Publications

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Nanostructured materials often display very unique properties related to their far-from-equilibrium nature. Due to these unique structures, many of these materials transform into other, more stable microstructures with minimal thermal excitation. This work will highlight examples of the unexpected routes taken during the microstructural evolution of pulsed-laser deposited (PLD) free-standing face-centered cubic (FCC) thin films as a function of deposition condition and annealing temperatures. A direct comparison between the grain growth dynamics observed during in situ TEM annealing experiments in PLD films of high-purity aluminum, copper, gold and nickel films, as well as aluminum-alumina alloys shows a multitude of kinetics. For high-purity systems film thickness, void density, grain size distribution, and deposition temperature were found to be the primary factors observed controlling the rate, extent, and nature of the grain growth. The growth dynamics ranged from nearly classical normal grain growth to abnormal grain growth resulting in a bimodal grain size distribution. The grain growth rate was found to be highly dependent on the materials system despite all of the films being nanograined FCC metals produced by similar PLD parameters. The investigation of the aluminum-alumina alloys produced under various compositions and deposition parameters suggests that particle pinning can be used to maintain nanostructured films, even after annealing treatments at high homologous temperatures. In addition to investigating the grain growth dynamics and the resulting grain size distribution, the variety of internal microstructures formed from thermal annealing were evaluated. These structures ranged from intergranular voids to stacking-fault tetrahedra. An unexpected, metastable hexagonal-closed packed phase was indentified in the high-purity nickel films. These in situ TEM observations have provided key insight into the microstructural evolution of nanograined free-standing metal films and the defect structure present in the grains resulting from various growth dynamics, in addition to suggesting multiple methods to tailor the structure and the resulting properties of nanostructured free-standing films.

One of the tenets of nanotechnology is that the electrical/optical/chemical/biological properties of a material may be changed profoundly when the material is reduced to sufficiently small dimensions - and we can exploit these new properties to achieve novel or greatly improved material's performance. However, there may be mechanical or thermodynamic driving forces that hinder the synthesis of the structure, impair the stability of the structure, or reduce the intended performance of the structure. Examples of these phenomena include de-wetting of films due to high surface tension, thermally-driven instability of nano-grain structure, and defect-related internal dissipation. If we have fundamental knowledge of the mechanical processes at small length scales, we can exploit these new properties to achieve robust nanodevices. To state it simply, the goal of this program is the fundamental understanding of the mechanical properties of materials at small length scales. The research embodied by this program lies at the heart of modern materials science with a guiding focus on structure-property relationships. We have divided this program into three Tasks, which are summarized: (1) Mechanics of Nanostructured Materials (PI Blythe Clark). This task aims to develop a fundamental understanding of the mechanical properties and thermal stability of nanostructured metals, and of the relationship between nano/microstructure and bulk mechanical behavior through a combination of special materials synthesis methods, nanoindentation coupled with finite-element modeling, detailed electron microscopic characterization, and in-situ transmission electron microscopy experiments. (2) Theory of Microstructures and Ensemble Controlled Deformation (PI Elizabeth A. Holm). The goal of this Task is to combine experiment, modeling, and simulation to construct, analyze, and utilize three-dimensional (3D) polycrystalline nanostructures. These full 3D models are critical for elucidating the complete structural geometry, topology, and arrangements that control experimentally-observed phenomena, such as abnormal grain growth, grain rotation, and internal dissipation measured in nanocrystalline metal. (3) Mechanics and Dynamics of Nanostructured and Nanoscale Materials (PI John P. Sullivan). The objective of this Task is to develop atomic-scale understanding of dynamic processes including internal dissipation in nanoscale and nanostructured metals, and phonon transport and boundary scattering in nanoscale structures via internal friction measurements.

