A new process for making high surface area tantalum and/or niobium powders via the reduction of the corresponding tantalum and/or niobium oxides is presented in the work, wherein the reduction is carried out by reacting the tantalum and/or niobium oxides with at least one metal halide selected from the group consisting of halides of Mg, Ca, Sr, Ba and Ce, and an alkali metal at elevated temperature so as to form the tantalum and/or niobium powders. As an embodiment, high surface area, high purity tantalum powder was obtained by reducing tantalum oxide with CaCl2 and Na, The granulate tantalum powder was obtained by which this crude powder with nanometer primary particle was thermal agglomerated and deoxidization. And the electrical properties of the tantalum powder were tested.