Replicating Spectral Baseline for Unambiguous Frequency Locking in Resonant Sensors.

Electrothermal piezoresistive resonant cantilever sensors have been fabricated with embedded actuating (heating resistor) and sensing (piezo resistors) parts, with the latter configured in a Wheatstone bridge circuit. Due to the close spacing between these two elements, a direct thermal parasitic effect on the resonant sensor during the actuating-sensing process leads to asymmetric amplitude and reversing phase spectral responses. Such a condition affects the precise determination of the cantilever's resonant frequency, f0. Moreover, in the context of phase-locked loop-based (PLL) resonance tracking, a reversing phase spectral response hinders the resonance locking due to its ambiguity. In this work, a replica of the baseline spectral was applied to remove the thermal parasitic effect on the resonance spectra of the cantilever sensor, and its capability was simulated through mathematical analysis. This replica spectral was subtracted from the parasitized spectral using a particular calculation, resulting in optimized spectral responses. An assessment using cigarette smoke particles performed a desired spectral shifting into symmetrical amplitude shapes and monotonic phase transitions, subsequently allowing for real-time PLL-based frequency tracking.

Unlocking High-Current Performance in Silicon Anode: Synergistic Phosphorus Doping and Nitrogen-Doped Carbon Encapsulation to Enhance Lithium Diffusivity.

The silicon (Si) offers enormous theoretical capacity as a lithium-ion battery (LIB) anode. However, the low charge mobility in Si particles hinders its application for high current loading. In this study, ball-milled phosphorus-doped Si nanoparticles encapsulated with nitrogen-doped carbon (P-Si@N-C) are employed as an anode for LIBs. P-doped Si nanoparticles are first obtained via ball-milling and calcination of Si with phosphoric acid. N-doped carbon encapsulation is then introduced via carbonization of the surfactant-assisted polymerization of pyrrole monomer on P-doped Si. While P dopant is required to support the stability at high current density, the encapsulation of Si particles with N-doped carbon is influential in enhancing the overall Li+ diffusivity of the Si anode. The combined approaches improve the anode's Li+ diffusivity up to tenfold compared to the untreated anode. It leads to exceptional anode stability at a high current, retaining 87 % of its initial capacity under a large current rate of 4000 mA g-1. The full-cell comprising P-Si@N-C anode and LiFePO4 cathode demonstrates 94 % capacity retention of its initial capacity after 100 cycles at 1 C. This study explores the effective strategies to improve Li+ diffusivity for high-rate Si-based anode.

Area-Selective Growth of Zinc Oxide Nanowire Arrays for Piezoelectric Energy Harvesting.

In this work, we present the area-selective growth of zinc oxide nanowire (NW) arrays on patterned surfaces of a silicon (Si) substrate for a piezoelectric nanogenerator (PENG). ZnO NW arrays were selectively grown on patterned surfaces of a Si substrate using a devised microelectromechanical system (MEMS)-compatible chemical bath deposition (CBD) method. The fabricated devices measured a maximum peak output voltage of ~7.9 mV when a mass of 91.5 g was repeatedly manually placed on them. Finite element modeling (FEM) of a single NW using COMSOL Multiphysics at an applied axial force of 0.9 nN, which corresponded to the experimental condition, resulted in a voltage potential of -6.5 mV. The process repeated with the same pattern design using a layer of SU-8 polymer on the NWs yielded a much higher maximum peak output voltage of ~21.6 mV and a corresponding peak power density of 0.22 µW/cm3, independent of the size of the NW array. The mean values of the measured output voltage and FEM showed good agreement and a nearly linear dependence on the applied force on a 3 × 3 µm2 NW array area in the range of 20 to 90 nN.

Linear extrapolation method based on multiple equiproportional models for thermal performance prediction of ultra-large array.

Strong demand for developing the photothermal (PT) and electrothermal devices with ultra-large array is increasing. Thermal performance prediction is vital to optimize the key properties of the devices with ultra-large array. Finite element method (FEM) provides a powerful numerical approach for solving complex thermophysics issues. However, for calculating the performance of devices with ultra-large array, it is very memory-consuming and time-consuming to build an equal scale three-dimensional (3D) FEM model. For an ultra-large periodic array irradiated with a local heating source, the use of periodic boundary conditions could lead to considerable errors. To solve this problem, a linear extrapolation method based on multiple equiproportional models (LEM-MEM) is proposed in this paper. The proposed method builds several reduced-size FEM models to carry out simulation and extrapolation, which avoids dealing with the ultra-large arrays directly and greatly reduces the computation consumption. To verify the accuracy of LEM-MEM, a PT transducer with beyond 4000 × 4000 pixels is proposed, fabricated, tested and compared with the prediction results. Four different pixel patterns are designed and fabricated to test their steady thermal properties. The experimental results demonstrate that LEM-MEM has great predictability, and the maximum percentage error of average temperature is within 5.22% in four different pixel patterns. In addition, the measured response time of the proposed PT transducer is within 2 ms. The proposed LEM-MEM not only provides design guidance for optimizing PT transducers, but is also very useful for other thermal engineering problems in ultra-large array that requires facile and efficient prediction strategy.

