Plasticity in nanoscale friction: Static and dynamic

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Wide dynamic range 2-D nanoindentation: Friction and partial slip at contacts

A new nanomechanical testing system is described. It provides the same force controlled displacement sensing capability as nanoindentation, but now with two completely separated orthogonal axes. Load modulation enables direct determination of contact area and stiffness, both lateral and vertical, along with energy losses from the phase shifts. Two features in particular, wide dynamic ranges of several orders of magnitude of stiffness and a very high degree of mechanical separation (low crosstalk) between the axes, distinguish the technique from AFM. AFM is one of the few techniques to date to investigate tribological single asperity contacts but its mechanical limitations make it difficult to discern the underlying mechanisms. With this new technique, the evolution of a contact under 2-D stresses from deformation-free atomistic scale to initial plasticity along with the associated changes in geometry, can be monitored. Results will be presented showing that unlike in elastic contacts, Mindlin partial slip does not occur immediately under lateral stress in plastically deformed contacts. The evolution of contact area in the initial stages of sliding in the presence of plastic flow will be described, and resembles the predictions of classical Tabor and Johnson models. It will be shown that energy dissipation measured from phase shift of a modulating signal is largely due to interfacial friction rather than volumetric deformation. Prospects for further studies using both shear and normal loading will be discussed

Densification of polymer glass film under combined high pressure and shear flow revealed via scanning X-ray microscopy

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Direct measurement of molecular stiffness and damping in confined water layers

We present {\em direct} and {\em linear} measurements of the normal stiffness and damping of a confined, few molecule thick water layer. The measurements were obtained by use of a small amplitude (0.36 $\textrm{\AA}$), off-resonance Atomic Force Microscopy (AFM) technique. We measured stiffness and damping oscillations revealing up to 7 layers separated by 2.56 $\pm$ 0.20 $\textrm{\AA}$. Relaxation times could also be calculated and were found to indicate a significant slow-down of the dynamics of the system as the confining separation was reduced. We found that the dynamics of the system is determined not only by the interfacial pressure, but more significantly by solvation effects which depend on the exact separation of tip and surface. Thus ` solidification\rq seems to not be merely a result of pressure and confinement, but depends strongly on how commensurate the confining cavity is with the molecule size. We were able to model the results by starting from the simple assumption that the relaxation time depends linearly on the film stiffness.Comment: 7 pages, 6 figures, will be submitted to PR

Direct observation of yield in films by flat punch indentation

In regular indentation many strain states are simultaneously present in the indented region, so measured parameters such as hardness and modulus are average values over a wide range of strains. Testing of structures such as pillars, levers or film bulges enables determination of yield point and modulus with uniform strains in the sample, but requires specialised sample preparation and can be significantly affected by surface condition. Here we show how in-situ indentation with a flat punch allows direct observation of a discrete yield point in soft films on more rigid substrates. The yield point is clearly observable from the load displacement behaviour and from post indent AFM imaging. The film is in uniform uniaxial strain. Finite element simulations show that effective self-confinement by surrounding film material leads to uniformity throughout the film material down to surprisingly low aspect ratios around 4:1. This occurs for a significant range of stresses above the yield point. Eventually at even higher stresses the film material is extruded laterally. The characteristics of the yield event will be described as a function of temperature and film thickness for thin to ultrathin films. At higher aspect ratio and with sufficient stiffness of punch and substrate, quantitative, in-situ measurement of intrinsic stress vs. strain to well beyond the elastic limit becomes possible for thin films. The extent to which full constitutive relations for polymer films can be determied will be discussed, along with limitations of the technique

Quantitative STM imaging of metal surfaces

Many deductions made about STM images are based upon the model of Tersoff and Hamann, in which images are given in principal by a combination of surface atomic positions and local charge density. There is a now a need for a fuller understanding of this technique in order to explain experimental evidence which indicates that the tip and sample can interact strongly during normal imaging. In order to investigate the fundamental STM imaging process, a method for deducing the tunnel barrier height has been developed which is based on corrugation height measurements of constant current topographs. From experiments on clean Cu(100), values of the tunnel barrier height have been shown to be somewhat below the workfunction (~ 1-2.5eV) but are in good agreement with other reports of atomically resolved barrier height data. At large values of the tunnel conductance (~ 1μS), a fall-off (based upon extrapolation of large separation data) in the corrugation heights is observed with increasing conductance. This effect is quantitatively explained using a Molecular Dynamics simulation of the tip approaching the sample. The simulation gives a good estimate of both the absolute tip-sample separation and site-dependent tip-surface forces. Distributions of corrugation heights indicate that variations in both tip geometry and chemistry are likely to occur in practice and strongly influence the phenomena described above. Similarly, it is found that increased local tunnel barrier heights are measured when the Cu(100) surface is modified with small numbers of single halogen atoms. This data has been used to estimate the contributions to the increase in local barrier height of both adsorbate induced dipoles and geometric topography. Values for the charge transfer between the surface and adsorbate have been established. The process of tip-induced adsorbate manipulation has also been demonstrated at room temperature.</p

A direct-write, resistless hard mask for rapid nanoscale patterning of diamond

We introduce a simple, resist-free dry etch mask for producing patterns in diamond, both bulk and thin deposited films. Direct gallium ion beam exposure of the native diamond surface to doses as low as 1016 cm-2 forms a top surface hard mask resistant to both oxygen plasma chemical dry etching and, unexpectedly, argon plasma physical dry etching. Gallium implant hard masks of nominal 50 nm thickness demonstrate oxygen plasma etch resistance to over 450 nm depth, or 9:1 selectivity. The process offers significant advantages over direct ion milling of diamond including increased throughput due to separation of patterning and material removal steps, allowing both nanoscale patterning resolution as well as rapid masking of areas approaching millimetre scales. Retention of diamond properties in nanostructures formed by the technique is demonstrated by fabrication of specially shaped nanoindenter tips that can perform imprint pattern transfer at over 14 GPa pressure into gold and silicon surfaces. This resistless technique can be applied to curved and non-planar surfaces for a variety of potential applications requiring high resolution structuring of diamond coatings

Quantitative electrostatic force measurement in AFM

We describe a method for measuring forces in the atomic force microscope (AFM), in which a small amplitude oscillation(similar to 1 Angstrom(p-p)) is applied to a stiff(similar to 40 N/m) cantilever below its first resonant frequency, and the force gradient is measured directly as a function of separation. We have used this instrument to measure electrostatic forces by applying an ac voltage between the tip and the sample, and observed a variation in contact potential difference with separation. We also show how the benefits of this instrument may be exploited to make meaningful capacitance measurements, especially at small tip-surface separations, and demonstrate the potential of this technique for quantitative dopant profiling in semiconductors