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Two novel carbon‐doped structures grown by metalorganic molecular beam epitaxy were used to study thermal stability over the temperature range from 650 to 800 °C. Each structure consists of several GaAs layers with different carbon concentrations to characterize thermal stability of GaAs layers with various carbon concentrations simultaneously. The structure shows no significant carbon diffusion even after an 800 °C‐240 min anneal. However, the hole concentration of each carbon‐doped GaAs layer in both structures has decreased, and a decrease of the hole concentration is more significant for a higher carbon concentration. With increasing the annealing time or temperature, the hole concentrations of all carbon‐doped GaAs layers approach to the same value, low 1019 cm-3.