NMR study of the synthesis of alkyl-terminated silicon nanoparticles from the reaction of SiCl4with the Zintl Salt, NaSi

D. Mayeri, B. L. Phillips, M. P. Augustine, S. M. Kauzlarich

Research output: Contribution to journalArticle

103 Citations (Scopus)

Abstract

The synthesis of silicon nanoclusters and their characterization by multinuclear solid-state nuclear magnetic resonance (NMR) is presented. A combination of 23Na, 29Si, and 13C magic angle spinning with and without cross polarization to 1H nuclei have been used to investigate the reaction of sodium silicide (NaSi) with silicon tetrachloride (SiCl4) followed by varying degrees of surface passivation. The 23Na and 29Si NMR spectra of NaSi distinguish the two crystallographically inequivalent sites for each, consistent with the crystal structure. This compound exhibits extreme diamagnetic chemical shifts for 29Si of -361 and -366 ppm. NaSi is reacted with SiCl4 in refluxing ethylene glycol dimethyl ether to produce both amorphous and crystalline Si nanoparticles with surfaces capped by chlorine. This reaction produces new 29Si resonances that survive subsequent capping and oxidation reactions. The 29Si NMR spectrum shows that the product is incompletely passivated with butyl groups and gives several peaks lying between -67 and -81 ppm that can be attributed to surface silicon atoms. Further reaction of this product with water produces a new NMR spectrum consistent with further termination of the surface by -OH groups.

Original languageEnglish (US)
Pages (from-to)765-770
Number of pages6
JournalChemistry of Materials
Volume13
Issue number3
DOIs
StatePublished - 2001

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Silicon
Salts
Nuclear magnetic resonance
Nanoparticles
Magic angle spinning
Nanoclusters
Chlorine
Chemical shift
Ethylene glycol
Passivation
Ethers
Crystal structure
Sodium
Polarization
Crystalline materials
Atoms
Oxidation
Water

ASJC Scopus subject areas

  • Materials Chemistry
  • Materials Science(all)

Cite this

NMR study of the synthesis of alkyl-terminated silicon nanoparticles from the reaction of SiCl4with the Zintl Salt, NaSi. / Mayeri, D.; Phillips, B. L.; Augustine, M. P.; Kauzlarich, S. M.

In: Chemistry of Materials, Vol. 13, No. 3, 2001, p. 765-770.

Research output: Contribution to journalArticle

Mayeri, D. ; Phillips, B. L. ; Augustine, M. P. ; Kauzlarich, S. M. / NMR study of the synthesis of alkyl-terminated silicon nanoparticles from the reaction of SiCl4with the Zintl Salt, NaSi. In: Chemistry of Materials. 2001 ; Vol. 13, No. 3. pp. 765-770.
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N2 - The synthesis of silicon nanoclusters and their characterization by multinuclear solid-state nuclear magnetic resonance (NMR) is presented. A combination of 23Na, 29Si, and 13C magic angle spinning with and without cross polarization to 1H nuclei have been used to investigate the reaction of sodium silicide (NaSi) with silicon tetrachloride (SiCl4) followed by varying degrees of surface passivation. The 23Na and 29Si NMR spectra of NaSi distinguish the two crystallographically inequivalent sites for each, consistent with the crystal structure. This compound exhibits extreme diamagnetic chemical shifts for 29Si of -361 and -366 ppm. NaSi is reacted with SiCl4 in refluxing ethylene glycol dimethyl ether to produce both amorphous and crystalline Si nanoparticles with surfaces capped by chlorine. This reaction produces new 29Si resonances that survive subsequent capping and oxidation reactions. The 29Si NMR spectrum shows that the product is incompletely passivated with butyl groups and gives several peaks lying between -67 and -81 ppm that can be attributed to surface silicon atoms. Further reaction of this product with water produces a new NMR spectrum consistent with further termination of the surface by -OH groups.

AB - The synthesis of silicon nanoclusters and their characterization by multinuclear solid-state nuclear magnetic resonance (NMR) is presented. A combination of 23Na, 29Si, and 13C magic angle spinning with and without cross polarization to 1H nuclei have been used to investigate the reaction of sodium silicide (NaSi) with silicon tetrachloride (SiCl4) followed by varying degrees of surface passivation. The 23Na and 29Si NMR spectra of NaSi distinguish the two crystallographically inequivalent sites for each, consistent with the crystal structure. This compound exhibits extreme diamagnetic chemical shifts for 29Si of -361 and -366 ppm. NaSi is reacted with SiCl4 in refluxing ethylene glycol dimethyl ether to produce both amorphous and crystalline Si nanoparticles with surfaces capped by chlorine. This reaction produces new 29Si resonances that survive subsequent capping and oxidation reactions. The 29Si NMR spectrum shows that the product is incompletely passivated with butyl groups and gives several peaks lying between -67 and -81 ppm that can be attributed to surface silicon atoms. Further reaction of this product with water produces a new NMR spectrum consistent with further termination of the surface by -OH groups.

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