Publications

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Objective: We will research how short (ns) and ultrashort (fs) laser pulses interact with the surfaces of various materials to create complex color layers and morphological patterns. Method: We are investigating the site-specific, formation of microcolor features. Also, research includes a fundamental study of the physics underlying periodic ripple formation during femtosecond laser irradiation. Status of effort: Laser induced color markings were demonstrated on an increased number of materials (including metal thin films) and investigated for optical properties and microstructure. Technology that allows for marking curved surfaces (and large areas) has been implemented. We have used electro-magnetic solvers to model light-solid interactions leading to periodic surface ripple patterns. This includes identifying the roles of surface plasmon polaritons. Goals/Milestones: Research corrosion resistance of oxide color markings (salt spray, fog, polarization tests); Through modeling, investigate effects of multi-source scattering and interference on ripple patterns; Investigate microspectrophotometry for mapping color; and Investigate new methods for laser color marking curved surfaces and large areas.

The mechanical properties, thermal stability, and electrical performance of Au-ZnO composite thin films are determined in this work. The co-deposition of ZnO with Au via physical vapor deposition leads to grain refinement over that of pure Au; the addition of 0.1 vol.% ZnO reduces the as-grown grain size by over 30%. The hardness of the as-grown films doubles with 2% ZnO, from 1.8 to 3.6 GPa as measured by nanoindentation. Films with ZnO additions greater than 0.5% show no significant grain growth after annealing at 350°C, while pure gold and smaller additions do exhibit grain growth and subsequent mechanical softening. Films with 1% and 2% ZnO show a decrease of approximately 50% in electrical resistivity and no change in hardness after annealing. A model accounting for both changes in the interface structure between dispersed ZnO particles and the Au matrix captures the changes in mechanical and electrical resistivity. The addition of 1-2% ZnO co-deposited with Au provides a method to create mechanically hard and thermally stable films with a resistivity less than 80 n-m. These results complement previous studies of other alloying systems, suggesting oxide dispersion strengthened (ODS) gold shows a desirable hardness-resistivity relationship that is relatively independent of the particular ODS chemistry.

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In this study we report a novel method of dispersing multi-walled carbon nanotubes (MWCNTs) using an electrospinning depositional process onto a conventional, uncured preimpregnated composite material. The main focus is the determination of the process parameters in order to consistently and homogeneously disperse MWCNTs onto a secondary substrate. Due to the exceptional thermal, mechanical, and electrical properties that can be exploited in CNTs, a homogenous dispersion can lead to isotropy in material properties of interest-mechanical, thermal, electrical etc. By combining these materials with structural composite materials, the true spirit of a tailored engineering material can be exploited even further to induce specific properties that are desired for a particular application. Through the use of scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images, as well as vertical scanning interferometry, the resulting electrospun fibers are imaged and correlated with process parameters.

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Localized heating of metals and alloys using a focused laser beam in ambient atmosphere produces dielectric oxide layers that have characteristic optical appearances including different colors. Nanoindentation probed the deformation and fracture of laser-fabricated oxides on 304L stainless steel. Conductive nanoindentation measured electrical contact resistance (ECR) of the same colored oxides indicating a correlation between laser exposure, conductance during loading, current-voltage (I-V) behavior at constant load, and indentation response. Microscopy and X-ray diffraction examined the microstructure and chemical composition of the oxides. Combining techniques provides a unique approach for correlating mechanical behavior and the resulting performance of the films in conditions that cause wear. © 2012 Materials Research Society.

