In this study, the effects of pyrolysis heating rate on microstructural and main mechanical properties of Novalac-based carbon/carbon composites were investigated by CHNS, optical microscope, FE-SEM, BET N 2 adsorption, XRD, Raman, FT-IR, wear analyzing, three-point bending test, tensile and Vickers micro-hardness tests. Firstly, PAN-derived carbon nanofibers (reinforcing agent) was synthesized using electrospinning followed by the functionalizing via the wet chemical oxidation to improve the strength of nanofiber bonding to the matrix of composites. Firstly, novalac resin (acting as a matrix), hexamethylenetetramine (hardener agent) and carbon nanofibers (reinforcing agent) were mixed and hot-pressed at 180 °C under the compression load of 40 kN to produce compressed CNFs-Novolac composites. Carbon/Carbon composites were obtained from the pyrolysis of CNFs-Novolac composites up to 1000 °C by the various heating rates under the compression press of 400 bar, finally. Structural and mechanical studies confirmed that the heating rates below or equal to 10 °C.min −1 resulted in the production of low porosity (≤17%) carbon composite with high carbon content (>90 wt%), high fracture strength (≥270 MPa), high toughness (≥9 MPa m 1/2 ), high hardness (≥156 Hv), and low friction coefficient (<0.6).
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