Removal of epoxy-attached thin-sections from glass slides by plasma-etching

Thin-sectioned samples mounted on glass slides with common petrographic epoxies cannot be easily removed (for subsequent ion-milling) by standard methods such as heating or dissolution in solvents. A method for the removal of such samples using a radio frequency (RF) generated oxygen plasma has been investigated for a number of typical petrographic and ceramic thin sections. Sample integrity and thickness were critical factors that determined the etching rate of adhesive and the survivability of the sample. Several tests were performed on a variety of materials in order to estimate possible heating or oxidation damage from the plasma. Temperatures in the plasma chamber remained below 138°C and weight changes in mineral powders etched for 76 hr were less than ±4%. A crystal of optical grade calcite showed no apparent surface damage after 48 hr of etching. Any damage from the oxygen plasma is apparently confined to the surface of the sample, and is removed during the ion-milling stage of transmission electron microscopy (TEM) sample preparation.

Matrix metalloproteinase biosensor based on a porous silicon reflector

Matrix metalloproteinases (MMPs) are proteolytic enzymes important to wound healing. In non-healing wounds, it has been suggested that MMP levels become dysfunctional, hence it is of great interest to develop sensors to detect MMP biomarkers. This study presents the development of a label-free optical MMP biosensor based on a functionalised porous silicon (pSi) thin film. The biosensor is fabricated by immobilising a peptidomimetic MMP inhibitor in the porous layer using hydrosilylation followed by amide coupling. The binding of MMP to the immobilised inhibitor translates into a change of effective optical thickness (EOT) over the time. We investigate the effect of surface functionalisation on the stability of pSi surface and evaluate the sensing performance. We successfully demonstrate MMP detection in buffer solution and human wound fluid at physiologically relevant concentrations. This biosensor may find application as a point-of-care device that is prognostic of the healing trajectory of chronic wounds.

In situ imaging of catalytic etching on silver during methanol oxidation conditions by environmental scanning electron microscopy

Polycrystalline silver is used to catalytically oxidise methanol to formaldehyde. This paper reports the results of extensive investigations involving the use of environmental scanning electron microscopy (ESEM) to monitor structural changes in silver during simulated industrial reaction conditions. The interaction of oxygen, nitrogen, and water, either singly or in combination, with a silver catalyst at temperatures up to 973 K resulted in the appearance of a reconstructed silver surface. More spectacular was the effect an oxygen/methanol mixture had on the silver morphology. At a temperature of ca. 713 K pinholes were created in the vicinity of defects as a consequence of subsurface explosions. These holes gradually increased in size and large platelet features were created. Elevation of the catalyst temperature to 843 K facilitated the wholescale oxygen induced restructuring of the entire silver surface. Methanol reacted with subsurface oxygen to produce subsurface hydroxyl species which ultimately formed water in the subsurface layers of silver. The resultant hydrostatic pressure forced the silver surface to adopt a "hill and valley" conformation in order to minimise the surface free energy. Upon approaching typical industrial operating conditions widespread explosions occurred on the catalyst and it was also apparent that the silver surface was extremely mobile under the applied conditions. The interaction of methanol alone with silver resulted in the initial formation of pinholes primarily in the vicinity of defects, due to reaction with oxygen species incorporated in the catalyst during electrochemical synthesis. However, dramatic reduction in the hole concentration with time occurred as all the available oxygen became consumed. A remarkable correlation between formaldehyde production and hole concentration was found.

Investigations of the physical origins of etching LiNbO3 during Ti in-diffusion

We investigate the physical origins of etching observed during Ti diffusion. The relationship between observed etch depth and water vapor content in the annealing environment is quantified. The dynamics of the etching process are also identified. It is discovered that water vapor content is essential for etching and that there is a characteristic delay before etching is observed. From these observations we can conclude that the process is electrochemical in nature with ionic defects diffusing into the Ti strip from the lithium niobate and these defects catalyzing the dissociation of water into reactive ions.

