Publications

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As electronic assemblies become more compact and increase in processing bandwidth, escalating thermal energy has become more difficult to manage. The major limitation has been nonmetallic joining using poor thermal interface materials (TIM). The interfacial, versus bulk, thermal conductivity of an adhesive is the major loss mechanism and normally accounts for an order magnitude loss in conductivity per equivalent thickness. The next generation TIM requires a sophisticated understanding of material and surface sciences, heat transport at submicron scales, and the manufacturing processes used in packaging of microelectronics and other target applications. Only when this relationship between bond line manufacturing processes, structure, and contact resistance is well-understood on a fundamental level will it be possible to advance the development of miniaturized microsystems. This report examines using thermal and squeeze-flow modeling as approaches to formulate TIMs incorporating nanoscience concepts. Understanding the thermal behavior of bond lines allows focus on the interfacial contact region. In addition, careful study of the thermal transport across these interfaces provides greatly augmented heat transfer paths and allows the formulation of very high resistance interfaces for total thermal isolation of circuits. For example, this will allow the integration of systems that exhibit multiple operational temperatures, such as cryogenically cooled detectors.

As electronic assemblies become more compact and with increased processing bandwidth, the escalating thermal energy has become more difficult to manage. The major limitation has been nonmetallic joining using poor thermal interface materials (TIM). The interfacial, versus bulk, thermal conductivity of an adhesive is the major loss mechanism and normally accounts for an order magnitude loss in conductivity per equivalent thickness. The next generation TIM requires a sophisticated understanding of material and surface sciences, heat transport at sub-micron scales and the manufacturing processes used in packaging of microelectronics and other target applications. Only when this relationship between bondline manufacturing processes, structure and contact resistance is well understood on a fundamental level, would it be possible to advance the development of miniaturized microsystems. We give the status of the study of thermal transport across these interfaces.

Nearly every manufacturing and many technologies central to Sandia's business involve physical processes controlled by interfacial wetting. Interfacial forces, e.g. conjoining/disjoining pressure, electrostatics, and capillary condensation, are ubiquitous and can surpass and even dominate bulk inertial or viscous effects on a continuum level. Moreover, the statics and dynamics of three-phase contact lines exhibit a wide range of complex behavior, such as contact angle hysteresis due to surface roughness, surface reaction, or compositional heterogeneities. These thermodynamically and kinetically driven interactions are essential to the development of new materials and processes. A detailed understanding was developed for the factors controlling wettability in multicomponent systems from computational modeling tools, and experimental diagnostics for systems, and processes dominated by interfacial effects. Wettability probed by dynamic advancing and receding contact angle measurements, ellipsometry, and direct determination of the capillary and disjoining forces. Molecular scale experiments determined the relationships between the fundamental interactions between molecular species and with the substrate. Atomistic simulations studied the equilibrium concentration profiles near the solid and vapor interfaces and tested the basic assumptions used in the continuum approaches. These simulations provide guidance in developing constitutive equations, which more accurately take into account the effects of surface induced phase separation and concentration gradients near the three-phase contact line. The development of these accurate models for dynamic multicomponent wetting allows improvement in science based engineering of manufacturing processes previously developed through costly trial and error by varying material formulation and geometry modification.

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Laser scanning confocal microscopy has been applied to study segregation in multi-component wetting. By labeling the two components of a blend with contrasting fluorescent dyes, the approximate local concentration can be determined from the relative fluorescence intensities. As a proof of concept, a coarsely blended mixture was imaged and parameters were adjusted to achieve good spectral separation of the two components. The technique was then applied to a well-blended drop of the two components and one component was observed to segregate to the air interface.

