Spin-Coated Heterogenous Stacked Electrodes for Performance Enhancement in CMOS-Compatible On-Chip Microsupercapacitors.

Integration of microsupercapacitors (MSCs) with on-chip sensors and actuators with nanoenergy harvesters can improve the lifetime of wireless sensor nodes in an Internet-of-Things (IoT) architecture. However, to be easy to integrate with such harvester technology, MSCs should be fabricated through a complementary-metal-oxide-semiconductor (CMOS) compatible technology, ubiquitous in electrode choice with the capability of heterogeneous stacking of electrodes for modulation in properties driven by application requirements. In this article, we address both these issues through fabrication of multielectrode modular, high energy density microsupercapacitors (MSC) containing reduced graphene oxide (GO), GO-heptadecane-9-amine (GO-HD9A), rGO-octadecylamine (rGO-ODA), and rGO-heptadecane-9-amine (rGO-HD9A) that stack through a scalable, CMOS compatible, high-wafer-yield spin-coating process. Furthermore, we compare the performance of the stack with individual electrode MSCs fabricated through the same process. The individual electrodes, in the presence of 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfony)imide (EMIM-TFSI), demonstrate a capacitance of 38, 30, 36, and 105 µF cm-2 at 20 mV s-1 whereas the fabricated stack of electrodes demonstrates a high capacitance of 280 µF cm-2 at 20 mV s-1 while retaining and enhancing the material-dependent capacitance, charge retention, and power density.

Dry Film Photoresist-Based Microfabrication: A New Method to Fabricate Millimeter-Wave Waveguide Components.

This paper presents a novel fabrication method based on dry film photoresists to realize waveguides and waveguide-based passive components operating at the millimeter-wave frequency (30-300 GHz). We demonstrate that the proposed fabrication method has a high potential as an alternative to other microfabrication technologies, such as silicon-based and SU8-based micromachining for realizing millimeter-wave waveguide components. Along with the nearly identical transfer of geometrical structures, the dry film photoresist offers other advantages such as fewer processing steps, lower production cost, and shorter prototyping time over the conventional micromachining technologies. To demonstrate the feasibility of the fabrication process, we use SUEX dry film to fabricate a ridge gap waveguide resonator. The resonator is designed to exhibit two resonances at 234.6 and 284 GHz. The measured attenuation at 234 GHz is 0.032 dB/mm and at 283 GHz is 0.033 dB/mm for the fabricated prototype. A comparative study among different existing technologies indicates that the reported method can give a better unloaded Q-value than other conventional processes. The measured unloaded Q-values are in good agreement with the simulated unloaded Q-values. The signal attenuation indicates that SUEX dry film photoresists can be used to fabricate passive devices operating at millimeter-wave frequencies. Moreover, this new fabrication method can offer fast and low-cost prototyping.

Enhanced Electrode Deposition for On-Chip Integrated Micro-Supercapacitors by Controlled Surface Roughening.

On-chip micro-supercapacitors (MSCs), integrated with energy harvesters, hold substantial promise for developing self-powered wireless sensor systems. However, MSCs have conventionally been manufactured through techniques incompatible with semiconductor fabrication technology, the most significant bottleneck being the electrode deposition technique. Utilization of spin-coating for electrode deposition has shown potential to deliver several complementary metal-oxide-semiconductor (CMOS)-compatible MSCs on a silicon substrate. Yet, their limited electrochemical performance and yield over the substrate have remained challenges obstructing their subsequent integration. We report a facile surface roughening technique for improving the wafer yield and the electrochemical performance of CMOS-compatible MSCs, specifically for reduced graphene oxide as an electrode material. A 4 nm iron layer is deposited and annealed on the wafer substrate to increase the roughness of the surface. In comparison to standard nonroughened MSCs, the increase in surface roughness leads to a 78% increased electrode thickness, 21% improvement in mass retention, 57% improvement in the uniformity of the spin-coated electrodes, and a high yield of 87% working devices on a 2″ silicon substrate. Furthermore, these improvements directly translate to higher capacitive performance with enhanced rate capability, energy, and power density. This technique brings us one step closer to fully integrable CMOS-compatible MSCs in self-powered systems for on-chip wireless sensor electronics.

