Static micromechanical measurements of the flexural modulus and strength of micrometre-diameter single fibres using deflecting microcantilever techniques.

The mechanical properties of natural and man-made fibres ultimately govern the robustness of products. Examples range from textiles to composite materials for mechanical parts in emerging technological applications. An accurate determination of the mechanical properties of microscopic single fibres is therefore important. Today, macroscopic mechanical techniques, such as tensile testing, are commonly employed to obtain this information. However, a relatively high dispersion of results is often encountered due to a relatively long sample size. As an alternative to tensile methods, we demonstrate here micromechanical techniques to accurately measure the flexural modulus and strength of micrometre-sized diameter fibres without the need of force sensing. To demonstrate our ideas, we use the example of single natural fibres (Linum Usitatissimum). The flexural modulus of the single fibres is first accurately measured in the low deflection regime of an inclined bending cantilever in an original setup. The flexural strength of the single fibres is then measured in the high deflection regime of a bending cantilever. Interestingly, the novel measurements have allowed the authors to quantify the flexural strength of two different failure modes in flax fibre, enabling a contribution to plant mechanics.

Skate, overtravel, and contact force of tilted triangular cantilevers for microcantilever-based MEMS probe technologies.

Microfabricated chip-edge microcantilevers are commonly used as surface probes, e.g. in near-field microscopy. Such probes normally function in the low-deflection regime, where their behaviour is very well understood and documented. In contrast, when microcantilevers are used for applications such as electrical testing probes, their deflection can be somewhat higher, taking them into the less well understood high-deflection regime of microelectromechanical systems (MEMS). Here, a scalable model for the relationship between the skate, overtravel, and resulting tip contact force in tilted triangular cantilevers-which are bending with high deflection and in contact with a flat surface-is presented. The model is tested experimentally using macroscopic triangular cantilevers-the experimental results agree well with the proposed model. The findings enable a practical solution for zero-skate in tapered MEMS probes to be suggested. It is hoped that the findings may be of use for probe engineers involved with on-wafer testing and designers of emerging MEMS micro cantilever-based probes.

Strong and weak polarization-dependent interactions in connected and disconnected plasmonic nanostructures.

We explore numerically and experimentally the formation of hybridized modes between a bright mode displayed by a gold nanodisc and either dark or bright modes of a nanorod - both elements being either separated by a nanometer-size gap (disconnected system) or relied on a metal junction (connected system). In terms of modeling, we compare the scattering or absorption spectra and field distributions obtained under oblique-incidence plane wave illumination with quasi-normal mode computation and an analytical model based on a coupled oscillator model. Both connected and disconnected systems have very different plasmon properties in longitudinal polarization. The disconnected system can be consistently understood in terms of the nature of hybridized modes and coupling strength using either QNMs or coupled oscillator model; however the connected configuration presents intriguing peculiarities based on the strong redistribution of charges implied by the presence of the metal connection. In practice, the fabrication of disconnected or connected configurations depends on the mitigation of lithographic proximity effects inherent to top-down lithography methods, which can lead to the formation of small metal junctions, while careful lithographic dosing allows one to fabricate disconnected systems with a gap as low as 20 nm. We obtained a very good agreement between experimentally measured scattering spectra and numerical predictions. The methods and analyses presented in this work can be applied to a wide range of systems, for potential applications in light-matter interactions, biosensing or strain monitoring.

Passivation of miniature microwave coplanar waveguides using a thin film fluoropolymer electret.

The insertion losses of miniature gold/silicon-on-insulator (SOI) coplanar waveguides (CPW) are rendered low, stable, and light insensitive when covered with a thin film (95 nm) fluoropolymer deposited by a trifluoromethane (CHF3) plasma. Microwave characterization (0-50 GHz) of the CPWs indicates that the fluoropolymer stabilizes a hydrogen-passivated silicon surface between the CPW tracks. The hydrophobic nature of the fluoropolymer acts as a humidity barrier, meaning that the underlying intertrack silicon surfaces do not re-oxidize over time-something that is known to increase losses. In addition, the fluoropolymer thin film also renders the CPW insertion losses insensitive to illumination with white light (2400 lx)-something potentially advantageous when using optical microscopy observations during microwave measurements. Capacitance-voltage (CV) measurements of gold/fluoropolymer/silicon metal-insulator-semiconductor (MIS) capacitors indicate that the fluoropolymer is an electret-storing positive charge. The experimental results suggest that the stored positive charge in the fluoropolymer electret and charge trapping influence surface-associated losses in CPW-MIS device modelling supports this. Finally, and on a practical note, the thin fluoropolymer film is easily pierced by commercial microwave probes and does not adhere to them-facilitating the repeatable and reproducible characterization of microwave electronic circuitry passivated by thin fluoropolymer.

