Standardized detection and characterization of graphene in textile fibers via an integrated SEM/XRD/Raman approach

The application of graphene in functional textiles is limited by detection challenges within complex fiber matrices. This study presents a standardized integrated protocol comprising “Pretreatment + SEM/XRD/Raman.” The fiber-specific chemical pretreatment facilitates efficient graphene enrichment, achieving a recovery rate exceeding 80% and a matrix removal rate surpassing 90%. Scanning Electron Microscopy (SEM) characterizes morphology, X-ray Diffraction (XRD) determines the layer count (≤10 layers) through Full Width at Half Maximum (FWHM) measurements (≤2.3°) at approximately 26°, and Raman spectroscopy analyzes defects and layers via 2D band FWHM (<30 cm⁻¹). This method exhibits high precision, with a relative standard deviation (RSD) of ≤10% across a mass fraction range of 0.01-10%, and reliability, achieving a discrimination accuracy of ≥95% between graphene and graphite. Furthermore, it reduces analysis time from 4 hours to 2.8 hours, thereby providing a robust solution for the quality control of graphene textiles.