Publications

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We propose and evaluate a linearized method to measure dynamic friction between micromachined surfaces. This linearized method reduces the number of data points needed to obtain dynamic friction data, minimizing the effect of wear on sliding surfaces during the measurement. We find that the coefficient of dynamic friction is lower than the coefficient of static friction, while the adhesive pressure is indistinguishable for the two measurements. Furthermore, after an initial detailed measurement is made on a device type, the number of trial runs required to take the data on subsequent devices can be reduced from 200 to approximately 20. © Society for Experimental Mechanics 2008.

We designed, fabricated and measured the performance of nanoelectromechanical (NEMS) switches. Initial data are reported with one of the switch designs having a measured switching time of 400 ns and an operating voltage of 5 V. The switches operated laterally with unmeasurable leakage current in the 'off' state. Surface micromachining techniques were used to fabricate the switches. All processing was CMOS compatible. A single metal layer, defined by a single mask step, was used as the mechanical switch layer. The details of the modeling, fabrication and testing of the NEMS switches are reported.

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Capillary condensation of water can have a significant effect on rough surface adhesion. To explore this phenomenon between micromachined surfaces, the authors perform microcantilever experiments as a function of surface roughness and relative humidity (RH). Below a threshold RH, the adhesion is mainly due to van der Waals forces across extensive noncontacting areas. Above the threshold RH, the adhesion jumps due to capillary condensation and increases towards the upper limit of Γ = 144 mJ/m2. A detailed model based on the measured surface topography qualitatively agrees with the experimental data only when the topographic correlations between the upper and lower surfaces are considered. © 2007 American Institute of Physics.

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The goal of this project was to design, build and test novel diagnostics to probe the effect of hydrodynamic forces on coalescence dynamics. Our investigation focused on how a drop coalesces onto a flat surface which is analogous to two drops coalescing, but more amenable to precise experimental measurements. We designed and built a flow cell to create an axisymmetric compression flow which brings a drop onto a flat surface. A computer-controlled system manipulates the flow to steer the drop and maintain a symmetric flow. Particle image velocimetry was performed to confirm that the control system was delivering a well conditioned flow. To examine the dynamics of the coalescence, we implemented an interferometry capability to measure the drainage of the thin film between the drop and the surface during the coalescence process. A semi-automated analysis routine was developed which converts the dynamic interferogram series into drop shape evolution data.

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This report details results from our last year of work (FY2005) on friction in MEMS as funded by the Campaign 6 program for the Microscale Friction project. We have applied different monolayers to a sensitive MEMS friction tester called the nanotractor. The nanotractor is also a useful actuator that can travel {+-}100 {micro}m in 40 nm steps, and is being considered for several MEMS applications. With this tester, we can find static and dynamic coefficients of friction. We can also quantify deviations from Amontons' and Coulomb's friction laws. Because of the huge surface-to-volume ratio at the microscale, surface properties such as adhesion and friction can dominate device performance, and therefore such deviations are important to quantify and understand. We find that static and dynamic friction depend on the monolayer lubricant applied. The friction data can be modeled with a non-zero adhesion force, which represents a deviation from Amontons' Law. Further, we show preliminary data indicating that the adhesion force depends not only on the monolayer, but also on the normal load applied. Finally, we also observe slip deflections before the transition from static to dynamic friction, and find that they depend on the monolayer.

Interfacial adhesion is an important factor in determining the performance and reliability of microelectromechanical systems (MEMS). Van der Waals dispersion forces are the dominant adhesion mechanism in the low relative humidity (RH) regime. At small roughness values, adhesion is mainly due to van der Waals dispersion forces acting across extensive non-contacting areas and is related to 1/Dave2, where Dave is the average surface separation. These contributions must be considered due to the close proximity of the surfaces, which is a result of the planar deposition technology. At large roughness values, van der Waals forces at contacting asperities become the dominating contributor to the adhesion. Capillary condensation of water has a significant effect on rough surface adhesion in the moderate to high RH regime. Above a threshold RH, which is a function of the surface roughness, the adhesion jumps due to meniscus formation at the interface and increases rapidly towards the upper limit of Γ=2γcosθ=44 mJ/m2, where γis the liquid surface energy and θis the contact angle. Copyright © 2006 by ASME.

