The Vapor Pressure of Silicon Tetrachloride

Kearby, K.K.

doi:10.1021/ja01293a503

Cited by 12 publications

(5 citation statements)

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“…The simplest method was to apply a sufficiently negative potential (−1.6 V vs E(Ag/AgCl)) for an extended period of time (Figure 2a,b). A consistent attenuation of the measured current was observed, with more rapid loss of current after ∼900 s. Due to the volatility of SiCl 4 (boiling point = 56 °C; vapor pressure = 235 mm Hg), 46 an initial assumption was that the attenuation in current was from loss of SiCl 4 . Attempts to periodically refresh the ec-LPE cell with a new electrolyte (Figure 2c,d) did not restore the electroreduction current.…”

Section: ■ Resultssupporting

confidence: 56%

Si Electrochemical Liquid Phase Epitaxy: Low-Temperature Growth of Hyperdoped Epitaxial Si Films

et al. 2022

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Epitaxial films of Si have been prepared at room temperature by electrochemical liquid phase epitaxy (ec-LPE). Crystalline Si films were grown on both Si(111) and Si(100) substrates, demonstrating clear evidence of low-temperature homoepitaxy. The ec-LPE method was demonstrated as a hybrid approach that combined elements of conventional electrodeposition and traditional liquid phase epitaxy. Voltammetric and amperometric data were collected that indicated conditions where Si ec-LPE is possible with SiCl 4 in propylene carbonate electrolyte and eutectic gallium indium (e-GaIn) thin-film electrodes. Scanning electron micrographs, scanning transmission electron micrographs, and electron and X-ray diffraction data demonstrated that epitaxy extended throughout films that were several microns in thickness. Raman spectra, high-resolution X-ray diffraction data, time-of-flight secondary ion mass spectrometry, and energy-dispersive elemental mapping indicated that the asprepared films were uniformly hyperdoped with Ga at >10 at %. These cumulative results demonstrate a distinct new way to realize crystalline Si films suitable for optoelectronic applications.

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Section: ■ Resultssupporting

confidence: 56%

Si Electrochemical Liquid Phase Epitaxy: Low-Temperature Growth of Hyperdoped Epitaxial Si Films

et al. 2022

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“…The cell was pressurized to 2.76 × 10 6 Pa (400 psi) to offset the volatility of SiCl 4 at elevated temperatures. 25 Figure 1b shows representative voltammograms for a Ga(l) working electrode scanned to negative potentials in propylene carbonate containing 0.2 M tetrabutylammonium chloride (TBACl) with or without 0.5 M SiCl 4 at 100 °C. The data have been corrected for the iR drop from solution resistance, as measured by impedance analysis [Figure S1 in the Supporting Information (SI)], and are the responses observed after the first scan.…”

mentioning

confidence: 99%

“…To determine whether any observable for the electroreduction of SiCl 4 at Ga( l ) electrodes would support Figure a, a two-compartment electrochemical cell was used to electrodeposit Si onto a Ga( l ) electrode at several temperatures up to 200 °C. The cell was pressurized to 2.76 × 10 6 Pa (400 psi) to offset the volatility of SiCl 4 at elevated temperatures . Figure b shows representative voltammograms for a Ga( l ) working electrode scanned to negative potentials in propylene carbonate containing 0.2 M tetrabutylammonium chloride (TBACl) with or without 0.5 M SiCl 4 at 100 °C.…”

