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Eddy sensors for small diameter stainless steel tubes

Morales, Alfredo M.; Andersen, Lisa E.; Skinner, J.L.; LaFord, Marianne L.; Korellis, Henry J.

The goal of this project was to develop non-destructive, minimally disruptive eddy sensors to inspect small diameter stainless steel metal tubes. Modifications to Sandia's Emphasis/EIGER code allowed for the modeling of eddy current bobbin sensors near or around 1/8-inch outer diameter stainless steel tubing. Modeling results indicated that an eddy sensor based on a single axial coil could effectively detect changes in the inner diameter of a stainless steel tubing. Based on the modeling results, sensor coils capable of detecting small changes in the inner diameter of a stainless steel tube were designed, built and tested. The observed sensor response agreed with the results of the modeling and with eddy sensor theory. A separate limited distribution SAND report is being issued demonstrating the application of this sensor.

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Material compatibility and thermal aging of thermoelectric materials

Morales, Alfredo M.; Chames, Jeffery M.; Cliff, Miles; Cliff, Miles; Gardea, Andrew D.; Whalen, Scott A.

In order to design a thermoelectric (TE) module suitable for long-term elevated temperature use, the Department 8651 has conducted parametric experiments to study material compatibility and thermal aging of TE materials. In addition, a comprehensive material characterization has been preformed to examine thermal stability of P- and N-based alloys and their interaction with interconnect diffusion barrier(s) and solder. At present, we have completed the 7-days aging experiments for 36 tiles, from ambient to 250 C. The thermal behavior of P- and N-based alloys and their thermal interaction with both Ni and Co diffusion barriers and Au-Sn solder were examined. The preliminary results show the microstructure, texture, alloy composition, and hardness of P-(Bi,Sb){sub 2}Te{sub 3} and N-Bi{sub 2}(Te,Se){sub 3} alloys are thermally stable up to 7 days annealing at 250 C. However, metallurgical reactions between the Ni-phosphor barriers and P-type base alloy were evident at temperatures {ge} 175 C. At 250 C, the depth (or distance) of the metallurgical reaction and/or Ni diffusion into P-(Bi,Sb){sub 2}Te{sub 3} is approximately 10-15 {micro}m. This thermal instability makes the Ni-phosphor barrier unsuitable for use at temperatures {ge} 175 C. The Co barrier appeared to be thermally stable and compatible with P(Bi,Sb){sub 2}Te{sub 3} at all annealing temperatures, with the exception of a minor Co diffusion into Au-Sn solder at {ge} 175 C. The effects of Co diffusion on long-term system reliability and/or the thermal stability of the Co barrier are yet to be determined. Te evaporation and its subsequent reaction with Au-Sn solder and Ni and Co barriers on the ends of the tiles at temperatures {ge} 175 C were evident. The Te loss and its effect on the long-term required stoichiometry of P-(Bi, Sb){sub 2}Te{sub 3} are yet to be understood. The aging experiments of 90 days and 180 days are ongoing and scheduled to be completed in 30 days and 150 days, respectively. Material characterization activities are continuing for the remaining tiles.

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Extreme solid state refrigeration using nanostructured Bi-Te alloys

Sharma, Peter A.; Morales, Alfredo M.; Spataru, Dan C.

Materials are desperately needed for cryogenic solid state refrigeration. We have investigated nanostructured Bi-Te alloys for their potential use in Ettingshausen refrigeration to liquid nitrogen temperatures. These alloys form alternating layers of Bi{sub 2} and Bi{sub 2}Te{sub 3} blocks in equilibrium. The composition Bi{sub 4}Te{sub 3} was identified as having the greatest potential for having a high Ettingshausen figure of merit. Both single crystal and polycrystalline forms of this material were synthesized. After evaluating the Ettingshausen figure of merit for a large, high quality polycrystal, we simulated the limits of practical refrigeration in this material from 200 to 77 K using a simple device model. The band structure was also computed and compared to experiments. We discuss the crystal growth, transport physics, and practical refrigeration potential of Bi-Te alloys.

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Metallurgy, thermal stability, and failure mode of the commercial Bi-Te-based thermoelectric modules

Yang, Nancy Y.; Morales, Alfredo M.

