The application of STEM and in situ controlled dehydration to bacterial systems using ESEM.

Transmission imaging with an environmental scanning electron microscope (ESEM) (Wet STEM) is a recent development in the field of electron microscopy, combining the simple preparation inherent to ESEM work with an alternate form of contrast available through a STEM detector. Because the technique is relatively new, there is little information available on how best to apply this technique and which samples it is best suited for. This work is a description of the sample preparation and microscopy employed by the authors for imaging bacteria with Wet STEM (scanning transmission electron microscopy). Three different bacterial samples will be presented in this study: first, used as a model system, is Escherichia coli for which the contrast mechanisms of STEM are demonstrated along with the visual effects of a dehydration-induced collapse. This collapse, although clearly in some sense artifactual, is thought to lead to structurally meaningful morphological information. Second, Wet STEM is applied to two distinct bacterial systems to demonstrate the novel types of information accessible by this approach: the plastic-producing Cupriavidus necator along with wild-type and ΔmreC knockout mutants of Salmonella enterica serovar Typhimurium. Cupriavidus necator is shown to exhibit clear internal differences between bacteria with and without plastic granules, while the ΔmreC mutant of S. Typhimurium has an internal morphology distinct from that of the wild type.

The application of STEM and in situ controlled dehydration to bacterial systems using ESEM

Transmission imaging with an environmental scanning electron microscope (ESEM) (Wet STEM) is a recent development in the field of electron microscopy, combining the simple preparation inherent to ESEM work with an alternate form of contrast available through a STEM detector. Because the technique is relatively new, there is little information available on how best to apply this technique and which samples it is best suited for. This work is a description of the sample preparation and microscopy employed by the authors for imaging bacteria with Wet STEM (scanning transmission electron microscopy). Three different bacterial samples will be presented in this study: first, used as a model system, is Escherichia coli for which the contrast mechanisms of STEM are demonstrated along with the visual effects of a dehydration-induced collapse. This collapse, although clearly in some sense artifactual, is thought to lead to structurally meaningful morphological information. Second, Wet STEM is applied to two distinct bacterial systems to demonstrate the novel types of information accessible by this approach: the plastic-producing Cupriavidus necator along with wild-type and δmreC knockout mutants of Salmonella enterica serovar Typhimurium. Cupriavidus necator is shown to exhibit clear internal differences between bacteria with and without plastic granules, while the δmreC mutant of S. Typhimurium has an internal morphology distinct from that of the wild type. © 2012 Wiley Periodicals, Inc.

Diameter and wall number control of carbon nanotubes by chemical vapor deposition

We analyze the relationship between the average wall number (N) and the diameter (d) for carbon nanotubes (CNTs) grown by chemical vapour deposition. It is found that N depends linearly on d for diameters in the range of 2.5-10 nm, while single wall nanotubes predominate for diameters under about 2.1 nm. The linear relationship is found to depend somewhat on the growth conditions. It is also verified that the mean diameter depends on the diameter of the originating catalyst nanoparticle, and thus on the initial catalyst thickness where a thin film catalyst is used. This simplifies the characterisation of CNTs by electron microscopy. We also find a linear relationship between nanotube diameter and initial catalyst film thickness. © 2013 AIP Publishing LLC.

Evidence of quantum lateral confinement in side-gated resonant tunnelling diodes formed by patterned substrate regrowth

MBE regrowth on patterned np-GaAs wafers has been used to fabricate GaAs/AlGaAs double barrier resonant tunnel diodes with a side-gate in the plane of the quantum well. The physical diameters vary from 1 to 20 μm. For a nominally 1 μm diameter diode the peak current is reduced by more than 95% at a side-gate voltage of -2 V at 1.5 K, which we estimate corresponds to an active tunnel region diameter of 75 nm ± 10 nm. At high gate biases additional structure appears in the conductance data. Differential I-V measurements show a linear dependence of the spacing of subsidiary peaks on gate bias indicating lateral quantum confinement. © 1996 American Institute of Physics.