Damped Cantilever Microprobes for High-Speed Contact Metrology with 3D Surface Topography.

We addressed the coating 5 mm-long cantilever microprobes with a viscoelastic material, which was intended to considerably extend the range of the traverse speed during the measurements of the 3D surface topography by damping contact-induced oscillations. The damping material was composed of epoxy glue, isopropyl alcohol, and glycerol, and its deposition onto the cantilever is described, as well as the tests of the completed cantilevers under free-oscillating conditions and in contact during scanning on a rough surface. The amplitude and phase of the cantilever's fundamental out-of-plane oscillation mode was investigated vs. the damping layer thickness, which was set via repeated coating steps. The resonance frequency and quality factor decreased with the increasing thickness of the damping layer for both the free-oscillating and in-contact scanning operation mode, as expected from viscoelastic theory. A very low storage modulus of E'≈100kPa, a loss modulus of E″≈434kPa, and a density of ρ≈1.2gcm-3 were yielded for the damping composite. Almost critical damping was observed with an approximately 130 µm-thick damping layer in the free-oscillating case, which was effective at suppressing the ringing behavior during the high-speed in-contact probing of the rough surface topography.

A Free-Standing Polyaniline/Silicon Nanowire Forest as the Anode for Lithium-ion Batteries.

Despite its high theoretical capacity, silicon anode has limited intrinsic conductivity and experiences significant volume changes during charge-discharge. To overcome these issues, facile metal-assisted chemical etching and in-situ polymerization of aniline are employed to produce a dense 1D polyaniline/silicon nanowire forest without noticeable agglomeration as a free-standing anode for lithium-ion batteries. This hybrid electrode possesses high cycling performance, delivering a stable capacity capped at 2 mAh cm-2 for 346 cycles of charge-discharge. Maximum capacity of 2 mAh cm-2 is also achievable at high-rate cell testing of 2 mA cm-2 , which cannot be obtained by the anode with plain silicon wafer and silicon nanowire only. The introduction of polyaniline on the silicon nanowire is shown to reduce the solid electrolyte interface (SEI) resistance, stabilize the SEI layer, further alleviate the effect of volume changes, and boost the conductivity of the hybrid anode, resulting in the high electrochemical performance of the anode.

Using a Tip Characterizer to Investigate Microprobe Silicon Tip Geometry Variation in Roughness Measurements.

Given their superior dynamics, microprobes represent promising probe candidates for high-speed roughness measurement applications. Their disadvantage, however, lies in the fact that the volume of the microprobe's silicon tip decreases dramatically during roughness measurement, and the unstable tip geometry leads to an increase in measurement uncertainty. To investigate the factors that influence tip geometry variation during roughness measurement, a rectangular-shaped tip characterizer was employed to characterize the tip geometry, and a method for reconstructing the tip geometry from the measured profile was introduced. Experiments were conducted to explore the ways in which the tip geometry is influenced by tip wear, probing force, and the relative movement of the tip with respect to the sample. The results indicate that tip fracture and not tip wear is the main reason for tip volume loss, and that the lateral dynamic load on the tip during scanning mode is responsible for more tip fracture than are other factors.

Vertically Aligned n-Type Silicon Nanowire Array as a Free-Standing Anode for Lithium-Ion Batteries.

Due to its high theoretical specific capacity, a silicon anode is one of the candidates for realizing high energy density lithium-ion batteries (LIBs). However, problems related to bulk silicon (e.g., low intrinsic conductivity and massive volume expansion) limit the performance of silicon anodes. In this work, to improve the performance of silicon anodes, a vertically aligned n-type silicon nanowire array (n-SiNW) was fabricated using a well-controlled, top-down nano-machining technique by combining photolithography and inductively coupled plasma reactive ion etching (ICP-RIE) at a cryogenic temperature. The array of nanowires ~1 µm in diameter and with the aspect ratio of ~10 was successfully prepared from commercial n-type silicon wafer. The half-cell LIB with free-standing n-SiNW electrode exhibited an initial Coulombic efficiency of 91.1%, which was higher than the battery with a blank n-silicon wafer electrode (i.e., 67.5%). Upon 100 cycles of stability testing at 0.06 mA cm-2, the battery with the n-SiNW electrode retained 85.9% of its 0.50 mAh cm-2 capacity after the pre-lithiation step, whereas its counterpart, the blank n-silicon wafer electrode, only maintained 61.4% of 0.21 mAh cm-2 capacity. Furthermore, 76.7% capacity retention can be obtained at a current density of 0.2 mA cm-2, showing the potential of n-SiNW anodes for high current density applications. This work presents an alternative method for facile, high precision, and high throughput patterning on a wafer-scale to obtain a high aspect ratio n-SiNW, and its application in LIBs.

