[en] Electrostatic modes of atomic force microscopy have shown to be non-destructive and relatively simple methods for imaging conductors embedded in insulating polymers. Here we use electrostatic force microscopy to image the dispersion of carbon nanotubes in a latex-based conductive composite, which brings forth features not observed in previously studied systems employing linear polymer films. A fixed-potential model of the probe-nanotube electrostatics is presented which in principle gives access to the conductive nanoparticle's depth and radius, and the polymer film dielectric constant. Comparing this model to the data results in nanotube depths that appear to be slightly above the film–air interface. Furthermore, this result suggests that water-mediated charge build-up at the film–air interface may be the source of electrostatic phase contrast in ambient conditions.

[en] Individual carbon nanotubes (CNTs) exhibit exceptional mechanical properties. However, difficulties remain in fully realizing these properties in CNT macro-assemblies, because the weak inter-tube forces result in the CNTs sliding past one another. Here in this study, a simple solid-state reaction is presented that enhances the mechanical properties of carbon nanotube fibers (CNTFs) through simultaneous covalent functionalization and crosslinking. This is the first chemical crosslinking proposed without the involvement of a catalyst or byproducts. The specific tensile strength of CNTFs obtained from the treatment employing a benzocyclobutene-based polymer is improved by 40%. Such improvement can be attributed to a reduced number of voids, impregnation of the polymer, and the formation of covalent crosslinks. This methodology is confirmed using both multiwalled nanotube (MWNT) powders and CNTFs. Thermogravimetric analysis, differential scanning calorimetry, x-ray photoelectron spectroscopy, and transmission electron microscopy of the treated MWNT powders confirm the covalent functionalization and formation of inter-tube crosslinks. This simple one-step reaction can be applied to industrial-scale production of high-strength CNTFs.

[en] We address the impact of metal co-deposition in the nanodot patterning dynamics of Si(100) surfaces under normal-incidence 1 keV Ar⁺ ion-beam sputtering (IBS). In particular, the effect of both the metal nature (Fe or Mo) and flux has been studied. Morphological and compositional evolution were followed by atomic force microscopy (AFM) and Rutherford backscattering spectrometry, respectively. For the same type of impurity, the dynamics is faster for a higher co-deposition flux, which also drives to larger asymptotic roughness and wavelength. Mo co-deposition yields rougher surfaces for a lower metal coverage than Fe and, remarkably, higher ordered patterns. X-ray photoelectron spectroscopy reveals the formation of silicide bonds even before pattern onset, stressing the relevant role of the affinity of the co-deposited metals for silicon. Further, current-sensing AFM performed at the initial and asymptotic stages indicates that the nanodot structures are metal-rich, resulting in coupled compositional and morphological patterns. These results are discussed in terms of phase segregation, morphology-driven local flux variations of impurities and silicide formation. This analysis reveals that the underlying (concurrent) mechanisms of pattern formation are complex since many processes can come into play with a different relative weight depending on the specific patterning conditions. From a practical point of view, it is shown that, by proper selection of the process parameters, IBS with metal co-deposition can be used to tune the dynamics and pattern properties and, interestingly, to produce highly ordered arrays. (paper)

[en] The antireflective characteristics of Si nanocone (NC) arrays were estimated using a theory devised for an inhomogeneous antireflection layer, and further verified by the Fourier modal method (FMM). Considering a better impedance matching from air to Si, a minimum depth of 400 nm is essentially required. Although Si NC arrays have usually been suggested to be at a base diameter of ∼300 nm for infinitely thick Si wafers, as wafers become thinner than 50 μm, the optimal base diameter of the NCs is suggested to be ∼500 nm so as to excite more resonant modes. Our simulation work indicates that geometrical parameters such as the top diameter and filling ratio of the NCs are much more sensitive in terms of optimizing the optical performance on ultrathin (∼5 μm) wafers, suggesting the need for strict control of the surface morphology in the nanostructure fabrication process. (paper)

[en] High-quality colloidal crystals (CCs) are important for use in photonic research and as templates for large-scale plasmonic SERS substrates. We investigated how variations in temperature, colloid concentration, and dip-drawing parameters (rate, incubation time, etc) affect the structure of 2D CCs formed by highly monodisperse silica nanoparticles (SiNPs) synthesized in an l-arginine solution and regrown by a modified Stöber method. The best quality 2D CCs were obtained with aqueous 12 wt% colloids at a temperature of 25 °C, an incubation time of 1 min, and a drawing rate of 50 mm min⁻¹. Assembling of gold nanorods (GNRs) on 2D CCs resulted in the formation of ring-like chains with a preferential tail-to-tail orientation along the hexagonal boundaries. To the best of our knowledge, this is the first time that such nanostructures have been prepared. Owing to the preferential tail-to-tail packing of GNRs, 2D SiNP CC + GNR substrates demonstrated an analytical SERS enhancement of about 8000, which was 10 to 15 times higher than that for self-assembled GNRs on a silicon wafer. In addition, the analytical SERS enhancement was almost 60 times lower after replacing the nanorods in 2D SiNP CC + GNR substrates with 25 nm gold nanospheres. (paper)

