gamma-Al2O3 (136 m(2)/g, capillaries 2.3 nm) incipient wetness impregnated with Ni(NO3)(2)(.)6H(2)O and/or RhCi(3)(.)3H(2)O, air-dried 12 h/105degreesC, calcined 3 h/500degreesC in O-2 and reduced 1 h/600degreesC with H-2, yielded xNi-(5-x)Rh/Al2O3 (x = 5, 3.75, 2.5, 1.25, 0%) catalysts, sp. surface 0.77 to 8.32 m(2)/g. Precursors decomposed in two steps: to NiO and 2NO at 304degreesC and to Ni at 500degreesC; to RhCl at 65degreesC and to Rh at 146degreesC. Dispersions of the x = 5, 3.75 and 2.5% Ni catalysts were close, 2.3-3.2%., vs. the 37.8% of the 5% Rh catalyst Each catalyst was studied, 0.1 g, in a fixed-bed reactor over 20-900degreesC and in a 24-h reaction of (1:1 v/v) CH4-CO2, 50 mL/min, at 700degreesC. Up to 500degreesC, the bimetallic were more active than the mono; above 500degreesC all were equally highly active. The x = 5, least stable, lost 10% of activity in 24 h, C deposited was 3.2%.