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Hierarchically microstructured tri-axial poly(vinyl alcohol)/graphene nanoplatelet (PVA/GNP) composite fibers were fabricated using a dry-jet wet spinning technique. The composites with distinct PVA/GNPs/PVA phases led to highly oriented and evenly distributed graphene nanoplatelets (GNPs) as a result of molecular chain-assisted interfacial exfoliation. With a concentration of 3.3 wt% continuously aligned GNPs, the composite achieved a ∼73.5% increase in Young's modulus (∼38 GPa), as compared to the pure PVA fiber, and an electrical conductivity of ∼0.38 S m −1 , one of the best mechanical/electrical properties reported for polymer/GNP nanocomposite fibers. This study has broader impacts on textile engineering, wearable robotics, smart sensors, and optoelectronic devices. 

Abstract There are advantages to polymer/nanoparticle composite‐based volatile organic compounds (VOCs) sensors, such as high chemical and physical stability, operability under extreme conditions, flexible use in manufacturing, and low cost. Nevertheless, their lower limit of detection due to thickness‐dependent diffusion has constrained their application. Inspired by the metaxylem in vascular plants and its vertical conduits and horizontal pits that enable efficient transpiration, a polymer/nanoparticle composite‐based sensor is fabricated with a controllable, spontaneously formed, hollow core for inline VOCs transportation, and porous microstructure for radial direction diffusion. The hollow core is surrounded by an inner porous layer (thermoplastic polyurethane (TPU)), a middle sensing layer (TPU/graphene nanoplatelets/multiwalled carbon nanotubes), and an outer mechanically durable layer (TPU). This multilayered structure shows a 600% higher response rate compared to a single‐layered composite fiber sensor, with a low limit of detection (e.g., ≈15 ppm for xylene) and high selectivity based on the Flory–Huggins interaction parameter. This flexible and stretchable sensor also demonstrates a dual parameter sensing capability from VOC concentrations and uniaxial strain deformation. Via a one‐step fiber spinning procedure, this self‐induced hollow fiber offers a unique method of microstructural design, which enables the detection of low‐concentration VOCs by polymer/nanoparticle‐based sensors.