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This report describes an Engineering Sciences Research Foundation (ESRF) project to characterize and understand fracture processes via molecular dynamics modeling and atom-to-continuum methods. Under this aegis we developed new theory and a number of novel techniques to describe the fracture process at the atomic scale. These developments ranged from a material-frame connection between molecular dynamics and continuum mechanics to an atomic level J integral. Each of the developments build upon each other and culminated in a cohesive zone model derived from atomic information and verified at the continuum scale. This report describes an Engineering Sciences Research Foundation (ESRF) project to characterize and understand fracture processes via molecular dynamics modeling and atom-to-continuum methods. The effort is predicated on the idea that processes and information at the atomic level are missing in engineering scale simulations of fracture, and, moreover, are necessary for these simulations to be predictive. In this project we developed considerable new theory and a number of novel techniques in order to describe the fracture process at the atomic scale. Chapter 2 gives a detailed account of the material-frame connection between molecular dynamics and continuum mechanics we constructed in order to best use atomic information from solid systems. With this framework, in Chapter 3, we were able to make a direct and elegant extension of the classical J down to simulations on the scale of nanometers with a discrete atomic lattice. The technique was applied to cracks and dislocations with equal success and displayed high fidelity with expectations from continuum theory. Then, as a prelude to extension of the atomic J to finite temperatures, we explored the quasi-harmonic models as efficient and accurate surrogates of atomic lattices undergoing thermo-elastic processes (Chapter 4). With this in hand, in Chapter 5 we provide evidence that, by using the appropriate energy potential, the atomic J integral we developed is calculable and accurate at finite/room temperatures. In Chapter 6, we return in part to the fundamental efforts to connect material behavior at the atomic scale to that of the continuum. In this chapter, we devise theory that predicts the onset of instability characteristic of fracture/failure via atomic simulation. In Chapters 7 and 8, we describe the culmination of the project in connecting atomic information to continuum modeling. In these chapters we show that cohesive zone models are: (a) derivable from molecular dynamics in a robust and systematic way, and (b) when used in the more efficient continuum-level finite element technique provide results that are comparable and well-correlated with the behavior at the atomic-scale. Moreover, we show that use of these same cohesive zone elements is feasible at scales very much larger than that of the lattice. Finally, in Chapter 9 we describe our work in developing the efficient non-reflecting boundary conditions necessary to perform transient fracture and shock simulation with molecular dynamics.

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Interfacial delamination is often the critical failure mode limiting the performance of polymer/metal interfaces. Consequently methods that measure the toughness of such interfaces are of considerable interest. One approach for measuring the toughness of a polymer/metal interface is to use the stressed-overlayer test. In this test a metal substrate is coated with a sub-micron thick polymer film to create the interface of interest. An overlayer, typically a few tenths of a micron of sputtered tungsten, is then deposited on top of the polymer in such a way as to generate a very high residual compressive stress within the sputtered layer ({approx} 1-2 GPa). This highly stressed overlayer induces delamination and blister formation. The measured buckle heights and widths are then used in conjunction with a fracture mechanics analysis to infer interfacial toughness. Here we use a finite element, cohesive-zone-based, fracture analysis to perform the required interfacial crack growth simulation. This analysis shows that calculated crack growth is sensitive to the polymer layer thickness even when the layer is only 10's of nanometers thick. The inward displacement of the overlayer at the buckle edge, which is enabled by the relatively low polymer compliance, is the primary cause of differences from a rigid substrate idealization.

Film durability is a primary factor governing the use of emerging thin film flexible substrate devices where compressive stresses can lead to delamination and buckling. It is of particular concern in gold film systems found in many submicron and nanoscale applications. We are therefore studying these effects in gold on PMMA systems using compressively stressed tungsten overlayers to force interfacial failure and simulations employing cohesive zone elements to model the fracture process. Delamination and buckling occurred spontaneously following deposition with buckle morphologies that differed significantly from existing model predictions. Moreover, use of thin adhesive interlayers had no discernable effect on performance. In this presentation we will use observations and simulations to show how substrate compliance and yielding affects the susceptibility to buckling of gold films on compliant substrates. We will also compare the fracture energies and buckle morphologies of this study with those of gold films on sapphire substrates to show how changing substrate compliance affects buckle formation.

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A cohesive zone, finite element fracture analysis is based upon a traction-separation relation. Our recent work has used molecular dynamics simulations to derive general traction-separation relationships for interfacial fracture between two brittle materials under mix-mode loading conditions. Here we apply our method to explore the effects of elastic constants of the two materials on the traction-separation relationship. A comparison and discussion of our results will be provided.

