Magnesium　aluminate　spinel　(MgAl2O4)　was　synthesized　via　layered　double　hydroxides　(LDHs)-containing　precursor　by　co-precipitation　method.　The　precursors　and　the　calcined　powders　were　characterized　by　various　techniques　including　N2　physical　adsorption,　powder　X-ray　diffraction　(XRD),　27Al　nuclear　magnetic　resonance　(NMR),　thermogravimetric　and　differential　thermal　analysis　(TG-DTA),　scanning　electron　microscopy　(SEM),　and　transmission　electron　microscopy　(TEM).　The　characterization　results　suggested　that　the　as-synthesized　precursor　was　mainly　composed　of　Mg[sbnd]Al　LDHs　and　gibbsite　Al(OH)3.　Upon　calcination　of　the　LDHs-containing　precursor　at　600 ~ 700 °C,　MgAl2O4　spinel　was　formed　and　a　high　BET　specific　surface　area　of　~ 193 m2 g− 1　was　achieved　at　700 °C,　demonstrating　the　effectiveness　of　LDHs-containing　precursor　for　the　preparation　of　high　surface　area　MgAl2O4　spinel.　It　was　suggested　that　the　poorly　crystalline　Mg(Al)O　solid　solution　resulted　from　the　thermal　decomposition　of　Mg[sbnd]Al　LDHs　might　facilitate　the　formation　of　MgAl2O4　spinel.　The　precipitation　procedure　had　significant　effect　on　the　textural　property　of　spinel.　The　MgAl2O4　prepared　by　constant　pH　precipitation　exhibited　much　higher　BET　specific　surface　area　than　those　prepared　by　decreasing　pH　precipitation　and　increasing　pH　precipitation.　This　high-surface　area　MgAl2O4　appeared　a　promising　catalyst　support.　The　prepared　MgAl2O4-supported　Ni　catalyst　possessed　well-dispersed　Ni　nanoparticles　and　exhibited　stable　activity　for　the　carbon　dioxide　reforming　of　methane.　©　2016　Elsevier　B.V.