Precise tailoring of evaporated gold nanocones using electron beam lithography and lift-off.

The ability to fabricate nanocones with precise dimensions is essential for several emerging applications. We demonstrate here a method which can be used to fabricate arrays of gold nanocones with high dimensional precision using lithographic and lift-off means. electron beam (ebeam) writing of a spin-coated PMMA-based bilayer resist deposited onto silicon wafers is used to form a shadow mask. This mask gradually closes as the deposition of gold (using ebeam evaporation) proceeds-the result is arrays of gold nanocones on the silicon wafer surface after lift-off of the resist. Observations using scanning electron microscopy enable a statistical study of the dimensions of 360 gold nanocones-the results demonstrate the high precision of the nanocones dimensions. The fabrication process enables the creation of arrays of nanocones with a base diameter varying from 53.6 ± 2.1 nm to 94.1 ± 2.4 nm, a vertical height ranging from 71.3 ± 4.1 nm to 153.4 ± 3.4 nm, and an apex radius of curvature ranging from 8.4 ± 1.2 nm to 11.6 ± 1.5 nm. The results are compared with the predictions of a deposition model which considers the evolving shadow masking during the gold deposition to compute the nanocone profile.

Size and shape control of a variety of metallic nanostructures using tilted, rotating evaporation and lithographic lift-off techniques.

Here, we demonstrate a simple top-down method for nanotechnology whereby electron beam (ebeam) lithography can be combined with tilted, rotated thermal evaporation to control the topography and size of an assortment of metallic objects at the nanometre scale. In order to do this, the evaporation tilt angle is varied between 1 and 24°. The technique allows the 3-dimensional tailoring of a range of metallic object shapes from sharp, flat bottomed spikes to hollow cylinders and rings-all of which have rotational symmetry and whose critical dimensions are much smaller than the lithographic feature size. The lithographic feature size is varied from 400 nm down to 40 nm. The nanostructures are characterized using electron microscopy techniques-the specific shape can be predicted using topographic modelling of the deposition. Although individual nanostructures are studied here, the idea can easily be extended to fabricate arrays for e.g. photonics and metamaterials. Being a generic technique-depending on easily controlled lithographic and evaporation parameters-it can be readily incorporated into any standard planar process and could be adapted to suit other thin-film materials deposited using physical means.

Cracking effects in squashable and stretchable thin metal films on PDMS for flexible microsystems and electronics.

Here, we study cracking of nanometre and sub-nanometre-thick metal lines (titanium, nickel, chromium, and gold) evaporated onto commercial polydimethylsiloxane (PDMS) substrates. Mechanical and electromechanical testing reveals potentially technologically useful effects by harnessing cracking. When the thin film metal lines are subjected to uniaxial longitudinal stretching, strain-induced cracks develop in the film. The regularity of the cracking is seen to depend on the applied longitudinal strain and film thickness-the findings suggest ordering and the possibility of creating metal mesas on flexible substrates without the necessity of lithography and etching. When the metal lines are aligned transversally to the direction of the applied strain, a Poisson effect-induced electrical 'self-healing' can be observed in the films. The Poisson effect causes process-induced cracks to short circuit, resulting in the lines being electrically conducting up to very high strains (~40%). Finally, cracking results in the observation of an enhanced transversal gauge factor which is ~50 times larger than the geometric gauge factor for continuous metal films-suggesting the possibility of high-sensitivity thin-film metal strain gauge flexible technology working up to high strains.

When is a surface foam-phobic or foam-philic?

It is commonly assumed that the liquid making up a sessile bubble completely wets the surface upon which the bubble lies. However, this need not be so, and the degree of wetting will determine how well a collection of bubbles - a foam - sticks to a surface. As a preliminary to this difficult problem, we study the shape of a single vertical soap film spanning the gap between two flat, horizontal solid substrates of given wettabilities. For this simple geometry, the Young-Laplace equation can be solved (quasi-)analytically to yield the equilibrium shapes, under gravity, of the two-dimensional Plateau borders along which the film contacts the substrates. We thus show that these Plateau borders, where most of a foam's liquid resides, can only exist if the values of the Bond number Bo and of the liquid contact angle θc lie within certain domains in (θc,Bo) space: under these conditions the substrate is foam-philic. For values outside these domains, the substrate cannot support a soap film and it is foam-phobic. In other words, on a substrate of a given wettability, only Plateau borders of a certain range of sizes can form. For given (θc,Bo), the top Plateau border can never have greater width or cross-sectional area than the bottom one. Moreover, the top Plateau border cannot exist in a steady state for contact angles above 90°. Our conclusions are validated by comparison with both experimental and numerical (Surface Evolver) data. We conjecture that these results will hold, with slight modifications, for non-planar soap films and bubbles. Our results are also relevant to the motion of bubbles and foams in channels, where the friction force of the substrate on the Plateau borders plays an important role.

