Publications

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The assembly of ceramic components often uses soldering technologies to attach metal structures to the ceramic base material. Because many suitable solder alloys do not readily wet and spread on ceramics, a metallization layer is deposited on the latter to support wetting and spreading by the molten solder for completion of the joint The metallization layer must be sufficiently robust to retain its integrity through the soldering process as well as not negatively impact the long-term reliability of the joint A study was performed to evaluate the mechanical properties of solder joints made to a 0.200Ti/W-40Cu-2.0Pt-0.375Au (pm) thin-film metallization deposited on low-temperature co-fired ceramic (LTCC) base materials. The solder joints were made with the 63Sn-37Pb solder (wt-%, abbreviated Sn-Pb). A pin pull test was developed to measure the tensile strength of the solder joint as a function of soldering parameters. Failure mode analysis was a critical metric for assessing the roles of interfaces, bulk solder, and the ceramic on mechanical performance. The Sn-Pb solder joints experienced a nominal strength loss with increased severity of the soldering process parameters. The strength decline was attributed to changes in the solder joint microstructure, and not degradation to the thin film structures.

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Pressure losses and aerosol collection efficiencies were measured for fibrous filter materials at air-flow rates consistent with high efficiency filtration (hundreds of cubic feet per minute). Microfiber filters coated with nanofibers were purchased and fabricated into test assemblies for a 12-inch duct system designed to mimic high efficiency filtration testing of commercial and industrial processes. Standards and specifications for high efficiency filtration were studied from a variety of institutions to assess protocols for design, testing, operations and maintenance, and quality assurance (e.g., DOE, ASHRAE, ASME). Three materials with varying Minimum Efficiency Reporting Values (MERV) were challenged with sodium chloride aerosol. Substantial filter loading was observed where aerosol collection efficiencies and pressure losses increased during experiments. Filter designs will be optimized and characterized in subsequent years of this study. Additional testing will be performed with higher hazard aerosols at Oak Ridge National Laboratory.

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This study examined the cause of nonwetted regions of the gold (Au) finish on iron-nickel (Fe-Ni) alloy lids that seal ceramic packages using the 80Au-20Sn solder (wt %, abbreviated Au-Sn) and their impact on the final lid-to-ceramic frame solder joint. The Auger electron spectroscopy (AES) surface and depth profile techniques identified surface and through-thickness contaminants in the Au metallization layer. In one case, the AES analysis identified background levels of carbon (C) contamination on the surface; however, the depth profile detected Fe and Ni contaminants that originated from the plating process. The Fe and Ni could impede the completion of wetting and spreading to the edge of the Au metallization. The Au layer of lids not exposed to a Au-Sn solder reflow step had significant surface and through-thickness C contamination. Inorganic contaminants were absent. Subsequent simulated reflow processes removed the C contamination from the Au layer without driving Ni diffusion from the underlying solderable layer. An Au metallization having negligible C contamination developed elevated C levels after exposure to a simulated reflow process due to C contamination diffusing into it from the underlying Ni layer. However, the second reflow step removed that contamination from the Au layer, thereby allowing the metallization to support the formation of lid-to-ceramic frame Au-Sn joints without risk to their mechanical strength or hermeticity.

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The run-out phenomenon was observed in Ag-Cu-Zr active braze joints made between the alumina ceramic and Kovar™ base material. Run-out introduces a significant yield loss by generating functional and/or cosmetic defects in brazements. A prior study identified a correlation between run-out and the aluminum (Al) released by the reduction/oxidation reaction with alumina and aluminum's reaction with the Kovar™ base material. A study was undertaken to understand the fundamental principles of run-out by examining the interface reaction between Ag-xAl filler metals (x = 2,5, and 10 wt-%) and Kovar™ base material. Sessile drop samples were fabricated using brazing temperatures of 965° (T769°F) or 995°C 0823°F) and times of 5 or 20 min. The correlation was made between the degree of wetting and spreading by the sessile drops and the run-out phenomenon. Wetting and spreading increased with Al content (x) of the. Ag-xAl filler metal, but was largely insensitive to the brazing process parameters. The increased Al concentration resulted in higher Al contents of the (Fe, Ni, Co)xAly reaction layer. Run-out was predicted when the filler metal has a locally elevated Al content exceeding 2-5 wt-%. Several mitigation strategies were proposed, based upon these findings.

