Study of fluorine in silicate glass with 19F nuclear magnetic resonance spectroscopy

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Abstract
We report an application of nuclear magnetic resonance (NMR) spectroscopy to the study of fluorine‐doped silicate glass prepared by the modified chemical vapor deposition process, prior to drawing the rod into fibers. The silica contains 1.03‐wt. % fluorine, as determined by the calibrated intensity of the 19F NMR spectrum. The isotropic chemical shift of the 19F spectrum shows that fluorine bonds only to silicon; there is no evidence of oxyfluorides. Analysis of the distribution of nuclear dipolar couplings between fluorine nuclei reveals that the relative populations of silicon monofluoride sites [Si(O–)3F] and species having near‐neighbor fluorines, such as silicon difluoride sites [Si(O–)2F2], are nearly statistically random. That is, to a good approximation, the fluorine substitutes randomly into the oxygen sites of the silica network. There is no evidence of local clusters of fluorine sites, silicon trifluoride sites [Si(O–)F3], or silicon tetrafluoride (SiF4).