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The radiolysis route is applied to synthesize nickel catalysts deposited on titanium dioxide. The TPR profile of radiation-induced Ni/TiO
2
catalyst indicates a more complete reduction of the irradiated catalysts compared to the conventionally H
2
-reduced one. When tested in the benzene hydrogenation, the radiolytic Ni/TiO
2
exhibits catalytic properties with higher efficiency than the H
2
-reduced catalyst. This observation is assigned to the presence of intermetallic Ni–Ti compounds (Ni
2.66
Ti
1.33
and Ni
3
Ti) evidenced by XRD. In contrast, the calcined and H
2
-reduced catalyst contains predominantly the oxidized Ni
5
TiO
7
phase, where the nickel is in strong interaction with the support. The TEM observations show highly dispersed nickel.
Graphical Abstract
When tested in the benzene hydrogenation reaction, the catalyst Ni/TiO
2
prepared by gamma-irradiation exhibits catalytic properties (the turn-over frequency at total conversion is 33.5 molecules Bz Ni
at
−1
s
−1
at 140 °C) with higher efficiency and at lower temperature than the H
2
-reduced catalyst. This observation is assigned to extremely dispersed nickel nanoparticles and to intermetallic Ni
2.66
Ti
1.33
and Ni
3
Ti compounds evidenced by XRD.