In this work, self-assembled NiFe2O4/carbon nanotubes (CNTs) sponge was prepared by ice-templating method. The device synergized the advantageous features of both the 3D porous nanostructure and the catalytic properties of CNTs with GOx and NiFe2O4 nanoparticles. The porous network construction of the NiFe2O4/CNTs sheets offered enlarged specific surface for GOx immobilization and opened channels for facilitating the electrons transport and reactants diffusion. With the help of the abnormal-valence elements Ni and Fe, double catalysis has happened and the enhanced glucose biosensing performance has been achieved. The fabricated glucose biosensor exhibited two large linear ranges (0-3.0 and 3.2-12.4 mM) and distinct sensitivities (84.1 and 24.6 mu AmM-1 cm(-2)). (C) 2015 Elsevier B.V. All rights reserved.