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The mechanical properties of rare earth tritide films evolve as tritium decays into {sup 3}He, which forms bubbles that influence long-term film stability in applications such as neutron generators. Ultralow load nanoindentation, combined with finite-element modeling to separate the mechanical properties of the thin films from their substrates, has been used to follow the mechanical properties of model ErT{sub 2} films as they aged. The size of the growing {sup 3}He bubbles was followed with transmission electron microscopy, while ion beam analysis was used to monitor total T and {sup 3}He content. The observed behavior is divided into two regimes: a substantial increase in layer hardness but elasticity changed little over {approx}18 months, followed by a decrease in elastic stiffness and a modest decease in hardness over the final 24 months. We show that the evolution of properties is explained by a combination of dislocation pinning by the bubbles, elastic softening as the bubbles occupy an increasing fraction of the material, and details of bubble growth modes.

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In-situ transmission electron microscopy (TEM) straining experiments provide direct detailed observation of the deformation and failure mechanisms active at a length scale relevant to nanomaterials. This presentation will detail continued investigations into the active mechanisms governing high purity nanograined pulsed-laser deposited (PLD) nickel, as well as recent work into dislocation-particle interactions in nanostructured PLD aluminum-alumina alloys. Straining experiments performed on nanograined PLD free-standing nanograined Ni films with an engineered grain size distribution revealed that the addition of ductility with limited decrease in strength, reported in such metals, can be attributed to the simultaneous activity of three deformation mechanisms in front of the crack tip. At the crack tip, a grain agglomeration mechanism occurs where several nanograins appear to rotate, resulting in a very thin, larger grain immediately prior to failure. In the classical plastic zone in front of the crack tip, a multitude of mechanisms were found to operate in the larger grains including: dislocation pile-up, twinning, and stress-assisted grain growth. The region outside of the plastic zone showed signs of elasticity with limited indications of dislocation activity. The insight gained from in-situ TEM straining experiments of nanograined PLD Ni provides feedback for models of the deformation and failure in nanograined FCC metals, and suggests a greater complexity in the active mechanisms. The investigation into the deformation and failure mechanisms of FCC metals via in-situ TEM straining experiments has been expanded to the effect of hard particles on the active mechanisms in nanograined aluminum with alumina particles. The microstructures investigated were developed with varying composition, grain size, and particle distribution via tailoring of the PLD conditions and subsequent annealing. In order to develop microstructures suitable for in-situ deformation testing, in-situ TEM annealing experiments were performed, revealing the effect of nanoparticle precipitates on grain growth. These films were then strained in the TEM and the resulting microstructural evolution will be discussed. In-situ TEM straining experiments currently provide a wealth of information into plasticity within nanomaterials and can potentially, with further development of TEM and nanofabrication tools, provide even greater investigative capabilities.

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Interfaces are a critical determinant of the full range of materials properties, especially at the nanoscale. Computational and experimental methods developed a comprehensive understanding of nanograin evolution based on a fundamental understanding of internal interfaces in nanocrystalline nickel. It has recently been shown that nanocrystals with a bi-modal grain-size distribution possess a unique combination of high-strength, ductility and wear-resistance. We performed a combined experimental and theoretical investigation of the structure and motion of internal interfaces in nanograined metal and the resulting grain evolution. The properties of grain boundaries are computed for an unprecedented range of boundaries. The presence of roughening transitions in grain boundaries is explored and related to dramatic changes in boundary mobility. Experimental observations show that abnormal grain growth in nanograined materials is unlike conventional scale material in both the level of defects and the formation of unfavored phases. Molecular dynamics simulations address the origins of some of these phenomena.

Radiation Effects Microscopy is an extremely useful technique in failure analysis of electronic parts used in radiation environment. It also provides much needed support for development of radiation hard components used in spacecraft and nuclear weapons. As the IC manufacturing technology progresses, more and more overlayers are used; therefore, the sensitive region of the part is getting farther and farther from the surface. The thickness of these overlayers is so large today that the traditional microbeams, which are used for REM are unable to reach the sensitive regions. As a result, higher ion beam energies have to be used (> GeV), which are available only at cyclotrons. Since it is extremely complicated to focus these GeV ion beams, a new method has to be developed to perform REM at cyclotrons. We developed a new technique, Ion Photon Emission Microscopy, where instead of focusing the ion beam we use secondary photons emitted from a fluorescence layer on top of the devices being tested to determine the position of the ion hit. By recording this position information in coincidence with an SEE signal we will be able to indentify radiation sensitive regions of modern electronic parts, which will increase the efficiency of radiation hard circuits.

