NiCuFe　layered　double　oxide　(LDO)　catalysts　were　synthesized　using　co-precipitation,　impregnation,　and　urea　hydrothermal　methods.　The　NH3-SCR　activity　of　NiCuFe-LDO　catalysts　was　investigated　to　determine　the　effect　of　different　synthesis　methods.　All　NiCuFe-LDO　samples　exhibited　good　catalytic　performance　at　low　temperatures,　with　the　sample　synthesized　using　the　urea　hydrothermal　method　(NiCuFe-LDO-3)　being　the　most　efficient　catalyst.　The　NiCuFe-LDO-3　catalyst　achieved　over　80%　NO　conversion　in　the　temperature　range　of　180 °C　to　280 °C,　with　a　peak　of　95.13%　at　240 °C.　The　physicochemical　properties　of　the　samples　were　systematically　characterized　using　XRD,　SEM,　BET,　NH3-TPD,　H2-TPR,　XPS,　and　in-situ　DRIFTS.　The　results　showed　that　the　NiCuFe-LDO-3　sample　had　the　best　crystallinity,　as　demonstrated　by　XRD　and　SEM.　BET　analysis　revealed　that　the　NiCuFe-LDO-3　sample　had　the　largest　specific　surface　area.　The　NiCuFe-LDO-3　sample　was　found　to　have　more　acidic　sites　and　a　better　redox　capacity　than　the　other　samples,　according　to　the　H2-TPR　and　NH3-TPD　results.　In-situ　DRIFTS　analysis　showed　that　the　catalyst　operates　through　both　E–R　and　L–H　reaction　mechanisms.　©　Akadémiai　Kiadó,　Budapest,　Hungary　2024.