The fracture energy of metal fibre reinforced ceramic composites (MFCs)

A model is presented for prediction of the fracture energy of ceramic-matrix composites containing dispersed metallic fibres. It is assumed that the work of fracture comes entirely from pull-out and/or plastic deformation of fibres bridging the crack plane. Comparisons are presented between these predictions and experimental measurements made on a commercially-available composite material of this type, containing stainless steel (304) fibres in a matrix predominantly comprising alumina and alumino-silicate phases. Good agreement is observed, and it's noted that there is scope for the fracture energy levels to be high (~20kJm-2). Higher toughness levels are both predicted and observed for coarser fibres, up to a practical limit for the fibre diameter of the order of 0.5mm. Other deductions are also made concerning strategies for optimisation of the toughness of this type of material. © 2010 Elsevier Ltd.

The performance of ejectors driven by sinusoidally unsteady jets

The operation of ejectors driven by a low-speed, sinusoidally unsteady jet has been studied. The thrust augmentation is shown to be highly dependent on the non-dimensional frequency of the driver jet, but independent of its Mach Number. Convective rather than acoustically propagated phenomena dominate the ejector flowfield. Unsteady pressure measurements on the internal surfaces of the ejector have enabled convecting ring vortices to be identified. The impingement of a ring vortex on the leading edge of the ejector causes the peak unsteady body force. The non-dimensional diameter of the ejector is shown to be the only geometric variable that affects the optimum non-dimensional frequency for thrust augmentation. An experimentally optimised geometry is presented. An expression relating the mechanical efficiency and thrust augmentation of the ejector is developed, and shown to be crucially dependent on the degree of unsteadiness in the ejector exit plane.

The elastic-plastic indentation response of a columnar thermal barrier coating

Thermal barrier coatings with a columnar microstructure are prone to erosion damage by a mechanism of surface cracking upon impact by small foreign particles. In order to explore this erosion mechanism, the elastic indentation and the elastic-plastic indentation responses of a columnar thermal barrier coating to a spherical indenter were determined by the finite element method and by analytical models. It was shown that the indentation response is intermediate between that of a homogeneous half-space and that given by an elastic-plastic mattress model (with the columns behaving as independent non-linear springs). The sensitivity of the indentation behaviour to geometry and to the material parameters was explored: the diameter of the columns, the gap width between columns, the coefficient of Coulomb friction between columns and the layer height of the thermal barrier coating. The calculations revealed that the level of induced tensile stress is sufficient to lead to cracking of the columns at a depth of about the column radius. It was also demonstrated that the underlying soft bond coat can undergo plastic indentation when the coating comprises parallel columns, but this is less likely for the more realistic case of a random arrangement of tapered columns. © 2009 Elsevier B.V.

Fabrication of an organic field effect transistor using nano imprinting of Ag inks and semiconducting polymers

A simple and cheap procedure for flexible electronics fabrication was demonstrated by imprinting metallic nanoparticles (NPs) on flexible substrates. Silver NPs with an average diameter of 10 nm were prepared via an improved chemical approach and Ag Np ink was produced in α-terpineol with a concentration up to 15%. Silver micro/nanostructures with a dimension varying from nanometres to microns were produced on a flexible substrate (polyimide) by imprinting the as-prepared silver ink. The fine fluidic properties of an Ag NP/α-terpineol solution and low melting temperatures of silver nanoparticles render a low pressure and low temperature procedure, which is well suited for flexible electronics fabrication. The effects of sintering and mechanical bending on the conductivity of imprinted silver contacts were also investigated. Large area organic field effect transistors (OFET) on flexible substrates were fabricated using an imprinted silver electrode and semiconducting polymer. The OFET with silver electrodes imprinted from our prepared oleic acid stabilized Ag nanoparticle ink show an ideal ohmic contact; therefore, the OFET exhibit high performance (Ion/Ioff ratio: 1 × 103; mobility: 0.071 cm2 V-1 s-1). © 2010 IOP Publishing Ltd.

