Metal borides are typically extremely hard, refractory compounds that may be used to increase the durability and strength of metallic materials. In the past, extreme conditions proved necessary to make these materials, with thin films being especially difficult to prepare. The most commonly employed thin film preparative method, chemical vapor deposition, required extremely high vacuum and high temperature conditions. Here, we describe gentler methods that we have employed to generate the metal boride nanostructured materials. These include the aerosol pyrolytic methods and electrochemical room temperature syntheses. The metal boride nanoparticles were grown onto substrates as thin films and may very well serve as corrosion resistant coatings. A new unique property of metal boride nanoparticles is that they have been observed to catalyze the growth of carbon nanotubes, nanorods, and nanospheres. Microscopic, such as SEM and TEM, and X-ray techniques have been employed to investigate the morphology and the composition of these metal boride nanoparticles, thin films and carbon nanotubes.