Microelectronic package characterisation using scanning acoustic microscopy

In a highly competitive market, reliable techniques for manufacturing quality control of electronic devices are demanded. Characterisation of modern microelectronic package integrity becomes more difficult due to the continued miniaturisation of electronic device and the complexity of advanced micro-assembling technologies such as chip-scale packages and 3D IC stacks. In this paper, sparse representations of acoustic signals are sought to improve the scanning acoustic microscopy (SAM), a common non-destructive tool for failure analysis of microelectronic packages. Sparse representation of an ultrasonic signal is obtained by decomposing it in an overcomplete dictionary. Detection and location of ultrasonic echoes are then performed on the basis of the resulting redundant representation. The method offers a solution to the deconvolution problem for restoration of the ultrasonic reflectivity function. It can restore closely space overlapping echoes beyond the resolution of the conventional SAM system. It also produces high resolution and accurate estimates for ultrasonic echo parameters, i.e., time-of-flight, amplitude, centre frequency, and bandwidth. These merits of the proposed method are explored in various potential applications for microelectronic package characterisation.     

Exploring the impact of formulation and temperature shock on metered dose inhaler priming

The interplay between canister, valve design, formulation, and environmental temperature is crucial to dose retention in metered dose inhalers (MDIs). Previous studies that have utilized MDIs with polymeric capillary retention valves, have shown that exposure to environmental changes can create a temporary temperature gradient between the formulation retained in the metering chamber and the formulation reservoir in the metal canister, which can cause inconsistencies in the dose delivered to the patient. The purpose of this study was to more fully quantify these effects. This was achieved by deliberately varying the temperature difference between inhalers and environment within ranges representative of routine usage, and assessing the resulting loss of prime effect via shot weight and delivered dose testing.

The shot weights delivered by three fixed-dose commercial MDIs—Foster®, flutiform® and Seretide®, were investigated under different experimental conditions. Exposure to temperature changes of up to 15°C did not appear to affect unprimed shot weights (USW) or subsequent doses from the Foster product. In contrast, flutiform maintained prime at a temperature differential of 8.6°C, but delivered a low USW following exposure to a ΔT of 15°C under both realistic and controlled conditions. Seretide exhibited loss of prime at lower temperature differentials (ΔT 8.6°C) and a reduction in USW. The results suggest that the inclusion of ethanol in a solution-based formulation may inhibit loss of prime, leading to more robust performance in the face of temperature variations.

Delivered dose testing was carried out to assess the effect of loss of prime on the device ability to deliver a dose to within 80–120% of the label claim. The results suggest that the drainage of propellant from the metering chamber of suspension MDIs leaves active pharmaceutical ingredient (API) residue, causing an increase in subsequent doses once the prime has been restored. Taken together, the results provide valuable insight into the likely performance of MDIs subjected to routine daily use, highlighting design and formulation strategies that could be applied to make performance more robust.     

Characterization of PAX‐21 Insensitive Munition Detonation Residues

Insensitive high explosives are being used in military munitions to counteract unintended detonations during storage and transportation. These formulations contain compounds such as 2,4‐dinitroanisole (DNAN) and 3‐nitro‐1,2,4‐triazol‐5‐one (NTO), which are less sensitive to shock and heat than conventional explosives. We conducted a series of four tests on snow‐covered ice utilizing 60‐mm mortar cartridges filled with 358 g of PAX‐21, a mixture of RDX, DNAN, and ammonium perchlorate. Rounds were detonated high‐ and low‐order using a fuze simulator to initiate detonation. Blow‐in‐place (BIP) operations were conducted on fuzed rounds using an external donor charge or a shaped‐charge initiator. Results indicate that 0.001 % of the original mass of RDX and DNAN were deposited during high‐order detonations, but up to 28 % of the perchlorate remained. For the donor block BIPs, 1 % of the RDX and DNAN remained. Residues masses for these operations were significantly higher than for conventional munitions. Low‐order detonations deposited 10–15 % of their original explosive filler in friable chunks up to 5.2 g in mass. Shaped‐charge BIPs scattered 15 % of the filler and produced chunks up to 15 g. Ammonium perchlorate residue masses were extremely high because of the presence of large AP crystals, up to 400 μm in the recovered particles.     

Failure of Adhesive Bonds at Constant Strain Rates

Shear strengths of adhesive bonds using AF126 and two thicknesses of aluminum were measured at constant rate of crosshead separation. It was found that the shear strength could be related to temperature and strain rate or failure time over the range of deformation rates used.     

