Various　Ni–Fe/Mg(Al)O　alloy　catalysts　were　obtained　by　calcination　of　Ni–Fe–Mg–Al　hydrotalcite-like　compounds,　followed　by　reduction　at　different　temperatures　(973–1173　K).　The　characterizations　of　XRD　and　STEM-EDX　suggest　that　the　resulting　Ni–Fe　alloy　particles　are　composition-uniform　and　size-controllable.　The　alloy　composition　is　little　affected　by　the　reduction　temperature,　whereas　the　particle　size　(5.8–8.2　nm)　increases　with　the　increase　of　reduction　temperature.　This　property　is　ascribed　to　the　homogeneous　distribution　of　nickel　and　iron　species　during　the　catalyst　preparation.　All　of　the　Ni–Fe/Mg(Al)O　alloy　catalysts　show　relatively　high　and　stable　activity　for　CH4–CO2　reforming　during　25　h　of　investigation　at　773–1073　K.　Particularly,　the　973　K-reduced　catalyst　exhibits　higher　coke-resistance　due　to　its　smaller　particle　size.　Ea-CH4　and　CH4-TPSR　measurements　indicate　that　Ni–Fe　alloying　inhibits　CH4　dissociation.　It　is　considered　that　during　DRM　CH4　is　dissociated　at　the　Ni　sites　and　CO2　may　be　activated　at　the　metal-support　interface　as　well　as　the　Fe　sites.　Ni–Fe　alloying　may　inhibit　CH4　dissociation　and/or　promote　CO2　activation,　thus　contributing　to　the　suppression　of　coke　deposition.　©　2020　Hydrogen　Energy　Publications　LLC