Impact of electrode geometry and thickness on planar on-chip microsupercapacitors.

We report an assessment of the influence of both finger geometry and vertically-oriented carbon nanofiber lengths in planar micro-supercapacitors. Increasing the finger number leads to an up-scaling in areal power densities, which increases with scan rate. Growing the nanofibers longer, however, does not lead to a proportional growth in capacitance, proposedly related to limited ion penetration of the electrode.

Maintaining Transparency of a Heated MEMS Membrane for Enabling Long-Term Optical Measurements on Soot-Containing Exhaust Gas.

Ensuring optical transparency over a wide spectral range of a window with a view into the tailpipe of the combustion engine, while it is exposed to the harsh environment of soot-containing exhaust gas, is an essential pre-requisite for introducing optical techniques for long-term monitoring of automotive emissions. Therefore, a regenerable window composed of an optically transparent polysilicon-carbide membrane with a diameter ranging from 100 µm up to 2000 µm has been fabricated in microelectromechanical systems (MEMS) technology. In the first operating mode, window transparency is periodically restored by pulsed heating of the membrane using an integrated resistor for heating to temperatures that result in oxidation of deposited soot (600-700 °C). In the second mode, the membrane is kept transparent by repelling soot particles using thermophoresis. The same integrated resistor is used to yield a temperature gradient by continuous moderate-temperature heating. Realized devices have been subjected to laboratory soot exposure experiments. Membrane temperatures exceeding 500 °C have been achieved without damage to the membrane. Moreover, heating of membranes to ΔT = 40 °C above gas temperature provides sufficient thermophoretic repulsion to prevent particle deposition and maintain transparency at high soot exposure, while non-heated identical membranes on the same die and at the same exposure are heavily contaminated.

Carbon-Based Electrode Materials for Microsupercapacitors in Self-Powering Sensor Networks: Present and Future Development.

There is an urgent need to fulfill future energy demands for micro and nanoelectronics. This work outlines a number of important design features for carbon-based microsupercapacitors, which enhance both their performance and integration potential and are critical for complimentary metal oxide semiconductor (CMOS) compatibility. Based on these design features, we present CMOS-compatible, graphene-based microsupercapacitors that can be integrated at the back end of the line of the integrated circuit fabrication. Electrode materials and their interfaces play a crucial role for the device characteristics. As such, different carbon-based materials are discussed and the importance of careful design of current collector/electrode interfaces is emphasized. Electrode adhesion is an important factor to improve device performance and uniformity. Additionally, doping of the electrodes can greatly improve the energy density of the devices. As microsupercapacitors are engineered for targeted applications, device scaling is critically important, and we present the first steps toward general scaling trends. Last, we outline a potential future integration scheme for a complete microsystem on a chip, containing sensors, logic, power generation, power management, and power storage. Such a system would be self-powering.

A Micromachined Coupled-Cantilever for Piezoelectric Energy Harvesters.

This paper presents a demonstration of the feasibility of fabricating micro-cantilever harvesters with extended stress distribution and enhanced bandwidth by exploiting an M-shaped two-degrees-of-freedom design. The measured mechanical response of the fabricated device displays the predicted dual resonance peak behavior with the fundamental peak at the intended frequency. This design has the features of high energy conversion efficiency in a miniaturized environment where the available vibrational energy varies in frequency. It makes such a design suitable for future large volume production of integrated self powered sensors nodes for the Internet-of-Things.

Tailor-made conductive inks from cellulose nanofibrils for 3D printing of neural guidelines.

Neural tissue engineering (TE), an innovative biomedical method of brain study, is very dependent on scaffolds that support cell development into a functional tissue. Recently, 3D patterned scaffolds for neural TE have shown significant positive effects on cells by a more realistic mimicking of actual neural tissue. In this work, we present a conductive nanocellulose-based ink for 3D printing of neural TE scaffolds. It is demonstrated that by using cellulose nanofibrils and carbon nanotubes as ink constituents, it is possible to print guidelines with a diameter below 1 mm and electrical conductivity of 3.8 × 10-1 S cm-1. The cell culture studies reveal that neural cells prefer to attach, proliferate, and differentiate on the 3D printed conductive guidelines. To our knowledge, this is the first research effort devoted to using cost-effective cellulosic 3D printed structures in neural TE, and we suppose that much more will arise in the near future.

