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Engineering the Microstructure and Morphology of Explosive Films via Control of Interfacial Energy

ACS Applied Materials and Interfaces

Forrest, Eric C.; Knepper, Robert; Brumbach, Michael T.; Rodriguez, Mark A.; Archuleta, Kim A.; Marquez, Michael P.; Tappan, Alexander S.

Physical vapor deposition of organic explosives enables growth of polycrystalline films with a unique microstructure and morphology compared to the bulk material. This study demonstrates the ability to control crystal orientation and porosity in pentaerythritol tetranitrate films by varying the interfacial energy between the substrate and the vapor-deposited explosive. Variation in density, porosity, surface roughness, and optical properties is achieved in the explosive film, with significant implications for initiation sensitivity and detonation performance of the explosive material. Various surface science techniques, including angle-resolved X-ray photoelectron spectroscopy and multiliquid contact angle analysis, are utilized to characterize interfacial characteristics between the substrate and explosive film. Optical microscopy and scanning electron microscopy of pentaerythritol tetranitrate surfaces and fracture cross sections illustrate the difference in morphology evolution and the microstructure achieved through surface energy modification. X-ray diffraction studies with the Tilt-A-Whirl three-dimensional pole figure rendering and texture analysis software suite reveal that high surface energy substrates result in a preferred (110) out-of-plane orientation of pentaerythritol tetranitrate crystallites and denser films. Low surface energy substrates create more randomly textured pentaerythritol tetranitrate and lead to nanoscale porosity and lower density films. This work furthers the scientific basis for interfacial engineering of polycrystalline organic explosive films through control of surface energy, enabling future study of dynamic and reactive detonative phenomena at the microscale. Results of this study also have potential applications to active pharmaceutical ingredients, stimuli-responsive polymer films, organic thin film transistors, and other areas.

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Materials compatibility and aging for flux and cleaner combinations

Archuleta, Kim A.; Piatt, Rochelle P.

A materials study of high reliability electronics cleaning is presented here. In Phase 1, mixed type substrates underwent a condensed contaminants application to view a worst- case scenario for unremoved flux with cleaning agent residue for parts in a silicone oil filled environment. In Phase 2, fluxes applied to copper coupons and to printed wiring boards underwent gentle cleaning then accelerated aging in air at 65% humidity and 30 O C. Both sets were aged for 4 weeks. Contaminants were no-clean (ORL0), water soluble (ORH1 liquid and ORH0 paste), and rosin (RMA; ROL0) fluxes. Defluxing agents were water, solvents, and engineered aqueous defluxers. In the first phase, coupons had flux applied and heated, then were placed in vials of oil with a small amount of cleaning agent and additional coupons. In the second phase, pairs of copper coupons and PWB were hand soldered by application of each flux, using tin-lead solder in a strip across the coupon or a set of test components on the PWB. One of each pair was cleaned in each cleaning agent, the first with a typical clean, and the second with a brief clean. Ionic contamination residue was measured before accelerated aging. After aging, substrates were removed and a visual record of coupon damage made, from which a subjective rank was applied for comparison between the various flux and defluxer combinations; more corrosion equated to higher rank. The ORH1 water soluble flux resulted in the highest ranking in both phases, the RMA flux the least. For the first phase, in which flux and defluxer remained on coupons, the aqueous defluxers led to worse corrosion. The vapor phase cleaning agents resulted in the highest ranking in the second phase, in which there was no physical cleaning. Further study of cleaning and rinsing parameters will be required.

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Effects of evolving surface morphology on yield during focused ion beam milling of carbon

Applied Surface Science

Adams, D.P.; Mayer, T.M.; Vasile, M.J.; Archuleta, Kim A.

