Selected Publications

G. B. Thompson and D. D. Allred

We report the preparation and structural characterization of lithium hydride and lithium fluoride thin films. These materials, due to their low absorption in the soft x-ray range, may have a role as spacer layers in multilayer mirrors. Theoretical reflection calculations suggest that an epitaxial crystalline multilayer stack of a nitride and a lithium compound spacer layer could produce respectable reflectance for short soft x-ray wavelengths (λ < 10 nm). Lithium targets were magnetron sputtered in the presence of hydrogen or ammonia to prepare the LiH films and nitrogen trifluoride to prepare the LiF films. The films were deposited on room temperature Si (100) or MgO (100) substrates. A near IR-Visible-UV spectrometer indicated a drop in reflectance at ~250 nm for a 100-nm-thick LiH film. This corresponds to a 5-eV band gap (characteristic of LiH). UV fluorescence indicated characteristic LiH defect bands at 2.5, 3.5, and 4.4 eV. The UV fluorescence characterization also indicated a possible lithium oxide (Li2O) contamination peak at 3.1 eV in some of our thin films. Film surface morphology, examined by scanning electron microscopy, appeared extremely rough. The roughness size varied with reactive gas pressure and the type of substrate surface. A LiH/MoN multilayer was constructed, but no significant d spacing peak was seen in a low angle CuKα XRD scan. It is believed that the roughness of the LiH film prevented smooth, uniform planar growth of the multilayer stack. Possible reasons of rough growth are briefly discussed.

Using perturbed-angular-correlation (PAC) spectroscopy, via the Hf-181-->Ta-181 probe, we have measured Mn-site electric-field gradients (EFG's) at Ta nuclei in ceramic samples of LaMnO3. Two crystallographic phases coexist over a temperature interval of approximate to 16 K near the orthorhombic-to-rhombohedral transition at approximate to 724 K, which shows a thermal hysteresis of approximate to 1.7+/-0.2 K. Concurrently, in the two phases, we determined the temperature dependence of the EFG parameters, V-zz, eta, and delta, and the ratio of the probe concentrations A(1)/A(2) To explain the apparent coexistence of two phases in this weakly first-order transition, we present a model that assumes a spatial distribution of T-c values. This distribution could arise from a spatially nonuniform distribution of Mn4+ ions. We show the PAC technique to be a uniquely powerful probe of local symmetries that reflect the effects of a local-distribution of valences, which drive the phase transition.
D. D. Allred (et al.)

We report the effect that thermal annealing in inert and oxidizing atmospheres, and with and without encapsulating layers, has on the structure of tungsten/carbon [W/C] multilayer thin films. This study focuses on the tungsten component and deals mainly with multilayers where the ratio of thickness of tungsten layers is equal to or greater than for the carbon layers (that is, γ ≤ 0.5). This is in contrast to prior studies where the tungsten layer thickness was generally held constant and the carbon layer was varied. Thermal annealing in inert atmospheres produces reactions and other structural changes in the tungsten and carbide layers which depend on the as-deposited multilayer structure which depends, in turn, on the thickness of the tungsten layer. In samples where both the tungsten and carbide fractions of the multilayer are completely amorphous as deposited, which is the case for thin tungsten layers (thickness of tungsten (tw) < 4 nm/period), the reactions in the tungsten layer forming crystalline tungsten and tungsten carbide occur at annealing temperatures above 900°C. The layer pair spacing, or period, (d), in this group shows an expansion of up to 10–15% of the original value as has been reported in the past. Changes in both the tungsten and carbide layers, and their interfaces, contribute to changes in d spacing and relative thickness of the high and low Z components. When the tungsten layer thickness exceeds 4 nm per period the tungsten is partially crystallized in as-prepared samples. In such multilayers interfacial reactions, producing an oriented partially crystalline W2C/C superlattice, occur at temperatures of 600°C and below. The fact that W2C crystallites in one period can form a structure which is correlated to W2C crystallites in neighboring layers is somewhat surprising, since layers are presumably still separated by amorphous carbon which is still visible via Raman. The expansion of the layer pair spacing is relatively small (<5%) in this group and, more importantly, mostly involves increases in the thickness of the high Z components. Samples annealed in air at temperatures below 300°C are progressively destroyed by the oxidation of both tungsten and carbide layers. Encapsulation of similar multilayers with a thin (30 nm) dielectric layer of any of several types can retard oxidation to 600°C. The silicon-containing encapsulants generally perform better. Failure at this temperature is seen to occur from pinhole formation.

We show that Raman spectral lines from H-2, D-2, T-2, HD, HT and DT are readily resolved, permitting an effective means to analyze isotopic hydrogen mixtures used in muon-catalyzed fusion experiments. We propose a Raman spectrographic system to allow for real-time analysis of targets involving all three isotopes of hydrogen.
A constrained non-linear deconvolution method was used to analyse the Raman spectrum of amorphous carbon. The method was tested by applying it to a model spectrum. Before the deconvolution the observed Raman spectrum was smoothed by a least-squares convoluting procedure. The proper width of the spread function used in the deconvolution was determined by examining the reversibility of the deconvolution process. The deconvolution result for the Raman spectrum of amorphous carbon has a form very similar to the phonon density of states of graphite. This is taken to be additional evidence for Shuker and Gamon's model for Raman spectra of amorphous materials. Potentially, the deconvolution method can also be used for other aspects of Raman spectrum analysis of amorphous materials, such as finding the relative intensity of each peak of study the structure of the material.
Wang Qi, David D. Allred, and Larry V. Knight (et al.)
Measurements of the circular polarization of Balmer-α radiation emitted by excited hydrogen atoms, following the transmission of (20-50)-keV protons through thin, tilted amorphous carbon foils, exhibit markedly unexpected behavior asa function of exposure of the foil to the proton beam. Specifically, the circular polarization changes from an initially well understood tilt-angle dependence to a behavior which, for low tilt angles, gives the opposite handedness of circular polarization from that predicted. In addition, the degree of alignment, indicated by the linear Stokes parameter M/I, is enhanced also as a function of dose. These changes in the tilt-angle dependence of the Stokes parameters have been systematically correlated with beam-induced graphitization of the foil, which is observed to occur from Raman measurements.