Versatilely tuned vertical silicon nanowire arrays by cryogenic reactive ion etching as a lithium-ion battery anode.

Production of high-aspect-ratio silicon (Si) nanowire-based anode for lithium ion batteries is challenging particularly in terms of controlling wire property and geometry to improve the battery performance. This report demonstrates tunable optimization of inductively coupled plasma reactive ion etching (ICP-RIE) at cryogenic temperature to fabricate vertically-aligned silicon nanowire array anodes with high verticality, controllable morphology, and good homogeneity. Three different materials [i.e., photoresist, chromium (Cr), and silicon dioxide (SiO2)] were employed as masks during the subsequent photolithography and cryogenic ICP-RIE processes to investigate their effects on the resulting nanowire structures. Silicon nanowire arrays with a high aspect ratio of up to 22 can be achieved by tuning several etching parameters [i.e., temperature, oxygen/sulfur hexafluoride (O2/SF6) gas mixture ratio, chamber pressure, plasma density, and ion energy]. Higher compressive stress was revealed for longer Si wires by means of Raman spectroscopy. Moreover, an anisotropy of lattice stress was found at the top and sidewall of Si nanowire, indicating compressive and tensile stresses, respectively. From electrochemical characterization, half-cell battery integrating ICP-RIE-based silicon nanowire anode exhibits a capacity of 0.25 mAh cm-2 with 16.67% capacity fading until 20 cycles, which has to be improved for application in future energy storage devices.

In-Line Measurement of the Surface Texture of Rolls Using Long Slender Piezoresistive Microprobes.

Long slender piezoresistive silicon microprobes are a new type of sensor for measurement of surface roughness. Their advantage is the ability to measure at speeds of up to 15 mm/s, which is much faster than conventional stylus probes. The drawbacks are their small measurement range and tendency to break easily when deflected by more than the allowed range of 1 mm. In this article, previously developed microprobes were tested in the laboratory to evaluate their metrological properties, then tested under industrial conditions. There are several industrial measurement applications in which microprobes are useful. Measurement of the roughness of paper machine rolls was selected for testing in this study. The integration of a microprobe into an existing roll measurement device is presented together with the measurement results. The results are promising, indicating that measurements using a microprobe can give useful data on the grinding process.

Performance of an Electrothermal MEMS Cantilever Resonator with Fano-Resonance Annoyance under Cigarette Smoke Exposure.

An electrothermal piezoresistive cantilever (EPC) sensor is a low-cost MEMS resonance sensor that provides self-actuating and self-sensing capabilities. In the platform, which is of MEMS-cantilever shape, the EPC sensor offers several advantages in terms of physical, chemical, and biological sensing, e.g., high sensitivity, low cost, simple procedure, and quick response. However, a crosstalk effect is generated by the coupling of parasitic elements from the actuation part to the sensing part. This study presents a parasitic feedthrough subtraction (PFS) method to mitigate a crosstalk effect in an electrothermal piezoresistive cantilever (EPC) resonance sensor. The PFS method is employed to identify a resonance phase that is, furthermore, deployed to a phase-locked loop (PLL)-based system to track and lock the resonance frequency of the EPC sensor under cigarette smoke exposure. The performance of the EPC sensor is further evaluated and compared to an AFM-microcantilever sensor and a commercial particle counter (DC1100-PRO). The particle mass-concentration measurement result generated from cigarette-smoke puffs shows a good agreement between these three detectors.

Ultrafine Aerosol Particle Sizer Based on Piezoresistive Microcantilever Resonators with Integrated Air-Flow Channel.

