Utilizing on-chip testing and electron microscopy to obtain a mechanistic understanding of fatigue and wear in polysilicon structural films
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Proposed for publication in Applied Physics Letters.
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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.
Journal of Manufacturing Processes
Deep X-ray lithography based techniques such as LIGA (German acronym representing Lithographie, Galvanoformung, and Abformung) are being currently used to fabricate net-shape components for microelectromechanical systems (MEMS). Unlike other microfabrication techniques, LIGA lends itself to a broad range of materials, including metals, alloys, polymers, as well as ceramics and composites. Currently, Ni and Ni alloys are the materials of choice for LIGA microsystems. While Ni alloys may meet the structural requirements for MEMS, their tribological (friction and wear) behavior poses great challenges for the reliable operation of LIGA-fabricated MEMS. Typical sidewall morphologies of LIGA-fabricated parts are described, and their role in the tribological behavior of MEMS is discussed. The adaptation of commercial plasma-enhanced chemical vapor deposition to coat the sidewalls of LIGA-fabricated parts with diamond-like nanocomposite is described.
Proposed for publication in Acta Materialia, 50th Anniversary.
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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.
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, the authors 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 WF{sub 6}, 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 cleanings 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.
The burgeoning new technology of Micro-Electro-Mechanical Systems (MEMS) shows great promise in the weapons arena. We can now conceive of micro-gyros, micro-surety systems, and micro-navigators that are extremely small and inexpensive. Do we want to use this new technology in critical applications such as nuclear weapons? This question drove us to understand the reliability and failure mechanisms of silicon surface-micromachined MEMS. Development of a testing infrastructure was a crucial step to perform reliability experiments on MEMS devices and will be reported here. In addition, reliability test structures have been designed and characterized. Many experiments were performed to investigate failure modes and specifically those in different environments (humidity, temperature, shock, vibration, and storage). A predictive reliability model for wear of rubbing surfaces in microengines was developed. The root causes of failure for operating and non-operating MEMS are discussed. The major failure mechanism for operating MEMS was wear of the polysilicon rubbing surfaces. Reliability design rules for future MEMS devices are established.
Annual Proceedings - Reliability Physics (Symposium)
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 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.
Predictive models of solid lubricant performance are needed to determine the dynamic behavior of electromechanical devices after long periods of storage. X-ray photoelectron spectroscopy has been used to determine the kinetics of oxidation and sulfate formation for solid lubricants and self-lubricating materials containing MoS{sub 2}, exposed to a variety of oxidation conditions. The frictional performance of the lubricant has then been determined as a fi.mction of its surface chemistry and the ambient environment in which sliding takes place. Results indicate that surface sulfate formation governs the initial or start-up friction coefficient of MoS{sub 2}-containing films, while the composition of the ambient gas determines the steady-state friction coefficient. The dependence of the steady-state friction coefficient on the environment in which sliding takes place has been examined, and the results show that dynamic oxidation of surfaces having exposed metal has a major impact on friction. Surface oxidation is also shown to influence the frictional behavior of a self-lubricating composite material containing MoS{sub 2}.
The solid lubricant used most extensively in strong links throughout the enduring stockpile contains MoS{sub 2}, which is known to react with oxygen and water vapor resulting in a change in the material`s friction and wear behavior. The authors have examined the frictional behavior of this lubricant as a function of oxidation, in support of efforts to quantify the impact of changes in the material on the dynamic behavior of the MC2969 strong link. Their results show that the friction response of oxidized lubricant is strongly influenced by the amount of burnishing performed on the lubricant after deposition. Low levels of burnish leave a thick film, of which only the near surface degrades during oxidation. Rapid wear of the oxidized material leaves a surface whose properties are the same as non-oxidized material. Higher levels of burnish leave a thinner film of lubricant such that the entire film may be oxidized. The friction coefficient on this surface reaches a steady state value greater than that of non oxidized material. In addition to these fundamental differences in steady state behavior, they have shown that the initial friction coefficient on oxidized surfaces is related to the amount of sulfide converted to sulfate, regardless of the oxidation conditions used. Measurements on parts returned from the stockpile show that the friction behavior of aged hardware is consistent with the behavior observed on controlled substrates containing thin lubricant films.
The oxidation and performance of the solid film lubricant used in a majority of the surety devices in the enduring stockpile have been investigated. Oxidation of this lubricant in air at 150 C produces a significant increase in the molybdenum oxide to sulfide ratio, indicative of degradation of the primary lubricating constituent of the composite lubricant. Oxidation is more extensive on samples that were burnished such that the substrate is exposed over a fraction of the surface, relative to those which were only lightly burnished. Friction results indicate that oxidation in air did not increase the initial or steady-state friction coefficient for lightly burnished surfaces. However, surfaces burnished to expose substrate material experienced a significant increase in both initial and steady-state friction. Oxidation of lubricated parts retrieved from aged stronglinks has also been demonstrated.
An aqueous-based process that uses electrophoresis to attract powdered lubricant in suspension to a charged target was developed. The deposition process yields coatings with low friction, complies with environmental safety regulations, requires minimal equipment, and has several advantages over processes involving organic binders or vacuum techniques. This work focuses on development of the deposition process, includes an analysis of the friction coefficient of the material in sliding contact with stainless steel under a range of conditions, and a functional evaluation of coating performance in a precision mechanical device application. Results show that solid lubricant films with friction coefficients as low as 0.03 can be produced. A 0.03 friction coefficient is superior to solid lubricants with binder systems and is comparable to friction coefficients generated with more costly vacuum techniques.
Sputtered MoS{sub 2} is a solid lubricant capable of ultralow friction coefficients (below 0.05) load-bearing capacity. Since it exhibits low friction in vacuum, low outgassing rate, is non-migrating and lacks organic binders, this material is an attractive lubricant for space mechanisms. To exploit these new materials to their fullest potential, designers of space-based motion systems require data on the effects of atomic oxygen exposure on dense, sputtered MoS{sub 2}. This paper describes the effects of atomic oxygen in low earth orbit on the friction and surface composition of sputtered MoS{sub 2} films. Sputtered multilayer films of MoS{sub 2} with nickel (0.7 nm Ni per 10 nm MoS{sub 2}, for 1 {mu}m total film thickness), and MoS{sub 2} cosputtered with antimony oxide (nominally 2 {mu}m thick) were exposed to 2.2 to 2.5 x 10{sup 20} oxygen/cm{sup 2} over a period of 42.25 hours in earth orbit on the United States space shuttle. Identical specimens were kept as controls in desiccated storage for the duration of the mission, and another set was exposed to an equivalent fluence of atomic oxygen in the laboratory. The friction coefficient in air and vacuum, and the composition of worn surfaces, were determined prior to the shuttle flight and again after the shuttle flight. Results are described.
Examination of the durability of zirconia-coated rigid disks in various environments reveals a sensitivity to the presence of water vapor during sliding. Vacuum and dry air yield contact durabilities of 300 to 400 m, while in 50% relative humidity air the contact life increases to about 20 km. The durability of amorphous carbon-coated disks was also found to be more sensitive to the presence of moisture than to oxygen. The dominant factors affecting wear are believed to be oxidation of metallic debris and interaction of the overcoat layer with water vapor. Tests with ferrite read/write sliders on carbon-coated disks suggest that the pin-on-disc test is a valid simulation of the tribological behavior of this system. Carbon film thickness measurements indicate that the carbon film remains intact without appreciable thinning until the point of failure. 25 refs., 12 figs., 1 tab.