This report summarizes a survey of several new methods for obtaining mechanical and rheological properties of single biological cells, in particular: (1) The use of laser Doppler vibrometry (LDV) to measure the natural vibrations of certain cells. (2) The development of a novel micro-electro-mechanical system (MEMS) for obtaining high-resolution force-displacement curves. (3) The use of the atomic force microscope (AFM) for cell imaging. (4) The adaptation of a novel squeezing-flow technique to micro-scale measurement. The LDV technique was used to investigate the recent finding reported by others that the membranes of certain biological cells vibrate naturally, and that the vibration can be detected clearly with recent instrumentation. The LDV has been reported to detect motions of certain biological cells indirectly through the motion of a probe. In this project, trials on Saccharomyces cerevisiae tested and rejected the hypothesis that the LDV could measure vibrations of the cell membranes directly. The MEMS investigated in the second technique is a polysilicon surface-micromachined force sensor that is able to measure forces to a few pN in both air and water. The simple device consists of compliant springs with force constants as low as 0.3 milliN/m and Moire patterns for nanometer-scale optical displacement measurement. Fields from an electromagnet created forces on magnetic micro beads glued to the force sensors. These forces were measured and agreed well with finite element prediction. It was demonstrated that the force sensor was fully functional when immersed in aqueous buffer. These results show the force sensors can be useful for calibrating magnetic forces on magnetic beads and also for direct measurement of biophysical forces on-chip. The use of atomic force microscopy (AFM) for profiling the geometry of red blood cells was the third technique investigated here. An important finding was that the method commonly used for attaching the cells to a substrate actually modified the mechanical properties of the cell membrane. Thus, the use of the method for measuring the mechanical properties of the cell may not be completely appropriate without significant modifications. The latest of the studies discussed in this report is intended to overcome the drawback of the AFM as a means of measuring mechanical and rheological properties. The squeezing-flow AFM technique utilizes two parallel plates, one stationary and the other attached to an AFM probe. Instead of using static force-displacement curves, the technique takes advantage of frequency response functions from force to velocity. The technique appears to be quite promising for obtaining dynamic properties. More research is required to develop this technique.

We describe the design and operation of a long-working-distance, incoherent light interference microscope that has been developed to address the growing demand for new microsystem characterization tools. The design of the new microscope is similar to that of a Linnik interference microscope and thus preserves the full working distance of the long-working-distance objectives utilized. However, in contrast to a traditional Linnik microscope, the new microscope does not rely on the use of matched objectives in the sample and the reference arms of the interferometer. An adjustable optical configuration has been devised that allows the total optical path length, wavefront curvature, and dispersion of the reference arm to be matched to the sample arm of the interferometer. The reference arm configuration can be adjusted to provide matching for 5×, 10×, and 20× long-working-distance objectives in the sample arm. In addition to retaining the full working distance of the sample arm objectives, the new design allows interference images to be acquired in situations in which intervening windows are necessary, such as occur with packaged microsystems, microfluidic devices, and cryogenic, vacuum, or environmental chamber studies of microsystem performance. The interference microscope is compatible with phase-shifting interferometry, vertical scanning interferometry, and stroboscopic measurement of dynamic processes. © 2005 Optical Society of America.

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The formation and functions of living materials and organisms are fundamentally different from those of synthetic materials and devices. Synthetic materials tend to have static structures, and are not capable of adapting to the functional needs of changing environments. In contrast, living systems utilize energy to create, heal, reconfigure, and dismantle materials in a dynamic, non-equilibrium fashion. The overall goal of the project was to organize and reconfigure functional assemblies of nanoparticles using strategies that mimic those found in living systems. Active assembly of nanostructures was studied using active biomolecules to drive the organization and assembly of nanocomposite materials. In this system, kinesin motor proteins and microtubules were used to direct the transport and interactions of nanoparticles at synthetic interfaces. In addition, the kinesin/microtubule transport system was used to actively assemble nanocomposite materials capable of storing significant elastic energy. Novel biophysical measurement tools were also developed for measuring the collective force generated by kinesin motor proteins, which will provide insight on the mechanical constraints of active assembly processes. Responsive reconfiguration of nanostructures was studied in terms of using active biomolecules to mediate the optical properties of quantum dot (QD) arrays through modulation of inter-particle spacing and associated energy transfer interaction. Design rules for kinesin-based transport of a wide range of nanoscale cargo (e.g., nanocrystal quantum dots, micron-sized polymer spheres) were developed. Three-dimensional microtubule organizing centers were assembled in which the polar orientation of the microtubules was controlled by a multi-staged assembly process. Overall, a number of enabling technologies were developed over the course of this project, and will drive the exploitation of energy-driven processes to regulate the assembly, disassembly, and dynamic reorganization of nanomaterials.

