In this work, NiMgAl and RhNiMgAl catalysts prepared from HTLCs precursors were investigated for the Partial Oxidation of Methane (POM) at 550 and 750 degrees C. Samples have been characterized by XRD, TPR, H-2 chemisorption, TPSR analyses, XPS, field emission scanning electron microscopy and Raman spectroscopy. NiMgAl catalysts with high Ni content (40 and 16 wt%) showed high stability and high methane conversion for POM. On the other hand those with lower Ni content (NiHT15 and NiHT25, with 6 and 4 wt%) exhibited low catalytic activity with low H-2/CO ratio (<2) and fast deactivation. In RhNiHT25 (0.6 wt. % Rh), the Ni reducibility was improved, increasing the methane conversion and hydrogen selectivity. In addition, the noticeable increase in stability was related to the absence of carbon deposition after 30 h on stream at 550 degrees C. These results show that RhNiHT25 is promising for application in membrane reactors to produce high purity hydrogen. Copyright (C) 2013, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.