Publications

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This report documents the strategies for verification and validation of the codes LSP and ICARUS used for simulating the operation of the neutron tubes used in all modern nuclear weapons. The codes will be used to assist in the design of next generation neutron generators and help resolve manufacturing issues for current and future production of neutron devices. Customers for the software are identified, tube phenomena are identified and ranked, software quality strategies are given, and the validation plan is set forth.

As part of a project with SEMATECH, detailed chemical reaction mechanisms have been developed that describe the gas-phase and surface chemistry occurring during the fluorocarbon plasma etching of silicon dioxide and related materials. The fluorocarbons examined are C{sub 2}F{sub 6}, CHF{sub 3} and C{sub 4}F{sub 8}, while the materials studied are silicon dioxide, silicon, photoresist, and silica-based low-k dielectrics. These systems were examined at different levels, ranging from in-depth treatment of C{sub 2}F{sub 6} plasma etch of oxide, to a fairly cursory examination of C{sub 4}F{sub 8} etch of the low-k dielectric. Simulations using these reaction mechanisms and AURORA, a zero-dimensional model, compare favorably with etch rates measured in three different experimental reactors, plus extensive diagnostic absolute density measurements of electron and negative ions, relative density measurements of CF, CF{sub 2}, SiF and SiF{sub 2} radicals, ion current densities, and mass spectrometric measurements of relative ion densities.

In October 1996, an interdisciplinary team began a three-year LDRD project to study the plasma processes of reactive ion etching and plasma-enhanced chemical vapor deposition on large-area silicon devices. The goal was to develop numerical models that could be used in a variety of applications for surface cleaning, selective etching, and thin-film deposition. Silicon solar cells were chosen as the experimental vehicle for this project because an innovative device design was identified that would benefit from immediate performance improvement using a combination of plasma etching and deposition processes. This report presents a summary of the technical accomplishments and conclusions of the team.

There has been considerable interest in developing dry processes which can effectively replace wet processing in the manufacture of large area photovoltaic devices. Environmental and health issues are a driver for this activity because wet processes generally increase worker exposure to toxic and hazardous chemicals and generate large volumes of liquid hazardous waste. Our work has been directed toward improving the performance of screen-printed solar cells while using plasma processing to reduce hazardous chemical usage.

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A pulsed rf plasma technique is capable of generating ceramic particles of 10 manometer dimension. Experiments using silane/ammonia and trimethylchlorosilane/hydrogen gas mixtures show that both silicon nitride and silicon carbide powders can be synthesized with control of the average particle diameter from 7 to 200 nm. Large size dispersion and much agglomeration appear characteristic of the method, in contrast to results reported by another research group. The as produced powders have a high hydrogen content and are air and moisture sensitive. Post-plasma treatment in a controlled atmosphere at elevated temperature (800{degrees}C) eliminates the hydrogen and stabilizes the powder with respect to oxidation or hydrolysis.

Silicon nitride powders with an average size as low as 7 nm are synthesized in a pulsed radio frequency glow discharge. The as-synthesized silicon nitride powder from a silane/ammonia plasma has a high hydrogen content and is sensitive to oxidation in air. Post-plasma heating of the powder in a vacuum results in nitrogen loss, giving silicon-rich powder. In contrast, heat treatment at 800 C for 20 minutes in an ammonia atmosphere (200 Torr pressure) yields a hydrogen-free powder which is stable with respect to atmospheric oxidation. Several approaches to synthesizing silicon carbide nano-size powders are presented. Experiments using silane/hydrocarbon plasmas produce particles with a high hydrogen content as demonstrated by Fourier transform infrared analysis. The hydrogen is present as both CH and SiH functionality. These powders are extremely air-sensitive. A second approach uses a gas mixture of methyltrichlorosilane and hydrogen. The particles have a low hydrogen content and resist oxidation. Particle morphology of the silicon carbide is more spherical and there is less agglomeration than is observed in the silicon nitride powder.

Silicon nitride (hydrogenated) particles are synthesized using a pulsed 13.56 MHz glow discharge. The plasma is modulated with a square-wave on/off cycle of varying period to study the growth kinetics. In situ laser light scattering and ex situ particle analysis are used to study the nucleation and growth. For SiH4/Ar and SiH4/NH3 plasmas, an initial very rapid growth phase is followed by slower growth, approaching the rate of thin film deposition on adjacent flat surfaces. The average particle size can be controlled in the 10-100 nm range by adjusting the plasma-on time. The size dispersion of the particles is large and is consistent with a process of continuous nucleation during the plasma-on period. The large polydispersity is also reported for silicon parties from silane and differs from that reported in other laboratories. The silicon nitride particle morphology is compared to that of silicon and silicon carbide particles generated by the same technique. Whereas Si particles appear as rough clusters of smaller subunits, the SiC particles are smooth spheres, and the Si3N4 particles are smooth but nonspherical. Postplasma oxidation kinetics of the particles are studied with Fourier transform infrared spectra and are consistent with a hydrolysis mechanism proposed in earlier work with continuous plasmas. Heat treatment of the powder in an ammonia atmosphere results in the elimination of hydrogen, rendering the silicon nitride resistant to atmospheric oxidation. © 1996 American Vacuum Society.

Nanometer size silicon nitride particles are synthesized using a pulsed radio frequency plasma technique. The plasma is modulated with a square-wave on/off cycle of varying period to control size and morphology and to deduce the growth kinetics. In situ laser light scattering and ex situ particle analysis are used to study the nucleation and growth. For SiH{sub 4}/Ar plasmas which nucleate silicon particles, an initial extremely rapid growth phase is followed by a slower growth rate, approaching the rate of thin film deposition on adjacent flat surfaces. In SiH{sub 4}/NH{sub 3} plasmas, silicon nitride particle size can be tightly controlled by adjusting the plasma-on time. The size dispersion of the particles is large and is consistent with a process of continual nucleation during the plasma-on period. The observed polydispersity differs dramatically from that reported from other laboratories.

The production, suspension and transport of fluorocarbon particulates in rf discharges have been studied using in situ laser light scattering and ex situ chemical analysis. The time evolution of the spatial distribution of suspended particles was obtained by 2-D imaging of the scattered light. The chemistry of the discharge was varied by the use of a range of pure fluorocarbon gases and mixtures with argon, oxygen and hydrogen-containing molecules. The addition of hydrogen to a fluorocarbon discharge increases the rate of formation of particles although these powders are found by FTIR to contain negligible hydrogen. Particle formation rates correlate with polymer deposition rates and are independent of apparatus history. It is proposed that this is a clear example of gas-phase rather than surface processes leading to particle nucleation and growth.