We investigate evolving surface morphology during focused ion beam bombardment of C and determine its effects on sputter yield over a large range of ion dose (10 17 -10 19 ions/cm 2 ) and incidence angles (Θ = 0-80°). Carbon bombarded by 20 keV Ga + either retains a smooth sputtered surface or develops one of two rough surface morphologies (sinusoidal ripples or steps/terraces) depending on the angle of ion incidence. For conditions that lead to smooth sputter-eroded surfaces there is no change in yield with ion dose after erosion of the solid commences. However, for all conditions that lead to surface roughening we observe coarsening of morphology with increased ion dose and a concomitant decrease in yield. A decrease in yield occurs as surface ripples increase wavelength and, for large Θ, as step/terrace morphologies evolve. The yield also decreases with dose as rippled surfaces transition to have steps and terraces at Θ = 75°. Similar trends of decreasing yield are found for H 2 O-assisted focused ion beam milling. The effects of changing surface morphology on yield are explained by the varying incidence angles exposed to the high-energy beam. © 2005 Elsevier B.V. All rights reserved.

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Effects of evolving surface morphology on yield during focused ion beam milling of carbon

Proposed for publication in Applied Surface Science.

Adams, David P.; Mayer, T.M.; Archuleta, Kim A.

We investigate evolving surface morphology during focused ion beam bombardment of C and determine its effects on sputter yield over a large range of ion dose (10{sup 17}-10{sup 19} ions/cm{sup 2}) and incidence angles ({Theta} = 0-80{sup o}). Carbon bombarded by 20 keV Ga{sup +} either retains a smooth sputtered surface or develops one of two rough surface morphologies (sinusoidal ripples or steps/terraces) depending on the angle of ion incidence. For conditions that lead to smooth sputter-eroded surfaces there is no change in yield with ion dose after erosion of the solid commences. However, for all conditions that lead to surface roughening we observe coarsening of morphology with increased ion dose and a concomitant decrease in yield. A decrease in yield occurs as surface ripples increase wavelength and, for large {Theta}, as step/terrace morphologies evolve. The yield also decreases with dose as rippled surfaces transition to have steps and terraces at {Theta} = 75{sup o}. Similar trends of decreasing yield are found for H{sub 2}O-assisted focused ion beam milling. The effects of changing surface morphology on yield are explained by the varying incidence angles exposed to the high-energy beam.

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Morphology evolution on diamond surfaces during ion sputtering

Proposed for publication in Journal of Vacuum Science and Technology A.

Mayer, T.M.; Adams, David P.; Archuleta, Kim A.

We have conducted an extensive study of the evolution of surface morphology of single crystal diamond surfaces during sputtering by 20 keV Ga{sup +} and Ga{sup +} + H{sub 2}O. We observe the formation of well-ordered ripples on the surface for angles of incidence between 40 and 70{sup o}. We have also measured sputter yields as a function of angle of incidence, and ripple wavelength and amplitude dependence on angle of incidence and ion fluence. Smooth surface morphology is observed for <40{sup o}, and a transition to a step-and-terrace structure is observed for >70{sup o}. The formation and evolution of well-ordered surface ripples is well characterized by the model of Bradley and Harper, where sputter-induced roughening is balanced by surface transport smoothing. Smoothing is consistent with an ion-induced viscous relaxation mechanism. Ripple amplitude saturates at high ion fluence, confirming the effect of nonlinear processes. Differences between Ga{sup +} and Ga{sup +} + H{sub 2}O in ripple wavelength, amplitude, and time to saturation of amplitude are consistent with the increased sputter yield observed for Ga{sup +} + H{sub 2}O. For angle of incidence <40{sup o}, an ion bombardment-induced 'atomic drift' mechanism for surface smoothing may be responsible for suppression of ripple formation. For Ga{sup +} + H{sub 2}O, we observe anomalous formation of very large amplitude and wavelength, poorly ordered surface ridges for angle of incidence near 40{sup o}. Finally, we observe that ripple initiation on smooth surfaces can take place by initial stochastic roughening followed by evolution of increasingly well-ordered ripples.

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24 Results
24 Results