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Ultrafast optical microscopy of metal z-pinch rods pulsed with megaampere current is contributing new data and critical insight into what provides the fundamental seed for the magneto-Rayleigh-Taylor (MRT) instability. A two-frame near infrared/visible intensified-charge-coupled device gated imager with 2-ns temporal resolution and 3-μm spatial resolution captured emissions from the nonuniformly Joule heated surfaces of ultrasmooth aluminum (Al) rods. Nonuniform surface emissions are consistently first observed from discrete, 10-μm scale, subelectronvolt spots. Aluminum 6061 alloy, with micrometer-scale nonmetallic resistive inclusions, forms several times more spots than 99.999% pure Al 5N; 5-10 ns later, azimuthally stretched elliptical spots and distinct strata (40-100μm wide by 10μm tall) are observed on Al 6061, but not on Al 5N. Such overheat strata, which are aligned parallel to the magnetic field, are highly effective seeds for MRT instability growth. These data give credence to the hypothesis that early nonuniform Joule heating, such as the electrothermal instability, may provide the dominant seed for MRT.

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Ferroelastic domain walls provide opportunities for deterministically controlling mechanical, optical, electrical, and thermal energy. Domain wall characterization in micro- and nanoscale systems, where their spacing may be of the order of 100 nm or less is presently limited to only a few techniques, such as piezoresponse force microscopy and transmission electron microscopy. These respective techniques cannot, however, independently characterize domain polarization orientation and domain wall motion in technologically relevant capacitor structures or in a non-destructive manner, thus presenting a limitation of their utility. In this work, we show how backscatter scanning electron microscopy utilizing channeling contrast yield can image the ferroelastic domain structure of ferroelectric films with domain wall spacing as narrow as 10 nm. Combined with electron backscatter diffraction to identify grain orientations, this technique provides information on domain orientation and domain wall type that cannot be readily measured using conventional non-destructive methods. In addition to grain orientation identification, this technique enables dynamic domain structure changes to be observed in functioning capacitors utilizing electrodes that are transparent to the high-energy backscattered electrons. This non-destructive, high-resolution domain imaging technique is applicable to a wide variety of ferroelectric thin films and a multitude of material systems where nanometer-scale crystallographic twin characterization is required.

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Amorphous titania thin films were examined for use as the active material in a polarimetry based HF sensor. The amorphous titania films were found to be sensitive to vapor phase HF and the reaction product was identified as a hydronium oxofluorotitanate phase, which has previously only been synthesized in aqueous solution. The extent of reaction varied both with vapor phase HF concentration, relative humidity, and the exposure time. HF concentrations as low as 1 ppm could be detected for exposure times of 120 h.

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Three balance of systems (BOS) connector designs common to industry were investigated as a means of assessing reliability from the perspective of arc fault risk. These connectors were aged in field and laboratory environments and performance data captured for future development of a reliability model. Comparison of connector resistance measured during damp heat, mixed flowing gas and field exposure in a light industrial environment indicated disparities in performance across the three designs. Performance was, in part, linked to materials of construction. A procedure was developed to evaluate new and aged connectors for arc fault risk and tested for one of the designs. Those connectors exposed to mixed flowing gas corrosion exhibited considerable Joule heating that may enhance arcing behavior, suggesting temperature monitoring as a potential method for arc fault prognostics. These findings, together with further characterization of connector aging, can provide operators of photovoltaic installations the information necessary to develop a data-driven approach to BOS connector maintenance as well as opportunities for arc fault prognostics.

