Novel materials having high surface area rendering them suitable for a variety of applications including, but not limited to: catalysts for methane reforming; ammonia synthesis; alcohol synthesis from syngas; hydrodesulfurization; electrocatalysis for hydrogen evolution reaction; and as corrosion-resistant supports for platinum in PEM fuel cells. In general the method comprises the formation of a high-surface area refractory metal-based material using a novel synthesis pathway that avoids the production of intermediate oxide. The method may include the in situ formation of a sacrificial support that can be removed using non-aggressive means, such as, for example, chemical etching with a mild acid or by altering reaction conditions.