Composites of magnetic particles in a polymeric matrix have received increasing interest due to their capacity to respond to external magnetic or electromagnetic fields. Algal polysaccharides such as agar are used extensively as gel-forming agents, thickeners, and stabilizers due to their low cost and high degree of biocompatibility and biodegradability. This study is focused on the preparation and characterization of algal polysaccharides–carbonyl iron composite films. The samples were analyzed using the photothermal radiometry (PTR) technique in the back-propagation emission configuration performing a modulation frequency scan. The amplitude and phase of the PTR experimental data were fitted simultaneously using a one-layer thermal-wave model considering homogeneous optical and thermal properties. The results indicate a systematic increase of the thermal diffusivity and optical absorption coefficient when the magnetic particle content increases. Scanning electron microscopy surface morphology of the agar/carbonyl iron composite indicates that a homogeneous distribution of particles can be obtained with the reported procedure and also provides evidence of agglomeration at high concentrations.