The glass fiber surface is metalized with electroless nickel-phosphorus deposition. The roughening and activation processes are optimized by the orthogonal experiments. A new nickel-catalyst method is developed to activate the glass fiber surface. When the activation is completed, a layer of continuous and dense film is formed on the substrate. The activated film contains a great deal of nickel oxide particles which can become the active sites after they are deoxidized in the electroless bath. In the activated film on the glass fiber, the content of Ni element is 41.01 wt.%, the content of O element is 45.64 wt.% and the content of P element is 13.35 wt.%. Scanning electron microscopy (SEM) shows that the Ni-P coatings obtained under the optimum pretreatment conditions are uniform, continuous and adhered to the glass fiber surface. Energy dispersive X-ray spectrometry (EDS) points out that the content of the nickel and the phosphorus in the deposits is 87.41 wt.% and 12.59 wt.%, respectively. X-ray photoelectron spectroscopy (XPS) analysis reveals that the 0 signal on electroless Ni-coated glass surface corresponds to oxygen in the glass substrate. X-ray diffraction pattern (XRD) indicates the Ni-P coatings are amorphous. Crown Copyright (C) 2011 Published by Elsevier B.V. All rights reserved.