Quantitative Texture Analysis with the HIPPO TOF Diffractometer

One of the design goals of the neutron time-of-flight (TOF) diffractometer HIPPO (HIgh Pressure - Preferred Orientation) at LANSCE (Los Alamos Neutron Science Center) was efficient quantitative texture analysis. In this paper, the effects of the HIPPO detector geometry and layout on texture analysis, particularly the shape and dimensions of the detector panels, are investigated. An aluminum sample with a strong and asymmetric texture was used to determine the methodological limitations of various methods of quantitative texture analysis. Several algorithms for extracting the orientation distribution function (ODF) from the TOF-spectra are compared: discrete orientations at arbitrary positions, harmonic method in Rietveld codes (MAUD and GSAS) and discrete methods in MAUD. All methods provide a similar representation of the main texture component, but discrete methods have a fundamental advantage over harmonic methods in characterizing regions of the ODF with low orientation densities. For HIPPO data of the present sample, harmonic expansions beyond lmax= 12 introduce subsidiary maxima and minima, which are consistently identified as artifacts. The results of our analysis establishes HIPPO as an efficient instrument to quantitatively determine preferred orientations in relatively short measuring times, if the texture features are not exceedingly sharp (full-width at half-maximum (FWHM) in the ODF > 20-30°).

ON THE CHARACTERIZATION OF METALLIC SUPERLATTICE STRUCTURES BY X-RAY DIFFRACTION

To solve the problem on the microstructural characterization of metallic superlattices, taking the NiFe/Cu superlattices as example, we show that the structures of metallic superlattices can be characterized exactly by combining low-angle X-ray diffraction with high-angle X-ray diffraction. First, we determine exactly the total film thickness by a straightforward and precise method based on a modified Bragg law from the subsidiary maxima around the low-angle X-ray diffraction peak. Then, by combining with the simulation of high-angle X-ray diffraction, we obtain the structural parameters such as the superlattice period, the sublayer and buffer thickness. This characterization procedure is also applicable to other types of metallic superlattices.

Suppression of subsidiary maxima in computer simulations of diffraction intensities

A simple method is described to suppress the subsidiary maxima occurring in computer simulations of diffraction intensities due to finite sizes of the simulated crystals. This is achieved by multiplying the scattering density of the model crystal by a suitably designed weighting function.

Column-by-column compositional imaging by z-contrast STEM

The use of a high-angle detector in STEM imparts incoherent characteristics to the image while simultaneously introducing a strong compositional sensitivity through the ∼Z2 dependence of the highangle scattering cross sections. The destruction of coherence is achieved in two ways. Firstly, the wide angular range of the detector averages interference fringes in the transverse plane, even if predominantly coherent scattering is detected, resulting in improved resolution and a lack of contrast reversals. Coherence along the beam direction largely remains so that with increasing thickness the intensity increases initially as t2, becoming oscillatory as the Ewald sphere intersects only subsidiary maxima of the crystal shape factor (see Fig. 1). Coherence along a column can effectively be broken by ensuring that the detector is dominated by diffuse scattering, which at large angles is dominated by multiphonon scattering (the simultaneous emission and/or absorption of several phonons in a single scattering event).

Distinguishing Between Coherent Interdiffusion and Incoherent Roughness in Synthetic Multilayers Using X-Ray Diffraction

ABSTRACT:: We have developed a method to separate coherent interfacial interdiffusion from incoherent interfacial roughness by extending an electromagnetic dynamical theory to calculate the reflectivity of a multilayer having an arbitrary interfacial profile with a variable degree of randomness in the repeating layer thicknesses. We find that the intensity of the subsidiary maxima are extremely sensitive to incoherent roughness while the intensity of the Bragg maxima are largely determined by the interfacial electron density profiles. Experimental data are modeled in a manner similar to that used by Warren and Averback to determine domain size of crystallites. We divide the multilayer into coherent domains differing from one another by small deviations from the average layer thicknesses. The diffraction intensity from each of these domains is then added to obtain the experimental pattern. The diffraction spectra of a set of Pt/Co multilayers with similar layer thicknesses but prepared with different sputtering gases illustrates the ability to separate the effects of coherent interdiffusion from incoherent roughness. The extent of incoherent roughness obtained using this model to analyze the diffraction data of these Pt-Co multilayers is in good agreement with TEM and STM results from the same samples. The diffraction patterns could not be simulated with abrupt concentration profiles and the extent of interdiffusion was found to be correlated with the energy of reflected neutrals present during the synthesis of the multilayers.

Signal-to-noise enhancement in bright field images by incoherent superposition

Bright field imaging of heavy single atoms with hollow cone illumination results in images with only slightly reduced central contrast, compared to axial illumination, but strongly suppressed subsidiary maxima. This holds for certain values for the cone angle and defocus and is due to the triangle-shaped contrast transfer function. Computer-simulated micrographs of Hg atoms on a carbon support film show that the inherent structural noise is suppressed as well, resulting in twice as good a signal-to-noise ratio compared to axial illumination. The phase grating approximation is used.The computer-generated carbon film with an area of 48 Å by 48 Å is a random network of atoms, the sampling distance corresponding to 0.75 Å. It is fitted to give a noise-to-background ratio N = 5% in the Scherzer focus with the data λ = 3.7 • 10-2 A; Cs = 0.5 mm; Cc = 0.8 mm of our microscope.