Ni–Co/Mg(Al)O　alloy　catalysts　with　different　Co/Ni　molar　ratios　have　been　prepared　from　Ni-　and　Co-substituted　Mg–Al　hydrotalcite-like　compounds　(HTlcs)　as　precursors　and　tested　for　dry　reforming　of　methane.　The　XRD　characterization　shows　that　Ni–Co–Mg–Al　HTlcs　are　decomposed　by　calcination　into　Mg(Ni,Co,Al)O　solid　solution,　and　by　reduction　finely　dispersed　alloy　particles　are　formed.　H2-TPR　indicates　a　strong　interaction　between　nickel/cobalt　oxides　and　magnesia,　and　the　presence　of　cobalt　in　Mg(Ni,Co,Al)O　enhances　the　metal-support　interaction.　STEM-EDX　analysis　reveals　that　nickel　and　cobalt　cations　are　homogeneously　distributed　in　the　HTlcs　precursor　and　in　the　derived　solid　solution,　and　by　reduction　the　resulting　Ni–Co　alloy　particles　are　composition-uniform.　The　Ni–Co/Mg(Al)O　alloy　catalysts　exhibit　relatively　high　activity　and　stability　at　severe　conditions,　i.e.,　a　medium　temperature　of　600　°C　and　a　high　space　velocity　of　120000　mL　g−1　h−1.　In　comparison　to　monometallic　Ni　catalyst,　Ni–Co　alloying　effectively　inhibits　methane　decomposition　and　coke　deposition,　leading　to　a　marked　enhancement　of　catalytic　stability.　From　CO2-TPD　and　TPSR,　it　is　suggested　that　alloying　Ni　with　Co　favors　the　CO2　adsorption/activation　and　promotes　the　elimination　of　carbon　species,　thus　improving　the　coke　resistance.　Furthermore,　a　high　and　stable　activity　with　low　coking　is　demonstrated　at　750　°C.　The　hydrotalcite-derived　Ni–Co/Mg(Al)O　catalysts　show　better　catalytic　performance　than　many　of　the　reported　Ni–Co　catalysts,　which　can　be　attributed　to　the　formation　of　Ni–Co　alloy　with　uniform　composition,　proper　size,　and　strong　metal-support　interaction　as　well　as　the　presence　of　basic　Mg(Al)O　as　support.　©　2022　Hydrogen　Energy　Publications　LLC