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.

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Two major research areas pertinent to microelectromechanical systems (MEMS) materials and material surfaces were explored and developed in this 5-year PECASE LDRD project carried out by Professor Roya Maboudian and her collaborators at the University of California at Berkeley. In the first research area, polycrystalline silicon carbide (poly-SiC) was developed as a structural material for MEMS. This material is potentially interesting for MEMS because compared to polycrystalline silicon (polysilicon), the structural material in Sandia National Laboratories' SUMMiTV process, it may exhibit high wear resistance, high temperature operation and a high Young's modulus to density ratio. Each of these characteristics may extend the usefulness of MEMS in Sandia National Laboratories' applications. For example, using polycrystalline silicon, wear is an important issue in microengines, temperature degradation is of concern in thermal actuators and the characteristics of resonators can be extended with the same lithography technology. Two methods of depositing poly-SiC from a 1,3-disilabutane source at 650 C to 800 C by low-pressure chemical vapor deposition (LPCVD) were demonstrated. These include a blanket method in which the material is made entirely out of poly-SiC and a method to coat previously released and fabricated polysilicon MEMS. This deposition method is much simpler to use than previous methods such as high temperature LPCVD and atmospheric CVD. Other major processing issues that were surmounted in this LDRD with the poly-SiC film include etching, doping, and residual strain control. SiC is inert and as such is notoriously difficult to etch. Here, an HBr-based chemistry was demonstrated for the first time to make highly selective etching of SiC at high etch rates. Nitrogen was incorporated from an NH3 gas source, resulting in high conductivity films. Residual strain and strain gradient were shown to depend on deposition parameters, and can be made negative or positive. The tribology of poly-SiC was also investigated. Much improved release stiction and in-use stiction performance relative to polysilicon MEMS was found. Furthermore, wear of poly-SiC-coated MEMS was much reduced relative to uncoated polysilicon MEMS. A prototype baseline process flow now exists to produce poly-SiC in the Berkeley Sensor and Actuator (BSAC) facility. In the second project, galvanic deposition of metals onto polysilicon surfaces has been developed. The possible applications include reflective and optical coatings for optical MEMS, microswitches and microrelays for radio frequency MEMS and catalytic surfaces for microchemical reactors. In contrast to electroless deposition, galvanic displacement deposition requires no prior activation of the surface and is truly selective to silicon surfaces. This approach was used to deposit copper, gold and rhodium onto polysilicon MEMS. A method to study the adhesion of these metals to polysilicon was developed. It was also shown that the surfaces could be rendered hydrophobic by applying thiol-based self-assembled monolayers. This procedure also lowered their surface energy to {approx}3 {micro}J/m{sup 2}, consistent with monolayer-coated polysilicon MEMS.

The primary goals of the present study are to: (1) determine how and why MEMS-scale friction differs from friction on the macro-scale, and (2) to begin to develop a capability to perform finite element simulations of MEMS materials and components that accurately predicts response in the presence of adhesion and friction. Regarding the first goal, a newly developed nanotractor actuator was used to measure friction between molecular monolayer-coated, polysilicon surfaces. Amontons law does indeed apply over a wide range of forces. However, at low loads, which are of relevance to MEMS, there is an important adhesive contribution to the normal load that cannot be neglected. More importantly, we found that at short sliding distances, the concept of a coefficient of friction is not relevant; rather, one must invoke the notion of 'pre-sliding tangential deflections' (PSTD). Results of a simple 2-D model suggests that PSTD is a cascade of small-scale slips with a roughly constant number of contacts equilibrating the applied normal load. Regarding the second goal, an Adhesion Model and a Junction Model have been implemented in PRESTO, Sandia's transient dynamics, finite element code to enable asperity-level simulations. The Junction Model includes a tangential shear traction that opposes the relative tangential motion of contacting surfaces. An atomic force microscope (AFM)-based method was used to measure nano-scale, single asperity friction forces as a function of normal force. This data is used to determine Junction Model parameters. An illustrative simulation demonstrates the use of the Junction Model in conjunction with a mesh generated directly from an atomic force microscope (AFM) image to directly predict frictional response of a sliding asperity. Also with regards to the second goal, grid-level, homogenized models were studied. One would like to perform a finite element analysis of a MEMS component assuming nominally flat surfaces and to include the effect of roughness in such an analysis by using a homogenized contact and friction models. AFM measurements were made to determine statistical information on polysilicon surfaces with different roughnesses, and this data was used as input to a homogenized, multi-asperity contact model (the classical Greenwood and Williamson model). Extensions of the Greenwood and Williamson model are also discussed: one incorporates the effect of adhesion while the other modifies the theory so that it applies to the case of relatively few contacting asperities.

