Selecting high-efficiency electrocatalysts of non-noble metals is significant for large-scale industrial applications of electrochemical water splitting. Currently, the synthesis of bimetal alloy nanoparticles is an ideal strategy to improve catalytic efficiency by optimizing adsorption energy and increasing the electrical conductivity of the catalysts. In this work, we report the successful synthesis of FeNi alloy nanoparticle embedded porous nitrogen-doped carbon fibers by a facile electrospinning and carbonizing technology. The effects of different carbonization temperatures on the structure of FeNi alloy nanoparticles in carbon fibers and the electrocatalytic properties were also investigated. The as-prepared composite of carbon fibers and FeNi alloy nanoparticles exhibited a small overpotential of 317 mV at 10 mA cm(-2) and low Tafel slope of 49 mV dec(-1) for oxygen evolution reaction, as well as good stability. The performance of the novel 1D composite material along with its low-cost and simple-preparation merits is suggestive of great potential for water splitting. (C) 2020 Elsevier Inc. All rights reserved.