Application of PM-IRRAS to study thin films on industrial and environmental samples

Polarization modulation–infrared reflection absorption spectroscopy (PM-IRRAS) was employed to analyze two unique samples: (1) an industrially prepared alkoxysilane-pretreated aluminum alloy (AA6111) in the absence and presence of a ～600-nm-thick lubricant coating and (2) a chemical warfare agent simulant, triethyl phosphate (TEP), on glass. For the pretreated aluminum samples, PM-IRRAS spectra were analyzed for three distinct regions; the SiO stretching vibration around 1120 cm^?1, the NH₂ bending mode at ～1600 cm^?1 and the CH stretching region around 2900 cm^?1. Our results showed that increasing the curing temperature (from 55 to 100 °C) improved the overall extent of cross-linking within the siloxane network. In addition, the spectra of lubricant (top coating) and the underlying siloxane layer for the aluminum samples with lubricant were collected for the same sample. Our results show that the nature of the siloxane film remains intact and unaltered after deposition of the lubricant top-coat. For detection of TEP on glass, the band at 1268 cm^?1, corresponding to the P═O vibration, was monitored. A droplet of TEP solution in dichloromethane was deposited on glass. After solvent evaporation had occurred, the intensity of the P═O vibration band was used to construct calibration curves to determine the experimental limit of detection, which was found to be ～200 μg for TEP on glass.

Specific heat of the dilute Ising magnet LiHoxY1-xF4

We present specific heat data on three samples of the dilute Ising magnet LiHoxY1-xF4 with x=0.018, 0.045, and 0.080. Previous measurements of the ac susceptibility of an x=0.045 sample showed the Ho3+ moments to remain dynamic down to very low temperatures, and the specific heat was found to have unusually sharp features. In contrast, our measurements do not exhibit these sharp features in the specific heat and instead show a broad feature, for all three samples studied, which is qualitatively consistent with a spin glass state. Integrating C/T, however, reveals an increase in residual entropy with lower Ho concentration, consistent with recent Monte Carlo simulations showing a lack of spin glass transition for low x.     

Enhanced x-ray phase determination by three-beam diffraction

For decades, solving the phase problem of x-ray scattering has been a goal that, in principle, could be achieved by means of n-beam diffraction (n-BD). However, the phases extracted by the actual n-BD phasing techniques are not very precise, mainly due to systematic errors that are difficult to estimate. We present an innovative theoretical approach and experimental procedure that, combined, eliminate two major sources of error. It is a high precision phasing technique that provides the triplet-phase angle with an error of about 2 degrees.     

3D composition of epitaxial nanocrystals by anomalous X-ray diffraction: observation of a Si-rich core in Ge domes on Si(100)

Three-dimensional composition maps of nominally pure Ge domes grown on Si(001) at 600 degrees C were obtained from grazing incidence anomalous x-ray scattering data at the Ge K edge. The data were analyzed in terms of a stack of layers with laterally varying concentration. The results demonstrated that the domes contained a Si-rich core covered by a Ge-rich shell and were independently supported by selective etch experiments. The composition profile resulted from substrate Si alloying into the Ge during growth to partially relax the stress in and under the domes.