This work demonstrates a polycrystalline silicon surface-micromachined inchworm actuator that exhibits high-performance characteristics such as large force (±0.5 millinewtons), large velocity range (0 to ±4.4 mm/sec), large displacement range (±100 microns), small step size (±10, ±40 or ±100 nanometers), low power consumption (nanojoules per cycle), continuous bidirectional operation and relatively small area (600 × 200μm2). An in situ load spring calibrated on a logarithmic scale from micronewtons to millinewtons, optical microscopy and Michelson interferometry are used to characterize its performance. The actuator consists of a force-amplifying plate that spans two voltage-controlled clamps, and walking is achieved by appropriately sequencing signals to these three components. In the clamps, normal force is borne by equipotential rubbing counterfaces, enabling friction to be measured against load. Using different monolayer coatings, we show that the static coefficient of friction can be changed from 0.14 to 1.04, and that it is load-independent over a broad range. We further find that the static coefficient of friction does not accurately predict the force generated by the actuator and attribute this to nanometer-scale presliding tangential deflections.

We have developed a new inchworm actuator, consisting of a plate and two frictional clamps, which utilizes leveraged bending for improved amplitude control. Here we investigate its friction characteristics. We measure its average slip per cycle as a function of friction load and independently measure the clamp friction coefficients. A model is developed that takes into account the electromechanics of the actuation plate, boundary conditions and clamp friction. We find that the model does not satisfactorily describe the operation of the actuator. We attribute this to pre-sliding tangential deflections and devise a test whose results are consistent with this phenomenon. This suggests that stable pre-sliding deflections control the behavior of nanometer-scale slip events in MEMS.

This report describes a new microsystems technology for the creation of microsensors and microelectromechanical systems (MEMS) using stress-free amorphous diamond (aD) films. Stress-free aD is a new material that has mechanical properties close to that of crystalline diamond, and the material is particularly promising for the development of high sensitivity microsensors and rugged and reliable MEMS. Some of the unique properties of aD include the ability to easily tailor film stress from compressive to slightly tensile, hardness and stiffness 80-90% that of crystalline diamond, very high wear resistance, a hydrophobic surface, extreme chemical inertness, chemical compatibility with silicon, controllable electrical conductivity from insulating to conducting, and biocompatibility. A variety of MEMS structures were fabricated from this material and evaluated. These structures included electrostatically-actuated comb drives, micro-tensile test structures, singly- and doubly-clamped beams, and friction and wear test structures. It was found that surface micromachined MEMS could be fabricated in this material easily and that the hydrophobic surface of the film enabled the release of structures without the need for special drying procedures or the use of applied hydrophobic coatings. Measurements using these structures revealed that aD has a Young's modulus of {approx}650 GPa, a tensile fracture strength of 8 GPa, and a fracture toughness of 8 MPa{center_dot}m {sup 1/2}. These results suggest that this material may be suitable in applications where stiction or wear is an issue. Flexural plate wave (FPW) microsensors were also fabricated from aD. These devices use membranes of aD as thin as {approx}100 nm. The performance of the aD FPW sensors was evaluated for the detection of volatile organic compounds using ethyl cellulose as the sensor coating. For comparable membrane thicknesses, the aD sensors showed better performance than silicon nitride based sensors. Greater than one order of magnitude increase in chemical sensitivity is expected through the use of ultra-thin aD membranes in the FPW sensor. The discoveries and development of the aD microsystems technology that were made in this project have led to new research projects in the areas of aD bioMEMS and aD radio frequency MEMS.