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Magnetically driven implosions (MDIs) on the Z Facility assemble high-energy-density plasmas for radiation effects and ICF experiments. MDIs are hampered by the Magneto-Rayleigh-Taylor (MRT) instability, which can grow to large amplitude from a small seed perturbation, limiting achievable stagnation pressures and temperatures. The metallic liners used in Magnetized Liner Inertial Fusion (MagLIF) experiments include astonishingly small (-10 nm RMS) initial surface roughness perturbations; nevertheless, unexpectedly large MRT amplitudes are observed in experiments. An electrothermal instability (ETI) may provide a perturbation which exceeds the initial surface roughness. For a condensed metal resistivity increases with temperature. Locations of higher resistivity undergo increased Ohmic heating, resulting in locally higher temperature, and thus still higher resistivity. Such unstable temperature (and pressure) growth produces density perturbations when the locally overheated metal changes phase, providing the seed perturbation for MRT growth. ETI seeding of MRT on thick conductors carrying current in a skin layer has thus far only been inferred by evaluating MRT amplitude late in the experiment. A direct observation of ETI is vital to ensure our simulation tools are accurately representing the seed of the deleterious MRT instability. In this LDRD project, ETI growth was directly observed on the surface of 1.0-mm-diameter solid Al rods which were pulsed with 1 MA of current in 100 ns. Fine structures resulting from ETI-driven temperature variations were observed directly through high resolution gated optical imaging. Data from two Aluminum alloys (6061 and 5N) and a variety fabrication techniques (conventional machining, single-point diamond turned, electropolished) enable evaluation of which imperfections provide a seed for ETI growth and subsequent plasma initiation. Data is relevant to the early stages of MagLIF liner implosions, when the ETI seed of MRT may be initiated, and provides a fundamentally new dataset with which to test our state-of-the-art simulation tools.

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Modification of the dipeptide of phenylalanine, FF, with a boronic acid (BA) functionality imparts unique aqueous self-assembly behavior that responds to multiple stimuli. Changes in pH and ionic strength are used to trigger hydrogelation via the formation of nanoribbon networks. Thus, we show for the first time that the binding of polyols to the BA functionality can modulate a peptide between its assembled and disassembled states.

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Dynamic control of thermal transport in solid-state systems is a transformative capability with the promise to propel technologies including phononic logic, thermal management, and energy harvesting. A solid-state solution to rapidly manipulate phonons has escaped the scientific community. We demonstrate active and reversible tuning of thermal conductivity by manipulating the nanoscale ferroelastic domain structure of a Pb(Zr0.3Ti0.7)O3 film with applied electric fields. With subsecond response times, the room-temperature thermal conductivity was modulated by 11%.

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The ability to integrate ceramics with other materials has been limited due to high temperature (>800degC) ceramic processing. Recently, researchers demonstrated a novel process , aerosol deposition (AD), to fabricate ceramic films at room temperature (RT). In this process, sub - micro n sized ceramic particles are accelerated by pressurized gas, impacted on the substrate, plastically deformed, and form a dense film under vacuum. This AD process eliminates high temperature processing thereby enabling new coatings and device integration, in which ceramics can be deposited on metals, plastics, and glass. However, k nowledge in fundamental mechanisms for ceramic particle s to deform and form a dense ceramic film is still needed and is essential in advancing this novel RT technology. In this wo rk, a combination of experimentation and atomistic simulation was used to determine the deformation behavior of sub - micron sized ceramic particle s ; this is the first fundamental step needed to explain coating formation in the AD process . High purity, singl e crystal, alpha alumina particles with nominal size s of 0.3 um and 3.0 um were examined. Particle characterization, using transmission electron microscopy (TEM ), showed that the 0.3 u m particles were relatively defect - free single crystals whereas 3.0 u m p articles were highly defective single crystals or particles contained low angle grain boundaries. Sub - micron sized Al 2 O 3 particles exhibited ductile failure in compression. In situ compression experiments showed 0.3um particles deformed plastically, fractured, and became polycrystalline. Moreover, dislocation activit y was observed within the se particles during compression . These sub - micron sized Al 2 O 3 particles exhibited large accum ulated strain (2 - 3 times those of micron - sized particles) before first fracture. I n agreement with the findings from experimentation , a tomistic simulation s of nano - Al 2 O 3 particles showed dislocation slip and significant plastic deformation during compressi on . On the other hand, the micron sized Al 2 O 3 particles exhibited brittle f racture in compression. In situ compression experiments showed 3um Al 2 O 3 particles fractured into pieces without observable plastic deformation in compression. Particle deformation behaviors will be used to inform Al 2 O 3 coating deposition parameters and particle - particle bonding in the consolidated Al 2 O 3 coatings.

