Publications

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Friction and wear are major concerns in the performance and reliability of micromechanical (MEMS) devices. While a variety of lubricant and wear resistant coatings are known which we might consider for application to MEMS devices, the severe geometric constraints of many micromechanical systems (high aspect ratios, shadowed surfaces) make most deposition methods for friction and wear-resistance coatings impossible. In this program we have produced and evaluate highly conformal, tribological coatings, deposited by atomic layer deposition (ALD), for use on surface micromachined (SMM) and LIGA structures. ALD is a chemical vapor deposition process using sequential exposure of reagents and self-limiting surface chemistry, saturating at a maximum of one monolayer per exposure cycle. The self-limiting chemistry results in conformal coating of high aspect ratio structures, with monolayer precision. ALD of a wide variety of materials is possible, but there have been no studies of structural, mechanical, and tribological properties of these films. We have developed processes for depositing thin (<100 nm) conformal coatings of selected hard and lubricious films (Al2O3, ZnO, WS2, W, and W/Al{sub 2}O{sub 3} nanolaminates), and measured their chemical, physical, mechanical and tribological properties. A significant challenge in this program was to develop instrumentation and quantitative test procedures, which did not exist, for friction, wear, film/substrate adhesion, elastic properties, stress, etc., of extremely thin films and nanolaminates. New scanning probe and nanoindentation techniques have been employed along with detailed mechanics-based models to evaluate these properties at small loads characteristic of microsystem operation. We emphasize deposition processes and fundamental properties of ALD materials, however we have also evaluated applications and film performance for model SMM and LIGA devices.

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Strength, friction, and wear are dominant factors in the performance and reliability of materials and devices fabricated using nickel based LIGA and silicon based MEMS technologies. However, the effects of frictional contacts and wear on long-term performance of microdevices are not well-defined. To address these effects on performance of LIGA nickel, we have begun a program employing nanoscratch and nanoindentation. Nanoscratch techniques were used to generate wear patterns using loads of 100, 200, 500, and 990 {micro}N with each load applied for 1, 2, 5, and 10 passes. Nanoindentation was then used to measure properties in each wear pattern correcting for surface roughness. The results showed a systematic increase in hardness with applied load and number of nanoscratch passes. The results also showed that the work hardening coefficient determined from indentation tests within the wear patterns follows the results established from tensile tests, supporting use of a nanomechanics-based approach for studying wear.

A commercial plasma enhanced chemical vapor deposition (PECVD) technique with planetary substrate rotation was used to apply a thin (200-400 nm thick) conformal diamond-like carbon (DLC) coating (known as a diamond-like nanocomposite (DLN)) on LIGA fabricated Ni-Mn alloy parts. The PECVD technique is known to overcome the drawbacks associated with the line-of-sight nature of physical vapor deposition (PVD) and substrate heating inherent with traditional chemical vapor deposition (CVD). The purpose of the present study is to characterize the coverage, adhesion, and tribological (friction and wear) behavior of DLN coatings applied to planar and sidewall surfaces of small featured LIGA Ni-Mn fabricated parts, e.g. 280 {micro}m thick sidewalls. Friction and wear tests were performed in dry nitrogen, dry air, and air with 50% RH at Hertzian contact pressures ranging from 0.3 to 0.6 GPa. The friction coefficient of bare Ni-Mn alloy was determined to be 0.9. In contrast, low friction coefficients ({approx}0.02 in dry nitrogen and {approx}0.2 in 50% RH air) and minimal amount of wear were exhibited for the DLN coated LIGA Ni-Mn alloy parts and test coupons. This behavior was due to the ability of the coating to transfer to the rubbing counterface providing low interfacial shear at the sliding contact; resultantly, coating one surface was adequate for low friction and wear. In addition, a 30 nm thick titanium bond layer was determined to be necessary for good adhesion of DLN coating to Ni-Mn alloy substrates. Raman spectroscopy and cross-sectional SEM with energy dispersive x-ray analysis revealed that the DLN coatings deposited by the PECVD with planetary substrate rotation covered both the planar and sidewall surfaces of LIGA fabricated parts, as well as narrow holes of 300 {micro}m (0.012 inch) diameter.

