A Combinatorial Approach to Reliable Quantitative Analysis of Small Nano-Sized Precipitates: A Case Study with α' Precipitates in Fe-20 at% Cr Alloy.

The quantitative characterization of small nano-sized precipitates poses genuine challenges and is often deficient in accuracy due to the inherent limitations inevitably associated with the individual experimental techniques. A convenient solution is to utilize multiple complementary techniques. The present work demonstrates an effective way to reliably quantify nano-sized precipitates using a combination of complementary techniques of atom probe tomography (APT), small angle neutron scattering (SANS), and transmission electron microscopy (TEM). As a case study, the size (radius, r), number density (NP), volume fraction (ϕ), and chemical composition of Cr-rich α' precipitates are determined in Fe­20 at% Cr alloy, thermally aged at 773 K for 1,000 h. This combinatorial approach utilizes the strength of each technique in such a way that the overall accuracy of quantitative precipitation analysis improves significantly. For example, the superior spatial resolution makes TEM the appropriate technique to estimate the size and size distribution of the precipitates, while APT provides the chemical composition. Similarly, SANS analysis incorporates both the size and the compositional information thus derived independently and provides statiscally averaged quantitative analysis overcoming the field-of-view limitations of both TEM and APT. This combinatorial approach improves the accuracy of quantification and provides the true representation of the microstructure.

Improving Compositional Accuracy in APT Analysis of Carbides Using a Decreased Detection Efficiency.

The composition of carbides in steel, measured by atom probe tomography, can be influenced by limitations in the ion detector system. When carbides are analyzed, many ions tend to field evaporate from the same region of the specimen during the same laser or voltage pulse. This results in a so-called multiple event, meaning that several ions impact the detector in close proximity both in time and space. Due to a finite detector dead-time not all ions can be detected, a phenomenon known as detector pile-up. The evaporation behavior of carbon is often different than the evaporation behavior of metals when analyzing alloy carbides, leading to preferential loss of carbon ions, and a measured carbon concentration below the expected value. This effect becomes stronger as the overall detection efficiency gets higher. Here, the detection efficiency was deliberately reduced by inserting a grid into the flight-path, which resulted in a higher and more correct carbon concentration, accompanied by an increase in the statistical uncertainty.

Elemental Distribution in CrNbTaTiW-C High Entropy Alloy Thin Films.

The microstructure and distribution of the elements have been studied in thin films of a near-equimolar CrNbTaTiW high entropy alloy (HEA) and films with 8 at.% carbon added to the alloy. The films were deposited by magnetron sputtering at 300°C. X-ray diffraction shows that the near-equimolar metallic film crystallizes in a single-phase body centered cubic (bcc) structure with a strong (110) texture. However, more detailed analyses with transmission electron microscopy (TEM) and atom probe tomography (APT) show a strong segregation of Ti to the grain boundaries forming a very thin Ti-Cr rich interfacial layer. The effect can be explained by the large negative formation enthalpy of Ti-Cr compounds and shows that CrNbTaTiW is not a true HEA at lower temperatures. The addition of 8 at.% carbon leads to the formation of an amorphous structure, which can be explained by the limited solubility of carbon in bcc alloys. TEM energy-dispersive X-ray spectroscopy indicated that all metallic elements are randomly distributed in the film. The APT investigation, however, revealed that carbide-like clusters are present in the amorphous film.

Correlation of microphotoluminescence spectroscopy, scanning transmission electron microscopy, and atom probe tomography on a single nano-object containing an InGaN/GaN multiquantum well system.

A single nanoscale object containing a set of InGaN/GaN nonpolar multiple-quantum wells has been analyzed by microphotoluminescence spectroscopy (µPL), high-resolution scanning transmission electron microscopy (HR-STEM) and atom probe tomography (APT). The correlated measurements constitute a rich and coherent set of data supporting the interpretation that the observed µPL narrow emission lines, polarized perpendicularly to the crystal c-axis and with energies in the interval 2.9-3.3 eV, are related to exciton states localized in potential minima induced by the irregular 3D In distribution within the quantum well (QW) planes. This novel method opens up interesting perspectives, as it will be possible to apply it on a wide class of quantum confining emitters and nano-objects.

Laser synthesized super-hydrophobic conducting carbon with broccoli-type morphology as a counter-electrode for dye sensitized solar cells.

A laser photochemical process is introduced to realize superhydrophobic conducting carbon coatings with broccoli-type hierarchical morphology for use as a metal-free counter electrode in a dye sensitized solar cell. The process involves pulsed excimer laser irradiation of a thin layer of liquid haloaromatic organic solvent o-dichlorobenzene (DCB). The coating reflects a carbon nanoparticle-self assembled and process-controlled morphology that yields solar to electric power conversion efficiency of 5.1% as opposed to 6.2% obtained with the conventional Pt-based electrode.

Controlled growth of well-aligned GaS nanohornlike structures and their field emission properties.

Here, we report the synthesis of vertically aligned gallium sulfide (GaS) nanohorn arrays using simple vapor-liquid-solid (VLS) method. The morphologies of GaS nano and microstructures are tuned by controlling the temperature and position of the substrate with respect to the source material. A plausible mechanism for the controlled growth has been proposed. It is important to note that the turn-on field value of GaS nanohorns array is found to be the low turn-on field 4.2 V/µm having current density of 0.1 µA/cm(2). The striking feature of the field emission behavior of the GaS nanohorn arrays is that the average emission current remains nearly constant over long time without any degradation.

Enhanced field-emission from SnO2:WO(2.72) nanowire heterostructures.

The field-emission properties of SnO(2):WO(2.72) hierarchical nanowire heterostructure have been investigated. Nanoheterostructure consisting of SnO(2) nanowires as stem and WO(2.72) nanothorns as branches are synthesized in two steps by physical vapor deposition technique. Their field emission properties were recorded. A low turn-on field of ~0.82 V/µm (to draw an emission current density ~10 µA/cm(2)) is achieved along with stable emission for 4 h duration. The emission characteristic shows the SnO(2):WO(2.72) nanoheterostructures are extremely suitable for field-emission applications.