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Tin (Sn) whiskers are conductive Sn filaments that grow from Sn-plated surfaces, such as surface finishes on electronic packages. The phenomenon of Sn whiskering has become a concern in recent years due to requirements for lead (Pb)-free soldering and surface finishes in commercial electronics. Pure Sn finishes are more prone to whisker growth than their Sn-Pb counterparts and high profile failures due to whisker formation (causing short circuits) in space applications have been documented. At Sandia, Sn whiskers are of interest due to increased use of Pb-free commercial off-the-shelf (COTS) parts and possible future requirements for Pb-free solders and surface finishes in high-reliability microelectronics. Lead-free solders and surface finishes are currently being used or considered for several Sandia applications. Despite the long history of Sn whisker research and the recently renewed interest in this topic, a comprehensive understanding of whisker growth remains elusive. This report describes recent research on characterization of Sn whiskers with the aim of understanding the underlying whisker growth mechanism(s). The report is divided into four sections and an Appendix. In Section 1, the Sn plating process is summarized. Specifically, the Sn plating parameters that were successful in producing samples with whiskers will be reviewed. In Section 2, the scanning electron microscopy (SEM) of Sn whiskers and time-lapse SEM studies of whisker growth will be discussed. This discussion includes the characterization of straight as well as kinked whiskers. In Section 3, a detailed discussion is given of SEM/EBSD (electron backscatter diffraction) techniques developed to determine the crystallography of Sn whiskers. In Section 4, these SEM/EBSD methods are employed to determine the crystallography of Sn whiskers, with a statistically significant number of whiskers analyzed. This is the largest study of Sn whisker crystallography ever reported. This section includes a review of previous literature on Sn whisker crystallography. The overall texture of the Sn films was also analyzed by EBSD. Finally, a short Appendix is included at the end of this report, in which the X-Ray diffraction (XRD) results are discussed and compared to the EBSD analyses of the overall textures of the Sn films. Sections 2, 3, and 4 have been or will be submitted as stand-alone papers in peer-reviewed technical journals. A bibliography of recent Sandia Sn whisker publications and presentations is included at the end of the report.

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In an aim to develop photo-responsive composites, the UV photo-reduction of aqueous titanium oxide nanoparticle-graphene oxide (TiO{sub 2}-GO) dispersions (Lambert et al. J Phys. Chem. 2010 113 (46), 19812-19823) was undertaken. Photo-reduction led to the formation of a black precipitate as well as a soluble portion, comprised of titanium oxide nanoparticle-reduced graphene oxide (TiO{sub 2}-RGO). When allowed to slowly evaporate, self assembled titanium oxide nanoparticle-graphene oxide (SA-TiO{sub 2}-RGO) films formed at the air-liquid interface of the solution. The thickness of SARGO-TiO{sub 2} films range from {approx}30-100 nm when deposited on substrates, and appear to be comprised of a mosaic assembly of graphene nanosheets and TiO{sub 2}, as observed by scanning electron microscopy. Raman spectroscopy and X-ray photoelectron spectroscopy indicate that the graphene oxide is only partially reduced in the SA-TiO{sub 2}-RGO material. These films were also deposited onto inter-digitated electrodes and their photo-responsive behavior was examined. UV-exposure lead to a {approx} 200 kOhm decrease in resistance across the device, resulting in a cathodically biased film. The cathodic bias of the films was utilized for the subsequent reduction of Ag(NO{sub 3}) into silver (Ag) nanoparticles, forming a ternary Ag-(SA-RGO-TiO{sub 2}) composite. Various aspects of the self assembled films, their photoconductive properties as well as potential applications will be presented.

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We have systematically studied the effect of pH and 1,3-diaminopropane additive concentration on the morphology of ZnO nanorod and nanoneedle arrays grown in aqueous solution using a variety of seed layers. Increase in the growth solution pH from 6.8 to 13.2 resulted in a near doubling of the growth rate in the [0001] direction possibly due to attractive interaction between the zinc species and the growth surface at high pH, leading to nanorod arrays with reduced faceting and higher aspect ratios. Increases in 1,3-diaminopropane concentration initially enhanced and subsequently inhibited growth of tapered ZnO nanoneedles on seed layers consisting of ZnO nanoparticles, oriented ZnO films, or columnar facets of ZnO microrods. The final nanoneedle dimensions, packing density, and alignment were strongly affected by 1,3-diaminopropane concentration and seed layer type, which can be explained in terms of the relative strength of zinc chelation by 1,3-diaminopropane, the areal density of seeds, and other factors. The precise tuning of ZnO crystalline morphology via the control of seeding and growth conditions may be beneficial to many potential applications that require these aligned crystalline nanostructures. © 2008 American Chemical Society.

