Publications

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Sandia National Laboratories (SNL) conducted accelerated atmospheric corrosion testing for the U.S. Consumer Product Safety Commission (CPSC) to help further the understanding of the development of corrosion products on conductor materials in household electrical components exposed to environmental conditions representative of homes constructed with problem drywall. The conditions of the accelerated testing were chosen to produce corrosion product growth that would be consistent with long-term exposure to environments containing humidity and parts per billion (ppb) levels of hydrogen sulfide (H{sub 2}S) that are thought to have been the source of corrosion in electrical components from affected homes. This report documents the test set-up, monitoring of electrical performance of powered electrical components during the exposure, and the materials characterization conducted on wires, screws, and contact plates from selected electrical components. No degradation in electrical performance (measured via voltage drop) was measured during the course of the 8-week exposure, which was approximately equivalent to 40 years of exposure in a light industrial environment. Analyses show that corrosion products consisting of various phases of copper sulfide, copper sulfate, and copper oxide are found on exposed surfaces of the conductor materials including wires, screws, and contact plates. The morphology and the thickness of the corrosion products showed a range of character. In some of the copper wires that were observed, corrosion product had flaked or spalled off the surface, exposing fresh metal to the reaction with the contaminant gasses; however, there was no significant change in the wire cross-sectional area.

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There are commercial and military applications in which a material needs to serve as a barrier that must subsequently be removed. In many cases it is desirable that once the barrier has served its function that it then be reduced to small pieces. For example, in pipelines and in downhole drilling applications, valves are needed to function as barriers that can sustain high pressures. Later the valves must be removed and essentially disappear or be rendered to such a small size that they do not interfere with the functioning of other equipment. Military applications include covers on missile silos or launch vehicles. Other applications might require that a component be used once as an actuator or for passive energy storage, and then be irreversibly removed, again so as not to interfere with the function or motion of other parts of the device. Brittle materials, especially those that are very strong, or are pre-stressed, are ideal candidates for these applications. Stressed glass can be produced in different sizes and shapes and the level of strength and pre-stress, both of which control the fragmentation, can be manipulated by varying the processing. Stressed glass can be engineered to fracture predictably at a specific stress level. Controlling the central tension allows the fragment size to be specified. The energy that is stored in the residual stress profile that results from ion exchange or thermal tempering processes can be harnessed to drive fragmentation of the component once it has been deliberately fractured. Energy can also be stored in the glass by mechanical loading. Energy from both of these sources can be released either to perform useful work or to initiate another reaction. Once the stressed glass has been used as a barrier or actuator it can never be ''used'' again because it fragments into many small unrecognizable pieces during the actuation. Under some circumstances it will interfere with the motion or functioning of other parts of a device. Our approach was to use stressed glass to develop capabilities for making components that can be used as barriers, as actuating devices that passively store energy, or as a mechanical weaklink that is destroyed by some critical shock or crush load. The objective of this project was to develop one or more prototype devices using stressed glass technology and demonstrate their potential for applications of interest. This work is intended to provide critical information and technologies for Sandia's NP&A and MT&A customers, and is relevant to commercial applications for these same materials. Most of the studies in this project were conducted using the Corning 0317 sodium aluminosilicate glass composition.

This paper discusses the design and use of low-temperature (850 C to 950 C) co-fired ceramic (LTCC) planar magnetic flyback transformers for applications that require conversion of a low voltage to high voltage (> 100V) with significant volumetric constraints. Measured performance and modeling results for multiple designs showed that the LTCC flyback transformer design and construction imposes serious limitations on the achievable coupling and significantly impacts the transformer performance and output voltage. This paper discusses the impact of various design factors that can provide improved performance by increasing transformer coupling and output voltage. The experiments performed on prototype units demonstrated LTCC transformer designs capable of greater than 2 kV output. Finally, the work investigated the effect of the LTCC microstructure on transformer insulation. Although this paper focuses on generating voltages in the kV range, the experimental characterization and discussion presented in this work applies to designs requiring lower voltage.

