Visualizing three-dimensional internal topology and quantifying morphometry of laser-induced porous graphene and MXene aerogel using x-ray micro-computed tomography

Laser-induced graphene (LIG) and MXene (Ti3C2Tx, where Tx = –OH, –F or –O) have emerged as versatile engineered electrode materials for next-generation energy conversion and storage, biochemical sensing, and environmental technologies. Realizing their full potential requires a detailed understanding of three-dimensional (3D) internal structures that govern transport phenomena and overall device performance. Here, we employ x-ray micro-computed tomography (μCT), complemented by electron microscopy, to quantitatively characterize the internal architecture of porous LIG and freeze-dried Ti3C2Tx MXene aerogels. The μCT approach enables nondestructive volumetric visualization and reconstruction of the internal microstructure from a series of two-dimensional projections. Three-dimensional analysis reveals interconnected, cross-linked networks formed by the spatial organization of graphene lamellae in LIG and stacked MXene nanosheets in the aerogels. Both materials exhibit hierarchical porous architecture consisting of honeycomb-like frameworks with interconnected micro- and nanoporous domains. Quantitative morphometric analysis further provides key structural descriptors—including pore size distribution, porosity, pore-wall thickness, and tortuosity—from reconstructed volumetric datasets, showing good agreement with complementary observed physicochemical characterization. These findings establish μCT as a powerful tool for correlating 3D morphology with material properties and provide design insights into layered porous materials used in applications where performance is strongly influenced by mass diffusion and mixed electron–ion transport within complex porous networks.