Publications

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.