In this chapter, two main superconducting compounds have been studied. The first study was focused on the preparation of magnesium diboride (MgB2) cryo-magnets by Spark Plasma Sintering (SPS). The role of the starting powder on the superconducting properties of MgB2 is investigated. Different sets of bulk MgB2 material were processed from: (i) a commercial available powder; (ii) a mixture of Mg metal and amorphous B using a single-step solid-state reaction process; and (iii) a mixture of amorphous boron coated with carbon and Mg metal. The samples were prepared in tungsten carbide molds, varying the processing conditions by the modulation of the temperature, the dwell time, and the applied pressure. The microstructures of the samples were i...