Blends of phenolphthalein poly(ether ether ketone) (PEK-C) and a thermotropic liquid crystalline copolyester (LCP), poly[(1-phenylethyl-p-phenylene terephthalate)-co-(1-cumyl-p-phenylene terephthalate)], was prepared via melt mixing. The studies of differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) indicate that the PEK-C/LCP blends display two glass transition temperatures which correspond to those of PEK-C-and LCP-rich phases, respectively. The PEK-C/ LCP blends were judged to be partially miscible. Scanning electron microscopy (SEM) was employed to examine the morphology of the blends, and it was observed that all the PEK-C/LCP blends displayed a phase-separated structure. The interface between the PEK-C-and LCP-rich phases is poor. The Young's modulus of the PEK-C/LCP blends was found to increase with LCP content due to the high modulus of the LCP. However, the tensile strength and the elongation at break of the blends greatly decreases with increase of LCP content, owing to the poor interfacial adhesion. From the thermogravity analysis (TGA), it was observed that all the blends exhibited a twostep weight loss mechanism, and the thermal degradation onset temperature of the blends was lowered with the addition of LCP content.