Fabrication of nanoporous carbon by electrical transformation of amorphous carbon nanospheres.

Nanoporous carbon nanospheres <150 nm in diameter have been fabricated for the first time by the transformation of amorphous carbon nanospheres under Joule heating. The process, initiated by current densities of 1.5-8 × 10(10) A m(-2), has been imaged in real time in situ in a transmission electron microscope. Significant atomic diffusion and carbon ordering results in the formation of a 3D network of buckled graphitic sheets bounding interlinked <5 nm diameter pores, with greatly enhanced conductivity. Porous carbon nanospheres offer new opportunities for biocompatible drug delivery, catalysis and energy storage.

Fabrication of a nickel nanowire mesh electrode suspended on polymer substrate.

We report on an efficient strategy for the fabrication of an ultra-long suspended nanowire mesh suitable for nanodevice architectures on a polymer surface. First, nickel nanowires are synthesized directly on a template substrate by magnetron sputtering. Laser interference lithography followed by deep reactive ion etching is used to create the nanograted template substrate constituted of one-dimensional line pattern arrays of 240 nm in periodicity. Ordered alignment of ultra-long nanowires (∼180 nm in diameter) with high fidelity to the template pattern is observed by scanning electron microscopy. The transfer of the pre-defined parallel nanowire array from the template surface to a target polymer substrate for electrical characterization of the system is demonstrated. The electrical behaviour of the nanowire mesh, suspended between two electrodes, was found to be linear, stable, and reproducible. This result suggests that this nanofabrication process will open an efficient way to the design and construction of novel nanodevices.

Friction-formed liquid droplets.

The formation of nanoscale liquid droplets by friction of a solid is observed in real-time. This is achieved using a newly developed in situ transmission electron microscope (TEM) triboprobe capable of applying multiple reciprocating wear cycles to a nanoscale surface. Dynamical imaging of the nanoscale cyclic rubbing of a focused-ion-beam (FIB) processed Al alloy by diamond shows that the generation of nanoscale wear particles is followed by a phase separation to form liquid Ga nanodroplets and liquid bridges. The transformation of a two-body system to a four-body solid-liquid system within the reciprocating wear track significantly alters the local dynamical friction and wear processes. Moving liquid bridges are observed in situ to play a key role at the sliding nanocontact, interacting strongly with the highly mobile nanoparticle debris. In situ imaging demonstrates that both static and moving liquid droplets exhibit asymmetric menisci due to nanoscale surface roughness. Nanodroplet kinetics are furthermore dependent on local frictional temperature, with solid-like surface nanofilaments forming on cooling. TEM nanotribology opens up new avenues for the real-time quantification of cyclic friction, wear and dynamic solid-liquid nanomechanics, which will have widespread applications in many areas of nanoscience and nanotechnology.

The formation of carbon nanostructures by in situ TEM mechanical nanoscale fatigue and fracture of carbon thin films.

A technique to quantify in real time the microstructural changes occurring during mechanical nanoscale fatigue of ultrathin surface coatings has been developed. Cyclic nanoscale loading, with amplitudes less than 100 nm, is achieved with a mechanical probe miniaturized to fit inside a transmission electron microscope (TEM). The TEM tribological probe can be used for nanofriction and nanofatigue testing, with 3D control of the loading direction and simultaneous TEM imaging of the nano-objects. It is demonstrated that fracture of 10-20 nm thick amorphous carbon films on sharp gold asperities, by a single nanoscale shear impact, results in the formation of <10 nm diameter amorphous carbon filaments. Failure of the same carbon films after cyclic nanofatigue, however, results in the formation of carbon nanostructures with a significant degree of graphitic ordering, including a carbon onion.

MRT letter: full-tilt electron tomography with a piezo-actuated rotary drive.

Piezoelectric nanoactuation, which is rapidly becoming established as state-of-the-art positioning control in transmission electron microscopy (TEM), is extended here to include a rotational degree of freedom. A piezoelectric goniometer with both translational and rotary drive action has been designed with high level of miniaturization to fit into a standard TEM specimen holder shaft without compromising any of the performance of the default TEM goniometer and without any modifications to the TEM. Enhanced functionality of such a goniometer-in-goniometer is outlined and experimental results for electron tomography of nanostructures over a full tilt range of views, without any missing angles, are demonstrated.