[en] Core–shell InSb-SiO₂ nanoballs/microballs were synthesized on a Si substrate by carbonthermal reactions at a temperature of 900 °C. High-resolution transmission microscopy (HRTEM) images revealed that the surfaces of the InSb nanoballs/microballs were covered by amorphous SiO₂ layers. On the basis of our theoretical calculation, the thermal expansion coefficient (TEC) of the InSb crystals is ten times higher than that of the SiO₂ shell. Therefore, the SiO₂ serves as a constraining shell for the InSb core so that the compressive stress of ∼−94 MPa can accumulate in the InSb core while a tensile stress of 196 MPa forms in the SiO₂ shell. The thermal excitation accumulated compressive stress in the InSb core, causing a partial structural phase transition from a cubic zinc-blende structure to a hexagonal wurtzite structure. Many lattice defects, such as stacking faults and Moiré fringes, have been observed on the surface of the InSb core. In situ temperature-dependent XRD patterns showed that a reversible InSb hexagonal (002) peak appeared and disappeared as the temperature increased and decreased at a transit point of 200 °C, respectively. As the temperature increased, the XRD diffraction peaks of the InSb wurtzite phase shifted significantly to lower angles because of the formation of compressive stress in the InSb nanoballs. The pressure-induced partial structural phase transitions of the nanostructured InSb occurred at −94 MPa of the compressive stress. This is the first report of this value, which is the lowest value in the pressure-induced phase transition of the nanostructure InSb from the cubic zinc-blende structure to the hexagonal wurtzite structure. (paper)

[en] AFM images are always affected by artifacts arising from tip convolution effects, resulting in a decrease in the lateral resolution of this technique. The magnitude of such effects is described by means of geometrical considerations, thereby providing better understanding of the convolution phenomenon. We demonstrate that for a constant tip radius, the convolution error is increased with the object height, mainly for the narrowest motifs. Certain influence of the object shape is observed between rectangular and elliptical objects with the same height. Such moderate differences are essentially expected among elongated objects; in contrast they are reduced as the object aspect ratio is increased. Finally, we propose an algorithm to study the influence of the size, shape and aspect ratio of different nanometric motifs on a flat substrate. Indeed, with this algorithm, convolution artifacts can be extended to any kind of motif including real surface roughness. From the simulation results we demonstrate that in most cases the real motif’s width can be estimated from AFM images without knowing its shape in detail. (paper)

[en] The transfer doping of diamond surfaces has been applied in various novel two-dimensional electronic devices. Its extension to nanodiamonds (ND) is essential for ND-based applications in many fields. In particular, understanding the influence of the crystallite size on transfer doping is desirable. Here, we report the results of a detailed study of the electronic energetic band structure of single, isolated transfer-doped nanodiamonds with nanometric resolution using a combination of scanning tunneling spectroscopy and Kelvin force microscopy measurements. The results show how the band gap, the valence band maximum, the electron affinity and the work function all depend on the ND’s size and nanoparticle surface properties. The present analysis, which combines information from both scanning tunneling spectroscopy and Kelvin force microscopy, should be applicable to any nanoparticle or surface that can be measured with scanning probe techniques. (paper)

[en] The process of the formation and disruption of nanometric conductive filaments in a HfO₂/TiN structure is investigated by conductive atomic force microscopy. The preforming state evidences nonhomogeneous conduction at high fields through conductive paths, which are associated with pre-existing defects and develop into conductive filaments with a forming procedure. The disruption of the same filaments is demonstrated as well, according to a bipolar operation. In addition, the conductive tip of the microscopy is exploited to perform electrical operations on single conductive spots, which evidences that neighboring conductive filaments are not electrically independent. We propose a picture that describes the evolution of the shape of the conductive filaments in the processes of their formation and disruption, which involves the development of conductive branches from a common root; this root resides in the pre-existing defects that lay at the HfO₂/TiN interface. (paper)

[en] We study charge transport in a monolayer MoS₂ nanoflake over a wide range of carrier density, temperature and electric bias. We find that the transport is best described by a percolating picture in which the disorder breaks translational invariance, breaking the system up into a series of puddles, rather than previous pictures in which the disorder is treated as homogeneous and uniform. Our work provides insight to a unified picture of charge transport in monolayer MoS₂ nanoflakes and contributes to the development of next-generation MoS₂-based devices. (paper)