The atomic structure of shear bands in Pd40Ni40P20 bulk metallic glass has been compared to an undeformed matrix phase using pair distribution functions (PDFs) derived from energy filtered nanobeam electron diffraction. Shear bands do not show any characteristic contrast in transmission electron microscopy (TEM) images when specimens are prepared with uniform thickness. PDFs from a shear band exhibit a slight decrease in the first peak, indicating a slight difference in packing density and short range order compared to the undeformed matrix.

Pre-irradiated thermodynamic and microstructural properties of nuclear fuels form the necessary set of data against which to gauge fuel performance and irradiation damage evolution. This paper summarizes recent efforts in mixed-oxide and minor actinide-bearing mixed-oxide ceramic fuels fabrication and characterization at Los Alamos National Laboratory. Ceramic fuels (U1-x-y-zPuxAmyNpz)O2 fabricated in the compositional ranges of 0.19≤x≤0.3 Pu, 0≤y≤0.05 Am, and 0≤z≤0.03 Np exhibited a uniform crystalline face-centered cubic phase with an average grain size of 14μm; however, electron microprobe analysis revealed segregation of NpO2 in minor actinide-bearing fuels. Immersion density and porosity analysis demonstrated an average density of 92.4% theoretical for mixed-oxide fuels and an average density of 89.5% theoretical density for minor actinide-bearing mixed-oxide fuels. Examined fuels exhibited mean thermal expansion value of 12.56×10−6/°C-1 for temperature range (100°C<T<1500°C) and ambient temperature Young's modulus and Poisson's ratio of 169 GPa and of 0.327, respectively. Internal dissipation as determined from mechanical resonances of these ceramic fuels has shown promise as a tool to gauge microstructural integrity and to interrogate fundamental properties.

Chemical Mechanical Planarization (CMP) has emerged as the central technology for polishing wafers in the semiconductor manufacturing industry to make integrated multi-level devices. Both chemical and mechanical processes work simultaneously to achieve local and global planarization. Although extensive research has been carried out to understand the various factors affecting the CMP process, many aspects remain unaddressed. One such aspect of CMP is the role of abrasives in the process of conditioning. Abrasives play an important role during conditioning to regenerate the clogged polishing pads. This research is focused on the study of abrasives in the process of conditioning with a focus on the size of abrasives. With diamond being widely used as an abrasive for conditioning the polishing pad, five different sizes of diamonds ranging from 0.25μm to 100μm were selected to condition the commercially available IC 1000 polishing pad. Properties like pad roughness and pad wear were measured to understand the effect of the abrasive size on the pad morphology and pad topography. In-situ ‘coefficient of friction’ was also monitored on the CETR bench top tester. The final impact was seen in the form of surface defects on the polished copper wafers using optical microscopy.

The strength of adhesion at the cell-substrate interface is an important parameter in the design of many prosthetic implant material surfaces, due to the desire to create and maintain a strong implant-tissue bond. This study focuses on the mechanical strength of the interface and the ease of cell removal from ceramic coatings using normal and shear forces, but also looks at cell proliferation rates on the same series of surfaces.This systematic study of cell proliferation and adhesion has been carried out on a series of oxide coated Ti6Al4V based substrates with a range of surface morphologies and chemistries. Oxide coatings were formed using Plasma Electrolytic Oxidation (the PEO process).Cells were seeded at a low concentration onto substrates and proliferation monitored for up to three weeks. The same cell concentrations were seeded on samples for adhesion testing. These were cultured for a few days to ensure well established adhesion of viable cells. The normal and shear strength of osteoblasts (bone cells) and chondrocytes (cartilage cells) adhered to these substrates was measured using accelerated negative buoyancy within an ultracentrifuge.The variation in proliferation rates on, and adhesive strengths to, the range of coatings, is discussed and related to morphological and chemical differences in the coatings. A comparison is made between the normal and shear strengths of the cell-coating bonds and the differences between the behaviour of the two cell types discussed.

