This work details the synthesis and characterization of novel ternary boride (MoAlB) and MAX phase particulates via pressureless reaction. Furthermore, porous MoAlB particulates were synthesized for the first time by selective deintercalation of Al from MoAlB. Finally, novel Ni-MoAlB composites were fabricated, and their mechanical and tribological properties were tested and analyzed. Chapter II describes the synthesis of Cr2AlC, Cr 2GaC, and V2AlC powders, and demonstrates the ability to engineer particle size of Ti3SiC2 by ball milling. Chapter III details the synthesis and characterization of a novel ternary boride, MoAlB, and their porous derivatives. These particulates showed a uniquely stacked 2D-like morphology and were riddled with pores of dimensions 257+/-126 nm and 35+/-10 nm, respectively. The EDS analysis showed that particulates had a chemistry of (Mo0.67Al0.33)B{O 0.19F0.02} due to partial deintercalation of Al from MoAlB. Chapter IV chronicles the fabrication of novel Ni-matrix composites using MoAlB powders as a multifunctional solid lubricant additive. During sliding against SS, the WR decreased gradually with MoAlB content, for example, it decreased from 3 x 10-3 mm3/Nm in Ni (240 MPa) to ∼2 x 10-4 mm3/Nm in Ni-30%MoAlB (1000 °C) (240 MPa). Chapter V discusses the conclusions and future studies of this work.