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29Si nuclear magnetic resonance study of plasma‐polymerized hexamethyldisiloxane

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4 Author(s)
Assink, R.A. ; Sandia National Laboratories, Albuquerque, New Mexico 87185 ; Hays, A.K. ; Bild, R.W. ; Hawkins, B.L.

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The structure of plasma‐polymerized hexamethyldisiloxane (PP‐HMDSO) was studied by 29Si nuclear magnetic resonance (NMR) using magic angle spinning and cross‐polarization techniques. Spectra of the PP‐HMDSO were recorded before and after it had been subjected to successive heat treatments in air at 100, 200, and 300 °C. The spectra exhibit major peaks at +11 ppm, -18 ppm, -55 to -64 ppm, and -99 to -106 ppm with respect to tetramethylsilane. These shifts correspond to silicon bonded to one, two, three, and four oxygens, respectively. The broadness of the tri‐ and tetrafunctional silicon peaks is attributed to SiOH or SiOCH3 functional groups in addition to the normal SiOSi moieties. Minor peaks at -5 and -33 ppm are attributed to mono‐ and difunctional silicons in which one of the methyl groups has been replaced by a hydrogen. As the material is heat treated there is a tendency for the PP‐HMDSO to form additional silicon–oxygen bonds. Spectra simulations show that the oxygen content increases from 16 to 30 wt. % during the course of the heat treatment. The silicon to oxygen weight percent ratios measured by NMR spectra simulation and neutron activation analysis are comparable and decrease monotonically as the heat treatment progresses.

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Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films  (Volume:3 ,  Issue: 6 )