Fabrication, densification, and replica molding of 3D carbon nanotube microstructures

The introduction of new materials and processes to microfabrication has, in large part, enabled many important advances in microsystems, labon- a-chip devices, and their applications. In particular, capabilities for cost-effective fabrication of polymer microstructures were transformed by the advent of soft lithography and other micromolding techniques 1,2, and this led a revolution in applications of microfabrication to biomedical engineering and biology. Nevertheless, it remains challenging to fabricate microstructures with well-defined nanoscale surface textures, and to fabricate arbitrary 3D shapes at the micro-scale. Robustness of master molds and maintenance of shape integrity is especially important to achieve high fidelity replication of complex structures and preserving their nanoscale surface texture. The combination of hierarchical textures, and heterogeneous shapes, is a profound challenge to existing microfabrication methods that largely rely upon top-down etching using fixed mask templates. On the other hand, the bottom-up synthesis of nanostructures such as nanotubes and nanowires can offer new capabilities to microfabrication, in particular by taking advantage of the collective self-organization of nanostructures, and local control of their growth behavior with respect to microfabricated patterns. Our goal is to introduce vertically aligned carbon nanotubes (CNTs), which we refer to as CNT "forests", as a new microfabrication material. We present details of a suite of related methods recently developed by our group: fabrication of CNT forest microstructures by thermal CVD from lithographically patterned catalyst thin films; self-directed elastocapillary densification of CNT microstructures; and replica molding of polymer microstructures using CNT composite master molds. In particular, our work shows that self-directed capillary densification ("capillary forming"), which is performed by condensation of a solvent onto the substrate with CNT microstructures, significantly increases the packing density of CNTs. This process enables directed transformation of vertical CNT microstructures into straight, inclined, and twisted shapes, which have robust mechanical properties exceeding those of typical microfabrication polymers. This in turn enables formation of nanocomposite CNT master molds by capillary-driven infiltration of polymers. The replica structures exhibit the anisotropic nanoscale texture of the aligned CNTs, and can have walls with sub-micron thickness and aspect ratios exceeding 50:1. Integration of CNT microstructures in fabrication offers further opportunity to exploit the electrical and thermal properties of CNTs, and diverse capabilities for chemical and biochemical functionalization 3. © 2012 Journal of Visualized Experiments.

Engineering of micro- and nanostructured surfaces with anisotropic geometries and properties

Widespread approaches to fabricate surfaces with robust micro- and nanostructured topographies have been stimulated by opportunities to enhance interface performance by combining physical and chemical effects. In particular, arrays of asymmetric surface features, such as arrays of grooves, inclined pillars, and helical protrusions, have been shown to impart unique anisotropy in properties including wetting, adhesion, thermal and/or electrical conductivity, optical activity, and capability to direct cell growth. These properties are of wide interest for applications including energy conversion, microelectronics, chemical and biological sensing, and bioengineering. However, fabrication of asymmetric surface features often pushes the limits of traditional etching and deposition techniques, making it challenging to produce the desired surfaces in a scalable and cost-effective manner. We review and classify approaches to fabricate arrays of asymmetric 2D and 3D surface features, in polymers, metals, and ceramics. Analytical and empirical relationships among geometries, materials, and surface properties are discussed, especially in the context of the applications mentioned above. Further, opportunities for new fabrication methods that combine lithography with principles of self-assembly are identified, aiming to establish design principles for fabrication of arbitrary 3D surface textures over large areas. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hierarchical carbon nanowire microarchitectures made by plasma-assisted pyrolysis of photoresist

We present a new approach for the fabrication and integration of vertically aligned forests of amorphous carbon nanowires (CNWs), using only standard lithography, oxygen plasma treatment, and thermal processing. The simplicity and scalability of this process, as well as the hierarchical organization of CNWs, provides a potential alternative to the use of carbon nanotubes and graphene for applications in microsystems and high surface area materials. The CNWs are highly branched at the nanoscale, and novel hierarchical microstructures with CNWs connected to a solid amorphous core are made by controlling the plasma treatment time. By multilayer processing we demonstrate deterministic joining of CNW micropillars into 3D sensing networks. Finally we show that these networks can be chemically functionalized and used for measurement of DNA binding with increased sensitivity. © 2011 American Chemical Society.

