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Abstract: Microcrystalline diamond has been successfully synthesized in a low-pressure inductively coupled plasma using di-t-alkyl peroxide. Di-t-alkyl peroxides are thermally decomposed into acetones and methyl radicals, which presumably serve as precursors for the formation of diamond on the silicon substrate at 943 K and 993 K. The deposits on the substrate were examined by scanning electron microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy. It was found that the deposits contained a microcrystalline diamond phase even at a low pressure of 11 Pa. Diamond formation over a large area in low-pressure plasmas has been demonstrated by the present novel diamond deposition process using di-t-alkyl peroxide thermally decomposed as a feed gas. [Copyright &y& Elsevier]