To monitor airborne nano-sized particles (NPs), a single-chip differential mobility particle sizer (DMPS) based on resonant micro cantilevers in defined micro-fluidic channels (µFCs) is introduced. A size bin of the positive-charged fraction of particles herein is separated from the air stream by aligning their trajectories onto the cantilever under the action of a perpendicular electrostatic field of variable strength. We use previously described µFCs and piezoresistive micro cantilevers (PMCs) of 16 ng mass fabricated using micro electro mechanical system (MEMS) technology, which offer a limit of detection of captured particle mass of 0.26 pg and a minimum detectable particulate mass concentration in air of 0.75 µg/m3. Mobility sizing in 4 bins of a nebulized carbon aerosol NPs is demonstrated based on finite element modelling (FEM) combined with a-priori knowledge of particle charge state. Good agreement of better than 14% of mass concentration is observed in a chamber test for the novel MEMS-DMPS vs. a simultaneously operated standard fast mobility particle sizer (FMPS) as reference instrument. Refreshing of polluted cantilevers is feasible without de-mounting the sensor chip from its package by multiply purging them alternately in acetone steam and clean air.

Investigating the Trackability of Silicon Microprobes in High-Speed Surface Measurements.

High-speed tactile roughness measurements set high demand on the trackability of the stylus probe. Because of the features of low mass, low probing force, and high signal linearity, the piezoresistive silicon microprobe is a hopeful candidate for high-speed roughness measurements. This paper investigates the trackability of these microprobes through building a theoretical dynamic model, measuring their resonant response, and performing tip-flight experiments on surfaces with sharp variations. Two microprobes are investigated and compared: one with an integrated silicon tip and one with a diamond tip glued to the end of the cantilever. The result indicates that the microprobe with the silicon tip has high trackability for measurements up to traverse speeds of 10 mm/s, while the resonant response of the microprobe with diamond tip needs to be improved for the application in high-speed topography measurements.

Sampling and Mass Detection of a Countable Number of Microparticles Using on-Cantilever Imprinting.

Liquid-borne particles sampling and cantilever-based mass detection are widely applied in many industrial and scientific fields e.g., in the detection of physical, chemical, and biological particles, and disease diagnostics, etc. Microscopic analysis of particles-adsorbed cantilever-samples can provide a good basis for measurement comparison. However, when a particles-laden droplet on a solid surface is vaporized, a cluster-ring deposit is often yielded which makes particles counting difficult or impractical. Nevertheless, in this study, we present an approach, i.e., on-cantilever particles imprinting, which effectively defies such odds to sample and deposit countable single particles on a sensing surface. Initially, we designed and fabricated a triangular microcantilever sensor whose mass m0, total beam-length L, and clamped-end beam-width w are equivalent to that of a rectangular/normal cantilever but with a higher resonant frequency (271 kHz), enhanced sensitivity (0.13 Hz/pg), and quality factor (~3000). To imprint particles on these cantilever sensors, various calibrated stainless steel dispensing tips were utilized to pioneer this study by dipping and retracting each tip from a small particle-laden droplet (resting on a hydrophobic n-type silicon substrate), followed by tip-sensor-contact (at a target point on the sensing area) to detach the solution (from the tip) and adsorb the particles, and ultimately determine the particles mass concentration. Upon imprinting/adsorbing the particles on the sensor, resonant frequency response measurements were made to determine the mass (or number of particles). A minimum detectable mass of ~0.05 pg was demonstrated. To further validate and compare such results, cantilever samples (containing adsorbed particles) were imaged by scanning electron microscopy (SEM) to determine the number of particles through counting (from which, the lowest count of about 11 magnetic polystyrene particles was obtained). The practicality of particle counting was essentially due to monolayer particle arrangement on the sensing surface. Moreover, in this work, the main measurement process influences are also explicitly examined.

In-Plane and Out-of-Plane MEMS Piezoresistive Cantilever Sensors for Nanoparticle Mass Detection.

In this study, we investigate the performance of two piezoresistive micro-electro-mechanical system (MEMS)-based silicon cantilever sensors for measuring target analytes (i.e., ultrafine particulate matters). We use two different types of cantilevers with geometric dimensions of 1000 × 170 × 19.5 µm3 and 300 × 100 × 4 µm3, which refer to the 1st and 2nd types of cantilevers, respectively. For the first case, the cantilever is configured to detect the fundamental in-plane bending mode and is actuated using a resistive heater. Similarly, the second type of cantilever sensor is actuated using a meandering resistive heater (bimorph) and is designed for out-of-plane operation. We have successfully employed these two cantilevers to measure and monitor the changes of mass concentration of carbon nanoparticles in air, provided by atomizing suspensions of these nanoparticles into a sealed chamber, ranging from 0 to several tens of µg/m3 and oversize distributions from ~10 nm to ~350 nm. Here, we deploy both types of cantilever sensors and operate them simultaneously with a standard laboratory system (Fast Mobility Particle Sizer, FMPS, TSI 3091) as a reference.

Cantilever-Droplet-Based Sensing of Magnetic Particle Concentrations in Liquids.