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This SAND report is the final report on Sandia's Grand Challenge LDRD Project 27328, 'A Revolution in Lighting -- Building the Science and Technology Base for Ultra-Efficient Solid-state Lighting.' This project, which for brevity we refer to as the SSL GCLDRD, is considered one of Sandia's most successful GCLDRDs. As a result, this report reviews not only technical highlights, but also the genesis of the idea for Solid-state Lighting (SSL), the initiation of the SSL GCLDRD, and the goals, scope, success metrics, and evolution of the SSL GCLDRD over the course of its life. One way in which the SSL GCLDRD was different from other GCLDRDs was that it coincided with a larger effort by the SSL community - primarily industrial companies investing in SSL, but also universities, trade organizations, and other Department of Energy (DOE) national laboratories - to support a national initiative in SSL R&D. Sandia was a major player in publicizing the tremendous energy savings potential of SSL, and in helping to develop, unify and support community consensus for such an initiative. Hence, our activities in this area, discussed in Chapter 6, were substantial: white papers; SSL technology workshops and roadmaps; support for the Optoelectronics Industry Development Association (OIDA), DOE and Senator Bingaman's office; extensive public relations and media activities; and a worldwide SSL community website. Many science and technology advances and breakthroughs were also enabled under this GCLDRD, resulting in: 55 publications; 124 presentations; 10 book chapters and reports; 5 U.S. patent applications including 1 already issued; and 14 patent disclosures not yet applied for. Twenty-six invited talks were given, at prestigious venues such as the American Physical Society Meeting, the Materials Research Society Meeting, the AVS International Symposium, and the Electrochemical Society Meeting. This report contains a summary of these science and technology advances and breakthroughs, with Chapters 1-5 devoted to the five technical task areas: 1 Fundamental Materials Physics; 2 111-Nitride Growth Chemistry and Substrate Physics; 3 111-Nitride MOCVD Reactor Design and In-Situ Monitoring; 4 Advanced Light-Emitting Devices; and 5 Phosphors and Encapsulants. Chapter 7 (Appendix A) contains a listing of publications, presentations, and patents. Finally, the SSL GCLDRD resulted in numerous actual and pending follow-on programs for Sandia, including multiple grants from DOE and the Defense Advanced Research Projects Agency (DARPA), and Cooperative Research and Development Agreements (CRADAs) with SSL companies. Many of these follow-on programs arose out of contacts developed through our External Advisory Committee (EAC). In h s and other ways, the EAC played a very important role. Chapter 8 (Appendix B) contains the full (unedited) text of the EAC reviews that were held periodically during the course of the project.

As electronic and optical components reach the micro- and nanoscales, efficient assembly and packaging require the use of adhesive bonds. This work focuses on resolving several fundamental issues in the transition from macro- to micro- to nanobonding. A primary issue is that, as bondline thicknesses decrease, knowledge of the stability and dewetting dynamics of thin adhesive films is important to obtain robust, void-free adhesive bonds. While researchers have studied dewetting dynamics of thin films of model, non-polar polymers, little experimental work has been done regarding dewetting dynamics of thin adhesive films, which exhibit much more complex behaviors. In this work, the areas of dispensing small volumes of viscous materials, capillary fluid flow, surface energetics, and wetting have all been investigated. By resolving these adhesive-bonding issues, we are allowing significantly smaller devices to be designed and fabricated. Simultaneously, we are increasing the manufacturability and reliability of these devices.

Biomanufacturing has the potential to be one of the defining technologies in the upcoming century. Research, development, and applications in the fields of biotechnology, bioengineering, biodetection, biomaterials, biocomputation and bioenergy will have dramatic impact on both the products we are able to create, and the ways in which we create them. In this report, we examine current research trends in biotechnology, identify key areas where biomanufacturing will likely be a major contributing field, and report on recent developments and barriers to progress in key areas.

Many microfabrication techniques are being developed for applications in microelectronics, microsensors, and micro-optics. Since the advent of microcomponents, designers have been forced to modify their designs to include limitations of current technology, such as the inability to make three-dimensional structures and the need for piece-part assembly. Many groups have successfully transferred a wide variety of patterns to both two-dimensional and three-dimensional substrates using microcontact printing. Microcontact printing is a technique in which a self-assembled monolayer (SAM) is patterned onto a substrate by transfer printing. The patterned layer can act as an etch resist or a foundation upon which to build new types of microstructures. We created a gold pattern with features as small as 1.2 {micro}m using microcontact printing and subsequent processing. This approach looks promising for constructing single-level structures such as microelectrode arrays and sensors. It can be a viable technique for creating three-dimensional structures such as microcoils and microsprings if the right equipment is available to achieve proper alignment, and if a means is available to connect the final parts to other components in subsequent assembly operations. Microcontact printing provides a wide variety of new opportunities in the fabrication of microcomponents, and increases the options of designers.

The autonomic healing ability of an epoxy adhesive containing micro-encapsulated dicyclopentadiene (DCPD) was evaluated. The epoxy resin used was Epon 828 cured with either Versamid 140 or diethylenetriamine (DETA). Variables included total weight percent of microcapsules (MCs) and catalyst, as well as the catalyst to DCPD ratio. The degree of healing was determined by the fracture toughness before and after ''healing'' using double-cantilever beam analysis. It was found that the degree of self-healing was most directly related to the contact area (i.e. crack width) during healing. Temperature also played a significant role. Observed differences between the results of this study and those in literature are discussed.

