Near-field optical taper antennas fabricated with a highly replicable ac electrochemical etching method.

This paper describes a novel chemical etching method to fabricate high quality near-field optical antennas-tapered metallic tips-from gold wire in a reproducible way for optically probing a specimen on the nanoscale. A new type of an electrochemical cell is introduced and different dc and ac etching regimes are studied in detail. The formation and dynamics of a meniscus around a gold wire immersed in an electrolyte when supplying a square wave voltage are considered. We show that in situ etching current kinetics allows one to improve a yield of tips with a well-defined geometry up to 95% by filtering these on the basis of a cutoff current and a power spectrum of etching current fluctuations. As a quantitative measure for estimating the yield we introduce a probability to find tips with curvature radii falling in the range of interest. Testing the tips for a plasmonic effect is implemented with tip-enhanced Raman spectroscopy and sub-wavelength imaging of a thin fullerene film.

Quantitative Conductive Atomic Force Microscopy on Single-Walled Carbon Nanotube-Based Polymer Composites.

Conductive atomic force microscopy (C-AFM) is a valuable technique for correlating the electrical properties of a material with its topographic features and for identifying and characterizing conductive pathways in polymer composites. However, aspects such as compatibility between tip material and sample, contact force and area between the tip and the sample, tip degradation and environmental conditions render quantifying the results quite challenging. This study aims at finding the suitable conditions for C-AFM to generate reliable, reproducible, and quantitative current maps that can be used to calculate the resistance in each point of a single-walled carbon nanotube (SWCNT) network, nonimpregnated as well as impregnated with a polymer. The results obtained emphasize the technique's limitation at the macroscale as the resistance of these highly conductive samples cannot be distinguished from the tip-sample contact resistance. Quantitative C-AFM measurements on thin composite sections of 150-350 nm enable the separation of sample and tip-sample contact resistance, but also indicate that these sections are not representative for the overall SWCNT network. Nevertheless, the technique was successfully used to characterize the local electrical properties of the composite material, such as sample homogeneity and resistance range of individual SWCNT clusters, at the nano- and microscale.

Single-walled carbon nanotube networks in conductive composite materials.

Electrically conductive composite materials can be used for a wide range of applications because they combine the advantages of a specific polymeric material (e.g., thermal and mechanical properties) with the electrical properties of conductive filler particles. However, the overall electrical behaviour of these composite materials is usually much below the potential of the conductive fillers, mainly because by mixing two different components, new interfaces and interphases are created, changing the properties and behaviours of both. Our goal is to characterize and understand the nature and influence of these interfaces on the electrical properties of composite materials. We have improved a technique based on the use of sodium carboxymethyl cellulose (CMC) to disperse single-walled carbon nanotubes (SWCNTs) in water, followed by coating glass substrates, and drying and removing the CMC with a nitric acid treatment. We used electron microscopy and atomic force microscopy techniques to characterize the SWCNT films, and developed an in situ resistance measurement technique to analyse the influence of both the individual components and the mixture of an epoxy/amine system on the electrical behaviour of the SWCNTs. The results showed that impregnating a SWCNT network with a polymer is not the only factor that affects the film resistance; air exposure, temperature, physical and chemical properties of the individual polymer components, and also the formation of a polymeric network, can all have an influence on the macroscopic electrical properties of the initial SWCNT network. These results emphasize the importance of understanding the effects that each of the components can have on each other before trying to prepare an efficient polymer composite material.