Twinning‐induced plasticity (Twip) steel is characterized by the presence of twins and austenite at room temperature. In the present work, Fe‐24Mn‐3Al‐1Ni‐2Si‐0.06C steel is cold‐rolled at 30, 50, and 80%, thickness reduction and subsequently annealed at temperatures between 300 and 1100°C for 15 min. The microstructure, and hardness are analyzed and dislocation density, stacking fault, and twin probability are calculated using the diffraction method based on the intensity of X‐rays generated in a synchrotron facility. The Rietveld analysis using Materials Analysis Using Diffraction (MAUD) software was performed, and Popa Model was employed. Cold rolling increases hardness due to the formation of deformation twins, stacking fault, and dislocation in different degrees depending on the thickness reduction. During annealing, recrystallization influences the parameters obtained by X‐ray diffraction such as stacking fault probability and dislocation density.This article is protected by copyright. All rights reserved.