We introduce a newly developed combinatorial electrostatic atomization system, "M-ist Combi," and demonstrate the effectiveness of the system by establishing a pseudo-temary Li-Ni-Co oxide phase diagram. After heating the starting materials with compositions in the range of 0.4 <= Li/(Li+Ni+Co) <= 0.6 at 973 K for 3 h, the diffraction of all of the products was indexed as single-phase with layer-type hexagonal structures such as LiCoO2 and LiNiO2. As the substitution quantity of Co to the Ni site increased, the value of 2 theta shifted to a high-angle. By combining the M-ist Combi system with combinatorial XRD apparatus, we successfully completed the high-throughput sample preparation and phase identification of over 150 samples in one day. (c) 2006 Elsevier B.V. All rights reserved.