An apparatus based on an atomic force microscope for implementing tip-controlled local breakdown.

Solid-state nanopores are powerful tools for sensing of single biomolecules in solution. Fabrication of solid-state nanopores is still challenging, however; in particular, new methods are needed to facilitate the integration of pores with larger nanofluidic and electronic device architectures. We have developed the tip-controlled local breakdown (TCLB) approach, in which an atomic force microscope (AFM) tip is brought into contact with a silicon nitride membrane that is placed onto an electrolyte reservoir. The application of a voltage bias at the AFM tip induces a dielectric breakdown that leads to the formation of a nanopore at the tip position. In this work, we report on the details of the apparatus used to fabricate nanopores using the TCLB method, and we demonstrate the formation of nanopores with smaller, more controlled diameters using a current limiting circuit that zeroes the voltage upon pore formation. Additionally, we demonstrate the capability of TCLB to fabricate pores aligned to embedded topographical features on the membranes.

One-to-one spatially matched experiment and atomistic simulations of nanometre-scale indentation.

We have carried out nanoindentation studies of gold in which the indenter is atomically characterized by field-ion microscopy and the scale of deformation is sufficiently small to be directly compared with atomistic simulations. We find that many features of the experiment are correctly reproduced by molecular dynamics simulations, in some cases only when an atomically rough indenter rather than a smooth repulsive-potential indenter is used. Heterogeneous nucleation of dislocations is found to take place at surface defect sites. Using input from atomistic simulations, a model of indentation based on stochastic transitions between continuum elastic-plastic states is developed, which accurately predicts the size distributions of plastic 'pop-in' events and their dependence on tip geometry.

Effect of using stencil masks made by focused ion beam milling on permalloy (Ni81Fe19) nanostructures.

Focused ion beam (FIB) milling is a common fabrication technique to make nanostencil masks which has the unintended consequence of gallium ion implantation surrounding milled features in silicon nitride membranes. We observe major changes in film structure, chemical composition, and magnetic behaviour of permalloy nanostructures deposited by electron beam evaporation using silicon nitride stencil masks made by a FIB as compared to stencil masks made by regular lithography techniques. We characterize the stenciled structures and both types of masks using transmission electron microscopy, electron energy loss spectroscopy, energy dispersive x-ray spectroscopy, magnetic force microscopy and kelvin probe force microscopy. All these techniques demonstrate distinct differences at a length scale of a 1-100 nm for the structures made using stencil mask fabricated using a FIB. The origin of these differences seems to be related to the presence of implanted ions, a detailed understanding of the mechanism however remains to be developed.

Field deposition from metallic tips onto insulating substrates.

The deposition of gold ions from atomic force microscope cantilever tips onto bulk insulating substrates with nearby surface electrodes is discussed. Numerical models of the potential distribution are used to estimate potential barriers for the desorption process. These models indicate deposition height thresholds of 7-10 nm with the tip 20-25 nm from the metallic electrode edge over a KBr surface but greater than 20 nm high for InP/GaAs/InP substrates with a two-dimensional electron gas (2DEG) as the back electrode. Experimental results for the deposition of gold clusters over KBr surfaces near metal electrodes in ultra-high vacuum (UHV) are presented and show promising agreement with calculations of the deposition threshold heights. Deposition of clusters over InP is discussed for comparison and indicates similar trends.

High Q optical fiber tips for NC-AFM in liquid.

Non-contact atomic force microscopy is rapidly expanding from ultra-high vacuum to include the study of surfaces and biomolecules in liquids by high resolution imaging and force spectroscopy. This is despite the additional frequency shift noise due to the inherently low Q factor of the cantilever oscillating in a liquid. In this paper we present a tip based on an optical fiber which can operate in liquid with Q factors in excess of 100 using a 'diving bell' arrangement which allows only a small portion of the tip to be submerged. We demonstrate stable imaging and force spectroscopy using this set-up. The tips are based on scanning near-field optical microscopy tips and, when used with NC-AFM, provide a method of combining both high resolution mechanical and fluorescence studies of biomolecules and cells.

Determination of the local contact potential difference of PTCDA on NaCl: a comparison of techniques.

There has been increasing focus on the use of Kelvin probe force microscopy (KPFM) for the determination of local electronic structure in recent years, especially in systems where other methods, such as scanning tunnelling microscopy/spectroscopy, may be intractable. We have examined three methods for determining the local apparent contact potential difference (CPD): frequency modulation KPFM (FM-KPFM), amplitude modulation KPFM (AM-KPFM), and frequency shift-bias spectroscopy, on a test system of 3,4,9,10-perylene tetracarboxylic dianhydride (PTCDA) on NaCl, an example of an organic semiconductor on a bulk insulating substrate. We will discuss the influence of the bias modulation on the apparent CPD measurement by FM-KPFM compared to the DC-bias spectroscopy method, and provide a comparison of AM-KPFM, AM-slope detection KPFM and FM-KPFM imaging resolution and accuracy. We will also discuss the distance dependence of the CPD as measured by FM-KPFM for both the PTCDA organic deposit and the NaCl substrate.