Copper-capped carbon nanocones on silicon : plasma-enabled growth control

Controlled self-organized growth of vertically aligned carbon nanocone arrays in a radio frequency inductively coupled plasma-based process is studied. The experiments have demonstrated that the gaps between the nanocones, density of the nanocone array, and the shape of the nanocones can be effectively controlled by the process parameters such as gas composition (hydrogen content) and electrical bias applied to the substrate. Optical measurements have demonstrated lower reflectance of the nanocone array as compared with a bare Si wafer, thus evidencing their potential for the use in optical devices. The nanocone formation mechanism is explained in terms of redistribution of surface and volumetric fluxes of plasma-generated species in a developing nanocone array and passivation of carbon in narrow gaps where the access of plasma ions is hindered. Extensive numerical simulations were used to support the proposed growth mechanism.

Plasma-made silicon nanograss and related nanostructures

Plasma-made nanostructures show outstanding potential for applications in nanotechnology. This paper provides a concise overview on the progress of plasma-based synthesis and applications of silicon nanograss and related nanostructures. The materials described here include black silicon, Si nanotips produced using a self-masking technique as well as self-organized silicon nanocones and nanograss. The distinctive features of the Si nanograss, two-tier hierarchical and tilted nanograss structures are discussed. Specific applications based on the unique features of the silicon nanograss are also presented.

Plasma nanoscience : setting directions, tackling grand challenges

This review paper presents historical perspectives, recent advances and future directions in the multidisciplinary research field of plasma nanoscience. The current status and future challenges are presented using a three-dimensional framework. The first and the largest dimension covers the most important classes of nanoscale objects (nanostructures, nanofeatures and nanoassemblies/nanoarchitectures) and materials systems, namely carbon nanotubes, nanofibres, graphene, graphene nanoribbons, graphene nanoflakes, nanodiamond and related carbon-based nanostructures; metal, silicon and other inorganic nanoparticles and nanostructures; soft organic nanomaterials; nano-biomaterials; biological objects and nanoscale plasma etching. In the second dimension, we discuss the most common types of plasmas and plasma reactors used in nanoscale plasma synthesis and processing. These include low-temperature non-equilibrium plasmas at low and high pressures, thermal plasmas, high-pressure microplasmas, plasmas in liquids and plasma–liquid interactions, high-energy-density plasmas, and ionized physical vapour deposition as well as some other plasma-enhanced nanofabrication techniques. In the third dimension, we outline some of the 'Grand Science Challenges' and 'Grand Socio-economic Challenges' to which significant contributions from plasma nanoscience-related research can be expected in the near future. The urgent need for a stronger focus on practical, outcome-oriented research to tackle the grand challenges is emphasized and concisely formulated as from controlled complexity to practical simplicity in solving grand challenges.

Different nanostructures from different plasmas : nanoflowers and nanotrees on silicon

Using the advanced radio-frequency plasma-assisted magnetron deposition system, various nanostructures such as nanoflowers of carbon nanotubes, ZnO nanobelts, and silicon nanotrees were successfully synthesized. In this paper, we present the photographs of ICP and magnetron discharges, the photograph of a complex plasma structure, and the SEM images of various nanostructures synthesized in the system with magnetron and ICP sources operating simultaneously.

Plasma-enabled growth of separated, vertically aligned copper-capped carbon nanocones on silicon

The formation of vertically aligned, clearly separated, copper-capped carbon nanocones with a length of up to 500 nm and base diameter of about 150 nm via three-stage process involving magnetron sputtering, N2 plasma treatment, and CH4 + N2 plasma growth is studied. The width of gaps between the nanocones can be controlled by the gas composition. The nanocone formation mechanism is explained in terms of strong passivation of carbon in narrow gaps, where the access of plasma ions is hindered and the formation of large Cn H2n+2 molecules is possible. This plasma-enabled approach can be used to fabricate nanoelectronic, nanofluidic, and optoelectronic components and devices. © 2010 American Institute of Physics.

