Correction: Highly-sensitive wafer-scale transfer-free graphene MEMS condenser microphones.

[This corrects the article DOI: 10.1038/s41378-024-00656-x.].

Highly-sensitive wafer-scale transfer-free graphene MEMS condenser microphones.

Since the performance of micro-electro-mechanical system (MEMS)-based microphones is approaching fundamental physical, design, and material limits, it has become challenging to improve them. Several works have demonstrated graphene's suitability as a microphone diaphragm. The potential for achieving smaller, more sensitive, and scalable on-chip MEMS microphones is yet to be determined. To address large graphene sizes, graphene-polymer heterostructures have been proposed, but they compromise performance due to added polymer mass and stiffness. This work demonstrates the first wafer-scale integrated MEMS condenser microphones with diameters of 2R = 220-320 µm, thickness of 7 nm multi-layer graphene, that is suspended over a back-plate with a residual gap of 5 µm. The microphones are manufactured with MEMS compatible wafer-scale technologies without any transfer steps or polymer layers that are more prone to contaminate and wrinkle the graphene. Different designs, all electrically integrated are fabricated and characterized allowing us to study the effects of the introduction of a back-plate for capacitive read-out. The devices show high mechanical compliances Cm = 0.081-1.07 µmPa-1 (10-100 × higher than the silicon reported in the state-of-the-art diaphragms) and pull-in voltages in the range of 2-9.5 V. In addition, to validate the proof of concept, we have electrically characterized the graphene microphone when subjected to sound actuation. An estimated sensitivity of S1kHz = 24.3-321 mV Pa-1 for a Vbias = 1.5 V was determined, which is 1.9-25.5 × higher than of state-of-the-art microphone devices while having a ~9 × smaller area.

Correction: Study on the controllability of the fabrication of single-crystal silicon nanopores/nanoslits with a fast-stop ionic current-monitored TSWE method.

[This corrects the article DOI: 10.1038/s41378-023-00532-0.].

Study on the controllability of the fabrication of single-crystal silicon nanopores/nanoslits with a fast-stop ionic current-monitored TSWE method.

The application of single-crystal silicon (SCS) nanopore structures in single-molecule-based analytical devices is an emerging approach for the separation and analysis of nanoparticles. The key challenge is to fabricate individual SCS nanopores with precise sizes in a controllable and reproducible way. This paper introduces a fast-stop ionic current-monitored three-step wet etching (TSWE) method for the controllable fabrication of SCS nanopores. Since the nanopore size has a quantitative relationship with the corresponding ionic current, it can be regulated by controlling the ionic current. Thanks to the precise current-monitored and self-stop system, an array of nanoslits with a feature size of only 3 nm was obtained, which is the smallest size ever reported using the TSWE method. Furthermore, by selecting different current jump ratios, individual nanopores of specific sizes were controllably prepared, and the smallest deviation from the theoretical value was 1.4 nm. DNA translocation measurement results revealed that the prepared SCS nanopores possessed the excellent potential to be applied in DNA sequencing.

An organ-on-chip device with integrated charge sensors and recording microelectrodes.

Continuous monitoring of tissue microphysiology is a key enabling feature of the organ-on-chip (OoC) approach for in vitro drug screening and disease modeling. Integrated sensing units are particularly convenient for microenvironmental monitoring. However, sensitive in vitro and real-time measurements are challenging due to the inherently small size of OoC devices, the characteristics of commonly used materials, and external hardware setups required to support the sensing units. Here we propose a silicon-polymer hybrid OoC device that encompasses transparency and biocompatibility of polymers at the sensing area, and has the inherently superior electrical characteristics and ability to house active electronics of silicon. This multi-modal device includes two sensing units. The first unit consists of a floating-gate field-effect transistor (FG-FET), which is used to monitor changes in pH in the sensing area. The threshold voltage of the FG-FET is regulated by a capacitively-coupled gate and by the changes in charge concentration in close proximity to the extension of the floating gate, which functions as the sensing electrode. The second unit uses the extension of the FG as microelectrode, in order to monitor the action potential of electrically active cells. The layout of the chip and its packaging are compatible with multi-electrode array measurement setups, which are commonly used in electrophysiology labs. The multi-functional sensing is demonstrated by monitoring the growth of induced pluripotent stem cell-derived cortical neurons. Our multi-modal sensor is a milestone in combined monitoring of different, physiologically-relevant parameters on the same device for future OoC platforms.

