Influences of, precipitate rinsing solvents oil Ni for methane decomposition to COx-free hydrogen has been investigated ill this study. Calcination of nickel hydroxide precipitates rinsed by ethanol leads to the formation of nanosheet needle-like NiO, whereas calcination of those rinsed by deionized water leads to the formation of Pure nanosheet NiO. When compared to Ni catalyst (Ni-et) reduced from nanosheet needle-like NiO, Ni catalyst (Ni-etwt), reduced front Pure nanosheet-like NiO, exhibits a better catalytic performance for methane decomposition. Among the different rinsing processes, nickel hydroxide precipitates, rinsed first by ethanol and subsequently by deionized water, were calcined to the most Suitable nanoshect NiO, which Could be reduced to Ni-etwt catalyst with the highest catalytic performance of methane decomposition. A total of 1954 mol(m2)/mol(Ni) of hydrogen yields could be obtained over Ni-etwt under suitable reaction conditions. Characterization. results indicate that Ni-etwt with the higher catalytic activity has the similar to 34 nm of average particle size.