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Pre-oxidized and glass-to-metal (GtM) sealed austenitic stainless steels were found to display a ferritic layer near the metal/oxide interface, as determined by electron backscatter diffraction (EBSD). Electron probe microanalysis (EPMA) showed that this layer was depleted in alloying elements due to the oxidation and sealing process. Characterization of the morphology suggested that it formed through the martensite transformation mechanism. Moreover, this observed layer was correlated to the composition gradient through published empirical relationships for martensite-start (Ms) temperatures. Due to Cr, Mn, and Si depletion during pre-oxidation and glass sealing, Ms temperatures near room temperature are possible in this surface region. Further support for a martensitic transformation was provided by thermochemical modeling. Possible detrimental ramifications of bulk composition, surface depletion, and phase transformations on GtM sealing are discussed. Copyright © 2007 MS&T'07®.

Microtubules and motor proteins are protein-based biological agents that work cooperatively to facilitate the organization and transport of nanomaterials within living organisms. This report describes the application of these biological agents as tools in a novel, interdisciplinary scheme for assembling integrated nanostructures. Specifically, selective chemistries were used to direct the favorable adsorption of active motor proteins onto lithographically-defined gold electrodes. Taking advantage of the specific affinity these motor proteins have for microtubules, the motor proteins were used to capture polymerized microtubules out of suspension to form dense patterns of microtubules and microtubule bridges between gold electrodes. These microtubules were then used as biofunctionalized templates to direct the organization of functionalized nanocargo including single-walled carbon nanotubes and gold nanoparticles. This biologically-mediated scheme for nanomaterials assembly has shown excellent promise as a foundation for developing new biohybrid approaches to nanoscale manufacturing.

An oxidation treatment, often termed "pre-oxidation", is performed on austenitic stainless steel prior to glass/metal joining to produce hermetic seals. The resulting thin oxide acts as a transitional layer and a source of Cr and other elements which diffuse into the glass during the subsequent bonding process. Pre-oxidation is performed in a low pO 2 atmosphere to avoid iron oxide formation and the final oxide is composed of Cr 2O 3, MnCr 2O 4 spinel, and SiO 2. Significant heat-to-heat variations in the oxidation behavior of 304L stainless steel have been observed, which result in inconsistent glass/metal seal behavior. The objectives of this work were to characterize the oxidation kinetics, the oxide morphology and composition, and the stainless steel attributes that lead to robust glass/metal seals. The oxidation kinetics were determined by thermogravimetric (TG) analysis and the oxide layers were characterized using metallography, SEM, focused ion beam (FIB) analysis, and image analysis. The results show that poor sealing behavior is associated with slower oxidation kinetics and a more continuous layer of SiO 2 at the metal/oxide interface. In addition, the effects of 304L heat composition on oxidation behavior will be discussed. Copyright © 2006 ASM International®.

An oxidation treatment, often termed "pre-oxidation", is performed on austenitic stainless steel prior to joining to alkali barium silicate glass to produce hermetic seals. The resulting thin oxide acts as a transitional layer and a source of Cr and other elements which diffuse into the glass during the subsequent bonding process. Pre-oxidation is performed in a low pO2 atmosphere to avoid iron oxide formation and the final oxide is composed of Cr2O3, MnCr2O4 spinel, and SiO2. Significant heat-to-heat variations in the oxidation behavior of 304L stainless steel have been observed, which result in inconsistent glass-to-metal (GTM) seal behavior. The objectives of this work were to characterize the stainless steel pre-oxidized layer and the glass/oxide/304L interface region after glass sealing. The 304L oxidation kinetics were determined by thermogravimetric (TG) analysis and the glass/metal seals characteristics were studied using sessile drop tests, in which wetting angles were measured and glass adhesion was analyzed. The pre-oxidized layers and glass/metal interface regions were characterized using metallography, focused ion beam (FIB) sectioning, scanning and transmission electron microscopy, and electron probe microanalysis (EPMA). The results show that poor glass sealing behavior is associated with a more continuous layer of SiO 2 at the metal/oxide interface.