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The synthesis and characterization of crystalline tungsten disulphide (WS2) solid lubricant thin films grown by atomic layer deposition (ALD) using WF6 and H2S gas precursors was studied. A new catalytic route was established to promote nucleation and growth of WS2 films on silicon surfaces with native oxide. Scanning electron microscopy with energy dispersive spectroscopy and Raman spectroscopy were used to determine the film morphology, composition, and crystallinity. The films exhibited solid lubricating behavior with a steady-state friction coefficient of 0.04 in a dry nitrogen environment.

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Micromachines have the potential to significantly impact future weapon component designs as well as other defense, industrial, and consumer product applications. For both electroplated (LIGA) and surface micromachined (SMM) structural elements, the influence of processing on structure, and the resultant effects on material properties are not well understood. The behavior of dynamic interfaces in present as-fabricated microsystem materials is inadequate for most applications and the fundamental relationships between processing conditions and tribological behavior in these systems are not clearly defined. We intend to develop a basic understanding of deformation, fracture, and surface interactions responsible for friction and wear of microelectromechanical system (MEMS) materials. This will enable needed design flexibility for these devices, as well as strengthen our understanding of material behavior at the nanoscale. The goal of this project is to develop new capabilities for sub-microscale mechanical and tribological measurements, and to exercise these capabilities to investigate material behavior at this size scale.

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We have conducted surface treatment and alloying experiments with Al, Fe, and Ti-based metals on the RHEPP-1 accelerator (0.8 MV, 20 W, 80 ns FHWM, up to 1 Hz repetition rate) at Sandia National Laboratories. Ions are generated by the MAP gas-breakdown active anode, which can yield a number of different beam species including H, N, and C, depending upon the injected gas. Beams of intense pulsed high-power ion beams have been used to produce surface modification by changes in microstructure caused by rapid heating and cooling of the surface. Increase of beam power leads to ablation of a target surface, and redeposition of ablated material onto a separate substrate. Experiments are described in which ion beams are used in an attempt to increase high-voltage breakdown of a treated surface. Surface alloying of coated Pt and Hf layers is also described. This mixing of a previously deposited thin-film layer into a Ti-alloy substrate leads to significantly enhanced surface wear durability, compared to either untreated Ti-alloy alone, or the Ti alloy alone treated with the ion beam. Thin-film layers have been produced from a number of target materials. Films of fine-grain Pt and Er are described, and are compared to conventionally formed films. First attempts to form high-dielectric constant BaTiO{sub 3} are described.

The nature of surfaces and the way they interact with each other during sliding contact can have a direct bearing on the performance of a microelectromechanical (MEMS) device. Therefore, a study was undertaken to characterize the surfaces of LIGA fabricated Ni and Cu components. Sidewall and planar surfaces were examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Surface roughness was quantified using the AFM. Post-processing (e.g. lapping, removal of polymer film) can profoundly influence the morphology of LIGA components. Edge rounding and smearing of ductile materials during lapping can result in undesirable sidewall morphologies. By judicious selection of AFM scan sizes, the native roughness ({approximately}10 nm RMS) can be distinguished from that arising due to post processing, e.g. scratches, debris, polymer films. While certain processing effects on morphology such as those due to lapping or release etch can be controlled, the true side wall morphology appears to be governed by the morphology of the polymer mold or by the electroforming process itself, and may be much less amenable to modification.

This report summarizes materials issues associated with advanced micromachines development at Sandia. The intent of this report is to provide a perspective on the scope of the issues and suggest future technical directions, with a focus on computational materials science. Materials issues in surface micromachining (SMM), Lithographic-Galvanoformung-Abformung (LIGA: lithography, electrodeposition, and molding), and meso-machining technologies were identified. Each individual issue was assessed in four categories: degree of basic understanding; amount of existing experimental data capability of existing models; and, based on the perspective of component developers, the importance of the issue to be resolved. Three broad requirements for micromachines emerged from this process. They are: (1) tribological behavior, including stiction, friction, wear, and the use of surface treatments to control these, (2) mechanical behavior at microscale, including elasticity, plasticity, and the effect of microstructural features on mechanical strength, and (3) degradation of tribological and mechanical properties in normal (including aging), abnormal and hostile environments. Resolving all the identified critical issues requires a significant cooperative and complementary effort between computational and experimental programs. The breadth of this work is greater than any single program is likely to support. This report should serve as a guide to plan micromachines development at Sandia.