Cantilever-based sensors have attracted considerable attention in the recent past due to their enormous and endless potential and possibilities coupled with their dynamic and unprecedented sensitivity in sensing applications. In this paper, we present a technique that involves depositing and vaporizing (at ambient conditions) a particle-laden water droplet onto a defined sensing area on in-house fabricated and commercial-based silicon microcantilever sensors. This process entailed the optimization of dispensing pressure and time to generate and realize a small water droplet volume (Vd = 49.7 ± 1.9 pL). Moreover, we monitored the water evaporation trends on the sensing surface and observed total evaporation time per droplet of 39.0 ± 1.8 s against a theoretically determined value of about 37.14 s. By using monodispersed particles in water, i.e., magnetic polystyrene particles (MPS) and polymethyl methacrylate (PMMA), and adsorbing them on a dynamic cantilever sensor, the mass and number of these particles were measured and determined comparatively using resonant frequency response measurements and SEM particle count analysis, respectively. As a result, we observed and reported monolayer particles assembled on the sensor with the lowest MPS particles count of about 19 ± 2.

Nanomechanical Characterization of Vertical Nanopillars Using an MEMS-SPM Nano-Bending Testing Platform.

Nanomechanical characterization of vertically aligned micro- and nanopillars plays an important role in quality control of pillar-based sensors and devices. A microelectromechanical system based scanning probe microscope (MEMS-SPM) has been developed for quantitative measurement of the bending stiffness of micro- and nanopillars with high aspect ratios. The MEMS-SPM exhibits large in-plane displacement with subnanometric resolution and medium probing force beyond 100 micro-Newtons. A proof-of-principle experimental setup using an MEMS-SPM prototype has been built to experimentally determine the in-plane bending stiffness of silicon nanopillars with an aspect ratio higher than 10. Comparison between the experimental results and the analytical and FEM evaluation has been demonstrated. Measurement uncertainty analysis indicates that this nano-bending system is able to determine the pillar bending stiffness with an uncertainty better than 5%, provided that the pillars' stiffness is close to the suspending stiffness of the MEMS-SPM. The MEMS-SPM measurement setup is capable of on-chip quantitative nanomechanical characterization of pillar-like nano-objects fabricated out of different materials.

Cantilever Sensors.

A cantilever is considered the most basic mechanical spring-mass system and has enormous application potential for sensors [...].

Long Slender Piezo-Resistive Silicon Microprobes for Fast Measurements of Roughness and Mechanical Properties inside Micro-Holes with Diameters below 100 µm.

During the past decade, piezo-resistive cantilever type silicon microprobes for high-speed roughness measurements inside high-aspect-ratio microstructures, like injection nozzles or critical gas nozzles have been developed. This article summarizes their metrological properties for fast roughness and shape measurements including noise, damping, tip form, tip wear, and probing forces and presents the first results on the measurement of mechanical surface parameters. Due to the small mass of the cantilever microprobes, roughness measurements at very high traverse speeds up to 15 mm/s are possible. At these high scanning speeds, considerable wear of the integrated silicon tips was observed in the past. In this paper, a new tip-testing artefact with rectangular grooves of different width was used to measure this wear and to measure the tip shape, which is needed for morphological filtering of the measured profiles and, thus, for accurate form measurements. To reduce tip wear, the integrated silicon tips were replaced by low-wear spherical diamond tips of a 2 µm radius. Currently, a compact microprobe device with an integrated feed-unit is being developed for high-speed roughness measurements on manufacturing machines. First measurements on sinusoidal artefacts were carried out successfully. Moreover, the first measurements of the elastic modulus of a polymer surface applying the contact resonance measurement principle are presented, which indicates the high potential of these microprobes for simultaneous high-speed roughness and mechanical parameter measurements.

Piezoelectric MEMS Resonators for Cigarette Particle Detection.

In this work, we demonstrate the potential of a piezoelectric resonator for developing a low-cost sensor system to detect microscopic particles in real-time, which can be present in a wide variety of environments and workplaces. The sensor working principle is based on the resonance frequency shift caused by particles collected on the resonator surface. To test the sensor sensitivity obtained from mass-loading effects, an Aluminum Nitride-based piezoelectric resonator was exposed to cigarette particles in a sealed chamber. In order to determine the resonance parameters of interest, an interface circuit was implemented and included within both open-loop and closed-loop schemes for comparison. The system was capable of tracking the resonance frequency with a mass sensitivity of 8.8 Hz/ng. Although the tests shown here were proven by collecting particles from a cigarette, the results obtained in this application may have interest and can be extended towards other applications, such as monitoring of nanoparticles in a workplace environment.