The authors present a method for the fast and efficient measurement of volumes of reciprocal space by x-ray diffraction using linear and area detectors. The goal of this technique is to obtain a complete overview of the reciprocal space to detect and characterize the nature and orientation of all the phases present. They first explain the detailed procedures and scan strategies required for transforming raw scattering data into three-dimensional maps of reciprocal space and present a complete open-source software package for advanced data processing, analysis, and visualization. Several case studies, chosen to highlight the overall capabilities of the technique, are then introduced. First, thermal diffuse scattering from a monocrystalline Si substrate is characterized by the presence of lines linking diffraction peaks in reciprocal space. Second, a detailed investigation of texture in multiphase thin layers permits us to reveal the unambiguous presence of fiber, axiotaxial, and epitaxial components in oriented films. The visualization of a significant fraction of reciprocal space has allowed us to identify an unexpected metastable phase, which could not be deduced from measurements carried out in the Bragg–Brentano geometry. The technique is then used to study planar defects in nickel silicides formed by solid-state reactions and micro twins in a GaP matrix containing coherent MnP precipitates. Overall, the authors show that the systematic acquisition of significant volumes of reciprocal space permits us to observe behaviors that might otherwise remain undetected when analyses are restricted to typical measurement scans.

Hybrid ferromagnetic-semiconductor GaP:MnP thin films were grown at 650 °C by metal-organic vapor phase epitaxy on GaP(001) using trimethylgallium, tertiarybutylphosphine, and methyl cyclopentadienyl manganese tricarbonyl (MCTMn). Overall Mn concentrations in the hybrid films, determined by Rutherford backscattering spectrometry, were found to be nearly proportional to the MCTMn precursor gas flow rate and ranged from 2 to 3.5 at. %. Cross-sectional transmission electron microscopy (TEM) analyses revealed the presence of a homogeneous distribution of 15–30 nm wide nanoclusters in a dislocation-free GaP matrix that is fully coherent with the substrate. The nanocluster facets are predominantly aligned along the (220) planes of the GaP matrix and selected-area electron diffraction patterns in TEM indicate that the nanoclusters are coherent (or semicoherent) with the single-crystal GaP matrix. The Mn:P composition ratio in the nanoclusters was determined to be 1.00±0.05 from parallel electron energy loss spectroscopy analyses. Increasing the MCTMn flow rate during film growth resulted in an increased concentration of MnP nanoclusters in the epilayer while their dimensions remained virtually unchanged. Magnetometric characterization indicates a ferromagnetic order, with a Curie temperature of about 294 K, originating from the MnP clusters.

GaP:MnP samples, which consist of GaP͑001͒ epilayers with embedded MnP nanoclusters occupying approximately 7% of the epilayer volume, were grown at three different substrate temperatures ͑600, 650, and 700°C͒ using metal-organic vapor phase epitaxy. Angle dependent ferromagnetic resonance ͑FMR͒ spectroscopy indicates that, in all samples, MnP clusters are crystallographically oriented along specific GaP directions and possess high magnetic anisotropy fields. FMR results also suggest that the growth temperature significantly modifies the distribution of clusters among the possible orientations. This is verified from the measured angular dependence of the remanent magnetization, which shows a different crystallographic orientation of the GaP:MnP effective magnetic easy axis for each growth temperature. Modeling of the remanent magnetization allowed the determination of the relative volume fraction of clusters corresponding to each MnP c-axis orientation at a given growth temperature. These results support our assumption that the clusters are monodomains and suggest that the growth temperature could eventually be used to adjust the magnetic properties of these GaP:MnP structures.