In this work, a mechanochemical process using high-energy milling conditions was employed to synthesize La 0.8 Sr 0.2 Ga 0.8 Mg 0.2 O 3-δ (LSGM) powders from the corresponding stoichiometric amounts of La 2 O 3 , SrO, Ga 2 O 3 , and MgO in a short time. After 60 min of milling, the desired final product was obtained without the need for any subsequent annealing treatment. A half solid oxide fuel cell (SOFC) was then developed using LSGM as an electrolyte and La 0.8 Sr 0.2 MnO 3 (LSM) as an electrode, both obtained by mechanochemistry. The characterization by X-ray diffraction of as-prepared powders showed that LSGM and LSM present a perovskite structure and pseudo-cubic symmetry. The thermal and chemical stability between the electrolyte (LSGM) and the electrode (LSM) were analyzed by dynamic X-ray diffraction as a function of temperature. The electrolyte (LSGM) is thermally stable up to 800 and from 900 • C, where the secondary phases of LaSrGa 3 O 7 and LaSrGaO 4 appear. The best sintering temperature for the electrolyte is 1400 • C, since at this temperature, LaSrGaO 4 disappears and the percentage of LaSrGa 3 O 7 is minimized . The electrolyte is chemically compatible with the electrode up to 800 • C. The powder sample of the electrolyte (LSGM) at 1400 • C observed by HRTEM indicates that the cubic symmetry Pm-3m is preserved. The SOFC was constructed using the brush-painting technique; the electrode-electrolyte interface characterized by SEM presented good adhesion at 800 • C. The electrical properties of the electrolyte and the half-cell were analyzed by complex impedance spectroscopy. It was found that LSGM is a good candidate to be used as an electrolyte in SOFC, with an Ea value of 0.9 eV, and the LSM sample is a good candidate to be used as cathode.