Spiral Tunneling Cracks Induced by Environmental Stress Cracking in LaRC™-TPI Adhesives

Some currently-available formulations of LaRC?-TPI, a thermoplastic polyimide originally developed at NASA-Langley, were found to be highly susceptible to environmental stress cracking when exposed to solvents such as acetone, toluene, diglyme and methyl ethyl ketone. The combination of stress and solvent led to rapid cracking in films and adhesive layers of this material system. Residual cool-down stresses induced when the LaRC-TPI is used as an adhesive or coating led, in the presence of a solvent, to dense “mud crack” patterns which relieve a portion of the stored energy. Because these through-the-thickness cracks are not able to relieve the stored energy in the vicinity of the adherends, additional fractures in the form of curious spiral tunnel cracks initiated and grew inward within each adhesive fragment. Micrographs of the spiral fractures are given, along with a qualitative explanation for the failure process as observed in adhesives and coatings.     

Effects of static axial strain on the tensile properties and failure mechanisms of self-assembled collagen fibers

Collagen fibers form the structural units of connective tissue throughout the body, transmitting force, maintaining shape, and providing a scaffold for cells. Our laboratory has studied collagen self-assembly since the 1970s. In this study, collagen fibers were self-assembled from molecular collagen solutions and then stretched to enhance alignment. Fibers were tested in uniaxial tension to study the mechanical properties and failure mechanisms. Results reported suggest that axial orientation of collagen fibrils can be achieved by stretching uncrosslinked collagen fibers. Stretching by about 30% not only results in decreased diameter and increased tensile strength but also leads to unusual failure mechanisms that inhibit crack propagation across the fiber. It is proposed that stretching serves to generate oriented fibrillar substructure in self-assembled collagen fibers. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 63: 1429–1440, 1997     

Soxhlet extraction of mucic acid from fungal biomass

Biologically produced mucic acid may form crystals before being separated from the biomass. Here we use Soxhlet extraction of fungal biomass to obtain mucic acid that was otherwise lost when separating biomass from the supernatant. Culture supernatant was used to extract the biomass, avoiding dilution of the mucic acid while retaining a cell-free suspension. Soxhlet extraction of biomass recovered 7% of total mucic acid produced at pH 4 and 24% at pH 6. The potential for mucic acid to cyclize to the 1,4-lactone was investigated by solid state NMR, confirming that very little lactone was present after the crystallization step.     

Recalibration of the Large Scale Gap‐Test to a Stress Scale

A series of gap‐test experiments were conducted in accordance with the EMTAP Test 22a guidelines to characterize the stress output from a donor charge of ROWANEX 3601. Forty eight successful gap‐tests were conducted at the University of Pardubice in addition to two supporting plate impact experiments performed at the Cavendish Laboratory, University of Cambridge. The experiments indicated that there are two principal release mechanisms, which produce the observed reduction in stress with increasing gap distance. The first is attenuation of the input wave, something which is expected during explosive loading due to the triangular nature of the loading pulse. The second is an interaction between the input wave and lateral release waves from the edges of the test sample at the measurement station. Attenuation of the input wave due to visco‐elastic loss in the PMMA “gap” used is likely to be less significant than these other two release mechanisms. The data generated by this investigation forms a robust dataset that gives an accurate calibration for ROWANEX 3601 for users of the EMTAP 22a test procedure. In addition the data represent an excellent “set problem” for those developing and wishing to validate, computational models of similar physical phenomena.     

Parametric study of a 2-d model of the nip region in a counter-rotating,non-intermeshing twin screw extruder

Within the polymer processing industry, the demand for more efficient mixing within the existing mixer geometries and keeping a tighter control over increasingly difficult applications calls for a quantitative understanding of the role of the mixer geometry on the mixing performance. An important extruder geometry to consider is the Counter-Rotating, Non-Intermeshing Twin Screw Extruder (CRTSE). Recent studies suggest that the greater than linear mixing performance in this geometry may be attributed to the flow in the nip region. Solution of the fluid dynamic equations for a 2-D model of the nip region was found in order to quantify mixing using a FEM software called FIDAP which was available to us on the CRAY X-MP supercomputer at San Diego Supercomputer Center. In order to study the effects of design parameters in the nip region, an arbitrary interface was placed in the entrance of the region. A program called “LINE” tracks the path and growth of the interface through the region. Measures of mixing are computed and compared. Effect of several design parameters on mixing performance are studied. Conclusions are presented as to the relative effect of various design parameters. Discussions regarding the measures of mixing and mixing efficiency are presented.