Diamond synthesized by CVD can be produced in different forms ranging from ballas material through to single crystal and polycrystalline films.[1±5] Diamond powders produced by conventional high-pressure/high-temperature or explosive methods are generally non-uniform and irregularly shaped. In this paper we describe the synthesis, using CVD, of diamond powders that are spherical and monodisperse, with diameters in the range 150±600 nm. Gas-phase nucleation [6±8] has been induced using a multi-cathode direct current plasma [9,10] in which the nanoscale diamond powders accumulate on a copper substrate. Transmission electron microscopy (TEM) patterns show that the internal structure comprises nanocrystalline diamond grains exhibiting a Raman peak at 1334 cm ±1 . This new form of diamond has many potential applications, including novel abrasives, cold cathode emitters, and drug delivery systems. Previously, polycrystalline diamond films have been deposited using a multi-cathode direct current (MCDC) plasma-activated (PA) CVD reactor. [9,10] With such a reactor (shown in Fig. 1a) diamond powders were also observed at the circumference of the copper disk. The presence of the copper disk lowered the surface temperature (<750 K) to a value where the diamond growth rate was negligible. As a result, it also yielded a suitable temperature gradient for the gas-phase nucleation of diamond outside the plasma boundary. The specified temperature gradient corresponds to a direction perpendicular to the lower substrate extending into the gas phase but just outside the plasma region. In the case where the tungsten anode was removed and the copper temperature was again reduced below 750 K, graphitic particles were co-deposited with diamond powder inside the plasma zone, on which the electric field concentrated, leading eventually to an arc discharge. [9,10] This caused an increase in the temperature resulting in localized film growth around the graphitic particles. Altering the configuration to that shown in Figure 1b restricted the individual DC plasmas to the regions between each pair of electrodes. Instead of the normal substrate, shown in Figure 1a, seven molybdenum disks (15 mm in Communications