Fabrication of high-aspect-ratio polymer microstructures and hierarchical textures using carbon nanotube composite master molds

Scalable and cost effective patterning of polymer structures and their surface textures is essential to engineer material properties such as liquid wetting and dry adhesion, and to design artificial biological interfaces. Further, fabrication of high-aspect-ratio microstructures often requires controlled deep-etching methods or high-intensity exposure. We demonstrate that carbon nanotube (CNT) composites can be used as master molds for fabrication of high-aspect-ratio polymer microstructures having anisotropic nanoscale textures. The master molds are made by growth of vertically aligned CNT patterns, capillary densification of the CNTs using organic solvents, and capillary-driven infiltration of the CNT structures with SU-8. The composite master structures are then replicated in SU-8 using standard PDMS transfer molding methods. By this process, we fabricated a library of replicas including vertical micro-pillars, honeycomb lattices with sub-micron wall thickness and aspect ratios exceeding 50:1, and microwells with sloped sidewalls. This process enables batch manufacturing of polymer features that capture complex nanoscale shapes and textures, while requiring only optical lithography and conventional thermal processing. © 2011 The Royal Society of Chemistry.

Controlled growth orientation of carbon nanotube pillars by catalyst patterning in microtrenches

We present a novel method for controlling the growth orientation of individual carbon nanotube (CNT) microstructures on a silicon wafer substrate. Our method controls the CNT forest orientation by patterning the catalyst layer used in the CNTs growth on slanted KOH edges. The overlap of catalyst area on the horizontal bottom and sloped sidewall surfaces of the KOH-etched substrate enables precise variation of the growth direction. These inclined structures can profit from the outstanding mechanical, electrical, thermal, and optical properties of CNTs and can therefore improve the performance of several MEMS devices. Inclined CNT microstructures could for instance be used as cantilever springs in probe card arrays, as tips in dip-pen lithography, and as sensing element in advanced transducers. ©2009 IEEE.

Design and testing of an ortho-planar micro-valve

This paper presents the production and testing of an ortho-planar one-way micro-valve. The main advantages of such valves are that they are very compact and can be made from a single flat piece of material. A previous paper presents and discusses a micro-valve assembly based on a spider spring. The present paper focuses on the valve assembly process and the valve performance.. Several prototypes with a bore of 0.2 mm have been built using two manufacturing techniques (μEDM and stereo-lithography) and tested for pressures up to 7 bars. © 2008 International Federation for Information Processing.

Plasmonic nanofocusing of light in an integrated silicon photonics platform.

The capability to focus electromagnetic energy at the nanoscale plays an important role in nanoscinece and nanotechnology. It allows enhancing light matter interactions at the nanoscale with applications related to nonlinear optics, light emission and light detection. It may also be used for enhancing resolution in microscopy, lithography and optical storage systems. Hereby we propose and experimentally demonstrate the nanoscale focusing of surface plasmons by constructing an integrated plasmonic/photonic on chip nanofocusing device in silicon platform. The device was tested directly by measuring the optical intensity along it using a near-field microscope. We found an order of magnitude enhancement of the intensity at the tip's apex. The spot size is estimated to be 50 nm. The demonstrated device may be used as a building block for "lab on a chip" systems and for enhancing light matter interactions at the apex of the tip.

High-performance nanowire oxide photo-thin film transistor.

A gate-modulated nanowire oxide photosensor is fabricated by electron-beam lithography and conventional dry etch processing.. The device characteristics are good, including endurance of up to 10(6) test cycles, and gate-pulse excitation is used to remove persistent photoconductivity. The viability of nanowire oxide phototransistors for high speed and high resolution applications is demonstrated, thus potentially expanding the scope of exploitation of touch-free interactive displays.

Flexible pneumatic twisting actuators

Compliant pneumatic actuators have attracted the interests of the robotics community especially for applications where large strokes are needed in delicate environments. This paper introduces a new type of compliant actuator that generates a large twisting deformation upon pressurization. This deformation is similar to torsion in solid mechanics, and can be characterized by a twisting angle along the longitudinal axis of the actuator. To produce prototype actuators, a new fabrication process is developed that uses soft lithography. With this process, prototype actuators with a width of 7mm and a thickness of 0.65mm have been produced that exhibit a twisting rotation of 6.5 degrees per millimeter length at a pressure of 178kPa. Besides design, fabrication and characterization, this paper will go into detail on stroke optimization. © 2013 IEEE.

Deterministic cold cathode electron emission from carbon nanofibre arrays.

The ability to accurately design carbon nanofibre (CN) field emitters with predictable electron emission characteristics will enable their use as electron sources in various applications such as microwave amplifiers, electron microscopy, parallel beam electron lithography and advanced Xray sources. Here, highly uniform CN arrays of controlled diameter, pitch and length were fabricated using plasma enhanced chemical vapour deposition and their individual emission characteristics and field enhancement factors were probed using scanning anode field emission mapping. For a pitch of 10 µm and a CN length of 5 µm, the directly measured enhancement factors of individual CNs was 242, which was in excellent agreement with conventional geometry estimates (240). We show here direct empirical evidence that in regular arrays of vertically aligned CNs the overall enhancement factor is reduced when the pitch between emitters is less than half the emitter height, in accordance to our electrostatic simulations. Individual emitters showed narrow Gaussian-like field enhancement distributions, in excellent agreement with electric field simulations.