Large Scale Nanomaterial Production Using Microfluidizer High Shear ProcessingKenneth. J. Chomistek and Thomai Panagiotou, Ph.D.Microfluidics Corporation, 30 Ossipee Rd., Newton, MA 02464, USA Microfluidics has developed scalable and low cost award winning technologies, capable of producing nanomaterials with desirable properties for a wide variety of applications. The industries served are pharmaceuticals and biotech, energy, specialty chemicals, cosmetics and nutraceuticals. Microfluidics approach is based on an in-depth understanding of applications, unique design of high shear fluid processors, and development of processes tailored for each individual application.The understanding of the requirements and ecosystem of specific applications includes the desired end properties of the material, the production environment requirements, time and cost restrictions. Pharmaceutical and biotech applications include the development and the production of FDA approved nanotechnology drugs such as vaccines, cancer drugs, anesthetics, controlled delivery systems that include polymers drugs and proteins, etc. Chemical applications include inkjet inks, fuel cell and battery electrodes, and carbon nanotube dispersion. Cosmetics include nanoencapsulation of oxygen carriers and nutrients, and collagen processing. Nutraceuticals include nanoencapsulation of fish oil for protection of omega-3 fatty acids and odor control, nanoemulsions that contain plant sterols and vitamins.Two main methods are used for production of nanomaterials: (a) the “top down”, particle size reduction method, and (b) the “bottom up”, Microfluidics reaction Technology (MRT) for production of nanoparticles through chemical reactions and physical processes, such as crystallization. This technology received the Nano50 Award in 2007. Both technologies are continuous and can be used in line with upstream or downstream processes such as premixing, filtration, etc., and are consistent with process intensification principals.The heart of the technology is the interaction chamber which consists of “fixed geometry” microchannels. Flow through the chamber is characterized by high fluid velocities (up to 500 m/s) and subsequent impingement of fluid jets to the chamber walls or to one another. The unique “fixed geometry” feature combined with the high shear rates ensure that varied formulations (emulsions, liposomes and dispersions) achieve the smallest particle size and the narrowest particle size distribution when compared to other particle reduction techniques.The technology is fully scalable and has been used extensively from lab scale to production of market drugs, nutraceuticals and inks, among others. Microfluidizer® processors offer a variety of options, such as steam sterility, cleanability and data acquisition capabilities, so they are cGMP compliant, CE certified, ATEX and explosion proof, and therefore are suitable for a variety of manufacturing environments.

A microfracture testing technique was applied for investigating the fracture properties of Mg-Zn-Y alloys with a long-period stacking ordered (LPSO) phase. Microsized cantilever beam specimens with dimensions ≈ 10×20×50 μm3 were prepared from Mg-Zn-Y alloys by focused ion beam (FIB) machining. Notches with widths of 0.5 μm and depths of 3.5–5 μm were also introduced into the specimens by FIB machining. In this study, three types of Mg-Zn-Y alloys―Mg99.2Zn0.2Y0.6, Mg97Zn1Y2, and Mg88Zn5Y7―were used. Fracture tests were successfully conducted using a mechanical testing machine for microsized specimens at room temperature. The fracture toughness values (K IC) could not be obtained as the specimen size was too small to satisfy the plane strain condition. Hence, provisional K Q values were considered. The K Q values of the Mg97Zn1Y2 alloy were 0.8–1.2 MPam½, and those of the Mg88Zn5Y7 alloy were 1.2–3.0 MPam½. As the fracture in the Mg99.2Zn0.2Y0.6 alloy specimen occurred in a ductile plastic deformation, it was impossible to evaluate K Q values of this specimen. The increasing volume fraction of the LPSO phase indicates that the fracture toughness of Mg-Zn-Y alloys increases in LPSO phase.

