The monolayer engineering diamond particles are aligned on the oxygen free Cu plates with electroless Ni plating layer. The mean diamond particle sizes of 15, 23 and 50 μm are used as thermal conductivity pathway for fabricating metal/carbon multi-layer composite material systems. Interconnected void structure of irregular shaped diamond particles allow dense electroless Ni plating layer on Cu plate and fixing them with 37-43% Ni thickness of their mean diameter. The thermal conductivity decrease with increasing measurement temperature up to 150°C in all diamond size conditions. When the diamond particle size is increased from 15 μm to 50 μm (Max. 304 W/mK at room temperature) tended to increase thermal conductivity, because the volume fraction of diamond is increased inside plating layer.