Evolution of residual stress and crack morphologies during 3D FIB tomographic analysis of alumina.

Three-dimensional focused ion beam (FIB) tomography is increasingly being used for 3D characterization of microstructures in the 50 nm-20 microm range. FIB tomography is a destructive, invasive process, and microstructural changes may potentially occur during the analysis process. Here residual stress and crack morphologies in single-crystal sapphire samples have been concurrently analyzed using Cr3+ fluorescence spectroscopy and FIB tomography. Specifically, maps of surface residual stress have been obtained from optically polished single-crystal alumina [surface orientation (1 i 0 2)], from FIB milled surface trenches, from Vickers micro-indentation sites (loads 50 g-300 g), and from Vickers micro-indentation sites during FIB serial sectioning. The residual stress maps clearly show that FIB sputtering generates residual stress changes. For the case of the Vickers micro-indentations, FIB sputtering causes significant changes in residual stress during the FIB tomographic serial sectioning. 3D reconstruction of the crack distribution around micro-indentation sites shows that the cracks observed are influenced by the location of the FIB milled surface trenches due to localized stress changes.

Thermal stability of Ti and Pt nanowires manufactured by Ga+ focused ion beam.

Ti and Pt nanowires have been produced by ultra high-vacuum molecular beam epitaxy deposition of Ti thin films and focused ion beam (FIB) deposition of Pt thin films, followed by cross-sectional FIB sputtering to form electron-transparent nanowires. The thermal stability of the nanowires has been investigated by in situ thermal cycling in a transmission electron microscope. Epitaxial single crystal Ti nanowires on (0001)Al(2)O(3) substrates are microstructurally stable up to 550-600 degrees C, above which limited dislocation motion is activated shortly before the Ti-wires oxidize. The amorphous FIB-deposited Pt wires are stable up to 580-650 degrees C where partial crystallization is observed in vacuum. Faceted nanoparticles grow on the wire surface, growing into free space by surface diffusion and minimizing contact area with the underlying wire. The particles are face-centred cubic (fcc) Pt with some dissolved Ga. Continued heating results in particle spheroidization, coalescence and growth, retaining the fcc structure.

Subsurface deformation of machined Al2O3 and Al2O3/5vol%SiC nanocomposite.

Under machine grinding, material removal in monolithic Al2O3 is by intergranular fracture and grain pull-out. In comparison, under the same grinding conditions, an Al2O3/5%SiC nanocomposite undergoes significant surface grooving and intragranular fracture. The subsurface deformation mechanisms were investigated by cross-sectional transmission electron microscopy. For Al2O3, the residual deformation zone was localized very close to the surface in the first layer of grains, with dislocations occurring only within 1.5 µm of the top surface and a high density of basal twins penetrating to a depth of one single grain. Cracks were present along grain boundaries or basal twin interfaces. For Al2O3/SiC nanocomposites, the main residual plastic deformation is observed to be dislocations activated to a depth of about 10 µm (approx. 3-4 grains), with twinning rarely observed. Possible mechanisms by which the SiC particles influence the subsurface deformation and material removal modes are discussed.

Subsurface nanoindentation deformation of Cu-Al multilayers mapped in 3D by focused ion beam microscopy.

A new technique for the three-dimensional analysis of subsurface damage of nanocomposites is presented. Cu-Al multilayers, grown epitaxially on (0001)Al2O3 single crystals by ultra high vacuum molecular beam epitaxy, have been deformed by nanoindentation. Systematic slicing and imaging of the deformed region by focused ion beam microscopy enables a 3D data set of the damaged region to be collected. From this 3D data set, profiles of the deformed sub-surface interfaces can be extracted. This enables the deformation of the individual layers, substrate and overall film thickness to be determined around the damage site. These 3D deformation maps have exciting implications for the analysis of mechanical deformation of nanocomposites on a sub-micrometre scale.