Integrated 64 pixel UV image sensor and readout in a silicon carbide CMOS technology.

This work demonstrates the first on-chip UV optoelectronic integration in 4H-SiC CMOS, which includes an image sensor with 64 active pixels and a total of 1263 transistors on a 100 mm2 chip. The reported image sensor offers serial digital, analog, and 2-bit ADC outputs and operates at 0.39 Hz with a maximum power consumption of 60 µW, which are significant improvements over previous reports. UV optoelectronics have applications in flame detection, satellites, astronomy, UV photography, and healthcare. The complexity of this optoelectronic system paves the way for new applications such harsh environment microcontrollers.

Direct Wafer-Scale CVD Graphene Growth under Platinum Thin-Films.

Since the transfer process of graphene from a dedicated growth substrate to another substrate is prone to induce defects and contamination and can increase costs, there is a large interest in methods for growing graphene directly on silicon wafers. Here, we demonstrate the direct CVD growth of graphene on a SiO2 layer on a silicon wafer by employing a Pt thin film as catalyst. We pattern the platinum film, after which a CVD graphene layer is grown at the interface between the SiO2 and the Pt. After removing the Pt, Raman spectroscopy demonstrates the local growth of monolayer graphene on SiO2. By tuning the CVD process, we were able to fully cover 4-inch oxidized silicon wafers with transfer-free monolayer graphene, a result that is not easily obtained using other methods. By adding Ta structures, local graphene growth on SiO2 is selectively blocked, allowing the controlled graphene growth on areas selected by mask design.

Sensitive Transfer-Free Wafer-Scale Graphene Microphones.

During the past decades micro-electromechanical microphones have largely taken over the market for portable devices, being produced in volumes of billions yearly. Because performance of current devices is near the physical limits, further miniaturization and improvement of microphones for mobile devices poses a major challenge that requires breakthrough device concepts, geometries, and materials. Graphene is an attractive material for enabling these breakthroughs due to its flexibility, strength, nanometer thinness, and high electrical conductivity. Here, we demonstrate that transfer-free 7 nm thick multilayer graphene (MLGr) membranes with diameters ranging from 85-155 to 300 µm can be used to detect sound and show a mechanical compliance up to 92 nm Pa-1, thus outperforming commercially available MEMS microphones of 950 µm with compliances around 3 nm Pa-1. The feasibility of realizing larger membranes with diameters of 300 µm and even higher compliances is shown, although these have lower yields. We present a process for locally growing graphene on a silicon wafer and realizing suspended membranes of patterned graphene across through-silicon holes by bulk micromachining and sacrificial layer etching, such that no transfer is required. This transfer-free method results in a 100% yield for membranes with diameters up to 155 µm on 132 fabricated drums. The device-to-device variations in the mechanical compliance in the audible range (20-20000 Hz) are significantly smaller than those in transferred membranes. With this work, we demonstrate a transfer-free method for realizing wafer-scale multilayer graphene membranes that is compatible with high-volume manufacturing. Thus, limitations of transfer-based methods for graphene microphone fabrication such as polymer contamination, crack formation, wrinkling, folding, delamination, and low-tension reproducibility are largely circumvented, setting a significant step on the route toward high-volume production of graphene microphones.

Multi-layer graphene pirani pressure sensors.

The operating principle of Pirani pressure sensors is based on the pressure dependence of a suspended strip's electrical conductivity, caused by the thermal conductance of the surrounding gas which changes the Joule heating of the strip. To realize such sensors, not only materials with high temperature dependent electrical conductivity are required, but also minimization of the suspended strip dimensions is essential to maximize the responsivity and minimize the power consumption. Due to this, nanomaterials are especially attractive for this application. Here, we demonstrate the use of a multi-layer suspended graphene strip as a Pirani pressure sensor and compare its behavior with existing models. A clear pressure dependence of the strip's electrical resistance is observed, with a maximum relative change of 2.75% between 1 and 1000 mbar and a power consumption of 8.5 mW. The use of graphene enables miniaturization of the device footprint by 100 times compared to state-of-the-art. Moreover, miniaturization allows for lower power consumption and/or higher responsivity and the sensor's nanogap enables operation near atmospheric pressure that can be used in applications such as barometers for altitude measurement. Furthermore, we demonstrate that the sensor response depends on the type of gas molecules, which opens up the way to selective gas sensing applications. Finally, the graphene synthesis technology is compatible with wafer-scale fabrication, potentially enabling future chip-level integration with readout electronics.

