of the nanotube membranes. Characteristic lifetimes of 60-80, 300-800, and ∼3000 s were present regardless of whether light or bias was applied and were also observed in the presence of a hole scavenger, which we attributed to oxygen adsorption and deep electron traps, whereas another characteristic lifetime >8000 s was only present when illumination was applied, and is attributed to the presence of hole traps.

Ultraviolet sensing using a TiO2 nanotube integrated high resolution planar microwave resonator device.

This paper presents a unique integrated UV light sensing concept and introduces a device with a detection limit of 1.96 nW cm-2. The combination of a high quality factor, a microwave planar resonator (Q ∼ 50 000) with a semiconducting nanomaterial enables a revolutionary potential paradigm for photodetection of low light intensities and small form factors. The presenting device employs a high-resolution microwave microstrip resonator as the signal transducer to convert the variant dielectric properties (permittivity and conductivity) of the nanotube membrane into electrical signals such as the resonant frequency, quality factor and resonant amplitude. The microwave resonator has an active feedback loop to improve the initial quality factor of the resonator from 200 to 50 000 and leads to boosting of the sensing resolution by orders of magnitude. Anatase TiO2 nanotubes are assembled on the surface of the microwave resonator. Upon exposure to UV light, electron-hole pair generation, trapping and recombination in the nanotubes are exploited as a unique signature to quantify the UV light intensity. The change of dielectric properties of the nanotube membrane is monitored using the underlying active microwave resonator. The proposed concept enables the detection and monitoring of UV light at high resolution, with very small exposure power and integrated form factors.

A Novel Technique for Determining the Adsorption Capacity and Breakthrough Time of Adsorbents Using a Noncontact High-Resolution Microwave Resonator Sensor.

A newly developed noncontact high-resolution real-time microwave sensor was used to determine the breakthrough time and adsorption capacity of adsorbents/adsorbates with different dielectric properties. The sensor is a microwave microstrip planar resonator with an enhanced quality factor using a regenerative feedback loop operating at 1.4 GHz and an adjustable quality factor of 200-200000. Beaded activated carbon (BAC, microwave-absorbing) and a polymeric adsorbent (V503, microwave transparent) were completely loaded with 1,2,4-trimethylbenzene (nonpolar) or 2-butoxyethanol (polar). During adsorption, variations in the dielectric properties of the adsorbents were monitored using two microwave parameters; quality factor and resonant frequency. Those parameters were related to adsorption breakthrough time and capacity. Adsorption tests were completed at select relative pressures (0.03, 0.1, 0.2, 0.4, and 0.6) of adsorbates in the influent stream. For all experiments, the difference between the breakthrough time (t5%) and the settling time of the quality factor variation (time that the quality factor was 0.95 of its final value) was <5%. Additionally, a linear relationship between the final value of the resonant frequency shift and adsorption capacity was observed. The proposed noncontact sensor can be used to determine the breakthrough time and adsorption capacity.

Effect of phosphonate monolayer adsorbate on the microwave photoresponse of TiO2 nanotube membranes mounted on a planar double ring resonator.

In this study, the effects of a phosphonate molecular monolayer adsorbed on the surface of a free-standing self-organized TiO2 nanotube membrane, on the microwave photoresponse of the membrane are presented. This phenomenon is monitored using planar microwave sensors. A double ring resonator is utilized to monitor the permittivity and conductivity variation on the monolayer coated membrane and the sensor environment separately. It is shown that the rise time and subsequent decay of the amplitude (A), resonance frequency (f 0) and quality factor (Q) of the resonator depend on the existence and the type of the monolayer coating the membrane. Three different monolayers of n-decylphosphonic acid (DPA), 1H, 1H', 2H, 2H'-perfluorodecyl phosphonic acid (PFDPA) and 16-phosphonohexadecanoic acid adsorbed on the titania nanotube membrane are investigated while monitoring their microwave properties during the illumination time period and in the relaxation period, which demonstrate different behavior in comparison to each other and to the bare nanotube membrane layer. The effect of humidity on the TiO2 nanotube membrane with and without different monolayers is also studied and the results demonstrate distinguishable microwave responses. While each of the monolayer-coated membranes exhibited an attenuation of the photo-induced change in A, f 0 and Q with respect to the bare membrane, PFDPA-coated membranes showed the smallest relative change in the monitored microwave parameters upon ultraviolet illumination and upon the introduction of different levels of humidity. These effects are explained on the basis of surface trap passivation by the monolayers as well as the hydrophobicity of the monolayers. Our work also shows how the interactions of self-assembled monolayers with charge carriers and surface states on metal oxides may be used to indirectly sense their presence through measurement of the microwave response.