Electrical control of nanoscale functionalization in graphene by the scanning probe technique

Functionalized graphene is a versatile material that has well-known physical and chemical properties depending on functional groups and their coverage. However, selective control of functional groups on the nanoscale is hardly achievable by conventional methods utilizing chemical modifications. We demonstrate electrical control of nanoscale functionalization of graphene with the desired chemical coverage of a selective functional group by atomic force microscopy (AFM) lithography and their full recovery through moderate thermal treatments. Surprisingly, our controlled coverage of functional groups can reach 94.9% for oxygen and 49.0% for hydrogen, respectively, well beyond those achieved by conventional methods. This coverage is almost at the theoretical maximum, which is verified through scanning photoelectron microscope measurements as well as first-principles calculations. We believe that the present method is now ready to realize 'chemical pencil drawing' of atomically defined circuit devices on top of a monolayer of graphene. © 2014 Nature Publishing Group All rights reserved.

Experimental investigation on submicron rib waveguide microring/racetrack resonators in silicon-on-insulator

in experiment, characteristics of silicon microring/racetrack resonators in submicron rib waveguides have been systematically investigated. It is demonstrated that only a transverse-electric mode is guided for a ratio of slab height to rib height h/H = 0.5. Thus, these microring/racetrack resonators can only function for quasi-transverse-electric mode, while they get rid of transverse-magnetic polarization. Electron beam lithography and inductively coupled plasma etching were employed and improved to reduce side-wall roughness for low propagation loss and high performance resonators. Then, the effects of waveguide dimensions, coupling region design, waveguide roughness, and oxide cladding for the resonators have been considered and analyzed. (C) 2008 Elsevier B.V. All rights reserved.

Design, fabrication and characterization of a high-performance microring resonator in silicon-on-insulator

A high-performance microring resonator in a silicon-on-insulator rib waveguide is realized by using the electron beam lithography followed by inductively coupled plasma etching. The design and the experimental realization of this device are presented in detail. In addition to improving relevant processes to minimize propagation loss, the coupling efficiency between the ring and the bus is carefully chosen to approach a critical coupling for high performance operating. We have measured a quality factor of 21,200 and an extinction ratio of 12.5dB at a resonant wavelength of 1549.32nm. Meanwhile, a low propagation loss of 0.89dB/mm in a curved waveguide with a bending radius of 40 mu m is demonstrated as well.

A photonic wire-based directional coupler based on SOI

A photonic wire-based directional coupler based on SOI was fabricated by e-beam lithography (EBL) and the inductively coupled plasma (ICP) etching method. The size of the sub-micron waveguide is 0.34 mu m x 0.34 mu m, and the length in the coupling region and the separation between the two parallel waveguides are 410 and 0.8 mu m, respectively. The measurement results are in good agreement with the results simulated by 3D finite-difference time-domain method. The transmission power from two output ports changed reciprocally with about 23 nm wavelength spacing between the coupled and direct ports. The extinction ratio of the device was between 5 and 10 dB, and the insertion loss of the device in the wavelength range 1520-1610 nm was between 22 and 24 dB, which included an about 18.4 +/- 0.4 dB coupling loss between the taper fibers and the polished sides of the device. (c) 2008 Elsevier B.V. All rights reserved.

Fabrication of nanoscale metallic air-bridges by introducing a SiO2 sacrificial layer

A new method to fabricate nanoscale metallic air-bridges has been investigated. The pillar patterns of the air-bridge were defined on a SiO2, sacrificial layer by electron-beam lithography combined with inductively coupled plasma etching. Thereafter, the span (suspended part between the pillars) patterns were defined with a second electron-beam exposure on a PMMA/PMMA-MAA resist system. The fabrication process was completed by subsequent metal electron-beam evaporation, lift-off in acetone, and removal of the sacrificial layer in a buffered hydrofluoric (HF) solution. Air-bridges with two different geometries (line-shaped and cross-shaped) were studied in detail. The narrowest width of the air-bridges was around 200 nm, and the typical length of the air-bridges was 2-5 mu m. The advantages of our method are the simplicity of carrying out electron-beam exposure with good reproducibility and the capability of more accurate control of the pillar sizes and shapes of the air-bridge. (C) 2007 Elsevier Ltd. All rights reserved.