HRTEM and TEM studies of amorphous structures in ZrNiTiCu base alloys obtained by rapid solidification or ball milling

Amorphous structure of Ti25Zr17Ni29Cu29 composition was studied. Alloys were prepared either by rapid solidification using melt spinning or by high-energy ball milling. The composition of multi-component eutectic in slowly cooled samples of ZrNiTiCu alloy was determined using EDS measurements in scanning microscope of slowly cooled cast samples. The alloys of eutectic composition were melt-spun or ball-milled. Transmission electron microscopy (TEM) studies of melt-spun ribbons from alloys near eutectic composition did not show presence of nanocrystals within the amorphous structure. TEM studies of ball-milled powders showed presence of nanocrystallites of size 2–5 nm. The electron diffraction pattern showed intense diffused ring due to the presence of the amorphous phase and a weak spot due to crystalline phases which were difficult to identify. The high temperature high-pressure compaction in vacuum of amorphous ball-milled powders resulted in a similar structure like in the powders showing nanocrystals embedded in the amorphous matrix. The crystallites were imaged using HREM. Interplanar distances were measured in pictures obtained by inverse fast Fourier transform (IFFT) of atomic planes to obtain better contrast. Analysis of the IFFT from high-resolution micrographs allowed to identify Cu10Zr7 phase. Point analysis and elemental mapping performed using nondispersive X-ray energy spectroscopy showed uniform elements distribution indicating that chemical segregation to nanocrystals is within measurement error.