Gregory B. Thompson

Lattice expansion in nanocrystalline niobium thin films

High-purity nanocrystalline niobium (Nb) thin films have been deposited using high-pressure magnetron sputter deposition. Increasing the pressure of the sputtering gas during deposition has systematically led to reduced crystallite sizes in these films. Based on x-ray and electron diffraction results, it is observed that the nanocrystalline Nb films exhibit a significantly large lattice expansion with reduction in crystallite size. There is however, no change in the bcc crystal structure on reduction in crystallite size to below 5 nm. The lattice expansion in nanocrystalline Nb has been simulated by employing a recently proposed model based on linear elasticity and by appropriately modifying it to incorporate a crystallite-size-dependent width of the grain boundary.

Phase stability of bcc Zr in Nb/Zr thin film multilayers

A change in phase stability from hcp Zr to bcc Zr occurs in Nb/Zr multilayers when the bilayer thickness is reduced to the nanometer scale. This phase stability in these multilayers has been described using a model based on classical thermodynamics. Using a previously reported experimental observation of hcp to bcc transformation in these multilayers, a phase stability diagram (referred to as the biphase diagram) has been proposed. Subsequently, a range of multilayers with varying volume fractions and bilayer thicknesses have been sputter deposited. The crystal structures in these multilayers have been determined using X-ray and electron diffraction. The hcp and bcc Zr phases within the Nb/Zr multilayers are in agreement with the predictions afforded by the proposed biphase diagram. The sequence of the Zr bcc phase stability was accomplished by forming its β-Zr (high temperature bcc phase) prior to forming a bcc coherent interface with Nb. First approximations of the structural and chemical contributions to the interfacial energy accompanying the changes in hcp to bcc phase stability for Zr have been evaluated.

Chemical ordering and texture in Ni–25 at% Al thin films

Abstract This paper describes a novel study of the microstructural development in sputter-deposited thin films from a target of the intermetallic compound Ni 3 Al. Films were deposited on oxidized Si substrates at different temperatures, namely 45°C, 200°C, and 400°C. These films have been characterized by X-ray diffraction and transmission electron microscopy. In contrast to the behavior of sputter-deposited elemental metals and disordered alloys, the films deposited at the two higher temperatures consisted of refined microstructures and exhibited a low degree of texturing. This anomalous behavior has been explained by the role of exothermic heating accompanying chemical ordering.

Formation mechanism and composition distribution of FePt nanoparticles

Self-assembled FePt nanoparticle arrays are candidate structures for ultrahigh density magnetic storage media. One of the factors limiting their application to this technology is particle-to-particle compositional variation. This variation will affect the A1 to L10 transformation as well as the magnetic properties of the nanoparticles. In the present study, an analysis is provided for the formation mechanism of these nanoparticles when synthesized by the superhydride reduction method. Additionally, a comparison is provided of the composition distributions of nanoparticles synthesized by the thermal decomposition of Fe(CO)5 and the reduction of FeCl2 by superhydride. The latter process produced a much narrower composition distribution. A thermodynamic analysis of the mechanism is described in terms of free energy perturbation Monte Carlo simulations.

Formation of FePt nanoparticles by organometallic synthesis

Our interest in determining the mechanism of FePt nanoparticle formation has led to this study of the evolution of particle size and composition during synthesis. FePt nanoparticles were prepared by the simultaneous reduction of platinum acetylacetonate and thermal decomposition of iron pentacarbonyl. During the course of the reaction, samples were removed and the particle structure, size, and composition were determined using x-ray diffraction, transmission electron microscopy (TEM), and scanning electron microscopy–energy dispersive x-ray spectrometry. Early in the reaction the particles were Pt rich (greater than 95at.% Pt) and as the reaction proceeded the Fe content increased to the target of 50%. The particle diameter increased from 3.1to4.6nm during the reaction. Energy dispersive x-ray spectrometry measurements of individual particle compositions using a high resolution TEM showed a broad distribution of particle compositions with a standard deviation greater than 15% of the average composition.