Enhanced growth of neural networks on conductive cellulose-derived nanofibrous scaffolds.

The problem of recovery from neurodegeneration needs new effective solutions. Tissue engineering is viewed as a prospective approach for solving this problem since it can help to develop healthy neural tissue using supportive scaffolds. This study presents effective and sustainable tissue engineering methods for creating biomaterials from cellulose that can be used either as scaffolds for the growth of neural tissue in vitro or as drug screening models. To reach this goal, nanofibrous electrospun cellulose mats were made conductive via two different procedures: carbonization and addition of multi-walled carbon nanotubes. The resulting scaffolds were much more conductive than untreated cellulose material and were used to support growth and differentiation of SH-SY5Y neuroblastoma cells. The cells were evaluated by scanning electron microscopy and confocal microscopy methods over a period of 15 days at different time points. The results showed that the cellulose-derived conductive scaffolds can provide support for good cell attachment, growth and differentiation. The formation of a neural network occurred within 10 days of differentiation, which is a promising length of time for SH-SY5Y neuroblastoma cells.

Low temperature and cost-effective growth of vertically aligned carbon nanofibers using spin-coated polymer-stabilized palladium nanocatalysts.

We describe a fast and cost-effective process for the growth of carbon nanofibers (CNFs) at a temperature compatible with complementary metal oxide semiconductor technology, using highly stable polymer-Pd nanohybrid colloidal solutions of palladium catalyst nanoparticles (NPs). Two polymer-Pd nanohybrids, namely poly(lauryl methacrylate)-block-poly((2-acetoacetoxy)ethyl methacrylate)/Pd (LauMA x -b-AEMA y /Pd) and polyvinylpyrrolidone/Pd were prepared in organic solvents and spin-coated onto silicon substrates. Subsequently, vertically aligned CNFs were grown on these NPs by plasma enhanced chemical vapor deposition at different temperatures. The electrical properties of the grown CNFs were evaluated using an electrochemical method, commonly used for the characterization of supercapacitors. The results show that the polymer-Pd nanohybrid solutions offer the optimum size range of palladium catalyst NPs enabling the growth of CNFs at temperatures as low as 350 °C. Furthermore, the CNFs grown at such a low temperature are vertically aligned similar to the CNFs grown at 550 °C. Finally the capacitive behavior of these CNFs was similar to that of the CNFs grown at high temperature assuring the same electrical properties thus enabling their usage in different applications such as on-chip capacitors, interconnects, thermal heat sink and energy storage solutions.

Electromechanically tunable carbon nanofiber photonic crystal.

We demonstrate an electrically tunable 2D photonic crystal array constructed from vertically aligned carbon nanofibers. The nanofibers are actuated by applying a voltage between adjacent carbon nanofiber pairs grown directly on metal electrodes, thus dynamically changing the form factor of the photonic crystal lattice. The change in optical properties is characterized using optical diffraction and ellipsometry. The experimental results are shown to be in agreement with theoretical predictions and provide a proof-of-principle for rapidly switchable photonic crystals operating in the visible that can be fabricated using standard nanolithography techniques combined with plasma CVD growth of the nanofibers.

Linear variable optical filter-based ultraviolet microspectrometer.

An IC-compatible linear variable optical filter (LVOF) for application in the UV spectral range between 310 and 400 nm has been fabricated using resist reflow and an optimized dry-etching. The LVOF is mounted on the top of a commercially available CMOS camera to result in a UV microspectrometer. A special calibration technique has been employed that is based on an initial spectral measurement on a xenon lamp. The image recorded on the camera during calibration is used in a signal processing algorithm to reconstruct the spectrum of the mercury lamp and the calibration data is subsequently used in UV spectral measurements. Experiments on a fabricated LVOF-based microspectrometer with this calibration approach implemented reveal a spectral resolution of 0.5 nm.

Cobalt (II) chloride promoted formation of honeycomb patterned cellulose acetate films.

