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The binder jetting printing technique enables in situ impregnation of alumina using a Ni(NO3)2-containing ink (NI), facilitating omission of impregnation. NI was compared to wet impregnation (WI). Full characterization by quasi-in situ XPS, XAS and TPR revealed the presence of Ni as NiAl2O4 spinel. TPR analysis identified surface NiO and NiAl2O4 species with facilitated reduction by NI, in addition to the respective species in bulk form. Post-processing affects active site accessibility by coverage. 3D printing limited the Ni loading, but XPS revealed higher metal dispersion by NI. CO2 hydrogenation confirmed active Ni/Al2O3 catalysts with enhanced activity by NI.