Microstructures and magnetic alignment of L10 FePt nanoparticles

Department of Physics, University of Texas at Arlington. Center for Materials for Information Technology, The University of Alabama

Gallium-enhanced phase contrast in atom probe tomography of nanocrystalline and amorphous Al–Mn alloys

Over a narrow range of composition, electrodeposited Al-Mn alloys transition from a nanocrystalline structure to an amorphous one, passing through an intermediate dual-phase nanocrystal/amorphous structure. Although the structural change is significant, the chemical difference between the phases is subtle. In this study, the solute distribution in these alloys is revealed by developing a method to enhance phase contrast in atom probe tomography (APT). Standard APT data analysis techniques show that Mn distributes uniformly in single phase (nanocrystalline or amorphous) specimens, and despite some slight deviations from randomness, standard methods reveal no convincing evidence of Mn segregation in dual-phase samples either. However, implanted Ga ions deposited during sample preparation by focused ion-beam milling are found to act as chemical markers that preferentially occupy the amorphous phase. This additional information permits more robust identification of the phases and measurement of their compositions. As a result, a weak partitioning tendency of Mn into the amorphous phase (about 2 at%) is discerned in these alloys.

The influence of voxel size on atom probe tomography data

A methodology for determining the optimal voxel size for phase thresholding in nanostructured materials was developed using an atom simulator and a model system of a fixed two-phase composition and volume fraction. The voxel size range was banded by the atom count within each voxel. Some voxel edge lengths were found to be too large, resulting in an averaging of compositional fluctuations; others were too small with concomitant decreases in the signal-to-noise ratio for phase identification. The simulated methodology was then applied to the more complex experimentally determined data set collected from a (Co(0.95)Fe(0.05))(88)Zr(6)Hf(1)B(4)Cu(1) two-phase nanocomposite alloy to validate the approach. In this alloy, Zr and Hf segregated to an intergranular amorphous phase while Fe preferentially segregated to a crystalline phase during the isothermal annealing step that promoted primary crystallization. The atom probe data analysis of the volume fraction was compared to transmission electron microscopy (TEM) dark-field imaging analysis and a lever rule analysis of the volume fraction within the amorphous and crystalline phases of the ribbon.

Sputter deposited nanocrystalline Ni-25Al alloy thin films and Ni/Ni3Al multilayers

Abstract Thin films of nominal composition Ni-25at%Al have been sputter deposited from a target of the intermetallic compound Ni3Al at different substrate deposition temperatures. The film deposited on an unheated substrate exhibited a strongly textured columnar growth morphology and consisted of a mixture of metastable phases. Nanoindentation studies carried out on this film exhibited a strong strain hardening tendency. In contrast, the film deposited at 200 °C exhibited a recrystallized non-textured microstructure consisting of grains of a partially ordered Ni3Al phase. At higher deposition temperatures (∼400 °C), larger grains of the bulk equilibrium, long-range ordered, Ll2 Ni3Al phase were observed in the film. Unlike the film deposited on an unheated substrate, the films deposited at elevated temperatures did not exhibit any dependence of the hardness on the indentation depth and, consequently no strain hardening. The average hardness of the film deposited at 200 °C was higher than the one deposited at 400 °C. In addition to monolithic Ni-25Al thin films, multilayered Ni/Ni3Al thin films were also deposited. Multilayers deposited non-epitaxially on unheated substrates exhibited a strong {111} fiber texture while those deposited epitaxially on (001) NaCl exhibited a {001} texture. Free-standing multilayers of both types of preferred orientations as well as of different layer thicknesses were deformed in tension untill fracture. Interestingly, the {111} oriented multilayers failed primarily by a brittle fracture while the {001} multilayers exhibited features of ductile fracture.

Grain Boundary Specific Segregation in Nanocrystalline Fe(Cr)

A cross-correlative precession electron diffraction – atom probe tomography investigation of Cr segregation in a Fe(Cr) nanocrystalline alloy was undertaken. Solute segregation was found to be dependent on grain boundary type. The results of which were compared to a hybrid Molecular Dynamics and Monte Carlo simulation that predicted the segregation for special character, low angle, and high angle grain boundaries, as well as the angle of inclination of the grain boundary. It was found that the highest segregation concentration was for the high angle grain boundaries and is explained in terms of clustering driven by the onset of phase separation. For special character boundaries, the highest Gibbsain interfacial excess was predicted at the incoherent ∑3 followed by ∑9 and ∑11 boundaries with negligible segregation to the twin and ∑5 boundaries. In addition, the low angle grain boundaries predicted negligible segregation. All of these trends matched well with the experiment. This solute-boundary segregation dependency for the special character grain boundaries is explained in terms of excess volume and the energetic distribution of the solute in the boundary.