Polycrystalline silicon (polysilicon) surface micromachining is a new technology for building micrometer ({micro}m) scale mechanical devices on silicon wafers using techniques and process tools borrowed from the manufacture of integrated circuits. Sandia National Laboratories has invested a significant effort in demonstrating the viability of polysilicon surface micromachining and has developed the Sandia Ultraplanar Micromachining Technology (SUMMiT V{trademark} ) process, which consists of five structural levels of polysilicon. A major advantage of polysilicon surface micromachining over other micromachining methods is that thousands to millions of thin film mechanical devices can be built on multiple wafers in a single fabrication lot and will operate without post-processing assembly. However, if thin film mechanical or surface properties do not lie within certain tightly set bounds, micromachined devices will fail and yield will be low. This results in high fabrication costs to attain a certain number of working devices. An important factor in determining the yield of devices in this parallel-processing method is the uniformity of these properties across a wafer and from wafer to wafer. No metrology tool exists that can routinely and accurately quantify such properties. Such a tool would enable micromachining process engineers to understand trends and thereby improve yield of micromachined devices. In this LDRD project, we demonstrated the feasibility of and made significant progress towards automatically mapping mechanical and surface properties of thin films across a wafer. The MEMS parametrics measurement team has implemented a subset of this platform, and approximately 30 wafer lots have been characterized. While more remains to be done to achieve routine characterization of all these properties, we have demonstrated the essential technologies. These include: (1) well-understood test structures fabricated side-by-side with MEMS devices, (2) well-developed analysis methods, (3) new metrologies (i.e., long working distance interferometry) and (4) a hardware/software platform that integrates (1), (2) and (3). In this report, we summarize the major focus areas of our LDRD project. We describe the contents of several articles that provide the details of our approach. We also describe hardware and software innovations we made to realize a fully automatic wafer prober system for MEMS mechanical and surface property characterization across wafers and from wafer-lot to wafer-lot.

The Microsystems Subgrid Physics project is intended to address gaps between developing high-performance modeling and simulation capabilities and microdomain specific physics. The initial effort has focused on incorporating electrostatic excitations, adhesive surface interactions, and scale dependent material and thermal properties into existing modeling capabilities. Developments related to each of these efforts are summarized, and sample applications are presented. While detailed models of the relevant physics are still being developed, a general modeling framework is emerging that can be extended to incorporate evolving material and surface interaction modules.

Stiction and friction in micromachines is commonly inhibited through the use of silane coupling agents such as 1H-, 1H-, 2H-, 2H-perfluorodecyltrichlorosilane (FDTS). FDTS coatings have allowed micromachine parts processed in water to be released without debilitating capillary adhesion occurring. These coatings are frequently considered as densely-packed monolayers, well-bonded to the substrate. In this paper, it is demonstrated that FDTS coatings can exhibit complex nanoscale structures, which control whether micromachine parts release or not. Surface images obtained via atomic force microscopy reveal that FDTS coating solutions can generate micellar aggregates that deposit on substrate surfaces. Interferometric imaging of model beam structures shows that stiction is high when the droplets are present and low when only monolayers are deposited. As the aggregate thickness (tens of nanometers) is insufficient to bridge the 2 μm gap under the beams, the aggregates appear to promote beam-substrate adhesion by changing the wetting characteristics of coated surfaces. Contact angle measurements and condensation figure experiments have been performed on surfaces and under coated beams to quantify the changes in interfacial properties that accompany different coating structures. These results may explain the irreproducibility that is often observed with these films.

A new instrument to accurately and verifiably measure mechanical properties across an entire MEMS wafer is under development. We have modified the optics on a conventional microelectronics probe station to enable three-dimensional imaging while maintaining the full working distance of a long working distance objective. This allows standard probes or probe cards to be used. We have proceeded to map out mechanical properties of polycrystalline silicon along a wafer column by the Interferometry for Material Property Measurement (IMaP) methodology. From interferograms of simple actuated cantilevers, out-of-plane deflection profiles at the nanometer scale are obtained. These are analyzed by integrated software routines that extract basic mechanical properties such as cantilever curvature and Young's modulus. Non-idealities such as support post compliance and beam take off angle are simultaneously quantified. Curvature and residual stress are found to depend on wafer position. Although deflections of cantilevers varied across the wafer, Young's modulus E - 161 GPa is independent of wafer position as expected. This result is achieved because the non-idealities have been taken into account.

