Three dimensional porous Li1.6Al0.6MnO4 (LAMO) nanofibers were successfully prepared for the first time, via a facile electrospinning homogenous solution of lithium acetate, manganese nitrate and aluminum nitrate in polyvinyl alcohol and polyvinylpyrolidone solution followed by calcination of the as-spun nanofibers at 500, 700 and 900 degrees C. The processing parameters were; voltage 25 kV, flow rate 0.7 ml/h, the distance between the needle and collector 10 cm and the inner diameter of the needle 0.499 mm. X-ray diffraction of the samples prepared by using electrospinning and sol-gel revealed that Li1.6Al0.6MnO4 phase was formed at; 500 degrees C and 700 degrees C, respectively. Field Emission Scanning Electron Microscopy revealed that the electrospun nanofibers at 700 degrees C were fabricated with diameter 250 nm, and the single fiber composed of 30 nm LAMO grains. On the other hand, samples calcined at 700 degrees C, prepared by sol-gel, show coalescence of the fine grains of LAMO in the form of microspheres with an average diameter of 1 mu m and each microsphere is composed of fine crystals of LAMO. The characteristics of the prepared spinel make them promising for use in lithium adsorption from polluted effluents. (C) 2015 Elsevier Ltd and Techna Group S.r.l. All rights reserved.