The simultaneous estimation of multi-mode heat transfer properties, conductive and radiative, is investigated for materials that include significant heat transfer by radiation. The focus is on insulative type materials with a relatively large optical thickness. Two basic models were developed for the combined conduction and radiation heat transfer: a diffusion solution and a more exact absorbing and isotropically scattering solution. Both solutions were written for one-dimensional heat transfer in gray, isotropically scattering materials. Different experimental setups were compared through a sensitivity analysis of the parameters to determine the best experiment for estimating the properties. An experiment was performed to collect real data to verify estimation procedures. The material used for the experiment was Styrofoam and the experiment consisted of a heat flux supplied by a thin film heater on one boundary and a constant temperature on the other boundary. The thermal capacitance of the heater proved to have an effect on the temperature measurements at the heated surface and had to be incorporated into the model. The estimation procedure involved the use of two methods, the modified Box Kanemasu algorithm and a genetic algorithm. Difficulties were encountered in simultaneously estimating all the properties due to correlation between the thermal conductivity and the radiation parameters, as well as some correlation between the heat capacity of the Styrofoam and the heat capacity of the heater. However, the genetic algorithm did provide fairly narrow and well-defined property ranges and confirmed that radiation transfer was significant in the Styrofoam. / Ph. D.