Transition pathway sampling was carried out for homogeneous dislocation nucleation in perfect crystal Si. The sampling algorithm employed was Nudged Elastic Band method. Results obtained were compared with corresponding results for Cu. The stress and activation barrier ranges were found to be much higher for Si than those reported for Cu. The results also showed that while for lower values of resolved shear stress the dislocation embryo approaches that of a perfect dislocation, for higher resolved shear stress values the embryo is far from perfect. That is, the shear displacement of most particles is considerably less than the Burger’s vector. This investigation also demonstrated for the first time that Athermal shear stress for homogeneous dislocation nucleation in Si does not exist, as the crystal undergoes twinning at such high stresses.

Embedded piezoresistive microcantilever (EPM) sensors provide a small, simple and robust platform for the detection of many different types of analytes. These inexpensive sensors may be deployed in battery-powered handheld units, or interfaced to small, battery-powered radio transmitter-receivers (motes), for deployment in mesh networks of many sensors. Previously, we have demonstrated the use of EPM sensors in the detection of hydrogen fluoride gas, organophosphate nerve agents, volatile organic compounds (VOC’s), chlorinated hydrocarbons in water, and others. Here, we report on the design of EPM sensors functionalized for the detection of chlorine gas, or Cl2. We have constructed EPM sensors using composite materials consisting of a polymer or hydrogel matrix loaded with agents specific for the detection of Cl2 such as NaI. These materials were tested in both controlled laboratory conditions and in outdoor releases. Stability of the sensing materials under conditions of high temperature were also studied. Results are presented for gas exposures ranging from 1000 ppm to 20 ppm.

Transformation of titanium dioxide (TiO2) nanotubes (NTs) to truncated bipyramidal shape nanoparticles (NPs) with a large fraction of photo-catalytically active {001} facet surface was observed after thermal annealing TiO2 ordered nanotube arrays in fluorine ambient. Size of the formed nanoparticles depended on fluorine concentration and can be controlled from 20 nm to 350 nm. The crystal and optical properties of nanoparticle layers are superior to those of nanotube arrays, which are also annealed but without geometrical transformation. Using nanoparticle layers formed by this method we have fabricated dye-sensitized solar cells (DSSCs) with different size NPs in the range 35-350 nm. The dependence of solar cell performance on NP size is discussed.

An enduring problem in the engineering of high-power semiconductor devices is how to mitigate the effect of heating. Heating means the proliferation of phonons, and phonons, interacting with electrons directly affect the electronic performance of the device. Nowhere is this more evident than the role of hot polar-optical phonons in reducing the drift velocity in the channel of an HFET and hence reducing its performance at high frequencies. The task of describing hot-phonon effects is complicated by the coupling to plasma modes. We present a theory of coupled plasmon-phonon modes in GaN, how they interact with electrons and how their lifetime becomes density-dependent. Raman scattering in bulk material shows a reduction of lifetime with increasing density and we offer an explanation for this in terms of the frequency dependence of the anharmonic decay mechanism. Hot-phonon effects, however, involve modes with wave-vectors beyond those probed by Raman scattering. By adopting a single-pole approximation for these modes we have obtained the lifetime dependence on wave vector, electron temperature and density.

Crystalline perfection of InGaN epi-layers is the missing design parameter for InGaN solar cells. Structural deterioration of InGaN epi-layers depends on the thickness, composition and growth conditions as well. Increasing the InGaN epi-layer thickness beyond a critical point introduces extended crystalline defects that hinder the optical absorption and electrical properties. Increasing the InGaN composition further reduces this critical layer thickness. The optical absorption band edge is sharp for III-nitride direct band gap materials. The band edge profile is deteriorated by creation of extended crystalline defects in the InGaN epitaxial material. The design of InGaN solar cells requires the growth of epi-layers where a trade off between crystalline perfection and optical absorption properties is reached.

This work reports on the changes of solid-state cells dye-sensitized solar cells performance with the variation of concentration of spiro-OMeTAD between 5% and 25% in the fabrication of the cell. The changes in charge recombination and capacitance correlate with the improvement of current-potential characteristics a increasing spiro-OMeTAD content, which is explained by reduction of transport resistance for hole transport, the increase of charge separation in the dye molecules, and importantly, with the increase of the β-factor in the recombination resistance, that causes a reduction of the diode ideality factor.