The most energy efficient solid state white light source will likely be a combination of individually efficient red, green, and blue LED. For any multi-color approach to be successful the efficiency of deep green LEDs must be significantly improved. While traditional approaches to improve InGaN materials have yielded incremental success, we proposed a novel approach using group IIIA and IIIB nitride semiconductors to produce efficient green and high wavelength LEDs. To obtain longer wavelength LEDs in the nitrides, we attempted to combine scandium (Sc) and yttrium (Y) with gallium (Ga) to produce ScGaN and YGaN for the quantum well (QW) active regions. Based on linear extrapolation of the proposed bandgaps of ScN (2.15 eV), YN (0.8 eV) and GaN (3.4 eV), we expected that LEDs could be fabricated from the UV (410 nm) to the IR (1600 nm), and therefore cover all visible wavelengths. The growth of these novel alloys potentially provided several advantages over the more traditional InGaN QW regions including: higher growth temperatures more compatible with GaN growth, closer lattice matching to GaN, and reduced phase separation than is commonly observed in InGaN growth. One drawback to using ScGaN and YGaN films as the active regions in LEDs is that little research has been conducted on their growth, specifically, are there metalorganic precursors that are suitable for growth, are the bandgaps direct or indirect, can the materials be grown directly on GaN with a minimal defect formation, as well as other issues related to growth. The major impediment to the growth of ScGaN and YGaN alloys was the low volatility of metalorganic precursors. Despite this impediment some progress was made in incorporation of Sc and Y into GaN which is detailed in this report. Primarily, we were able to incorporate up to 5 x 10{sup 18} cm{sup -3} Y atoms into a GaN film, which are far below the alloy concentrations needed to evaluate the YGaN optical properties. After a no-cost extension was granted on this program, an additional more 'liquid-like' Sc precursor was evaluated and the nitridation of Sc metals on GaN were investigated. Using the Sc precursor, dopant level quantities of Sc were incorporated into GaN, thereby concluding the growth of ScGaN and YGaN films. Our remaining time during the no-cost extension was focused on pulsed laser deposition of Sc metal films on GaN, followed by nitridation in the MOCVD reactor to form ScN. Finally, GaN films were deposited on the ScN thin films in order to study possible GaN dislocation reduction.

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Radiation effects microscopy (REM) for the next generation integrated circuits (ICs) will require GeV ions both to provide high ionization and to penetrate the thick overlayers in present day ICs. These ion beams can be provided by only a few cyclotrons in the world. Since it is extremely hard to focus these higher-energy ions, we have proposed the ion photon emission microscope (IPEM) that allows the determination of the ion hits by focusing the emitted photons to a position sensitive detector. The IPEM needs a thin luminescent foil that has high brightness, good spatial resolution and does not change the incident ion's energy and direction significantly. Available organic-phosphor foils require a large thickness to produce enough photons, which results in poor spatial resolution. To solve this problem, we have developed thin, lightly doped n-type GaN films that are extremely bright. We have grown high quality GaN films on sapphire using metal organic chemical vapor deposition (MOCVD), detached the films from the substrate using laser ablation, and made them self-supporting. The smallest foils have 1 mm2 area and 1 μm thickness. The optical properties, such as light yield, spectrum and decay times were measured and compared to those of conventional phosphors, by using both alpha particles from a radioactive source and 250 keV ions from an implanter. We found that the GaN performance strongly depends on composition and doping levels. The conclusion is that 1-2 μm GaN film of a 1 mm2 area may become an ideal ion position detector. © 2007 Elsevier B.V. All rights reserved.

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