This　paper　describes　a　facile　method　to　produce　mesoporous　nanostructure　Ni/Al2O3,　Ni/MgO,　and　Ni/xMgO.Al2O3　(x:　MgO/Al2O3　molar　ratio)　catalysts　prepared　by　＂one-pot＂　evaporation-induced　self-assembly　(EISA)　method　with　some　modifications　for　investigating　in　the　thermocatalytic　decomposition　of　methane.　Detailed　characterizations　of　the　material　were　performed　with　X-ray　diffraction　(XRD),　Brunauer-Emmett-Teller　(BET)　and　N-2　adsorption/desorption,　hydrogen　temperature-programmed　reduction　(H-2-TPR),　scanning　electron　microscopy　(SEM),　high-resolution　transmission　electron　microscopy　(HRTEM),　and　temperature-programmed　oxidation　(TPO).　The　characterizations　demonstrated　that　the　synthesized　catalysts　with　various　MgO/Al2O3　molar　ratios　possessed　mesoporous　structure　with　the　high　BET　area　in　the　range　of　216.79　to　31.74　m(2)　g(-1).　The　effect　of　different　surfactants　and　calcination　temperatures　on　the　characterizations　and　catalytic　activity　of　the　catalysts　were　also　examined　in　details.　The　experimental　results　showed　that　the　catalysts　exhibited　high　catalytic　potential　in　this　process　and　the　55　wt.%　Ni/2　MgO　center　dot　Al2O3　catalyst　calcined　at　600　degrees　C　possessed　an　acceptable　methane　conversion　(similar　to　60%)　under　the　harsh　reaction　conditions　(GHSV　=　48000　(mL　h(-1)　g(cat)(-1))).　(C)　2018　Hydrogen　Energy　Publications　LLC.　Published　by　Elsevier　Ltd.　All　rights　reserved.