Nanoscale, LiNiPO4-core and carbon-shell high voltage (>5 V) LiNiPO4@C cathode materials have been synthesized using a microwave & solvothermal methodology using different solvents, ethylene glycol, isopropanol, isobutanol and water as the reaction medium. The effects of these solvents on the crystalquality, morphology and electrochemical qualification of the produced materials have been evaluated in terms of the heating efficiency in the microwave field by using various opto-analytical techniques and electrochemical measurements. The heating characteristics in terms of the absorption of the energy as part of the microwave-material interaction phenomenon is also discussed. X-ray diffraction analyses demonstrate that it is possible to synthesize substantially pure LiNiPO4 crystal using isopropanol as the reaction medium. High-resolution transmission electron microscopy analysis reveals that this combined methodology can provide core-shell morphology with a 5-6 nm coating thickness. The LiNiPO4@C cathode material produced in an isopropanol environment exhibits the best electrochemical properties, achieving a discharge capacity of 157 mAh g(-1) at a 0.l C-rate, and shows almost 81% capacity retention at the end of the 80th cycle. Thus, this paper offers a perspective for solving the difficulties encountered in modifying a high voltage LiNiPO4 cathode, especially the deficiency in terms of cycle life behavior, and the further benefits are highlighted. (C) 2017 Elsevier Ltd. All rights reserved.