The effects of corona treatment on impact and spreading of ink-jet drops on a polymeric film substrate

The effects of varying corona surface treatment on ink drop impact and spreading on a polymer substrate have been investigated. The surface energy of substrates treated with different levels of corona was determined from static contact angle measurement by the Owens and Wendt method. A drop-on-demand print-head was used to eject 38 μm diameter drops of UV-curable graphics ink travelling at 2.7 m/s on to a flat polymer substrate. The kinematic impact phase was imaged with a high speed camera at 500k frames per second, while the spreading phase was imaged at 20k frames per secoiui. The resultant images were analyzed to track the changes in the drop diameter during the different phases of drop spreading. Further experiments were carried out with white-light intetferometry to accurately measure the final diameter of drops which had been printed on different corona treated substrates and UV cured. The results are correlated to characterize the effects of corona treatment on drop impact behavior and final print quality.

Growth of ultrahigh density single-walled carbon nanotube forests by improved catalyst design.

We have grown vertically aligned single-walled carbon nanotube forests with an area density of 1.5 × 10(13) cm(-2), the highest yet achieved, by reducing the average diameter of the nanotubes. We use a nanolaminate Fe-Al(2)O(3) catalyst design consisting of three layers of Al(2)O(3), Fe, and Al(2)O(3), in which the lower Al(2)O(3) layer is densified by an oxygen plasma treatment to increase its diffusion barrier properties, to allow a thinner catalyst layer to be used. This high nanotube density is desirable for using carbon nanotubes as interconnects in integrated circuits.

Thermal plasma synthesis of superparamagnetic iron oxide nanoparticles

Superparamagnetic iron oxide nanoparticles were synthesized by injecting ferrocene vapor and oxygen into an argon/helium DC thermal plasma. Size distributions of particles in the reactor exhaust were measured online using an aerosol extraction probe interfaced to a scanning mobility particle sizer, and particles were collected on transmission electron microscopy (TEM) grids and glass fiber filters for off-line characterization. The morphology, chemical and phase composition of the nanoparticles were characterized using TEM and X-ray diffraction, and the magnetic properties of the particles were analyzed with a vibrating sample magnetometer and a magnetic property measurement system. Aerosol at the reactor exhaust consisted of both single nanocrystals and small agglomerates, with a modal mobility diameter of 8-9 nm. Powder synthesized with optimum oxygen flow rate consisted primarily of magnetite (Fe 3O 4), and had a room-temperature saturation magnetization of 40.15 emu/g, with a coercivity and remanence of 26 Oe and 1.5 emu/g, respectively. © Springer Science+Business Media, LLC 2011.

Micromachining of glassy carbon toolsets for micro embossing applications

Laser micro machining is fast gaining popularity as a method of fabricating micro scale structures. Lasers have been utilised for micro structuring of metals, ceramics and glass composites and with advances in material science, new materials are being developed for micro/nano products used in medical, optical, and chemical industries. Due to its favourable strength to weight ratio and extreme resistance to chemical attack, glassy carbon is a new material that offers many unique properties for micro devices. The laser machining of SIGRADUR® G grade glassy carbon was characterised using a 1065 nm wavelength Ytterbium doped pulsed fiber laser. The laser system has a selection of 25 preset waveforms with optimised peak powers for different pulsing frequencies. The optics provide spot diameter of 40 μm at the focus. The effect of fluence, transverse overlap and pulsing frequency (as waveform) on glassy carbon was investigated. Depth of removal and surface roughness were measured as machining quality indicators. The damage threshold fluence was determined to be 0.29 J/cm2 using a pulsing frequency of 250 kHz and a pulse width of 18 ns (waveform 3). Ablation rates of 17 < V < 300 μm3/pulse were observed within a fluence range of 0.98 < F < 2.98 J/cm2. For the same fluence variation, 0.6 μm to 6.8 μm deep trenches were machined. Trench widths varied from 29 μm at lower fluence to 47 μm at the higher fluence. Square pockets, 1 mm wide, were machined to understand the surface machining or milling. The depth of removal using both waveform 3 and 5 showed positive correlation with fluence, with waveform 5 causing more removal than waveform 3 for the same fluence. Machined depths varied from less than 1 μm to nearly 40 μm. For transverse overlap variation using waveform 3, the best surface finish with Rz = 1.1 μm was obtained for fluence 0.792 J/cm2 for transverse overlap of 1 μm, 6 μm, and 9 μm at machined depths of 22.9 μm, 6.6 μm, and 4.6 μm respectively. For fluence of 1.426 J/cm2, the best surface finish with Rz = 1.2 μm was obtained for transverse overlap of 6 μm, and 9 μm at machined depths of 12.46 μm, and 8.6 μm respectively. The experimental data was compiled as machining charts and utilised for fabricating a micro-embossing glassy carbon master toolsets as a capability demonstration.

