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Firing experiments have been carried out on a clay containing naturally occurring fragments of mollusc shell. The transformation and/or decomposition of mineral phases with temperature was monitored by thermal analysis on the starting material and compared with X‐ray diffraction data on the fired specimens. Scanning electron microscopy revealed systematic changes in the internal microstructure of the shell fragments. Micrometer‐sized intra‐ and inter‐layer pores formed in the shells before the complete decomposition of calcite. The shape, dimension and location of the pores within the shell microstructure were found to be directly related to the firing temperature. The analysis of these microstructural features in archaeometric studies offers a good constraint on the estimation of the firing temperature in shell‐bearing pottery.