Bi-Te-based thermoelectric (TE) alloys are excellent candidates for power generation modules. We are interested in reliable TE modules for long-term use at or below 200 C. It is known that the metallurgical characteristics of TE materials and of interconnect components affect the performance of TE modules. Thus, we have conducted an extensive scientific investigation of several commercial TE modules to determine whether they meet our technical requirements. Our main focus is on the metallurgy and thermal stability of (Bi,Sb){sup 2}(Te,Se){sup 3} TE compounds and of other materials used in TE modules in the temperature range between 25 C and 200 C. Our study confirms the material suite used in the construction of TE modules. The module consists of three major components: AlN cover plates; electrical interconnects; and the TE legs, P-doped (Bi{sub 8}Sb{sub 32})(Te{sub 60}) and N-doped (Bi{sub 37}Sb{sub 3})(Te{sub 56}Se{sub 4}). The interconnect assembly contains Sn (Sb {approx} 1wt%) solder, sandwiched between Cu conductor with Ni diffusion barriers on the outside. Potential failure modes of the TE modules in this temperature range were discovered and analyzed. The results show that the metallurgical characteristics of the alloys used in the P and N legs are stable up to 200 C. However, whole TE modules are thermally unstable at temperatures above 160 C, lower than the nominal melting point of the solder suggested by the manufacture. Two failure modes were observed when they were heated above 160 C: solder melting and flowing out of the interconnect assembly; and solder reacting with the TE leg, causing dimensional swelling of the TE legs. The reaction of the solder with the TE leg occurs as the lack of a nickel diffusion barrier on the side of the TE leg where the displaced solder and/or the preexisting solder beads is directly contact the TE material. This study concludes that the present TE modules are not suitable for long-term use at temperatures above 160 C due to the reactivity between the Sn-solder and the (Bi,Sb){sup 2}(Te,Se){sup 3} TE alloys. In order to deploy a reliable TE power generator for use at or below 200 C, alternate interconnect materials must be used and/or a modified module fabrication technique must be developed.

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Fundamental enabling issues in nanotechnology :

Foiles, Stephen M.; Hearne, Sean J.; Morales, Alfredo M.; Webb, Edmund B.; Zimmerman, Jonathan A.

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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Universal bioprocessor LDRD final report

Davalos, Rafael V.; Krafcik, Karen L.; Salmi, Allen J.; Van De Vreugde, James L.; Mosier, Bruce P.; Morales, Alfredo M.

Microsystems pose unparalleled opportunity in the realm of real-time sample analysis for multiple applications, including Homeland Security monitoring devices, environmental monitoring, and biomedical diagnostics. The need for a universal means of processing, separating, and delivering a sample within these devices is a critical need if these systems are to receive widespread implementation in the industry and government sectors. Efficient particle separation and enrichment techniques are critical for a range of analytical functions including pathogen detection, sample preparation, high-throughput particle sorting, and biomedical diagnostics. Previously, using insulator-based dielectrophoresis (iDEP) in microfluidic glass devices, we demonstrated simultaneous particle separation and concentration. As an alternative to glass, we evaluate the performance of similar iDEP structures produced in polymer-based microdevices and their enhancement through dynamic surface coatings. There are numerous processing and operational advantages that motivate our transition to polymers such as the availability of numerous innate chemical compositions for tailoring performance, mechanical robustness, economy of scale, and ease of thermoforming and mass manufacturing. The polymer chips we have evaluated are fabricated through an injection molding process of the commercially available cyclic olefin copolymer Zeonor{reg_sign}. We demonstrate that the polymer devices achieve the same performance metrics as glass devices. Additionally, we show that the nonionic block copolymer surfactant Pluronic F127 has a strong interaction with the cyclic olefin copolymer at very low concentrations, positively impacting performance by decreasing the magnitude of the applied electric field necessary to achieve particle trapping. The presence of these dynamic surface coatings, therefore, lowers the power required to operate such devices and minimizes Joule heating. The results of this study demonstrate that polymeric microfluidic devices with surfactant coatings for insulator-based dielectrophoresis provide an affordable engineering strategy for selective particle enrichment and sorting.

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Design and fabrication of a meso-scale stirling engine and combustor

Haroldsen, Brent L.; Chen, Jacqueline H.; Morales, Alfredo M.; Hekmaty, Michelle A.; Krafcik, Karen L.; Raber, Thomas N.; Mills, Bernice E.; Ceremuga, Joseph T.