Development of flexible thin film systems for biomedical, homeland security and environmental sensing applications has increased dramatically in recent years [1,2,3,4]. These systems typically combine traditional semiconductor technology with new flexible substrates, allowing for both the high electron mobility of semiconductors and the flexibility of polymers. The devices have the ability to be easily integrated into components and show promise for advanced design concepts, ranging from innovative microelectronics to MEMS and NEMS devices. These devices often contain layers of thin polymer, ceramic and metallic films where differing properties can lead to large residual stresses [5]. As long as the films remain substrate-bonded, they may deform far beyond their freestanding counterpart. Once debonded, substrate constraint disappears leading to film failure where compressive stresses can lead to wrinkling, delamination, and buckling [6,7,8] while tensile stresses can lead to film fracture and decohesion [9,10,11]. In all cases, performance depends on film adhesion. Experimentally it is difficult to measure adhesion. It is often studied using tape [12], pull off [13,14,15], and peel tests [16,17]. More recent techniques for measuring adhesion include scratch testing [18,19,20,21], four point bending [22,23,24], indentation [25,26,27], spontaneous blisters [28,29] and stressed overlayers [7,26,30,31,32,33]. Nevertheless, sample design and test techniques must be tailored for each system. There is a large body of elastic thin film fracture and elastic contact mechanics solutions for elastic films on rigid substrates in the published literature [5,7,34,35,36]. More recent work has extended these solutions to films on compliant substrates and show that increasing compliance markedly changes fracture energies compared with rigid elastic solution results [37,38]. However, the introduction of inelastic substrate response significantly complicates the problem [10,39,40]. As a result, our understanding of the critical relationship between adhesion, properties, and fracture for hard films on compliant substrates is limited. To address this issue, we integrated nanomechanical testing and mechanics-based modeling in a program to define the critical relationship between deformation and fracture of nanoscale films on compliant substrates. The approach involved designing model film systems and employing nano-scale experimental characterization techniques to isolate effects of compliance, viscoelasticity, and plasticity on deformation and fracture of thin hard films on substrates that spanned more than two orders of compliance magnitude exhibit different interface structures, have different adhesion strengths, and function differently under stress. The results of this work are described in six chapters. Chapter 1 provides the motivation for this work. Chapter 2 presents experimental results covering film system design, sample preparation, indentation response, and fracture including discussion on the effects of substrate compliance on fracture energies and buckle formation from existing models. Chapter 3 describes the use of analytical and finite element simulations to define the role of substrate compliance and film geometry on the indentation response of thin hard films on compliant substrates. Chapter 4 describes the development and application of cohesive zone model based finite element simulations to determine how substrate compliance affects debond growth. Chapter 5 describes the use of molecular dynamics simulations to define the effects of substrate compliance on interfacial fracture of thin hard tungsten films on silicon substrates. Chapter 6 describes the Workshops sponsored through this program to advance understanding of material and system behavior.

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In ductile metals, sliding contact induces plastic deformation resulting in subsurfaces, the mechanical properties of which are different from those of the bulk. This article describes a novel combination of nanomechanical test methods and analysis techniques to evaluate the mechanical behavior of the subsurfaces generated underneath a wear surface. In this methodology, nanoscratch techniques were first used to generate wear patterns as a function of load and number of cycles using a Hysitron TriboIndenter. Measurements were made on a (001) single crystal plane along two crystallographic directions, <001> and <011>. Nanoindentation was then used to measure mechanical properties in each wear pattern. The results on the (001) single crystal nickel plane showed that there was a strong increase in hardness with increasing applied load that was accompanied by a change in surface deformation. The amount of deformation underneath the wear patterns was examined from focused ion beam cross-sections of the wear patterns. © 2009 Materials Research Society.

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The performance and the reliability of many devices are controlled by interfaces between thin films. In this study we investigated the use of patterned, nanoscale interfacial roughness as a way to increase the apparent interfacial toughness of brittle, thin-film material systems. The experimental portion of the study measured the interfacial toughness of a number of interfaces with nanoscale roughness. This included a silicon interface with a rectangular-toothed pattern of 60-nm wide by 90-nm deep channels fabricated using nanoimprint lithography techniques. Detailed finite element simulations were used to investigate the nature of interfacial crack growth when the interface is patterned. These simulations examined how geometric and material parameter choices affect the apparent toughness. Atomistic simulations were also performed with the aim of identifying possible modifications to the interfacial separation models currently used in nanoscale, finite element fracture analyses. The fundamental nature of atomistic traction separation for mixed mode loadings was investigated.

