Diffuse scattering data acquisition techniques

Techniques are presented for acquiring and reducing X-ray diffuse scattering data from disordered crystalline materials. These methods are part of a comprehensive approach to study disorder in novel quasicrystalline phases as a function of temperature, but can be applied without further adaptation to periodic crystalline systems. By fully exploiting the possibilities of modern two-dimensional X-ray detector systems - using imaging plates or charge coupled devices (CCD) - large volumes of reciprocal space can be measured in a quantitative and rapid way. For this purpose, the classical rotation method for collecting integrated Bragg intensities is extended for acquiring quasi-continuous diffuse diffraction data. A new high-temperature furnace and helium beam path, designed for the diffraction geometry of the rotation method, are integral parts of the diffraction system. New methods are presented for handling the reduction of diffuse diffraction data from area detectors. One of the key techniques is the reconstruction of arbitrary slices and volumes in reciprocal space from a single series of rotation images taken from an arbitrarily oriented single-crystal (reciprocal space mapping).