The foundations of a new approach to additive manufacturing: Characteristics of free space metal deposition

In this paper, we report on the realisation of a free space deposition process (FSD). For the first time the use of a moving support structure to deposit tracks of metal starting from a substrate and extending into free space is characterised. The ability to write metal shapes in free space has wide ranging applications in additive manufacturing and rapid prototyping where the tracks can be layered to build overhanging features without the use of fixed support structures (such as is used in selective laser melting (SLM) and stereo lithography (SLA)). We demonstrate and perform a preliminary characterisation of the process in which a soldering iron was used to deposit lead free solder tracks. The factors affecting the stability of tracks and the effect of operating parameters, temperature, velocity, initial track starting diameter and starting volume were measured. A series of 10 tracks at each setting were compared with a control group of tracks; the track width, taper and variation between tracks were compared. Notable results in free space track deposition were that the initial track diameter and volume affected the repeatability and quality of tracks. The standard deviation of mean track width of tracks from the constrained initial diameter group were half that of the unconstrained group. The amount of material fed to the soldering iron before commencing deposition affected the taper of tracks. At an initial volume of 7 mm3 and an initial track diameter of 0.8 mm, none of the ten tracks deposited broke or showed taper > ∼1°. The maximum deposition velocity for free space track deposition using lead-free solder was limited to 1.5 mm s-1. © 2011 Elsevier B.V. All rights reserved.

Synthesis of 10 nm Ag nanoparticle polymer composite pastes for low temperature production of high conductivity films

The conversion of silver nanoparticle (NP) paste films into highly conductive films at low sintering temperature is an important requirement for the developing areas of additive fabrication and printed electronics. Ag NPs with a diameter of ∼10 nm were prepared via an improved chemical process to produce viscous paste with a high wt%. The paste consisted of as-prepared Ag NP and an organic vehicle of ethylcellulose that was deposited on glass and Si substrates using a contact lithographic technique. The morphology and conductivity of the imprinted paste film were measured as a function of sintering temperature, sintering time and the percentage ratio of Ag NP and ethylcellulose. The morphology and conductivity were examined using scanning electron microscopy (SEM) and a two-point probe electrical conductivity measurement. The results show that the imprinted films were efficiently converted into conducting states when exposed to sintering temperature in the range of 200-240 °C, this temperature is lower than the previously reported values for Ag paste. © 2010 Elsevier B.V. All rights reserved.

CFD modeling of single-phase flow in a packed bed with MRI validation

Computational fluid dynamics (CFD) simulations are becoming increasingly widespread with the advent of more powerful computers and more sophisticated software. The aim of these developments is to facilitate more accurate reactor design and optimization methods compared to traditional lumped-parameter models. However, in order for CFD to be a trusted method, it must be validated using experimental data acquired at sufficiently high spatial resolution. This article validates an in-house CFD code by comparison with flow-field data obtained using magnetic resonance imaging (MRI) for a packed bed with a particle-to-column diameter ratio of 2. Flows characterized by inlet Reynolds numbers, based on particle diameter, of 27, 55, 111, and 216 are considered. The code used employs preconditioning to directly solve for pressure in low-velocity flow regimes. Excellent agreement was found between the MRI and CFD data with relative error between the experimentally determined and numerically predicted flow-fields being in the range of 3-9%. © 2012 American Institute of Chemical Engineers (AIChE).