As the technology for diamond film preparation by plasma-assisted CVD and related procedures has advanced, Raman spectroscopy has emerged as one of the principal characterization tools for diamond materials. Cubic diamond has a single Raman-active first order phonon mode at the center of the Brillouin zone. The presence of sharp Raman lines allows cubic diamond to be recognized against a background of graphitic carbon and also to characterize the graphitic carbon. Small shifts in the band wavenumber have been related to the stress state of deposited films. The effect is most noticeable in diamond films deposited on hard substrates such as alumina or carbides. The Raman line width varies with mode of preparation of the diamond and has been related to degree of structural order. The Raman spectrum of hexagonal diamond (lonsdaleite) is distinct from that of the cubic diamond and allows it to be recognized.

High quality diamond thin films were deposited on different substrates at temperatures from 300 to 1000 °C by the microwave plasma enhanced chemical vapor deposition (MPCVD) system. The quality of deposited diamond films was improved by adding oxygen in the gas mixtures. Different ratios of methane to oxygen concentration in hydrogen at different temperatures have been studied. At high temperatures (800–1000 °C), the addition of oxygen will not only enhance the growth rate of deposited films but also extend the region of diamond formation. At low temperatures (<500 °C), the oxygen plays an important role in diamond film growth by preferentially etching the non-diamond carbon. Without the addition of oxygen, the films deposited at high temperatures (>900 °C) were either graphitic or diamond containing a large amount of graphitic or amorphous carbon and at low temperatures (<500 °C) were white, soot-like coatings which were easily scraped off. The quality of the deposited films was characterized by Raman spectroscopy and scanning electron microscopy.

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By using surface-enhanced Raman spectroscopy it was possible to clearly identify very thin diamond and amorphous carbon coatings which were not detectable by normal Raman spectroscopy. A very small amount of silver was sputtered onto the surface of thin diamond depositions. Raman spectra measured through the silver layer exhibited the 1332 cm−1 diamond line and broadbands due to other forms of carbon. Raman scattering measured through silver coatings directly on the silicon substrate revealed extremely thin layers of amorphous carbon.

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