Pyrolysis chemistry of an organometallic precursor to silicon carbide

Schmidt, Wayde R.; Interrante, L. V.; Doremus, Robert H.; Trout, Todd K.; Marchetti, Paul S.; Maciel, Gary E.

doi:10.1021/cm00014a011

Cited by 90 publications

(70 citation statements)

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“…As the FWHM of this absorption band reaches 50 cm 1 , it is probably composed of many different types of bonds and configurations. We suggest that energetically these chemical groups could be a silylene radical SiH 2 (900-930 cm 1 ), 34 deformation mode of a silyl group SiH 3 (920, 843.5, 939.6, 941 cm 1 ), 35 Si-H bending (937 cm 1 ) 36 or Si-H 2 scissor mode (910 cm 1 ). 37 The time evolution of infrared absorption suggests that hydrogen tends to further react with silicon in the buffer/SLG interface layer.…”

Section: Discussionmentioning

confidence: 90%

Hydrogen intercalation of epitaxial graphene and buffer layer probed by mid-infrared absorption and Raman spectroscopy

2018

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We have measured optical absorption in mid-infrared spectral range on hydrogen intercalated single layer epitaxial graphene and buffer layer grown on silicon face of SiC. We have used attenuated total reflection geometry to enhance absorption related to the surface and SiC/graphene interface. The Raman spectroscopy is used to show presence of buffer layer and single layer graphene prior to intercalation. We also present Raman spectra of quasi free standing monolayer and bilayer graphene after hydrogen intercalation at temperatures between 790 and 1510°C. We have found that although the Si-H bonds form at as low temperatures as 790°C, the well developed bond order has been reached only for samples intercalated at temperatures exceeding 1000°C. We also study temporal stability of hydrogen intercalated samples stored in ambient air. The optical spectroscopy shows on a formation of silyl and silylene groups on the SiC/graphene interface due to the residual atomic hydrogen left from the intercalation process.

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Section: Discussionmentioning

confidence: 90%

Hydrogen intercalation of epitaxial graphene and buffer layer probed by mid-infrared absorption and Raman spectroscopy

2018

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“…NMR spectra were obtained using a Bruker 300 MHz spectrometer a 5 mm tube and benzene-d 6 as solvent and internal standard; a trace of Cr(AcAc) 3 (AE1 mol%) was added to the sample solution to reduce the 29 Si spin-lattice relaxation time (T 1 ). FTIR spectra were recorded on a PerkinElmer PE1700 spectrometer.…”

Section: Methodsmentioning

confidence: 99%

Stoichiometric silicon carbide from borate‐catalyzed polymethylsilane–polyvinylsilane formulations

Boury

Bryson²,

Soula³

1999

Appl. Organometal. Chem.

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Polymethylsilane (PMS) and polyvinysilane (PVS) were prepared by Wurtz condensation of chlorosilanes and characterized by spectroscopy (1H, 13C and 29Si NMR, and infrared), viscosity and GPC analysis. Mixtures of the PMS and PVS were prepared and stabilized with 2,6‐di‐t‐butyl‐4‐methylphenol (BHT; 0.5 wt%) to which was added a catalytic amount of tris(trimethylsilyl)borate, B(OSiMe3)3 (BTMS; 2 wt% by weight). The resulting liquid materials were pyrolyzed to 950 °C and to 1400 °C under argon. The formulation, composed of 60% PMS / 40% PVS / 2% BTMS, was pyrolyzed and gives nearly stoichiometric silicon carbide in 73% yield. The pyrolyzate was analyzed spectroscopically at intermediate stages in order to study its thermal transformations and the influence of the boron catalyst. The ceramic obtained from the formulation 60% PMS / 40% PVS / 2% BTMS shows good stability at 1500 °C under oxygen. Copyright © 1999 John Wiley & Sons, Ltd.

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“…Pyrolysis of several Si-containing polymers, including poly(dimethylsilane) (Yajima et al, 1978), polycarbosilane (PCS) (Liu et al, 1999;Schmidt et al, 1991), and polysilane-containing chlorine (Martin et al, 1997), is well-known to produce -silicon carbide exclusively (-SiC). This fact engendered the idea that SNPs might also produce -SiC as a result of pyrolysis.…”

Section: Pyrolysis Of Si-containing Polymersmentioning

confidence: 99%

“…Based on pyrolysis experiments with PCS (Liu et al, 1999;Schmidt et al, 1991), -H elimination from alkyl C-H (Scheme 2) is postulated to be the key for producing elemental Si without significant interference by the Kumada rearrangement reaction responsible for SiC production (Shini and Kumada, 1958). Peripheral SNP structures may be terminated with Si-Cl and Si-H, as exemplified in chlorine-containing polysilane (Martin et al, 1997).…”

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confidence: 99%