We have investigated the spatiotemporal development of the plasma duri
ng the bias pre-treatment that precedes the chemical vapour deposition
(CVD) of diamond and the chemical composition, the identity of carbon
modifications, and the topography of the substrate surfaces after sel
ected stages of the biasing. The methods employed were X-ray photoelec
tron spectroscopy (XPS) and Raman spectroscopy as well as scanning ele
ctron microscopy (SEM). Areas of high diamond nucleation density were
identified at each stage by interrupting the bias pre-treatment, switc
hing to growth conditions and screening for diamond crystals after gro
wth for Ih with SEM. After about 10 min the biasing alone yields an al
most pure diamond surface as judged by the loss features in XPS althou
gh neither Raman spectroscopy nor SEM give any indication thereof. In
particular, for the growth of highly oriented textured diamond films,
the stage at which the biasing is stopped is crucial since prolonged g
rowth of diamond under biasing conditions destroys the initial orienta
tion of the diamond nuclei.