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Glass can have lethal effects including fatalities and injuries when it breaks and then flies through the air under blast loading (''the glass problem''). One goal of this program was to assess the glass problem and solutions being pursued to mitigate it. One solution to the problem is the development of new glass technology that allows the strength and fragmentation to be controlled or selected depending on the blast performance specifications. For example the glass could be weak and fail, or it could be strong and survive, but it must perform reliably. Also, once it fails it should produce fragments of a controlled size. Under certain circumstances it may be beneficial to have very small fragments, in others it may be beneficial to have large fragments that stay together. The second goal of this program was to evaluate the performance (strength, reliability, and fragmentation) of Engineered Stress Profile (ESP) glass under different loading conditions. These included pseudo-static strength and pressure tests and free-field blast tests. The ultimate goal was to provide engineers and architects with a glass whose behavior under blast loading is less lethal. A near-term benefit is a new approach for improving the reliability of glass and modifying its fracture behavior.

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The purpose of the report is to summarize discussions from a Ceramic/Metal Brazing: From Fundamentals to Applications Workshop that was held at Sandia National Laboratories in Albuquerque, NM on April 4, 2001. Brazing experts and users who bridge common areas of research, design, and manufacturing participated in the exercise. External perspectives on the general state of the science and technology for ceramics and metal brazing were given. Other discussions highlighted and critiqued Sandia's brazing research and engineering programs, including the latest advances in braze modeling and materials characterization. The workshop concluded with a facilitated dialogue that identified critical brazing research needs and opportunities.

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The main objective of this project was to develop reliable, low-cost techniques for joining silicon nitride (Si{sub 3}N{sub 4}) to itself and to metals. For Si{sub 3}N{sub 4} to be widely used in advanced turbomachinery applications, joining techniques must be developed that are reliable, cost-effective, and manufacturable. This project addressed those needs by developing and testing two Si{sub 3}N{sub 4} joining systems; oxynitride glass joining materials and high temperature braze alloys. Extensive measurements were also made of the mechanical properties and oxidation resistance of the braze materials. Finite element models were used to predict the magnitudes and positions of the stresses in the ceramic regions of ceramic-to-metal joints sleeve and butt joints, similar to the geometries used for stator assemblies.

Computational materials simulations have traditionally focused on individual phenomena: grain growth, crack propagation, plastic flow, etc. However, real materials behavior results from a complex interplay between phenomena. In this project, the authors explored methods for coupling mesoscale simulations of microstructural evolution and micromechanical response. In one case, massively parallel (MP) simulations for grain evolution and microcracking in alumina stronglink materials were dynamically coupled. In the other, codes for domain coarsening and plastic deformation in CuSi braze alloys were iteratively linked. this program provided the first comparison of two promising ways to integrate mesoscale computer codes. Coupled microstructural/micromechanical codes were applied to experimentally observed microstructures for the first time. In addition to the coupled codes, this project developed a suite of new computational capabilities (PARGRAIN, GLAD, OOF, MPM, polycrystal plasticity, front tracking). The problem of plasticity length scale in continuum calculations was recognized and a solution strategy was developed. The simulations were experimentally validated on stockpile materials.

Microstructure-level residual stresses arise in polycrystalline ceramics during processing as a result of thermal expansion anisotropy and crystallographic disorientation across the grain boundaries. Depending upon the grain size, the magnitude of these stresses can be sufficiently high to cause spontaneous microcracking during the processing of these materials. They are also likely to affect where cracks initiate and propagate under macroscopic loading. The magnitudes of residual stresses in untextured and textured alumina samples were predicted using object oriented finite (OOF) element analysis and experimentally determined grain orientations. The crystallographic orientations were obtained by electron-backscattered diffraction (EBSD). The residual stresses were lower and the stress distributions were narrower in the textured samples compared to those in the untextured samples. Crack initiation and propagation were also simulated using the Griffith fracture criterion. The grain boundary to surface energy ratios required for computations were estimated using AFM groove measurements.

Microstructural-level residual stresses arise in ceramics due to thermal expansion anisotropy. The magnitude of these stresses can be very high and may cause spontaneous microcracking during the processing of these materials. The orientation data obtained by backscattered electron diffraction and grain boundary energies obtained by AFM were used in conjunction with an object oriented finite element analysis package (OOF) to predict the magnitude of residual stresses in alumina. Crack initiation and propagation were also simulated based on the Griffith fracture criterion.

