The　Li-rich　cathode　materials　Li[NixLi1/3-2x/3　Mn2/3-x/3]O2(x=1/5,　1/4,　1/3)　were　synthesized　with　co-precipitated　metal　hydroxide　precursors　M(OH)2(M=Mn,　Ni).　The　results　of　X-ray　diffraction(XRD)　and　selected　area　electron　diffraction(SAED)　analysis　confirmed　the　Li,　Ni　and　Mn　atoms　are　ordered　in　the　M　layer　to　form　the　superstrucutre.　Images　of　scanning　electron　microscopy(SEM)　show　the　Li-rich　materials　particles　are　about　1-3　μm,　aggregated　of　submicron　grains.　Electrochemical　behavior　was　examined　by　charge-discharge　cycling.　The　Li[NixLi1/3-2x/3　Mn2/3-x/3]O2(x=1/5,　1/4,　1/3)　materials　exhibited　high　reversible　capacity　of　200-240　mA·h/g　and　excellent　cycle　performance　between　2.0　and　4.8　V　at　10　mA/g　current　density.