Leakage-Safe Machine Learning for Hydrogen Embrittlement Detection in 316L Stainless Steel: A Region-Held-Out Evaluation of Texture and Deep Features in SEM Micrographs

Abstract

Scanning electron microscopy (SEM) is routinely used to characterize the microstructural changes caused by hydrogen embrittlement (HE) in structural steels. Machine learning can automate this characterization, but models are often evaluated using image-level splits. When several images come from the same specimen region, such splits leak information between the training and test sets. Here, we propose a region-held-out protocol for classifying as-received (AR) and hydrogen-charged (H2) SEM micrographs of 316L stainless steel, based on Leave-One-Region-Out (LORO) cross-validation over 14 spatial regions (8 AR, 6 H2; 31 images). We compared six feature-classifier combinations built on local binary patterns (LBP), grey-level co-occurrence matrices (GLCM), self-supervised convolutional embeddings pretrained on 143 unlabeled SEM images, and a convolutional neural network (CNN). The simplest texture approach, LBP with a support vector machine (LBP+SVM), performed best, achieving a balanced accuracy of 0.79, H2 recall of 0.69, and H2 precision of 0.82, outperforming every deep-learning and combined-feature model. A group-level permutation test (500 permutations sampled from the 3,003 possible region-to-label assignments) yielded p = 0.008, indicating that the result cannot be explained by a chance alignment of the region structure. Grad-CAM maps from a CNN trained on the full dataset tended to concentrate on localized surface and grain-boundary features, where hydrogen-induced morphological changes are known to occur. Under a leakage-safe, statistically validated protocol, texture descriptors recover a hydrogen-charging signature from SEM micrographs even with few samples, and the same protocol can be extended to larger HE detection studies in other alloy systems.