Kinetics of the initial stage of silicon surface oxidation : Deal–Grove or surface nucleation?

The nucleation-initiated oxidation of a Si surface at very low temperatures in plasmas is demonstrated experimentally, in contrast to the Deal-Grove mechanism, which predicts Si oxidation at a Si/SiO interface and cannot adequately describe the formation of SiO nanodots and oxidation rates at very low (several nanometers) oxide thickness. Based on the experimental results, an alternative oxidation scenario is proposed and supported by multiscale numerical simulations suggesting that saturation of micro- and nanohillocks with oxygen is a trigger mechanism for initiation of Si surface oxidation. This approach is generic and can be applied to describe the kinetics of low-temperature oxidation of other materials. © 2009 American Institute of Physics.

Controlled-bandgap silicon nitride nanomaterials : deterministic nitrogenation in high-density plasmas

To overcome major problems associated with insufficient incorporation of nitrogen in hydrogenated amorphous silicon nitride (a-SiNx:H) nanomaterials, which in turn impedes the development of controlled-bandgap nanodevices, here we demonstrate the possibility to achieve effective bandgap control in a broad range by using high-density inductively coupled plasmas. This achievement is related to the outstanding dissociation ability of such plasmas. It is shown that the compositional, structural, optical, and morphological properties of the synthesized a-SiNx:H nanomaterials can be effectively tailored through the manipulation of the flow rate ratio of the silane to nitrogen gases X. In particular, a wide bandgap of 5.21 eV can be uniquely achieved at a low flow rate ratio of the nitrogen to silane gas of 1.0, whereas typically used values often exceed 20.0. These results are highly-relevant to the development of the next-generation nanodevices that rely on the effective control of the functional nano-layer bandgap energies.

Effect of input power and gas pressure on the roughening and selective etching of SiO2/Si surfaces in reactive plasmas

We report on the application low-temperature plasmas for roughening Si surfaces which is becoming increasingly important for a number of applications ranging from Si quantum dots to cell and protein attachment for devices such as "laboratory on a chip" and sensors. It is a requirement that Si surface roughening is scalable and is a single-step process. It is shown that the removal of naturally forming SiO2 can be used to assist in the roughening of the surface using a low-temperature plasma-based etching approach, similar to the commonly used in semiconductor micromanufacturing. It is demonstrated that the selectivity of SiO2 /Si etching can be easily controlled by tuning the plasma power, working gas pressure, and other discharge parameters. The achieved selectivity ranges from 0.4 to 25.2 thus providing an effective means for the control of surface roughness of Si during the oxide layer removal, which is required for many advance applications in bio- and nanotechnology.

Self-organized carbon connections between catalyst particles on a silicon surface exposed to atmospheric-pressure Ar + CH4 microplasmas

Ag nanoparticles and Fe-coated Si micrograins were separately deposited onto Si(1 0 0) surfaces and then exposed to an Ar + CH4 microplasma at atmospheric pressure. For the Ag nanoparticles, self-organized carbon nanowires, up to 400 nm in length were produced, whereas for the Fe-coated Si micrograins carbon connections with the length up to 100 μm were synthesized on the plasma-exposed surface area of about 0.5 mm2. The experiment has revealed that long carbon connections and short nanowires demonstrate quite similar behavior and structure. While most connections/nanowires tended to link the nearest particles, some wires were found to 'dissolve' into the substrate without terminating at the second particle. Both connections and nanowires are mostly linear, but long carbon connections can form kinks which were not observed in the carbon nanowire networks. A growth scenario explaining the carbon structure nucleation and growth is proposed. Multiscale numerical simulations reveal that the electric field pattern around the growing connections/nanowires strongly affects the surface diffusion of carbon adatoms, the main driving force for the observed self-organization in the system. The results suggest that the microplasma-generated surface charges can be used as effective controls for the self-organized formation of complex carbon-based nano-networks for integrated nanodevices.