New bulky layers of metal mixed ceramic nanofibers were fabricated through two-nozzle electrospinning method followed by calcination. Solutions of PAN in DMF with various concentrations were prepared as: 11, 12, 13, 14, and 15 wt% to which the constant amounts of 2.1 g of Aluminum acetate, 0.3 g of Copper acetate and 0.3 g of Boehmite nanoparticles were added. A stepwise calcination process was utilized to obtain the ceramic nanofibers. The nanofibers were characterized by FTIR spectroscopy, TG-DTA, XRD, SEM and EDS techniques. The formulation with 12 wt% of PAN in DMF was proved to be the optimum spinable sample. The average diameter of as spun nanofibers was detected as 568 nm, which decreased to 181 nm after calcination and thermal degradation. Ceramic nanofibers were composed of CuO, Al2O3 and Cu2Al4O7 phases. The average density of the sample was about 0.090 (g/cm(3)) and the porosity of the mat was 94.5% and thus, production of a 3D structure may be claimed. The ceramic nanofibers performed well as catalyst in the C-C coupling reaction (Suzuki reaction) by facilitating the synthesis of biaryl compound from aryl iodide in 20 min with isolated yield of 89% only by using 15 mg of ceramic nano fibers as the nano catalyst. (C) 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.