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Solution-based synthesis is a powerful approach for creating nano-structured materials. Although there have been significant recent successes in its application to fabricating nanomaterials, the general principles that control solution synthesis are not well understood. The purpose of this LDRD project was to develop the scientific principles required to design and build unique nanostructures in crystalline oxides and II/VI semiconductors using solution-based molecular self-assembly techniques. The ability to synthesize these materials in a range of different nano-architectures (from controlled morphology nanocrystals to surface templated 3-D structures) has provided the foundation for new opportunities in such areas as interactive interfaces for optics, electronics, and sensors. The homogeneous precipitation of ZnO in aqueous solution was used primarily as the model system for the project. We developed a low temperature, aqueous solution synthesis route for preparation of large arrays of oriented ZnO nanostructures. Through control of heterogeneous nucleation and growth, methods to predicatively alter the ZnO microstructures by tailoring the surface chemistry of the crystals were established. Molecular mechanics simulations, involving single point energy calculations and full geometry optimizations, were developed to assist in selecting appropriate chemical systems and understanding physical adsorption and ultimately growth mechanisms in the design of oxide nanoarrays. The versatility of peptide chemistry in controlling the formation of cadmium sulfide nanoparticles and zinc oxide/cadmium sulfide heterostructures was also demonstrated.

We report for the first time a one-step, templateless method to directly prepare large arrays of oriented TiO{sub 2}-based nanotubes and continuous films. These titania nanostructures can also be easily prepared as conformal coatings on a substrate. The nanostructured films were formed on a Ti substrate seeded with TiO{sub 2} nanoparticles. SEM and TEM results suggested that a folding mechanism of sheetlike structures was involved in the formation of the nanotubes. The oriented arrays of TiO{sub 2} nanotubes, continuous films, and coatings are expected to have potentials for applications in catalysis, filtration, sensing, photovoltaic cells, and high surface area electrodes.

The Materials Chemistry Department 1846 has developed a lab-scale chem-prep process for the synthesis of PNZT 95/5, referred to as the ''SP'' process (Sandia Process). This process (TSP) has been successfully transferred to and scaled-up by Department 14192 (Ceramics and Glass Department), producing the larger quantities of PZT powder required to meet the future supply needs of Sandia for neutron generator production. The particle size distributions of TSP powders routinely have been found to contain a large particle size fraction that was absent in development (SP) powders. This SAND report documents experimental studies focused on characterizing these particles and assessing their potential impact on material performance. To characterize these larger particles, fractionation of several TSP powders was performed. The ''large particle size fractions'' obtained were characterized by particle size analysis, SEM, and ICP analysis and incorporated into compacts and sintered. Large particles were found to be very similar in structure and composition as the bulk of the powder. Studies showed that the large-size fractions of the powders behave similarly to the non-fractionated powder with respect to the types of microstructural features once sintered. Powders were also compared that were prepared using different post-synthesis processing (i.e. differences in precipitate drying). Results showed that these powders contained different amounts and sizes of porous inclusions when sintered. How this affects the functional performance of the PZT 95/5 material is the subject of future investigations.

This paper reports the preparation of cubically ordered, self-assembled nanostructural crystals on micropatterned surfaces. Large ordered arrays of octahedral crystals were formed on substrates with triangular-shaped micropatterns that match the shape of the {111} surface morphology of the crystals. Many crystals became self-aligned in X, Y, and Z orientations through the interaction with the matching micropatterns. However, line micropatterns did not produce such well-defined crystals and crystal alignment. This work is among the first examples to show 3D crystal alignment independent of the long rodlike micellar structure that is characteristic of the hexagonal phases. Significantly, it also suggests that the geometry of the underline patterns has a large effect on the crystal morphology and orientation. We hope that these results will be helpful in developing microdevices based on self-assembled nanoscale materials.

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