In this work, pre-oxidized polyacrylonitrile fibers are treated with ultrasonic etching and solution etching to produce ultra-thin sections. The evolution of the fibers’ microstructure in the pre-oxidation process is observed, and the transformation model of the microstructure of the pre-oxidized fibers is proposed. Scanning electron microscopy and high-resolution transmission electron microscopy were used to observe the microstructure changes of the fibers. Fourier transform infrared spectroscopy and X-ray diffraction were used to observe the chemical structure transformation and crystallization degree of the fibers in the pre-oxidation process. The results revealed that pre-oxidized fibers exhibited a smooth surface, while their interior consisted of fibrils. The longitudinal microfibrils were connected by the transverse microfibrils and amorphous regions. The fracture morphology of the fibers shifted from ductile to brittle, and the cross-section gradually became smoother. The linear molecular chain of PAN transformed into a ring structure as pre-oxidation progressed, subsequently leading to the cross-linking of this ring structure into an orderly trapezoidal configuration. The connection between the fibrils was enhanced, and the fiber structure became more compact and stable.

Silk nanofibers (SNF) have great applications in high-performance functional nanocomposites due to their excellent mechanical properties, biocompatibility, and degradability. However, the preparation of SNF by traditional methods often requires the use of some environmentally harmful or toxic reagents, limiting its application in green chemistry. In this paper, we successfully prepared SNF using natural silk as raw material and solvent stripping technology by adjusting the solvent concentration and solution ratio (the diameter of about 120 nm). Using the above SNFs as raw materials, SNF membranes were prepared by vacuum filtration technology. In addition, we prepared an SNF/MXene nanocomposite material with excellent humidity sensitivity by simply coating MXene nanosheets with silk fibers. The conductivity of the material can approach 1400.6 S m⁻¹ with excellent mechanical strength (51.34 MPa). The SNF/MXene nanocomposite material with high mechanical properties, high conductivity, and green degradability can be potentially applied in the field of electromagnetic interference (EMI) shielding, providing a feasible approach for the development of functional nanocomposite materials.

With the increasing demand for effective electromagnetic wave (EMW) absorbers due to the proliferation of electronic devices and 5G communication systems, traditional wave-absorbing materials can no longer meet the current requirements. Thus, this research introduces a three-dimensional (3D) composite material consisting of PMMA@Mxene@Co₃O₄ microspheres, prepared through in situ self-assembly and hydrothermal growth. The strong electrical conductivity of Mxene, combined with the magnetic loss of Co₃O₄, ensures enhanced dielectric–magnetic synergy, leading to excellent EMW absorption. The study investigates the influence of varying Co₃O₄ content on the electromagnetic properties of the composite. Experimental results show that the optimal sample, with a thickness of 2.5 mm, achieves a minimum reflection loss (RL_min) of −52.88 dB at 6.88 GHz and an effective absorption bandwidth (EAB) of 5.28 GHz. This work highlights the potential of 3D PMMA@Mxene@Co₃O₄ composites as high-performance microwave absorbers, providing a promising solution to EMW pollution. The findings offer valuable insights into material design strategies, demonstrate a promising pathway for developing lightweight, high-performance EMW absorbing materials by optimizing impedance matching and utilizing advanced microstructure design techniques.