Indium acetylacetonate, a β-diketonate complex, was pyrolyzed at 700 °C in inert ambient in a sealed quartz tube, to yield a powder composite of nanocrystalline In 2 O 3 and elemental carbon (In 2 O 3 /C), as deduced from characterization by powder X-ray diffraction and Raman spectroscopy. Scanning electron microscopy shows that the metal oxide is embedded in micrometer-sized spherical structures, composed largely of carbon. The spherical entities are likely formed when the metal complex melts, decomposes, and vaporizes during pyrolysis, with the vapour condensing into spherical "droplets" as the sealed tube cools gradually to room temperature. The In 2 O 3 /C composite was tested (in pellet form) as a gas sensor, specifically the conductometric sensing of H 2 S. At 5 ppm of H 2 S, the composite shows a high response of 225% at 250 °C, with the response and recovery being swift (~ 5 s and ~ 15 s, respectively). At 250 °C, the detection limit is found to be of 500 ppb of H 2 S, with selectivity over NH 3 , NO 2 , CH 4 , and SO 2 being considerable. The In 2 O 3 /C sensor also displays good cyclability. When carbon in the composite is removed by annealing it in air (550 °C, 60 min), the resulting In 2 O 3 powder (in pellet form) shows a much poorer response to H 2 S at 250 °C (25% to 5 ppm), illustrating that the elemental carbon in In 2 O 3 /C enhances sensitivity to H 2 S. The advantages of a simple fabrication process and low power consumption make the carbonaceous composite sensor potentially useful.