Nd:11Fe:Ti alloys prepared by arc melting followed by splat quenching and annealing have been investigated by electron microscopy. The as-cast microstructure evidenced an α-Fe(Ti) → NdFe11Ti → Nd2(Fe,Ti)17 solidification sequence compatible with a cascade of peritectic reactions. The Nd2(Fe,Ti)17 phase was not detected in the microstructure of the splat-quenched materials, but after annealing the ternary compound grains consisted of a mixture of ThMn12-type and Th2Zn17-type structures exhibiting a consistent (020)1:12//(003)2:17 and [100]1:12//[110]2:17, orientation relation, with the invariant plane sitting at (022)1:12//(333)2:17. A series of 3D microdiffraction experiments carried out on grains presenting a random distribution of planar defects has been used to map the reciprocal space of the intergrown phases.

Two-dimensional proportional detectors with their faster data collection, large dynamic range, and more available information than point or linear proportional detectors make them ideal for microdiffraction analysis. The unique capabilities of these detectors coupled with a rotating anode source, capillary optics, and a variety of accessories allow for a wide range of applications.

The performance of a tapered, monocapillary optic was compared to double-pinhole optics by measuring the intensity and widths of powder diffraction peaks generated using Cr Kα and Cu Kα X-rays (46 kV, 46 mA). A microdiffractometer and curved image-plate system was used to collect diffraction patterns displayed by an alumina intensity standard. A monocapillary optic with a 20 μm beam width (measured at half the maximum intensity, FWHM) was compared to collimating pinhole optics with two apertures: one with 30 μm diameter pinholes and another with 50 μm pinholes. The average, integrated intensity of the diffraction peaks in the patterns collected using the 20 μm monocapillary optic was 6 to 7 times greater than the average diffraction intensity obtained with the 50 μm pinhole collimator and 25 times greater than the intensity obtained with the 30 μm collimator. The average increase in the FWHM of the diffraction peaks in the patterns obtained with the monocapillary optic was ∼2 times greater than the pinhole collimators.

In this article, the authors describe the principle and application of differential-aperture x-ray microscopy (DAXM). This recently developed scanning x-ray microprobe technique uses a confocal or traveling pinhole camera approach to determine the crystal structure, crystallographic orientation, and elastic and plastic strain tensors within bulk materials. The penetrating properties of x-rays make the technique applicable to optically opaque as well as transparent materials, and it is nondestructive; this provides for in situ, submicrometer-resolution characterization of local crystal structure and for measurements of microstructure evolution on mesoscopic length scales from tenths to hundreds of micrometers. Examples are presented that illustrate the use of DAXM to study grain and subgrain morphology, grain-boundary types and networks, and local intra- and intergranular elastic and plastic deformation. Information of this type now provides a direct link between the actual structure and evolution in materials and increasingly powerful computer simulations and multiscale modeling of materials microstructure and evolution.