This report summarizes the results of a study to develop and evaluate low temperature glass sealing technologies for photovoltaic applications. This work was done as part of Cooperative Research and Development Agreement (CRADA) No. SC95/01408. The sealing technologies evaluated included low melting temperature glass frits and solders. Because the glass frit joining required a material with a melting temperature that exceeded the allowable temperature for the active elements on the photovoltaic panels a localized heating scheme was required for sealing the perimeter of the glass panels. Thermal and stress modeling were conducted to identify the feasibility of this approach and to test strategies designed to minimize heating of the glass panel away from its perimeter. Hardware to locally heat the glass panels during glass frit joining was designed, fabricated, and successfully tested. The same hardware could be used to seal the glass panels using the low temperature solders. Solder adhesion to the glass required metal coating of the glass. The adhesion strength of the solder was dependent on the surface finish of the glass. Strategies for improving the polyisobutylene (PIB) adhesive currently being used to seal the panels and the use of Parylene coatings as a protective sealant deposited on the photovoltaic elements were also investigated. Starting points for further work are included.

Ceramic materials are used extensively in non-nuclear components in the weapons stockpile including neutron tubes, firing sets, radar, strong link and weak link assemblies, batteries, and current/voltage stacks. Ceramics also perform critical functions in electronics, passively as insulators and actively as resistors and capacitors. Glass and ceramic seals also provide hermetic electrical feedthroughs in connectors for many weapons components. The primary goal of the ceramic material lifetime prediction program is to provide the enhanced surveillance program with the capability to specify the reliability and lifetimes of glass and ceramic-containing components under conditions typical of the stockpile environment. The authors have studied the reliability and subcritical crack growth (SCG) behavior of 94% alumina (Al{sub 2}O{sub 3}), which is likely the most common ceramic in the stockpile. Measurements have been made on aluminas manufactured by four war reserve qualified vendors (Coors, Wesgo, AlSiMag, and Diamonite). These materials are expected to be representative of typical product obtained from vendors who have supplied alumina for weapons components during the past several decades.

This report describes the results to date of a program that was initiated to predict and measure residual stresses in Mo-Al{sub 2}O{sub 3} cermet-containing components and to develop new materials and processes that would lead to the reduction or elimination of the thermal mismatch stresses. The period of performance includes work performed CY95-97. Excessive thermal mismatch stresses had produced cracking in some cermet-containing neutron tube components. This cracking could lead to a loss of hermeticity or decreased tube reliability. Stress predictions were conducted using finite element models of the various components, along with the thermal coefficient of expansion (CTE), Young`s modulus, and strength properties. A significant portion of the program focused on the property measurements for the existing cermet materials, processing conditions, and the measurement technique. The effects of differences in the properties on the predicted residual stresses were calculated for existing designs. Several potential approaches were evaluated for reducing the residual stresses and cracking in cermet-containing parts including reducing the Mo content of the cermet, substituting a ternary alloy with a better CTE match with alumina, and substituting Nb for Mo. Processing modifications were also investigated for minimizing warpage that occurs during sintering due to differential sintering. These modifications include changing the pressing of the 94ND2 alumina and changing to a 96% alumina powder from AlSiMag.

Diametral compression strength distributions and the compaction behavior and of irregular shape 150-200 μm ceramic granules and uniform-size 210 μm glass spheres were measured to determine how granule strength variability relates to compaction behavior of granular assemblies. High variability in strength, represented by low Weibull modulus values (m<3) was observed for ceramic granules having a distribution of sizes and shapes, and for uniform-size glass spheres. Compaction pressure data were also analyzed using a Weibull distribution function, and the results were very similar to those obtained from the diametral compression strength tests for the same material. This similarity suggests that it may be possible to model granule compaction using a weakest link theory, whereby an assemblage of granules is viewed as the links of a chain, and failure of the weakest granule (i.e., the weakest link) leads to rearrangement and compaction. Additionally, with the use of Weibull statistics, it appears to be possible to infer the variability in strength of individual granules from a simple pressure compaction test, circumventing the tedious task of testing individual granules.

A fiberglass-reinforced plastic (FRP) pressure vessel containing sulfuric acid failed catastrophically in service. Preliminary investigations ruled out failure due to sabotage and chemical or mechanical overpressure. Subsequent examination of the fiber fracture surfaces and measurements of mirror radii indicated that fiber failure had occurred at stresses significantly below the fibers` expected strength. Further examination by scanning electron microscopy and energy dispersive spectroscopy indicated that the glass fibers had been exposed to sulfuric acid, a reagent that corrodes this type of glass and degrades its strength. Finite element analysis indicated stresses in an exposed region of the vessel that exceeded the strengths of the FRP during normal vessel operation. Numerous cracks were detected in this region using a vicinal optical illumination technique. We concluded that vessel failure was caused by progressive degradation and rupture of fibers starting at the outer surface of the FRP and extending inwards and laterally, until a crack of critical size was produced.