Zipping-Depinning: Dissolution of Droplets on Micropatterned Concentric Rings.

The control of the surface wettability is of great interest for technological applications as well as for the fundamental understanding of surface phenomena. In this article, we describe the dissolution behavior of droplets wetting a micropatterned surface consisting of smooth concentric circular grooves. In the experiments, a droplet of alcohol (1-pentanol) is placed onto water-immersed micropatterns. When the drops dissolve, the dynamics of the receding contact line occurs in two different modes. In addition to the stick-jump mode with jumps from one ring to the next inner one, our study reveals a second dissolution mode, which we refer to as zipping-depinning. The velocity of the zipping-depinning fronts is governed by the dissolution rate. At the early stage of the droplet dissolution, our experimental results are in good agreement with the theoretical predictions by Debuisson et al. [ Appl. Phys. Lett. 2011 , 99 , 184101 ]. With an extended model, we can accurately describe the dissolution dynamics in both stick-jump and zipping-depinning modes.

Dynamic Chemically Driven Dewetting, Spreading, and Self-Running of Sessile Droplets on Crystalline Silicon.

A chemically driven dewetting effect is demonstrated using sessile droplets of dilute hydrofluoric acid on chemically oxidized silicon wafers. The dewetting occurs as the thin oxide is slowly etched by the droplet and replaced by a hydrogen-terminated surface; the result of this is a gradual increase in the contact angle of the droplet with time. The time-varying work of adhesion is calculated from the time-varying contact angle; this corresponds to the changing chemical nature of the surface during dewetting and can be modeled by the well-known logistic (sigmoid) function often used for the modeling of restricted growth, in this case, the transition from an oxidized surface to a hydrogen-terminated silicon surface. The observation of the time-varying contact angle allows one to both measure the etch rate of the silicon oxide and estimate the hydrogenation rate as a function of HF concentration and wafer type. In addition to this, at a certain HF concentration, a self-running droplet effect is observed. In contrast, on hydrogen-terminated silicon wafers, a chemically induced spreading effect is observed using sessile droplets of nitric acid. The droplet spreading can also be modeled using a logistical function, where the restricted growth is the transition from hydrogen-terminated to a chemically induced oxidized silicon surface. The chemically driven dewetting and spreading observed here add to the methods available to study dynamic wetting (e.g., the moving three-phase contact line) of sessile droplets on surfaces. By slowing down chemical kinetics of the wetting, one is able to record the changing profile of the sessile droplet with time and gather information concerning the time-varying surface chemistry. The data also indicates a chemical interface hysteresis (CIH) that is compared to contact angle hysteresis (CAH). The approach can also be used to study the chemical etching and deposition behavior of thin films using liquids by monitoring the macroscopic droplet profile and relating this to the time-varying physical and chemical interface phenomena.

Stick-Jump (SJ) Evaporation of Strongly Pinned Nanoliter Volume Sessile Water Droplets on Quick Drying, Micropatterned Surfaces.

We present an experimental study of stick-jump (SJ) evaporation of strongly pinned nanoliter volume sessile water droplets drying on micropatterned surfaces. The evaporation is studied on surfaces composed of photolithographically micropatterned negative photoresist (SU-8). The micropatterning of the SU-8 enables circular, smooth, trough-like features to be formed which causes a very strong pinning of the three phase (liquid-vapor-solid) contact line of an evaporating droplet. This is ideal for studying SJ evaporation as it contains sequential constant contact radius (CCR) evaporation phases during droplet evaporation. The evaporation was studied in nonconfined conditions, and forced convection was not used. Micropatterned concentric circles were defined having an initial radius of 1000 µm decreasing by a spacing ranging from 500 to 50 µm. The droplet evaporates, successively pinning and depinning from circle to circle. For each pinning radius, the droplet contact angle and volume are observed to decrease quasi-linearly with time. The experimental average evaporation rates were found to decrease with decreasing pining radii. In contrast, the experimental average evaporation flux is found to increase with decreasing droplet radii. The data also demonstrate the influence of the initial contact angle on evaporation rate and flux. The data indicate that the total evaporation time of a droplet depends on the specific micropattern spacing and that the total evaporation time on micropatterned surfaces is always less than on flat, homogeneous surfaces. Although the surface patterning is observed to have little effect on the average droplet flux-indicating that the underlying evaporation physics is not significantly changed by the patterning-the total evaporation time is considerably modified by patterning, up to a factor or almost 2 compared to evaporation on a flat, homogeneous surface. The closely spaced concentric circle pinning maintains a large droplet radius and small contact angle from jump to jump; the result is a large evaporation rate leading to faster evaporation.