Nucleation is the rate-determining step in the initial stages of most chemical vapour deposition processes. In order to achieve uniform deposition of diamond thin films it is necessary to seed non-diamond substrates. Here we discuss a simple electrospray deposition technique for application of 5 nm diamond seed particles onto substrates of various sizes. The influence of selected parameters, such as experimental spatial arrangement and colloidal properties, are analysed in optimizing the method by optical and electron microscopy, both before and after nanocrystalline diamond deposition on the seed layer. The advantages and limitations of the electrospray method are highlighted in relation to other commonly exploited nucleation techniques.

We report on the fabrication of nano-crystalline silicon-carbide (nc-SiC) using pulse modulated RF-PECVD technique, from silane (SiH4) and methane (CH4) gas mixtures which is highly diluted in hydrogen (H2). The microstructure of nc-SiC material is nanometer-size silicon crystallites embedded in amorphous silicon-carbide (a-SiC) matrix. As carbon incorporation in nc-Si film increases, the bandgap is enlarged from 1.1eV to 1.55eV as measured by Photothermal Deflection Spectroscopy (PDS) while the crystalline volume fraction decreases from 70% to about 20%. It is found that the crystalline volume fraction, grain size and dark conductivity of nc-SiC films can be enhanced with applying a negative DC bias to substrate during deposition.

This research work deals the influence of boron content on the high temperature deformation behavior of a low carbon advanced high strength steel (AHSS). For this purpose high temperature tensile and compression tests are carried out at different temperatures and constant true strain rates by using an Instron testing machine equipped with a radiant cylindrical furnace. Tensile tests are carried out at different temperatures (650, 750, 800, 900 and 1000°C) at a constant true strain rate of 0.001 s-1. Uniaxial hot compression tests are also performed over a wide range of temperatures (950, 1000, 1050 and 1100°C) and constant true strain rates (10-3, 10-2 and 10-1 s-1). In general, experimental results of hot tensile tests show an improvement of the hot ductility of the AHSS microalloyed with boron, although poor ductility at low temperatures (650 and 750°C). The fracture surfaces of the AHSS tested at temperatures showing the higher ductility (800, 900 and 1000°C) indicate that the fracture mode is a result of ductile failure, whereas in the region of poor ductility the fracture mode is of the ductile-brittle type failure. On the other hand, experimental results of hot compression tests show that both peak stress and peak strain tend to decrease in the AHSS microalloyed with boron, which indicates that boron generates a sort of solid solution softening effect in similar a way to other interstitial alloying elements in steel. Likewise, hot flow curves of the AHSS microalloyed with boron show an acceleration of the onset of dynamic recrystallization (DRX) and a delay of the recrystallization kinetics. Results are discussed in terms of boron segregation towards austenitic grain boundaries and second phase particles precipitation during plastic deformation and cooling.

The knowledge of composition and strain with high spatial resolution is highly important for the understanding of the chemical and electronic properties of alloyed nanostructures. Several applications require a precise knowledge of both composition and strain, which can only be extracted by self-consistent methodologies. Here, we demonstrate the use of a quantitative high resolution transmission electron microscopy (QHRTEM) technique to obtain two-dimensional (2D) projected chemical maps of epitaxially grown Ge-Si:Si(001) islands, with high spatial resolution, at different crystallographic orientations. By a combination of these data with an iterative simulation, it was possible infer the three-dimensional (3D) chemical arrangement on the strained Ge-Si:Si(001) islands, showing a four-fold chemical distribution which follows the nanocrystal shape/symmetry. This methodology can be applied for a large variety of strained crystalline systems, such as nanowires, epitaxial islands, quantum dots and wells, and partially relaxed heterostructures.

