The location of Ti containing phases after the completion of the NaAlH sub(4 + x)TiCl sub(3) milling process

The NaAlH sub(4 + x)TiCl sub(3) (x < 0.1) system has been studied by X-ray synchrotron diffraction and transmission electron microscopy (TEM) after the completion of the milling process, for both planetary (PM) and cryo milled (CM) samples. Comparison of the NaAlH sub(4) mosaic size (coherence length) determined from the X-ray synchrotron diffraction lineshape, and measurement of the external powder grain dimensions of ca. 250-300 particles by TEM, reveals that after the completion of the milling process, a arrow right 1 0a[control] {1 1 1} edge dislocated 2-20 nm Al crystallites are dispersed in a Ti rich amorphous (a-)Al sub(1-x)Ti sub(x) (0.3 < x < 0.5) matrix. This nano Al/Al sub(50)Ti sub(50) composite is embedded on the surface of single crystalline NaAlH sub(4) powder grains. The NaAlH sub(4) single crystal powder grains are moderately defected with uncorrelated defects, induced from the milling process.