Effect of aluminum content on the mechanochemical synthesis of in-situ TiN in the Al-Ti-AlN system and subsequent shock consolidation

To determine the effect of aluminum content on the formation of in-situ TiN in the Al-Ti-AlN system, a mixture of aluminum, titanium and aluminum nitride powders was subjected to high energy milling. Al content of the mixture was changed according to the following stoichiometric reaction: Ti+AlN+XAl→TiN+(1+X)Al. The value of X was varied from 5.35 to 19.65 based on the stoichiometric calculation of the molar mass of each component expected to result in aluminum matrix composite with TiN weights of 30%, 20% and 10%, respectively, in addition to reaction corresponding to X=0(Ti+AlN→TiN+Al). Thermodynamic factors determine that the amount of Al in the mixture plays a key role in the formation of in-situ TiN. XRD and EPMA results showed that at lower Al content (X=0, 5.35), reaction proceed through a gradual mode. By increasing Al content (X=19.65), no mechanochemical reaction occurred between Ti and AlN. Continuation of the milling process allowed acquisition of in-situ TiN in the designed compositions of AlN-TiN, Al-Ti-AlN-30%TiN, and to some extent, of Al-Ti-AlN-20%TiN. A nanocrystalline solid solution evolved by mechanical alloying (MA) was sustained for prolonged milling time. The mean TiN crystallite size obtained was 10 nm for the AlN-TiN composition. The end product milled powder after 40 h of milling time, equating to the Al-Ti-AlN-30%TiN composition was consolidated into bulk compact using the underwater shock compaction method. The milled specimens were characterized by XRD, scanning electron microscopy (SEM), electron probe microanalysis (EPMA) and microhardness testing. The sample had a uniform and fine-grained composite structure with 99% theoretical density and average microhardness of 434 HV0.1. The results confirmed the possibility of fabricating reliable bulk nanostructured materials by imposing shock compaction on submicron sized powders.