Publications

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To effectively integrate nanotechnology into functional devices, fundamental aspects of material behavior at the nanometer scale must be understood. Stresses generated during thin film growth strongly influence component lifetime and performance; stress has also been proposed as a mechanism for stabilizing supported nanoscale structures. Yet the intrinsic connections between the evolving morphology of supported nanostructures and stress generation are still a matter of debate. This report presents results from a combined experiment and modeling approach to study stress evolution during thin film growth. Fully atomistic simulations are presented predicting stress generation mechanisms and magnitudes during all growth stages, from island nucleation to coalescence and film thickening. Simulations are validated by electrodeposition growth experiments, which establish the dependence of microstructure and growth stresses on process conditions and deposition geometry. Sandia is one of the few facilities with the resources to combine experiments and modeling/theory in this close a fashion. Experiments predicted an ongoing coalescence process that generates signficant tensile stress. Data from deposition experiments also supports the existence of a kinetically limited compressive stress generation mechanism. Atomistic simulations explored island coalescence and deposition onto surfaces intersected by grain boundary structures to permit investigation of stress evolution during later growth stages, e.g. continual island coalescence and adatom incorporation into grain boundaries. The predictive capabilities of simulation permit direct determination of fundamental processes active in stress generation at the nanometer scale while connecting those processes, via new theory, to continuum models for much larger island and film structures. Our combined experiment and simulation results reveal the necessary materials science to tailor stress, and therefore performance, in nanostructures and, eventually, integrated nanocomponents.

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A new nuclear microscopy technique called ion photon emission microscopy or IPEM was recently invented. IPEM allows analysis involving single ions, such as ion beam induced charge (IBIC) or single event upset (SEU) imaging using a slightly modified optical microscope. The spatial resolution of IPEM is currently limited to more than 10 μm by the scattering and reflection of ion-induced photons, i.e. light blooming or spreading, in the ionoluminescent phosphor layer. We are developing a "Microscopic Gridded Phosphor" (also called Black Matrix) where the phosphor nanocrystals are confined within the gaps of a micrometer scale opaque grid, which limits the amount of detrimental light blooming. MeV-energy proton beam lithography is ideally suited to lithographically form masks for the grid because of high aspect ratio, pattern density and sub-micron resolution of this technique. In brief, the fabrication of the grids was made in the following manner: (1) a MeV proton beam focused to 1.5-2 μm directly fabricated a matrix of pillars in a 15 μm thick SU-8 lithographic resist; (2) 7:1 aspect ratio pillars were then formed by developing the proton exposed area; (3) Ni (Au) was electrochemically deposited onto Cu-coated Si from a sulfamate bath (or buffered CN bath); (4) the SU-8 pillars were removed by chemical etching; finally (5) the metal micro-grid was freed from its substrate by etching the underlying Cu layer. Our proposed metal micro-grids promise an order-of-magnitude improvement in the resolution of IPEM. © 2005 Elsevier B.V. All rights reserved.

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The ability to integrate metal and semiconductor micro-systems to perform highly complex functions, such as RF-MEMS, will depend on developing freestanding metal structures that offer improved conductivity, reflectivity, and mechanical properties. Three issues have prevented the proliferation of these systems: (1) warpage of active components due to through-thickness stress gradients, (2) limited component lifetimes due to fatigue, and (3) low yield strength. To address these issues, we focus on developing and implementing techniques to enable the direct study of the stress and microstructural evolution during electrodeposition and mechanical loading. The study of stress during electrodeposition of metal thin films is being accomplished by integrating a multi-beam optical stress sensor into an electrodeposition chamber. By coupling the in-situ stress information with ex-situ microstructural analysis, a scientific understanding of the sources of stress during electrodeposition will be obtained. These results are providing a foundation upon which to develop a stress-gradient-free thin film directly applicable to the production of freestanding metal structures. The issues of fatigue and yield strength are being addressed by developing novel surface micromachined tensile and bend testers, by interferometry, and by TEM analysis. The MEMS tensile tester has a ''Bosch'' etched hole to allow for direct viewing of the microstructure in a TEM before, during, and after loading. This approach allows for the quantitative measurements of stress-strain relations while imaging dislocation motion, and determination of fracture nucleation in samples with well-known fatigue/strain histories. This technique facilitates the determination of the limits for classical deformation mechanisms and helps to formulate a new understanding of the mechanical response as the grain sizes are refined to a nanometer scale. Together, these studies will result in a science-based infrastructure to enhance the production of integrated metal--semiconductor systems and will directly impact RF MEMS and LIGA technologies at Sandia.

The stress evolution during electrodeposition of NiMn from a sulfamate-based bath was investigated as a function of Mn concentration and current density. The NiMn stress evolution with film thickness exhibited an initial high transitional stress region followed by a region of steady-state stress with a magnitude that depended on deposition rate, similar to the previously reported stress evolution in electrodeposited Ni [S. J. Hearne and J. A. Floro, J. Appl. Phys. 97, 014901-1 (2005)]. The incorporation of increasing amounts of Mn resulted in a linear increase in the steady-state stress at constant current density. However, no significant changes in the texture or grain size were observed, which indicates that an atomistic process is driving the changes in steady-state stress. Additionally, microstrain measured by ex situ x-ray diffraction increased with increasing Mn content, which was likely the result of localized lattice distortions associated with substitutional incorporation of Mn and/or increased twin density.

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The ability of future integrated metal-semiconductor micro-systems such as RF MEMS to perform highly complex functions will depend on developing freestanding metal structures that offer improved conductivity and reflectivity over polysilicon structures. For example, metal-based RF MEMS technology could replace the bulky RF system presently used in communications, navigation, and avionics systems. However, stress gradients that induce warpage of active components have prevented the implementation of this technology. Figure 1, is an interference micrograph image of a series of cantilever beams fabricated from electrodeposited Ni. The curvature in the beams was the result of stress gradients intrinsic to the electrodeposition process. To study the sources of the stress in electrodeposition of Ni we have incorporated a wafer curvature based stress sensor, the multibeam optical stress sensor, into an electrodeposition cell. We have determined that there are two regions of stress induced by electrodepositing Ni from a sulfamate-based bath (Fig 2). The stress evolution during the first region, 0-1000{angstrom}, was determined to be dependent only on the substrate material (Au vs. Cu), whereas the stress evolution during the second region, >1000{angstrom}, was highly dependent on the deposition conditions. In this region, the stress varied from +0.5 GPa to -0.5GPa, depending solely on the deposition rate. We examined four likely sources for the compressive intrinsic stress, i.e. reduction in tensile stress, and determined that only the adatom diffusion into grain boundaries model of Sheldon, et al. could account for the observed compressive stress. In the presentation, we shall discuss the compressive stress generation mechanisms considered and the ramifications of these results on fabrication of electrodeposited Ni for MEMS applications.

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We report the growth and characterization of quaternary AlGaInN. A combination of photoluminescence (PL), high-resolution x-ray diffraction (XRD), and Rutherford backscattering spectrometry (RBS) characterizations enables us to explore the contours of constant PL peak energy and lattice parameter as functions of the quaternary compositions. The observation of room temperature PL emission at 351nm (with 20% Al and 5% In) renders initial evidence that the quaternary could be used to provide confinement for GaInN (and possibly GaN). AlGaInN/GrdnN MQW heterostructures have been grown; both XRD and PL measurements suggest the possibility of incorporating this quaternary into optoelectronic devices.