Point-by-point compositional analysis for atom probe tomography.

This new alternate approach to data processing for analyses that traditionally employed grid-based counting methods is necessary because it removes a user-imposed coordinate system that not only limits an analysis but also may introduce errors. We have modified the widely used "binomial" analysis for APT data by replacing grid-based counting with coordinate-independent nearest neighbour identification, improving the measurements and the statistics obtained, allowing quantitative analysis of smaller datasets, and datasets from non-dilute solid solutions. It also allows better visualisation of compositional fluctuations in the data. Our modifications include:.•using spherical k-atom blocks identified by each detected atom's first k nearest neighbours.•3D data visualisation of block composition and nearest neighbour anisotropy.•using z-statistics to directly compare experimental and expected composition curves. Similar modifications may be made to other grid-based counting analyses (contingency table, Langer-Bar-on-Miller, sinusoidal model) and could be instrumental in developing novel data visualisation options.

Influence of seeding and bath conditions in hydrothermal growth of very thin (∼20 nm) single-crystalline rutile TiO2 nanorod films.

New seeding conditions have been examined for the hydrothermal growth of single-crystalline rutile TiO2 nanorods. Rutile nanorods of ∼20 nm diameter are grown from seed layers consisting of either (A) TiO2 or MnOOH nanocrystals deposited from suspension, or (B) a continuous sheet of TiO2. These seed layers are more effective for seeding the growth of rutile nanorods compared to the use of bare F-SnO2 substrates. The TiO2 sheet seeding allows lower concentration of titanium alkoxide precursor relative to previously reported procedures, but fusion of the resulting TiO2 nanorods into bundles occurs at higher precursor concentration and/or longer growth duration. Performance of polymer-oxide solar cells prepared using these nanorods shows a dependence on the extent of bundling as well as rod height.

Microstructure and electronic band structure of pulsed laser deposited iron fluoride thin film for battery electrodes.

Battery electrodes in thin-film form are free of the binders used with traditional powder electrodes and present an ideal platform to obtain basic insight to the evolution of the electrode-electrolyte interface passivation layer, the formation of secondary phases, and the structural underpinnings of reversibility. This is particularly relevant to the not yet fully understood conversion electrode materials, which possess enormous potential for providing transformative capacity improvements in next-generation lithium-ion batteries. However, this necessitates an understanding of the electronic charge transport properties and band structure of the thin films. This work presents an investigation of the electron transport properties of iron fluoride (FeF2) thin-film electrodes for Li-ion batteries. FeF2 thin films were prepared by pulsed-laser deposition, and their phase purity was characterized by electron microscopy and diffraction. The grown materials are polycrystalline FeF2 with a P42/mnm crystallographic symmetry. Room-temperature Hall measurements reveal that as-deposited FeF2 is n-type: the Hall coefficients were negative, electron mobility was 0.33 cm2/(V s) and resistivity was 0.255 Ω cm. The electronic band diagram of FeF2 was obtained using a combination of ultraviolet photoelectron spectroscopy, photoluminescence, photoluminescence excitation and optical absorption, which revealed that FeF2 is a direct bandgap, n-type semiconductor whose band structure is characterized by a 3.4 eV bandgap, a workfunction of ∼4.51 eV, and an effective Fermi level that resides approximately 0.22 eV below the conduction band edge. We propose that the shallow donor levels at 0.22 eV are responsible for the measured n-type conductivity. The band diagram was used to understand electron transport in FeF2 thin film and FeF2-C composite electrodes.

Laser deposited biocompatible Ca-P coatings on Ti-6Al-4V: microstructural evolution and thermal modeling.

A high intensity continuous wave diode pumped ytterbium laser source was used to deposit Ca-P coatings on a Ti-6Al-4V biocompatible alloy in order to generate a physically textured surface, enhancing osseointegration. Scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM) and energy dispersive spectroscopy (EDS) studies were coupled with X-ray and micro diffraction work to determine the structure, composition, and phases present in various zones of a sample prepared across the coating/substrate interaction zone. Three-dimensional thermal modeling was also carried out to determine the cooling rate and maximum temperature experienced by different regions of the substrate. Combining these results provide us with valuable insights regarding the thermo-physical as well as chemical interactions that take place across the coating-substrate interface.

Laser surface modification for synthesis of textured bioactive and biocompatible Ca-P coatings on Ti-6Al-4V.

A textured calcium phosphate based bio-ceramic coating was synthesized by continuous wave Nd:YAG laser induced direct melting of hydroxyapatite precursor on Ti-6Al-4V substrate. Two different micro-textured patterns (100 µm and 200 µm line spacing) of Ca-P based phases were fabricated by this technique to understand the alignment and focal adhesion of the bone forming cells on these surfaces. X-ray diffraction studies of the coated samples indicated the presence of CaTiO3, α-Ca3(PO4)2, Ca(OH)2, TiO2 (anatase) and TiO2 (rutile) phases as a result of the intermixing between the precursor and substrate material during laser processing. A two dimensional elemental mapping of the cross-section of the coated samples exhibited the presence of higher phosphorous concentration within the coating and a thin layer of calcium concentration only at the top of the coating. Improved in vitro bioactivity and in vitro biocompatibility was observed for the laser processed samples as compared to the control.

Corrosion resistance and in vitro response of laser-deposited Ti-Nb-Zr-Ta alloys for orthopedic implant applications.

While direct metal deposition of metallic powders, via laser deposition, to form near-net shape orthopedic implants is an upcoming and highly promising technology, the corrosion resistance and biocompatibility of such novel metallic biomaterials is relatively unknown and warrants careful investigation. This article presents the results of some initial studies on the corrosion resistance and in vitro response of laser-deposited Ti-Nb-Zr-Ta alloys. These new generation beta titanium alloys are promising due to their low elastic modulus as well as due the fact that they comprise of completely biocompatible alloying elements. The results indicate that the corrosion resistance of these laser-deposited alloys is comparable and in some cases even better than the currently used commercially-pure (CP) titanium (Grade 2) and Ti-6Al-4V ELI alloys. The in vitro studies indicate that the Ti-Nb-Zr-Ta alloys exhibit comparable cell proliferation but enhanced cell differentiation properties as compared with Ti-6Al-4V ELI.

Strengthening mechanisms in Ti-Nb-Zr-Ta and Ti-Mo-Zr-Fe orthopaedic alloys.

The microstructural evolution and attendant strengthening mechanisms in two novel orthopaedic alloy systems, Ti-Nb-Zr-Ta and Ti-Mo-Zr-Fe, have been compared and contrasted in this paper. Specifically, the alloy compositions considered are Ti-34Nb-9Zr-8Ta and Ti-13Mo-7Zr-3Fe. In the homogenized condition, both alloys exhibited a microstructure consisting primarily of a beta matrix with grain boundary alpha precipitates and a low-volume fraction of intra-granular alpha precipitates. On ageing the homogenized alloys at 600 degrees C for 4 hr, both alloys exhibited the precipitation of refined scale secondary alpha precipitates homogeneously in the beta matrix. However, while the hardness of the Ti-Mo-Zr-Fe alloy marginally increased, that of the Ti-Nb-Zr-Ta alloy decreased substantially as a result of the ageing treatment. In order to understand this difference in the mechanical properties after ageing, TEM studies have been carried out on both alloys prior to and post the ageing treatment. The results indicate the existence of a metastable B2 ordering in the Ti-Nb-Zr-Ta alloy in the homogenized condition which is destroyed by the ageing treatment, consequently leading to a decrease in the hardness.