Publications

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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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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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Deformation and fracture of thin films on compliant substrates are key factors constraining the performance of emerging flexible substrate devices. These systems often contain layers of thin polymer, ceramic and metallic films and stretchable interconnects where differing properties induce high normal and shear stresses. As long as the films remain bonded to the substrates, they may deform far beyond their freestanding form. Once debonded, substrate constraint disappears leading to film failure. Experimentally it is very difficult to measure properties in these systems at sub-micron and nanoscales. Theoretically it is very difficult to determine the contributions from the films, interfaces, and substrates. As a result our understanding of deformation and fracture behavior in compliant substrate systems is limited. This motivated a study of buckle driven delamination of thin hard tungsten films on pure PMMA substrates. The films were sputter deposited to thicknesses of 100 nm, 200 nm, and 400 nm with a residual compressive stress of 1.7 GPa. An aluminum oxide interlayer was added on several samples to alter interfacial composition. Buckles formed spontaneously on the PMMA substrates following film deposition. On films without the aluminum oxide interlayer, an extensive network of small telephone cord buckles formed following deposition, interspersed with regions of larger telephone cord buckles. On films with an aluminum oxide interlayer, telephone cord buckles formed creating a uniform widely spaced pattern. Through-substrate optical observations revealed matching buckle patterns along the film-substrate interface indicating that delamination occurred for large and small buckles with and without an interlayer. The coexistence of large and small buckles on the same substrate led to two distinct behaviors as shown in Figure 2 where normalized buckle heights are plotted against normalized film stress. The behaviors deviate significantly from behavior predicted by rigid elastic solutions. To address this issue we developed a finite element analysis technique that employed a cohesive zone model to simulate interfacial crack growth. Specifying the traction-separation relationship, cohesive strength, and work of separation along with film thickness, film stress, and film and substrate properties, buckle width and height were determined as a function of interfacial toughness. The simulations indicate that an analysis based on rigid substrate solutions significantly underestimate toughness for prescribed buckle widths: a result consistent with an analysis by Yu and Hutchinson that pieced together a solution based on non-linear plate theory with a solution for the linear film on substrate problem. More importantly, the results defined a lower limiting bound to seemingly disparate buckle deflection data. The variance from linear elastic behavior, especially for the small buckles, indicates more than substrate compliance is controlling behavior. Comparison of the experimental results with cohesive zone simulations suggests that the two buckle behaviors are associated with different levels of substrate yielding. In this presentation we will use the results to show how substrate compliance and deformation affect delamination and buckling of films on compliant substrates and provide a means to predict device performance.

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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.

Activation energies for the intermixing reaction of textured metal-metal multilayer thin films have been determined using X-ray diffraction analysis. Kinetic data were collected utilizing an area detector so as to reduce intensity bias from changes in out-of-plane texture during the intermixing reaction. Activation energies for Al/Pt, Ni/Ti, and Co/Al metal-metal multilayer thin films have been determined as 95.4(2) kJ/mol, 201(13) kJ/mol, and 247(19) kJ/mol, respectively. © 2009 International Centre for Diffraction Data.