Rapid Prototyping of Organ-on-a-Chip Devices Using Maskless Photolithography.

Organ-on-a-chip (OoC) and microfluidic devices are conventionally produced using microfabrication procedures that require cleanrooms, silicon wafers, and photomasks. The prototyping stage often requires multiple iterations of design steps. A simplified prototyping process could therefore offer major advantages. Here, we describe a rapid and cleanroom-free microfabrication method using maskless photolithography. The approach utilizes a commercial digital micromirror device (DMD)-based setup using 375 nm UV light for backside exposure of an epoxy-based negative photoresist (SU-8) on glass coverslips. We show that microstructures of various geometries and dimensions, microgrooves, and microchannels of different heights can be fabricated. New SU-8 molds and soft lithography-based polydimethylsiloxane (PDMS) chips can thus be produced within hours. We further show that backside UV exposure and grayscale photolithography allow structures of different heights or structures with height gradients to be developed using a single-step fabrication process. Using this approach: (1) digital photomasks can be designed, projected, and quickly adjusted if needed; and (2) SU-8 molds can be fabricated without cleanroom availability, which in turn (3) reduces microfabrication time and costs and (4) expedites prototyping of new OoC devices.

Low-Humidity Sensing Properties of Multi-Layered Graphene Grown by Chemical Vapor Deposition.

Humidity sensing is fundamental in some applications, as humidity can be a strong interferent in the detection of analytes under environmental conditions. Ideally, materials sensitive or insensitive towards humidity are strongly needed for the sensors used in the first or second case, respectively. We present here the sensing properties of multi-layered graphene (MLG) upon exposure to different levels of relative humidity. We synthesize MLG by chemical vapor deposition, as shown by Raman spectroscopy, Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM). Through an MLG-based resistor, we show that MLG is scarcely sensitive to humidity in the range 30%-70%, determining current variations in the range of 0.005%/%relative humidity (RH) well below the variation induced by other analytes. These findings, due to the morphological properties of MLG, suggest that defective MLG is the ideal sensing material to implement in gas sensors operating both at room temperature and humid conditions.

Self-aligned micro-optic integrated photonic platform.

In this work, we present the fabrication technology of a monolithically integrated photonic platform combining key components for optical coherence tomography (OCT) imaging, thereby including a photonic interferometer, a collimating lens, and a 45° reflecting mirror that directs the light from the interferometer to the collimator. The proposed integration process simplifies the fabrication of an interferometric system and inherently overcomes the complexity of costly alignment procedures while complying with the necessarily stringent optical constraints. Fabricated waveguide characterization shows total optical losses as low as 3 dB, and less than 1 dB of additional loss due to the Si 45° mirror facet. The alignment standard deviation of all components is within 15 nm. The integrated lens profile achieves a divergence angle smaller than 0.7°, which is close to that of a collimator. The proposed photonic platform provides the premise for low-cost and small-footprint single-chip OCT systems.

Suspended tungsten trioxide (WO3) gate AlGaN/GaN heterostructure deep ultraviolet detectors with integrated micro-heater.

A suspended WO3-gate AlGaN/GaN heterostructure photodetector integrated with a micro-heater is micro-fabricated and characterized for ultraviolet photo detection. The transient optical characteristics of the photodetector at different temperatures are studied. The 2DEG-based photodetector shows a recovery (170 s) time under 240 nm illumination at 150 ℃. The measured spectral response of WO3-gate AlGaN/GaN heterostructure shows a high response in deep ultraviolet range. Responsivity at 240 nm wavelength is 4600 A/W at 0.5 V bias. These characteristics support the feasibility of a high accuracy deep UV detector based on the suspended AlGaN/GaN heterostructure integrated with a micro-heater.

