S.V. Raju

Large area strain analysis using scanning transmission electron microscopy across multiple images

Here, we apply revolving scanning transmission electron microscopy to measure lattice strain across a sample using a single reference area. To do so, we remove image distortion introduced by sample drift, which usually restricts strain analysis to a single image. Overcoming this challenge, we show that it is possible to use strain reference areas elsewhere in the sample, thereby enabling reliable strain mapping across large areas. As a prototypical example, we determine the strain present within the microstructure of a Ni-based superalloy directly from atom column positions as well as geometric phase analysis. While maintaining atomic resolution, we quantify strain within nanoscale regions and demonstrate that large, unit-cell level strain fluctuations are present within the intermetallic phase.

Laser-assisted processing of Ni-Al-Co-Ti under high pressure

ABSTRACT Laser-assisted processing and in-situ characterization of a Ni0.7-Al0.1235-Co0.15-Ti0.0265 alloy were carried out under a range of simultaneous hydrostatic high pressures of ∼30 GPa and high temperature conditions ∼2000°C using a laser-assisted heating in diamond anvil cell with synchrotron X-ray micro-diffraction. The characterization of the microstructure and X-ray diffraction analysis at ambient conditions confirmed the formation of the cuboids of ordered γ′ phase in the disordered γ matrix. The isothermal bulk modulus (B0) and its first-order derivative (B0’) of the alloy were determined to be B0 = 123 ± 9 GPa and B0’ = 5.7 ± 2.8. The in-situ characterization of the alloy at high temperatures under high pressures revealed that the γ′ phase transforms into the tetragonaly distorted D022-type structure. This transformation is similar to the transformation that occurs in the ordered Ni3Al, responsible for the improved strength at high temperatures. High pressure was found to increase the onset temperature of the structural distortion. The pressure–temperature phase diagram of the Ni0.7-Al0.1235-Co0.15-Ti0.0265 up to ∼30 GPa and ∼2000°C was determined and is reported here.

Pressure-induced frustration in charge ordered spinel AlV2O4

AlV2O4 is the only spinel compound so far known that exists in the charge ordered state at room temperature. It is known to transform to a charge frustrated cubic spinel structure above 427 ° C. The presence of multivalent V ions in the pyrochlore lattice of the cubic spinel phase brings about the charge frustration that is relieved in the room temperature rhombohedral phase by the clustering of vanadium into a heptamer molecular unit along with a lone V atom. The present work is the first demonstration of pressure-induced frustration in the charge ordered state of AlV2O4. Synchrotron powder x-ray diffraction studies carried out at room temperature on AlV2O4 subjected to high pressure in a diamond anvil cell show that the charge ordered rhombohedral phase becomes unstable under the application of pressure and transforms to the frustrated cubic spinel structure. The frustration is found to be present even after pressure recovery. The possible role of pressure on vanadium t2g orbitals in understanding these observations is discussed.

High pressure and temperature structure of liquid and solid Cd: implications for the melting curve of Cd

The structure of cadmium was characterized in both the solid and liquid forms at pressures to 10 GPa using in situ x-ray diffraction measurements in a resistively heated diamond anvil cell. The distorted hexagonal structure of solid cadmium persists at high pressures and temperatures, with anomalously large c/a ratio of Cd becoming larger as the melting curve is approached. The measured structure factor S(Q) for the melt reveals that the cadmium atoms are spaced about 0.6 Angstroms apart. The melt structure remains notably constant with increasing pressure, with the first peak in the structure factor remaining mildly asymmetric, in accord with the persistence of an anisotropic bonding environment within the liquid. Evolution of powder diffraction patterns up to the temperature of melting revealed the stability of the ambient-pressure hcp structure up to a pressure of 10 GPa. The melting curve has a positive Clausius–Clapeyron slope, and its slope is in good agreement with data from other techniques. We find deviations in the melting curve from Lindemann law type behavior for pressures above 1 GPa.

Direct Lattice Parameter Measurements Using HAADF-STEM

Lattice strain is generated in crystal structures as a result of atomic size differences between host atom and solute elements during substitutional alloying. Extensive work has been performed to study lattice parameter variation with alloying elements, primarily using diffraction methods. The global information provided by reciprocal space analysis, however, limits access to local structural details. In contrast, atomic resolution STEM enables direct imaging of the crystal structure, but drift distortion currently limits capabilities to measure lattice parameters. This is particularly relevant for Ni-based superalloys as the microstructure consists of cuboidal intermetallic γ’ phase precipitate (L12 structure) within a γ phase matrix (FCC structure). As the coherent γ/ γ ’ interface is responsible for limiting dislocation motion [1], direct measurement of lattice parameters and strain provides critical information to further next generation alloy design.