Two major problems associated with Si-based MEMS (MicroElectroMechanical Systems) devices are stiction and wear. Surface modifications are needed to reduce both adhesion and friction in micromechanical structures to solve these problems. In this paper, we will present a CVD (Chemical Vapor Deposition) process that selectively coats MEMS devices with tungsten and significantly enhances device durability. Tungsten CVD is used in the integrated-circuit industry, which makes this approach manufacturable. This selective deposition process results in a very conformal coating and can potentially address both stiction and wear problems confronting MEMS processing. The selective deposition of tungsten is accomplished through the silicon reduction of WF6. The self-limiting nature of this selective. We deposition process ensures the consistency necessary for process control. The tungsten is deposited after the removal of the sacrificial oxides to minimize stress and process integration problems. Tungsten coating adheres well and is hard and conducting, requirements for device performance. Furthermore, since the deposited tungsten infiltrates under adhered silicon parts and the volume of W deposited is less than the amount of Si consumed, it appears to be possible to release stuck parts that are contacted over small areas such as dimples. The wear resistance of selectively coated W parts has been shown to be significantly improved on microengine test structures.

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.

The authors have developed a new experimental approach for measuring hysteresis in the adhesion between micromachined surfaces. By accurately modeling the deformations in cantilever beams that are subject to combined interfacial adhesion and applied electrostatic forces, they determine adhesion energies for advancing and receding contacts. They draw on this new method to examine adhesion hysteresis for silane coated micromachined structures and found significant hysteresis for surfaces that were exposed to high relative humidity (RH) conditions. Atomic force microscopy studies of these surfaces showed spontaneous formation of agglomerates that they interpreted as silages that have irreversibly transformed from uniform surface layers at low RH to isolated vesicles at high RH. They used contact deformation models to show that the compliance of these vesicles could reasonably account for the adhesion hysteresis that develops at high RH as the surfaces are forced into contact by an externally applied load.

Two major problems associated with Si-based MEMS (MicroElectroMechanical Systems) devices are stiction and wear. Surface modifications are needed to reduce both adhesion and friction in micromechanical structures to solve these problems. In this paper, the authors present a CVD (Chemical Vapor Deposition) process that selectively coats MEMS devices with tungsten and significantly enhances device durability. Tungsten CVD is used in the integrated-circuit industry, which makes this approach manufacturable. This selective deposition process results in a very conformal coating and can potentially address both stiction and wear problems confronting MEMS processing. The selective deposition of tungsten is accomplished through the silicon reduction of WF{sub 6}. The self-limiting nature of the process ensures consistent process control. The tungsten is deposited after the removal of the sacrificial oxides to minimize stress and process integration problems. The tungsten coating adheres well and is hard and conducting, which enhances performance for numerous devices. Furthermore, since the deposited tungsten infiltrates under adhered silicon parts and the volume of W deposited is less than the amount of Si consumed, it appears to be possible to release adhered parts that are contacted over small areas such as dimples. The wear resistance of tungsten coated parts has been shown to be significantly improved by microengine test structures.

We have developed a new process for applying a hydrophobic, low adhesion energy coating to microelectromechanical (MEMS) devices. Monolayer films are synthesized from tridecafluoro-1,1,2,2-tetrahydrooctyltrichlorosilane (FOTS) and water vapor in a low-pressure chemical vapor deposition process at room temperature. Film thickness is self-limiting by virtue of the inability of precursors to stick to the fluorocarbon surface of the film once it has formed. We have measured film densities of {approx}3 molecules nm{sup 2} and film thickness of {approx}1 nm. Films are hydrophobic, with a water contact angle >110{sup o}. We have also incorporated an in-situ downstream microwave plasma cleaning process, which provides a clean, reproducible oxide surface prior to film deposition. Adhesion tests on coated and uncoated MEMS test structures demonstrate superior performance of the FOTS coatings. Cleaned, uncoated cantilever beam structures exhibit high adhesion energies in a high humidity environment. An adhesion energy of 100 mJ m{sup -2} is observed after exposure to >90% relative humidity. Fluoroalkylsilane coated beams exhibit negligible adhesion at low humidity and {<=} 20 {micro}J m{sup -2} adhesion energy at >90% relative humidity. No obvious film degradation was observed for films exposed to >90% relative humidity at room temperature for >24 hr.