Metal and Polymeric Strain Gauges for Si-Based, Monolithically Fabricated Organs-on-Chips.

Organ-on-chip (OOC) is becoming the alternative tool to conventional in vitro screening. Heart-on-chip devices including microstructures for mechanical and electrical stimulation have been demonstrated to be advantageous to study structural organization and maturation of heart cells. This paper presents the development of metal and polymeric strain gauges for in situ monitoring of mechanical strain in the Cytostretch platform for heart-on-chip application. Specifically, the optimization of the fabrication process of metal titanium (Ti) strain gauges and the investigation on an alternative material to improve the robustness and performance of the devices are presented. The transduction behavior and functionality of the devices are successfully proven using a custom-made set-up. The devices showed resistance changes for the pressure range (0-3 kPa) used to stretch the membranes on which heart cells can be cultured. Relative resistance changes of approximately 0.008% and 1.2% for titanium and polymeric strain gauges are respectively reported for membrane deformations up to 5%. The results demonstrate that both conventional IC metals and polymeric materials can be implemented for sensing mechanical strain using robust microfabricated organ-on-chip devices.

Analysis of a calibration method for non-stationary CVD multi-layered graphene-based gas sensors.

Limitations such as lack of detected stationary signal and slow signal recovery after detection currently affect graphene-based chemi-sensors operating at room temperature. In this work, we model the behavior of a sensor in a test chamber having limited volume and simulating the environmental conditions. From this model, we mathematically derive the calibration method for the sensor. The approach, focused on the time differential of the signal output, is tested on multi-layered graphene (MLG)-based sensors towards the chosen target gas (nitrogen dioxide) in the range from 0.12 to 1.32 ppm. MLG acting as sensing layer is synthesized by chemical vapor deposition. Our study paves the route for a wider applicability of the analysis to calibrate the class of devices affected by non-stationary and recovery issues.

Effects of Conformal Nanoscale Coatings on Thermal Performance of Vertically Aligned Carbon Nanotubes.

The high aspect ratio and the porous nature of spatially oriented forest-like carbon nanotube (CNT) structures represent a unique opportunity to engineer a novel class of nanoscale assemblies. By combining CNTs and conformal coatings, a 3D lightweight scaffold with tailored behavior can be achieved. The effect of nanoscale coatings, aluminum oxide (Al2 O3 ) and nonstoichiometric amorphous silicon carbide (a-SiC), on the thermal transport efficiency of high aspect ratio vertically aligned CNTs, is reported herein. The thermal performance of the CNT-based nanostructure strongly depends on the achieved porosity, the coating material and its infiltration within the nanotube network. An unprecedented enhancement in terms of effective thermal conductivity in a-SiC coated CNTs has been obtained: 181% compared to the as-grown CNTs and Al2 O3 coated CNTs. Furthermore, the integration of coated high aspect ratio CNTs in an epoxy molding compound demonstrates that, next to the required thermal conductivity, the mechanical compliance for thermal interface applications can also be achieved through coating infiltration into foam-like CNT forests.

Effects of graphene defects on gas sensing properties towards NO2 detection.

The crystal structure of graphene flakes is expected to significantly affect their sensing properties. Here we report an experimental investigation on the crystalline structure of graphene aimed at exploring the effects on the gas sensing properties. The morphology of graphene, prepared via Chemical Vapor Deposition (CVD), Liquid Phase Exfoliation (LPE) and Mechanical Exfoliation (ME), is inspected through Raman spectroscopy, Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM). CVD and LPE-graphene structures are found to be more defective with respect to ME-graphene. The defects are due to the jagged morphology of the films rather than originating from intrinsic disorder. The flatness of ME-graphene flakes, instead, explains the absence of defects. Chemiresistors based on the three different graphene preparation methods are subsequently exposed to NO2 in the concentration range 0.1-1.5 ppm (parts per million). The device performance is demonstrated to be strongly and unambiguously affected by the material structure: the less defective the material is, the higher the response rate is. In terms of signal variation, at 1.5 ppm, for instance, ME-graphene shows the highest value (5%) among the three materials. This study, comparing simultaneously graphene and sensors prepared via different routes, provides the first experimental evidence of the role played by the graphene level of defectiveness in the interaction with analytes. Moreover, these findings can pave the path for tailoring the sensor behavior as a function of graphene morphology.