Power sources capable of supplying tens of watts are needed for a wide variety of applications including portable electronics, sensors, micro aerial vehicles, and mini-robotics systems. The utility of these devices is often limited by the energy and power density capabilities of batteries. A small combustion engine using liquid hydrocarbon fuel could potentially increase both power and energy density by an order of magnitude or more. This report describes initial development work on a meso-scale external combustion engine based on the Stirling cycle. Although other engine designs perform better at macro-scales, we believe the Stirling engine cycle is better suited to small-scale applications. The ideal Stirling cycle requires efficient heat transfer. Consequently, unlike other thermodynamic cycles, the high heat transfer rates that are inherent with miniature devices are an advantage for the Stirling cycle. Furthermore, since the Stirling engine uses external combustion, the combustor and engine can be scaled and optimized semi-independently. Continuous combustion minimizes issues with flame initiation and propagation. It also allows consideration of a variety of techniques to promote combustion that would be difficult in a miniature internal combustion engine. The project included design and fabrication of both the engine and the combustor. Two engine designs were developed. The first used a cylindrical piston design fabricated with conventional machining processes. The second design, based on the Wankel rotor geometry, was fabricated by through-mold electroforming of nickel in SU8 and LIGA micromolds. These technologies provided the requisite precision and tight tolerances needed for efficient micro-engine operation. Electroformed nickel is ideal for micro-engine applications because of its high strength and ductility. A rotary geometry was chosen because its planar geometry was more compatible with the fabrication process. SU8 lithography provided rapid prototypes to verify the design. A final high precision engine was created via LIGA. The micro-combustor was based on an excess enthalpy concept. Development of a micro-combustor included both modeling and experiments. We developed a suite of simulation tools both in support of the design of the prototype combustors, and to investigate more fundamental aspects of combustion at small scales. Issues of heat management and integration with the micro-scale Stirling engine were pursued using CFD simulations. We found that by choice of the operating conditions and channel dimensions energy conversion occurs by catalysis-dominated or catalysis-then-homogeneous phase combustion. The purpose of the experimental effort in micro-combustion was to study the feasibility and explore the design parameters of excess enthalpy combustors. The efforts were guided by the necessity for a practical device that could be implemented in a miniature power generator, or as a stand-alone device used for heat generation. Several devices were fabricated and successfully tested using methane as the fuel.

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The mechanical properties, dimensional tolerance and microstructural characterization of micro-molded ceramic and metal components

Microsystem Technologies

Garino, Terry J.; Morales, Alfredo M.; Boyce, B.L.

Metal and ceramic micro-components with ∼10 μm features were fabricated by molding nano-powder-binder mixtures in micro-molds produced from LiGA-formed masters and then sintering to achieve the desired density and properties. The mechanical properties of the metals nickel and 316L stainless steel were measured in tension using miniature dog bone shaped, micro-molded test specimens. The sintering temperature controlled yield stress (YS), the ultimate tensile strength (UTS) and the ductility of the nickel with the YS and the UTS decreasing and the ductility increasing with increasing sintering temperature. For the stainless steel, the YS was nearly 400 MPa, UTS was 650 MPa and the ductility was 3%. The mechanical properties of aluminum oxide ceramics were determined using 4-point bending on miniature micro-molded bend bars. The average modulus of rupture (MOR) was 260 MPa. Careful measurements were made of the dimensional tolerance of the micro-molded parts both before and after sintering using automated optical metrology. The variability in the dimensions of a sintered SS gear after sintering was <3 μm. Finally microscopic examination of the micromolded components indicated that the final grain size was generally less than 1 μm with minimal residual porosity.

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Assembly and electrical characterization of DNA-wrapped carbon nanotube devices

Proposed for publication in Journal of Vacuum Science and Technology B.

Dentinger, Paul M.; Pathak, Srikant P.; Jones, Frank E.; Hunter, Lucas L.; Leonard, Francois L.; Morales, Alfredo M.

In this article we report on the electrical characteristics of single wall carbon nanotubes (SWCNTs) wrapped with single-stranded deoxyribonucleic acid (ssDNA). We fabricate these devices using a solution-based method whereby SWCNTs are dispersed in aqueous solution using 20-mer ssDNA, and are placed across pairs of Au electrodes using alternating current dielectrophoresis (ACDEP). In addition to current voltage characteristics, we evaluate our devices using scanning electron microscopy and atomic force microscopy. We find that ACDEP with ssDNA based suspensions results in individual SWCNTs bridging metal electrodes, free of carbon debris, while similar devices prepared using the Triton X-100 surfactant yield nanotube bundles, and frequently have carbon debris attached to the nanotubes. Furthermore, the presence of ssDNA around the nanotubes does not appear to appreciably affect the overall electrical characteristics of the devices. In addition to comparing the properties of several devices prepared on nominally clean Au electrodes, we also investigate the effects of self-assembled monolayers of C{sub 14}H{sub 29}-SH alkyl thiol and benzyl mercaptan on the adhesion and electrical transport across the metal/SWCNT/metal devices.

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Autonomic Healing of Epoxy Using Micro-Encapsulated Dicyclopentadiene

Giunta, Rachel K.; Thoma, Steven T.; Giunta, Rachel K.; Stavig, Mark E.; Emerson, John A.; Morales, Alfredo M.

The autonomic healing ability of an epoxy adhesive containing micro-encapsulated dicyclopentadiene (DCPD) was evaluated. The epoxy resin used was Epon 828 cured with either Versamid 140 or diethylenetriamine (DETA). Variables included total weight percent of microcapsules (MCs) and catalyst, as well as the catalyst to DCPD ratio. The degree of healing was determined by the fracture toughness before and after ''healing'' using double-cantilever beam analysis. It was found that the degree of self-healing was most directly related to the contact area (i.e. crack width) during healing. Temperature also played a significant role. Observed differences between the results of this study and those in literature are discussed.

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41 Results
41 Results