Metallic　nickel　is　known　to　be　an　active,　but　not　a　selective　hydrogenation　catalyst　for　conversion　of　alkynes　to　alkenes.　On　the　other　hand,　nickel　oxide　is　not　active.　Recently,　we　have　demonstrated　that　nickel　doped　into　ceria　provides　an　inexpensive　catalyst　for　selective　hydrogenation　of　acetylene　in　the　presence　of　ethylene.　Here,　we　evaluate　various　synthesis　methods　to　achieve　optimal　selective　hydrogenation　performance.　We　examined　incipient　wetness　impregnation,　coprecipitation,　solution　combustion,　and　sol-gel　synthesis　to　study　how　the　method　of　preparation　affects　catalytic　structure　and　behavior.　Sol-gel　synthesis,　coprecipitation,　and　solution　combustion　synthesis　methods　favor　nickel　incorporation　into　the　ceria　lattice,　while　incipient　wetness　impregnation　creates　segregated　nickel　species　on　the　ceria　surface.　For　hydrogenation　of　acetylene,　these　nickel　surface　species　lead　to　poor　ethylene　selectivity　due　to　ethane　and　oligomer　formation.　However,　when　nickel　is　incorporated　into　the　ceria　lattice,　ethane　formation　is　prevented　even　while　achieving　100　%　conversion　of　acetylene.　Coke　formation　is　also　significantly　reduced　on　these　catalysts　compared　to　conventional　nanoparticle　counterparts.　We　conclude　that　sol-gel　synthesis　provides　the　optimal　method　for　creating　a　uniform　dopant　distribution　within　the　high　surface　area　ceria.　©　2019　Wiley-VCH　Verlag　GmbH　&　Co.　KGaA,　Weinheim