Mixtures (1-x)LiGdF4+xLiLuF(4) (0.50 <= x <= 0.75) were melted and submitted to one zone melting cycle under a reactive HF atmosphere, aiming the study of the crystal growth of LiGd1-xLuxF4 solid solutions. Phase identification and compositional studies of the ingots were performed by scanning electron microscopy, energy dispersive X-ray spectrometry, and X-ray powder diffraction. Transparent regions of the bar related to the formation of LiGd1-xLuxF4 solid solutions were found to be enlarged proportionally to the initial amount of Lu in the mixtures. Gd segregates to the end of the ingot. (C) 2012 Elsevier B.V. All rights reserved.