What is the Shape of an Air Bubble on a Liquid Surface?

We have calculated the equilibrium shape of the axially symmetric meniscus along which a spherical bubble contacts a flat liquid surface by analytically integrating the Young-Laplace equation in the presence of gravity, in the limit of large Bond numbers. This method has the advantage that it provides semianalytical expressions for key geometrical properties of the bubble in terms of the Bond number. Results are in good overall agreement with experimental data and are consistent with fully numerical (Surface Evolver) calculations. In particular, we are able to describe how the bubble shape changes from hemispherical, with a flat, shallow bottom, to lenticular, with a deeper, curved bottom, as the Bond number is decreased.

Controlled mud-crack patterning and self-organized cracking of polydimethylsiloxane elastomer surfaces.

Exploiting pattern formation - such as that observed in nature - in the context of micro/nanotechnology could have great benefits if coupled with the traditional top-down lithographic approach. Here, we demonstrate an original and simple method to produce unique, localized and controllable self-organised patterns on elastomeric films. A thin, brittle silica-like crust is formed on the surface of polydimethylsiloxane (PDMS) using oxygen plasma. This crust is subsequently cracked via the deposition of a thin metal film - having residual tensile stress. The density of the mud-crack patterns depends on the plasma dose and on the metal thickness. The mud-crack patterning can be controlled depending on the thickness and shape of the metallization - ultimately leading to regularly spaced cracks and/or metal mesa structures. Such patterning of the cracks indicates a level of self-organization in the structuring and layout of the features - arrived at simply by imposing metallization boundaries in proximity to each other, separated by a distance of the order of the critical dimension of the pattern size apparent in the large surface mud-crack patterns.

SU-8 as a material for lab-on-a-chip-based mass spectrometry.

This short review focuses on the application of SU-8 for the microchip-based approach to the miniaturization of mass spectrometry. Chip-based mass spectrometry will make the technology commonplace and bring benefits such as lower costs and autonomy. The chip-based miniaturization of mass spectrometry necessitates the use of new materials which are compatible with top-down fabrication involving both planar and non-planar processes. In this context, SU-8 is a very versatile epoxy-based, negative tone resist which is sensitive to ultraviolet radiation, X-rays and electron beam exposure. It has a very wide thickness range, from nanometres to millimetres, enabling the formation of mechanically rigid, very high aspect ratio, vertical, narrow width structures required to form microfluidic slots and channels for laboratory-on-a-chip design. It is also relatively chemically resistant and biologically compatible in terms of the liquid solutions used for mass spectrometry. This review looks at the impact and potential of SU-8 on the different parts of chip-based mass spectrometry - pre-treatment, ionization processes, and ion sorting and detection.

Moving liquids with light: photoelectrowetting on semiconductors.

By linking semiconductor physics and wetting phenomena a brand new effect termed "photoelectrowetting-on-semiconductors" is demonstrated here for a conducting droplet resting on an insulator-semiconductor stack. Optical generation of carriers in the space-charge region of the underlying semiconductor alters the capacitance of the liquid-insulator-semiconductor stack; the result of this is a modification of the wetting contact angle of the droplet upon illumination using above band gap light. The effect is demonstrated using commercial silicon wafers, both n- and p-type having a doping range spanning four orders of magnitude (6×10(14)-8×10(18) cm(-3)), coated with a commercial amorphous fluoropolymer insulating film (Teflon®). Impedance measurements confirm that the observations are semiconductor space-charge related effects. The impact of the work could lead to new silicon-based technologies in areas such as Laboratory-on-a-Chip, Microfluidics and Optofluidics.

Nanoscale devices for online dielectric spectroscopy of biological cells.

Nanoscale probes have been developed for the online characterization of the electrical properties of biological cells by dielectric spectroscopy. Two types of sensors have been designed and fabricated. The first one is devoted to low (<10 MHz) frequency range analysis and consists of gold nanoelectrodes. The second one works for high (>40 Hz) frequency range analysis and consists of a gold nanowire. The patterning of the sensors is performed by electron beam lithography. These devices are integrated in a microfluidic channel network for the manipulation of the cells and for the improvement of the performances of the sensors. These devices are used for the analysis of a well-characterized biological model in the area of the ligand-receptor interaction. The purpose is to monitor the interaction between the lactoferrin (the ligand) and the nucleolin and sulfated proteoglycans (the receptors) present or not on a set of mutant Chinese hamster ovary cell lines and their following internalization into the cytoplasm. Initial measurements have been performed with this microsystem and they demonstrate its capability for label-free, real-time, analysis of a dynamic mechanism involving biological cells.

