This work investigates the electrical properties of NiO-SDC/SDC anode sintered at approximately 1200 °C for 1 h via the microwave method. Nanopowders Sm 0.2 Ce 0.8 O 1.9 (SDC) and NiO were mixed using a high-energy ball mill and subsequently co-pressed at three different compaction pressures of 200, 300, and 400 MPa. This study determines the effect of compaction pressure on the electrochemical performance of Ni-SDC/SDC anode, with no binder used between layers. The electrical behavior of the prepared anode was studied via electrochemical impedance spectroscopy in controlled atmospheres, operating at high temperatures (600 °C-800 °C). The results indicate that decreasing the compaction pressure and increasing the operating temperature lead to a high electrochemical performance of the non-symmetrical NiO-SDC/SDC anode. The mechanism for manufacturing NiO-SDC/SDC involves ball milling, dry pressing, and microwave furnace sintering processes.