CoCl(2) containing honeycomb patterned films were prepared from cellulose acetate (CA)/CoCl(2)/acetone solutions by the breath figure method in a wide range of humidities. Size and pore regularity depend on the CA/CoCl(2) molar ratio and humidity. When replacing CoCl(2) with Co(NO(3))(2) or CoBr(2), no formation of ordered porosity in the cellulose acetate films is observed. According to data from scanning electron microscopy (SEM), Energy Dispersive X-ray Microanalysis (EDX), X-ray Diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy, the key role in the formation of honeycomb structures can be attributed to the physical and chemical properties of CoCl(2) - hygroscopicity, low interaction with CA, and extraction from CA/CoCl(2)/acetone solution by water droplets condensed on the surface of the CA/CoCl(2) solution. Obtained films are prospective for using in catalysis, hydrogen fuel cells, and optical sensing materials.

Optical label-free nanoplasmonic biosensing using a vertical-cavity surface-emitting laser and charge-coupled device.

We present a compact platform for biochemosensing based on the combination of a vertical-cavity surface-emitting laser (VCSEL) light source, microelectromechanical systems (MEMS)-based microoptics, a specially designed nanoplasmonic sensing chip, and charge-coupled device (CCD) detector. The platform does not require any spectral analyzer for signal evaluation, showing good promise for facile integration, neither does it use any microscope setup for the signal collection or imaging. The analytical capabilities of the developed biochemosensing platform are demonstrated by evaluation of the protein-substrate (biotinylated bovine serum albumin-gold) and the protein-protein (biotin-NeutrAvidin) binding kinetics, which is further compared to detection based on conventional optical extinction spectroscopy. The instrument is able to detect low femtomoles of adsorbed proteins with the limit of detection comparable to the state-of-the-art research and commercial optical label-free biochemosensors.

Towards an electrowetting-based digital microfluidic platform for magnetic immunoassays.

We demonstrate ElectroWetting-On-Dielectric (EWOD) transport and SQUID gradiometer detection of magnetic nanoparticles (MNPs) suspended in a 2 microl de-ionized water droplet. This proof-of-concept methodology constitutes the first development step towards a highly sensitive magnetic immunoassay platform with SQUID readout and droplet-based sample handling. Magnetic AC-susceptibility measurements were performed on MNPs with a hydrodynamic diameter of 100 nm using a high-Tc dc Superconducting Quantum Interference Device (SQUID) gradiometer as detector. We observed that the signal amplitude per unit volume is 2.5 times higher for a 2 microl sample droplet compared to a 30 microl sample volume.

Compatibility assessment of CVD growth of carbon nanofibers on bulk CMOS devices.

We compare the level of deterioration in the basic functionality of individual transistors on ASIC chips fabricated in standard 130 nm bulk CMOS technology when subjected to three disparate CVD techniques with relatively low processing temperature to grow carbon nanostructures. We report that the growth technique with the lowest temperature has the least impact on the transistor behavior.

Replication of continuous-profiled micro-optical elements for silicon integration.

A novel scheme for the integration of diffractive optical elements onto silicon is presented. The processing is made in reverse order, meaning that the process of structuring the optical elements on the wafer precedes the silicon microstructuring. The first processing step on the wafer is the hot embossing of the optical microstructures into an amorphous fluorocarbon polymer spin coated on the wafer. The cured polymer forms a highly stable material with excellent optical properties. The remaining silicon processing is thus performed with the diffractive optical elements already in place. Two different diffractive structures were used in the development of the method-a (Fresnel) lens with a rather low f-number and a diffractive element producing a fan-out of a large number of paraxial beams.

Electrical properties of Si-SiO(2)-Si nanogaps.

The chances of attaching organic molecules to silicon surfaces can be considerably enhanced if a robust nanogap structure with silicon electrodes can be used to connect the molecules. We describe the electrical properties of such an electrode structure, with a separation of the silicon surfaces in the 3-7 nm range. These silicon nanogaps are manufactured by partly removing the silicon dioxide insulator from a silicon-oxide-silicon material stack, by using a selective oxide etchant. After the activation of the gap (the etching), current instabilities appear, which are comparable to the properties of thin oxides after soft breakdown. Applying a constant voltage can reduce these current instabilities. We also address the issue of surface leakage currents for these nanogap structures.