Liquid identification by using a micro-electro-mechanical interdigital transducer.

A surface-acoustic-mode aluminum nitride (AlN) transducer is utilized to determine the type of liquid dropped on the propagation path. It is based on tracking the shrinking droplet radius and observing stagnant liquid molecules during and after the liquid evaporation process. The device configuration is suitable to test small amounts of liquids, in the microliter range. According to both mass loading and physical property mechanisms, eight samples of liquids, isopropanol (IPA), ethanol (ETH), deionized-water (DW), tap water (TW), heptane (HEP), propylene glycol monomethyl ether acetate (PGMEA), hexamethyldisilazane (HMDS) and acetone (ACE), which have different equilibrium vapor pressures, molecular weights and boiling points, are accurately detected. The experimental results show that the rate of the change in the energy loss including a slow and fast attenuation region depends on the change of physical properties, such as density, sound speed in liquids and evaporation rate, during the evaporation process. As the evaporation rate of the DW is rather slow, the slow attenuation region occurs for a longer time than the fast one. Consequently, the whole oscillation duration of the attenuation occurs for a longer time, whereas that of the other liquids studied, like ACE, ETH, and IPA, having a faster evaporation rate is shorter. Sensitivities of the surface-acoustic-mode transducer to the evaporation process of liquids such as DW, TW, PGMEA, HMDS, HEP, IPA, ETH and ACE are -29.39, -29.53, -31.79, -34.12, -33.62, -32.87, -32.67, and -32.82 dB µm-2, respectively. The concentration of stagnant liquid molecules causes a change in the surface mass of the micro-electro-mechanical transducer, which causes a frequency shift and increases the signal noise at the receiver after the liquid evaporation process. The average frequency shifts of ACE, HEP, HMDS, ETH, IPA, PGMEA, TW and DW are 241, 206, 172, 117, 76, 27.3, 11.6 and 0 kHz, respectively, coherent with the type of formed liquid pattern on the device surface, thus allowing to detect liquid samples effectively.

Stretchable Binary Fresnel Lens for Focus Tuning.

This paper presents a tuneable binary amplitude Fresnel lens produced by wafer-level microfabrication. The Fresnel lens is fabricated by encapsulating lithographically defined vertically aligned carbon nanotube (CNT) bundles inside a polydimethyl-siloxane (PDMS) layer. The composite lens material combines the excellent optical absorption properties of the CNT with the transparency and stretchability of the PDMS. By stretching the elastomeric composite in radial direction, the lens focal length is tuned. Good focusing response is demonstrated and a large focus change (≥24%) was achieved by stretching lenses up to 11.4%.

Thermal characterization of carbon nanotube foam using MEMS microhotplates and thermographic analysis.

Thermal material properties play a fundamental role in the thermal management of microelectronic systems. The porous nature of carbon nanotube (CNT) arrays results in a very high surface area to volume ratio, which makes the material attractive for surface driven heat transfer mechanisms. Here, we report on the heat transfer performance of lithographically defined micropins made of carbon nanotube (CNT) nanofoam, directly grown on microhotplates (MHPs). The MHP is used as an in situ characterization platform with controllable hot-spot and integrated temperature sensor. Under natural convection, and equivalent power supplied, we measured a significant reduction in hot-spot temperature when augmenting the MHP surface with CNT micropins. In particular, a strong enhancement of convective and radiative heat transfer towards the surrounding environment is recorded, due to the high aspect ratio and the foam-like morphology of the patterned CNTs. By combining electrical characterizations with high-resolution thermographic microscopy analysis, we quantified the heat losses induced by the integrated CNT nanofoams and we found a unique temperature dependency of the equivalent convective heat transfer coefficient, Hc. The obtained results with the proposed non-destructive characterization method demonstrate that significant improvements can be achieved in microelectronic thermal management and hierarchical structured porous material characterization.