Molecular dewetting on insulators.

Recent attention given to the growth and morphology of organic thin films with regard to organic electronics has led to the observation of dewetting (a transition from layer(s) to islands) of molecular deposits in many of these systems. Dewetting is a much studied phenomenon in the formation of polymer and liquid films, but its observation in thin films of the 'small' molecules typical of organic electronics requires additional consideration of the structure of the interface between the molecular film and the substrate. This review covers some key concepts related to dewetting and molecular film growth. In particular, the origins of different growth modes and the thickness dependent interactions which give rise to dewetting are discussed in terms of surface energies and the disjoining pressure. Characteristics of molecular systems which may lead to these conditions, including the formation of metastable interface structures and commensurate-incommensurate phase transitions, are also discussed. Brief descriptions of some experimental techniques which have been used to study molecular dewetting are given as well. Examples of molecule-on-insulator systems which undergo dewetting are described in some detail, specifically perylene derivatives on alkali halides, C(60) on alkali halides, and the technologically important system of pentacene on SiO(2). These examples point to some possible predicting factors for the occurrence of dewetting, most importantly the formation of an interface layer which differs from the bulk crystal structure.

Strain induced dewetting of a molecular system: bimodal growth of PTCDA on NaCl.

Submonolayer coverages of the molecule 3,4,9,10-perylene tetracarboxylic dianhydride (PTCDA) deposited on NaCl(001) surfaces were imaged with high resolution noncontact-atomic force microscopy. Two island types were observed: monolayer islands with a p3x3 epitaxy at low coverage and a mixture of these and bulklike crystallites at higher coverage. The transition between the pure monolayer islands and mixed islands occurs at approximately 0.85 ML, corresponding to a complete p3x3 layer. Calculations show the p3x3 epitaxy to be incompatible with a multilayer crystal of PTCDA. Consequently, the growth of additional layers results in an adaptation of the interface structure forcing a dewetting transition.

Comment on 'Temperature dependence of the energy dissipation in dynamic force microscopy'.

A recent article in this journal by Roll et al (2008 Nanotechnology 19 045703) presents experimental results of the temperature dependence of dissipation in dynamic force microscopy which they use to elucidate the mechanisms of such a dissipation signal in the PTCDA on KBr system. We argue here that dissipation results are often highly dependent upon the tip structure, and urge caution in the interpretation of single sets of experimental data.

Nucleation and submonolayer growth of C60 on KBr.

Noncontact atomic force microscopy has been applied to the prototypical molecule-insulator system C60 on KBr to study nucleation and submonolayer growth. Overview images reveal an island growth mode with unusual branching structures. Simultaneous molecular and atomic resolution on the C60 and KBr surfaces, respectively, was obtained revealing a coincident 8x3 superstructure. Also, a 21+/-3 pm apparent height difference was observed in atomic force microscopy topographies between some first layer molecules. One of the initial nucleation sites of the C60 islands was determined by observation of loosely bound molecules at kink sites in monatomic KBr steps, in conjunction with the observation that islands form preferentially at step edges.

Surface relaxations, current enhancements, and absolute distances in high resolution scanning tunneling microscopy.

We have performed the most realistic simulation to date of the operation of a scanning tunneling microscope. Probe-sample distances from beyond tunneling to actual surface contact are covered. We simultaneously calculate forces, atomic displacements, and tunneling currents, allowing quantitative comparison with experimental values. A distance regime below which the probe becomes unstable is identified. It is shown that the real distance differs substantially from previous estimates because of large atomic displacements on the surface and at the probe tip.

Creation of liquid crystal waveguides with scanning force microscopy.

The rubbing of a polymer layer, a commonly applied process, leads to an anisotropic surface morphology, aligning liquid crystal molecules. Scanning force microscopy can be used to intentionally create areas with a similar anisotropy by operating the instrument at loads in the range of 10(-7) to 10(-5) newtons. These areas have an orientation effect on liquid crystals indistinguishable from the rubbing process, which allows a systematic investigation of the orientation properties of an alignment layer as a function of its nanometer-scale morphology. Refractive index patterns can be tailored with this method by scratching a suitable area, as demonstrated by fabrication of an optical waveguide 6 micrometers wide and 5 millimeters long.