An open design microfabricated nib-like nanoelectrospray emitter tip on a conducting silicon substrate for the application of the ionization voltage.

This paper describes a novel emitter tip having the shape of a nib and based on an open structure for nano-electrospray ionization mass spectrometry (nanoESI-MS). The nib structure is fabricated with standard lithography techniques using SU-8, an epoxy-based negative photoresist. The tip is comprised of a reservoir, a capillary slot and a point-like feature, and is fabricated on a silicon wafer. We present here a novel scheme for interfacing such nib tips to MS by applying the ionization voltage directly onto the semi-conductor support. The silicon support is in direct contact with the liquid to be analyzed at the reservoir and microchannel level, thus allowing easy use in ESI-MS. This scheme is especially advantageous for automated analysis as the manual step of positioning a metallic wire into the reservoir is avoided. In addition, the analysis performance was enhanced compared with the former scheme, as demonstrated by the tests of standard peptides (gramicidin S, Glu-fibrinopeptide B). The limit of detection was determined to be lower than 10(-2) microM. Due to their enhanced performance, these microfabricated sources might be of great interest for analysis requiring very high sensitivity, such as proteomics analysis using nanoESI-MS.

Integrated microfabricated systems including a purification module and an on-chip nano electrospray ionization interface for biological analysis.

We report here on an integrated microfabricated device dedicated to the preparation of biological samples prior to their on-line analysis by electrospray ionization-mass spectrometry (ESI-MS). This microfluidic device is fabricated using the negative photoresist SU-8 by microtechnology techniques. The device includes a chromatographic module plus an ESI interface for MS. The chromatographic module is dedicated to sample purification and is based on a polymer monolithic phase which includes hydrophobic moieties. The ESI interface is integrated onto the chip and is based on a capillary slot. We present here the integration of these different modules onto a single system that is fabricated via a SU-8-based microtechnology route. We present also their testing for the purification of peptide samples. This started with a partial integration step with the combination of at least two of the modules (microsystem + monolith; microsystem + nib) and their test before the fabrication and testing of fully integrated microsystems.

A nanofluidic emitter tip obtained by focused ion beam nanofabrication.

We report here the design, fabrication and testing of a novel nanofluidic device which we term a 'nano-nib' due to its resemblance to a nano-fountain pen. The nanofluidic device is an emitter tip which incorporates a nanofluidic capillary slot coupled to a microfluidic capillary slot. The microfluidic capillary slot is fabricated using reactive ion etching (RIE) whilst the nanofluidic capillary slot is fabricated using focused ion beam (FIB) etching. The microfluidic capillary slot has a length of 2 mm and capillary slot dimensions (w x h) of 1 microm x 4 microm, i.e. a volume of a few picolitres (pl). The smallest nanofluidic capillary slot has a length of 3 microm and capillary slot dimensions as small as 21 nm x 300 nm, i.e. a volume of a few attolitres (al). Current-voltage characterization in electrospray mode revealed a current of 1 nA at an applied voltage as low as 40 V. The applications for this nanofluidic device lie in high sensitivity electrospray mass spectrometry, direct nanowriting, ultralow volume sample extraction/spotting and printing.

A novel nib-like design for microfabricated nanospray tips.

We present here novel tips for nanoelectrosray ionization-mass spectrometry (ESI-MS) applications. These ionization sources have a planar geometry in the shape of a nib. Their functioning is based on a principle much akin to that of a fountain pen in that fluids are actuated by capillarity. Once a voltage is applied, an electrospray is formed at the nib tip. The nib fabrication relies on micromachining techniques using the epoxy-based negative photoresist SU-8 and a double exposure photolithographic process. Two types of nib-like sources were fabricated; they were made either conductive by metallization with a nickel layer or non-conductive but hydrophilic by covering them with a SiO(2) layer. In the latter case, the HV was applied via a Pt wire inserted into the reservoir feature of the nib. The nib-like sources were tested on an ion trap mass spectrometer using Gramicidin S samples at concentrations as low as 1 microM and ionization voltages as low as 1.2 kV. We have observed a good overall stability of the spray during the tests with no marked decrease in the signal intensity even under extreme conditions.