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.

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While surface cleaning is the most common process step in DOE manufacturing operations, the link between a successful adhesive bond and the surface clean performed before adhesion is not well understood. An innovative approach that combines computer modeling expertise, fracture mechanics understanding, and cleaning experience to address how to achieve a good adhesive bond is discussed here to develop a capability that would result in reduced cleaning development time and testing, improved bonds, improved manufacturability, and even an understanding that leads to improved aging. A simulation modeling technique, polymer reference interaction site model applied near wall (Wall PRISM), provided the capability to include contaminants on the surface. Calculations determined an approximately 8% reduction in the work of adhesion for 1% by weight of ethanol contamination on the structure of a silicone adhesive near a surface. The demonstration of repeatable coatings and quantitative analysis of the surface for deposition of controlled amounts of contamination (hexadecane and mineral oil) was based on three deposition methods. The effect of the cleaning process used on interfacial toughness was determined. The measured interfacial toughness of samples with a Brulin cleaned sandblasted aluminum surface was found to be {approximately} 15% greater than that with a TCE cleaned aluminum surface. The sensitivity of measured fracture toughness to various test conditions determined that both interfacial toughness and interface corner toughness depended strongly on surface roughness. The work of adhesion value for silicone/silicone interface was determined by a contact mechanics technique known as the JKR method. Correlation with fracture data has allowed a better understanding between interfacial fracture parameters and surface energy.

The authors are particularly interested in the work of adhesion measurements as a means to facilitate the understanding of the adhesive failure mechanisms for systems containing encapsulated and bonded components. Of the several issues under investigation, one is the effect of organic contamination on the adhesive strength for several types of polymer/metal interface combinations. The specific question that the authors are trying to address is at what level of contamination does adhesive strength decrease. The use of contact mechanics, the JKR method, is a good approach for studying this question. Another approach being studied is the use of interracial fracture mechanics. The model contaminant is hexadecane--non-polar, medium molecular weight hydrocarbon fluid. They choose hexadecane because it replicates typical machining fluids, is nonreactive with Al surfaces, and should not dissolve readily into the adhesive systems of interest. The application of a uniform, controllable and reproducible hexadecane layer on Al surfaces has proven to be difficult. A primary concern is whether studies of model systems can be extended to systems of technological interest. The JKR theory is a continuum mechanics model of contact between two solid spheres that was developed by Johnson, Kendall and Roberts. The JKR theory is an extension of Hertzian contact theory and attributes the additional increase in the contact area between a soft elastomeric hemisphere to adhesive forces between the two surfaces. The JKR theory allows a direct estimate of the surface free energy of interface as well as the work of adhesion (Wa) between solids. Early studies performed in this laboratory involved the determination of Wa between silicone (PDMS) and Al surfaces in order to establish the potential adhesive failure mechanisms. However, the JKR studies using commercial based PDMS [poly(dimethylsiloxane)] was fraught with difficulty that were attributed to the additives used in commercial PDMS systems. The authors could not discriminate hydrogen-bonding effects between Al{sub 2}O{sub 3} and hydroxyl groups in the PDMS, and other possible bonding mechanisms. A model PDMS elastomer and polymer treatments were developed for studying solid surfaces by measuring the degree of self-adhesion hysteresis as indicator of surface properties. The goal of this work is to measure the adhesion between PDMS/Al surfaces -- contaminated and two cleaning techniques. A custom-made JKR apparatus is used to determine the amount of hysteresis and Wa.

The contact adhesive forces between two surfaces, one being a soft hemisphere and the other being a hard plate, can readily be determined by applying an external compressive load to mate the two surfaces and subsequently applying a tensile load to peel the surfaces apart. The contact region is assumed the superposition of elastic Hertzian pressure and of the attractive surface forces that act only over the contact area. What are the effects of the degree of surface contamination on adhesive forces? Clean aluminum surfaces were coated with hexadecane as a controlled contaminant. The force required to pull an elastomeric hemisphere from a surface was determined by contact mechanics, via the JKR model, using a model siloxane network for the elastomeric contact sphere. Due to the dispersive nature of the elastomer surface, larger forces were required to pull the sphere from a contaminated surface than a clean aluminum oxide surface.