Due to extreme surface to volume ratios, adhesion and friction are critical properties for reliability of Microelectromechanical Systems (MEMS), but are not well understood. In this LDRD the authors established test structures, metrology and numerical modeling to conduct studies on adhesion and friction in MEMS. They then concentrated on measuring the effect of environment on MEMS adhesion. Polycrystalline silicon (polysilicon) is the primary material of interest in MEMS because of its integrated circuit process compatibility, low stress, high strength and conformal deposition nature. A plethora of useful micromachined device concepts have been demonstrated using Sandia National Laboratories' sophisticated in-house capabilities. One drawback to polysilicon is that in air the surface oxidizes, is high energy and is hydrophilic (i.e., it wets easily). This can lead to catastrophic failure because surface forces can cause MEMS parts that are brought into contact to adhere rather than perform their intended function. A fundamental concern is how environmental constituents such as water will affect adhesion energies in MEMS. The authors first demonstrated an accurate method to measure adhesion as reported in Chapter 1. In Chapter 2 through 5, they then studied the effect of water on adhesion depending on the surface condition (hydrophilic or hydrophobic). As described in Chapter 2, they find that adhesion energy of hydrophilic MEMS surfaces is high and increases exponentially with relative humidity (RH). Surface roughness is the controlling mechanism for this relationship. Adhesion can be reduced by several orders of magnitude by silane coupling agents applied via solution processing. They decrease the surface energy and render the surface hydrophobic (i.e. does not wet easily). However, only a molecular monolayer coats the surface. In Chapters 3-5 the authors map out the extent to which the monolayer reduces adhesion versus RH. They find that adhesion is independent of RH up to a threshold value, depending on the coating chemistry. The mechanism for the adhesion increase beyond this threshold value is that the coupling agent reconfigures from a surface to a bulk phase (Chapter 3). To investigate the details of how the adhesion increase occurs, the authors developed the mechanics for adhesion hysteresis measurements. These revealed that near-crack tip compression is the underlying cause of the adhesion increase (Chapter 4). A vacuum deposition chamber for silane coupling agent deposition was constructed. Results indicate that vapor deposited coatings are less susceptible to degradation at high RH (Chapter 5). To address issues relating to surfaces in relative motion, a new test structure to measure friction was developed. In contrast to other surface micromachined friction test structures, uniform apparent pressure is applied in the frictional contact zone (Chapter 6). The test structure will enable friction studies over a large pressure and dynamic range. In this LDRD project, the authors established an infrastructure for MEMS adhesion and friction metrology. They then characterized in detail the performance of hydrophilic and hydrophobic films under humid conditions, and determined mechanisms which limit this performance. These studies contribute to a fundamental understanding for MEMS reliability design rules. They also provide valuable data for MEMS packaging requirements.

Two major problems associated with Si-based MEMS devices are stiction and wear. Surface modifications are needed to reduce both adhesion and friction in micromechanical structures to solve these problems. In this paper, we will present a process used to selectively coat MEMS devices with tungsten using a CVD (Chemical Vapor Deposition) process. The selective W deposition process results in a very conformal coating and can potentially solve both stiction and wear problems confronting MEMS processing. The selective deposition of tungsten is accomplished through silicon reduction of WF6, which results in a self-limiting reaction. The selective deposition of W only on polysilicon surfaces prevents electrical shorts. Further, the self-limiting nature of this selective W deposition process ensures the consistency necessary for process control. Selective tungsten is deposited after the removal of the sacrificial oxides to minimize process integration problems. This tungsten coating adheres well and is hard and conducting, requirements for device performance. Furthermore, since the deposited tungsten infiltrates under adhered silicon parts and the volume of W deposited is less than the amount of Si consumed, it appears to be possible to release stuck parts that are contacted over small areas such as dimples. Results from tungsten deposition on MEMS structures with dimples will be presented. The effect of wet and vapor phase cleans prior to the deposition will be discussed along with other process details. The W coating improved wear by orders of magnitude compared to uncoated parts. Tungsten CVD is used in the integrated-circuit industry, which makes this approach manufacturable.