Nanocrystalline copper lms were created by both repetitive high-energy pulsed power, to produce material without internal nanotwins; and pulsed laser deposition, to produce nan- otwins. Samples of these lms were indented at ambient (298K) and cryogenic temperatures by immersion in liquid nitrogen (77K) and helium (4K). The indented samples were sectioned through the indented regions and imaged in a scanning electron microscope. Extensive grain growth was observed in the lms that contained nanotwins and were indented cryogenically. The lms that either lacked twins, or were indented under ambient conditions, were found to exhibit no substantial grain growth by visual inspection. Precession transmission elec- tron microscopy was used to con rm these ndings quantitatively, and show that 3 and 7 boundaries proliferate during grain growth, implying that these interface types play a key role in governing the extensive grain growth observed here. Molecular dynamics sim- ulations of the motion of individual grain boundaries demonstrate that speci c classes of boundaries - notably 3 and 7 - exhibit anti- or a-thermal migration, meaning that their mobilities either increase or do not change signi cantly with decreasing temperature. An in-situ cryogenic indentation capability was developed and implemented in a transmission electron microscope. Preliminary results do not show extensive cryogenic grain growth in indented copper lms. This discrepancy could arise from the signi cant di erences in con g- uration and loading of the specimen between the two approaches, and further research and development of this capability is needed.
The goal of this LDRD project is to develop a rapid first-order experimental procedure for the testing of advanced cladding materials that may be considered for generation IV nuclear reactors. In order to investigate this, a technique was developed to expose the coupons of potential materials to high displacement damage at elevated temperatures to simulate the neutron environment expected in Generation IV reactors. This was completed through a high temperature high-energy heavy-ion implantation. The mechanical properties of the ion irradiated region were tested by either micropillar compression or nanoindentation to determine the local properties, as a function of the implantation dose and exposure temperature. In order to directly compare the microstructural evolution and property degradation from the accelerated testing and classical neutron testing, 316L, 409, and 420 stainless steels were tested. In addition, two sets of diffusion couples from 316L and HT9 stainless steels with various refractory metals. This study has shown that if the ion irradiation size scale is taken into consideration when developing and analyzing the mechanical property data, significant insight into the structural properties of the potential cladding materials can be gained in about a week.
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.
The development of a new radiation effects microscopy (REM) technique is crucial as emerging semiconductor technologies demonstrate smaller feature sizes and thicker back end of line (BEOL) layers. To penetrate these materials and still deposit sufficient energy into the device to induce single event effects, high energy heavy ions are required. Ion photon emission microscopy (IPEM) is a technique that utilizes coincident photons, which are emitted from the location of each ion impact to map out regions of radiation sensitivity in integrated circuits and devices, circumventing the obstacle of focusing high-energy heavy ions. Several versions of the IPEM have been developed and implemented at Sandia National Laboratories (SNL). One such instrument has been utilized on the microbeam line of the 6 MV tandem accelerator at SNL. Another IPEM was designed for ex-vacu use at the 88 cyclotron at Lawrence Berkeley National Laboratory (LBNL). Extensive engineering is involved in the development of these IPEM systems, including resolving issues with electronics, event timing, optics, phosphor selection, and mechanics. The various versions of the IPEM and the obstacles, as well as benefits associated with each will be presented. In addition, the current stage of IPEM development as a user instrument will be discussed in the context of recent results.
The ion photon emission microscope (IPEM), a new radiation effects microscope for the imaging of single event effects from penetrating radiation, is being developed at Sandia National Laboratories and implemented on the 88' cyclotron at Lawrence Berkeley National Laboratories. The microscope is designed to permit the direct correlation between the locations of high-energy heavy-ion strikes and single event effects in microelectronic devices. The development of this microscope has required the production of a robust optical system that is compatible with the ion beam lines, design and assembly of a fast single photon sensitive measurement system to provide the necessary coincidence, and the development and testing of many scintillating films. A wide range of scintillating material for application to the ion photon emission microscope has been tested with few meeting the stringent radiation hardness, intensity, and photon lifetime requirements. The initial results of these luminescence studies and the current operation of the ion photon emission microscope will be presented. Finally, the planned development for future microscopes and ion luminescence testing chambers will be discussed.
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.