Micro-scale Focused Ion Beam (FIB) machined cantilevers were manufactured in single crystal copper, polycrystalline copper and a copper-bismuth alloy. These were imaged and tested in bending using a nanoindenter. Cantilevers machined inside a single grain of polycrystalline copper were tested to determine their (anisotropic) Young's modulus: results were in good agreement with values calculated from literature values for single crystal elastic constants. The size dependence of yield behavior in the Cu microcantilevers was also investigated. As the thickness of the specimen was reduced from 23μm to 1.7μm the yield stress increased from 300MPa to 900MPa. Microcantilevers in Cu-0.02%Bi were manufactured containing a single grain boundary of known character, with a FIB-machined sharp notch on the grain boundary. The cantilevers were loaded to fracture allowing the fracture toughness of grain boundaries of different misorientations to be determined.

Electric transport properties of chemically modificated carbon nanotubes (CNT) using Si-containing organic molecules and polymers were investigated by means of the field effect transistors (FET) technique. From the results of FET measurements for each chemically surface modified CNT, it was shown that p-type semiconducting CNT can be converted to n-type ones by physical adsorption of Si-containing organic molecules and polymers having Ph-groups. It is suggested that the electron carrier are doped into CNT from the adsorbed molecules and polymers, and it was also confirmed by the results of adsorption spectra. That is, it can be said that the electronic properties of CNT can be controlled by chemically modifications of outer surface.

Microstructures of BiFeO3 (BFO) thin films epitaxially grown on SrRuO3 (SRO) buffered SrTiO3 (STO) (001) substrates by laser molecular beam epitaxy were investigated by means of transmission electron microscopy (TEM). The results showed that the films grown under the oxygen pressures of 1Pa and 0.3Pa, respectively, contain parasitic phase embedded in the BFO phase. The parasitic phase was revealed to be poor in Bi and rich in Fe by high-angle annular dark-field (HAADF) imaging and energy dispersive X-ray spectroscopy (EDS) compositional analysis. In combination with selected area electron diffraction patterns, the parasitic phase was determined to be α-Fe2O3. By lowering oxygen pressure, the density and the size of α-Fe2O3 phase increases whereas the regularity decreases. High resolution TEM images showed that approximately periodic misfit dislocations exist at the interface between the α-Fe2O3 phase and the BFO matrix, indicating that the α-Fe2O3 particles are semi-coherently embedded in the BFO films. Less misfit dislocations were detected at the interfaces between the BFO films and the SRO/STO substrates, implying that the misfit strains in the films may be fully relaxed by the formation of α-Fe2O3 phase.

A new fabrication technique to prepare ultra-thin barrier layers for nano-scale Cu wires was proposed in our previous studies. Ti-rich layers formed at the Cu(Ti)/dielectric-layer interfaces consisted of crystalline TiC or TiSi and amorphous Ti oxides. The primary control factor for Ti-rich interface layer composition was the C concentration in the dielectric layers rather than the formation enthalpy of the Ti compounds. To investigate Ti-rich interface layer growth in Cu(Ti)/dielectric-layer samples annealed in ultra high vacuum, Rutherford Backscattering Spectrometry (RBS) was employed in the present study. Ti peaks were obtained only at the interface for all the samples. Molar amounts of Ti atoms segregated to the interface (n) were estimated from Ti peak areas. The n value was defined by n = Z·exp(-E/RT) · tm, where Z is a preexponential factor and E the activation energy for the reaction. The Z, E, and m values were estimated from plots of log n vs log t and log n vs 1/T. The m values are similar in all the samples. The E values for Ti atoms reacting with the dielectric layers containing carbon (except SiO2) tended to decrease with decreasing C concentration (decreasing k), while reaction rate coefficients (Z·exp(-E/RT)) were insensitive to C concentration in the dielectric layers. These factors lead to conclusion that growth of the Ti-rich interface layers is controlled by chemical reactions of the Ti atoms with the dielectric layers represented by the Z and E values, rather than diffusion in the Ti-rich interface layers.