The reliability of thin film systems is important to the continued development of microelectronic and micro-electro-mechanical systems (MEMS). The reliability of these systems is often tied to the ability of the films to remain adhered to its substrate. By measuring the amount of energy to separate the film from the substrate, researchers can predicts film lifetimes. Recent work has resulted in several different testing techniques to measure this energy including spontaneous buckling, indentation induced delamination and four point bending. This report focuses on developing quantifiable adhesion measurements for multiple thin film systems used in MEMS and other thin film systems of interest to Sandia programs. First, methods of accurately assessing interfacial toughness using stressed overlayer methods are demonstrated using both the W/Si and Au/Si systems. For systems where fracture only occurs along the interface, such as Au/Si, the calculated fracture energies between different tests are identical if the energy put into the system is kept near the needed strain energy to cause delamination. When the energy in the system is greater than needed to cause delamination, calculated adhesion energies can increase by a factor of three due to plastic deformation. Dependence of calculated adhesion energies on applied energy in the system was also shown when comparisons of four point bending and stressed overlayer test methods were completed on Pt/Si systems. The fracture energies of Pt/Ti/SiO{sub 2} were studied using four-point bending and compressive overlayers. Varying the thickness of the Ti film from 2 to 17 nm in a Pt/Ti/SiO{sub 2} system, both test methods showed an increase of adhesion energy until the nominal Ti thickness was 12nm. Then the adhesion energy began to decrease. While the trends in toughness are similar, the magnitude of the toughness values measured between the test methods is not the same, demonstrating the difficulty in extracting mode I toughness as mixed mode loading approaches mode II conditions.

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Frictional contact results in surface and subsurface damage that could influence the performance, aging, and reliability of moving mechanical assemblies. Changes in surface roughness, hardness, grain size and texture often occur during the initial run-in period, resulting in the evolution of subsurface layers with characteristic microstructural features that are different from those of the bulk. The objective of this LDRD funded research was to model friction-induced microstructures. In order to accomplish this objective, novel experimental techniques were developed to make friction measurements on single crystal surfaces along specific crystallographic surfaces. Focused ion beam techniques were used to prepare cross-sections of wear scars, and electron backscattered diffraction (EBSD) and TEM to understand the deformation, orientation changes, and recrystallization that are associated with sliding wear. The extent of subsurface deformation and the coefficient of friction were strongly dependent on the crystal orientation. These experimental observations and insights were used to develop and validate phenomenological models. A phenomenological model was developed to elucidate the relationships between deformation, microstructure formation, and friction during wear. The contact mechanics problem was described by well-known mathematical solutions for the stresses during sliding friction. Crystal plasticity theory was used to describe the evolution of dislocation content in the worn material, which in turn provided an estimate of the characteristic microstructural feature size as a function of the imposed strain. An analysis of grain boundary sliding in ultra-fine-grained material provided a mechanism for lubrication, and model predictions of the contribution of grain boundary sliding (relative to plastic deformation) to lubrication were in good qualitative agreement with experimental evidence. A nanomechanics-based approach has been developed for characterizing the mechanical response of wear surfaces. Coatings are often required to mitigate friction and wear. Amongst other factors, plastic deformation of the substrate determines the coating-substrate interface reliability. Finite element modeling has been applied to predict the plastic deformation for the specific case of diamond-like carbon (DLC) coated Ni alloy substrates.

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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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A test method, the Tensile Brazil Nut Sandwich (TBNS) specimen, was developed to measure mixed-mode interfacial toughness of bonded materials. Interfacial toughness measured by this technique is compared to the interfacial toughness of thin film adhesive coatings using a nanoindentation technique. The interfacial toughness of solvent-cast and melt-spun adhesive thin films is compared and found to be similar. Finally, the Johnson-Kendall-Roberts (JKR) technique is used to evaluate the cleanliness of aluminum substrates.