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confidence: 99%

Direct Electrodeposition of Crystalline Silicon at Low Temperatures

Fahrenkrug

Maldonado

2013

J. Am. Chem. Soc.

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An electrochemical liquid-liquid-solid (ec-LLS) process that yields crystalline silicon at low temperature (80 °C) without any physical or chemical templating agent has been demonstrated. Electroreduction of dissolved SiCl(4) in propylene carbonate using a liquid gallium [Ga(l)] pool as the working electrode consistently yielded crystalline Si. X-ray diffraction and electron diffraction data separately indicated that the as-deposited materials were crystalline with the expected patterns for a diamond cubic crystal structure. Scanning and transmission electron microscopies further revealed the as-deposited materials (i.e., with no annealing) to be faceted nanocrystals with diameters in excess of 500 nm. Energy-dispersive X-ray spectra further showed no evidence of any other species within the electrodeposited crystalline Si. Raman spectra separately showed that the electrodeposited films on the Ga(l) electrodes were not composed of amorphous carbon from solvent decomposition. The cumulative data support two primary contentions. First, a liquid-metal electrode can serve simultaneously as both a source of electrons for the heterogeneous reduction of dissolved Si precursor in the electrolyte (i.e., a conventional electrode) and a separate phase (i.e., a solvent) that promotes Si crystal growth. Second, ec-LLS is a process that can be exploited for direct production of crystalline Si at much lower temperatures than ever reported previously. The further prospect of ec-LLS as an electrochemical and non-energy-intensive route for preparing crystalline Si is discussed.

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“…Vapor pressure of tetrachlorosilane (note: the temperature axis has been scaled inversely): blue ◊, Regnault; black □, Becker and Meyer; red ∗, Stock et al; blue □, Wintgen; green △, Kearby; purple ×, Jenkins and Chambers; black ○, Korchemskaya et al; blue +, Nisel’son and Seryakov; red ◊, Nisel’son and Lapidus; black ◊, King and Canjar; red △, Crookston and Canjar; blue ○, Capkova and Fried; black ∗, Jain and Yadav; green ○, Weiwad et al; green + , Toczylkin and Young; black △, Dow Corning Private Communication; , red □, this work. The inset shows an expanded scale for 280 < T /K < 320.…”

Section: Discussionmentioning

confidence: 99%

“…The vapor pressure of trichlorosilane has been studied in more detail, ,− but most measurements were at lower temperatures than those reported here. The vapor pressure of tetrachlorosilane has also been extensively studied ,− with all but the study by Toczylkin and Young (whose measurements were close to the critical temperature) and the industry measurements of Dow Corning (a private communication in the DIPPR database) being at lower temperatures. In the majority of the studies reported above the purity of the samples and the uncertainties in the measurements were not reported.…”

Section: Introductionmentioning

confidence: 99%

Vapor Pressure of Dichlorosilane, Trichlorosilane, and Tetrachlorosilane from 300 K to 420 K

et al. 2016

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The method for the preparation of elemental silicon of sufficient purity for the fabrication of electronic devices is by first converting silicon oxide to silicon–hydrogen-chloride compounds, purifying the material as a fluid mixture, and then converting the product to solid silicon. During the purification process a mixture of dichlorosilane (SiH2Cl2), trichlorosilane (SiHCl3), and tetrachlorosilane or silicon tetrachloride (SiCl4) are formed with each of the components in significant quantities. Models that describe the vapor–liquid equilibrium behavior for the mixtures are required to design appropriate separation and purification processes. Pure fluid properties form the starting point for most mixture models, hence the importance of vapor pressures for the pure materials. In this work we report measurements of the vapor pressures for three of the most important fluids in the silicon production process, dichlorosilane, trichlorosilane, and tetrachlorosilane. Our results are compared with measurements reported previously. The instability of chlorosilanes complicates the experimental procedures because of the corrosive nature of the products formed, and in particular the potential for self-ignition upon exposure to moist air. The experimental procedures used to minimize the hazards and to avoid contamination of the fluids are described.

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The Vapor Pressure of Silicon Tetrachloride

Cited by 12 publications

References 0 publications

Si Electrochemical Liquid Phase Epitaxy: Low-Temperature Growth of Hyperdoped Epitaxial Si Films

Si Electrochemical Liquid Phase Epitaxy: Low-Temperature Growth of Hyperdoped Epitaxial Si Films

Direct Electrodeposition of Crystalline Silicon at Low Temperatures

Vapor Pressure of Dichlorosilane, Trichlorosilane, and Tetrachlorosilane from 300 K to 420 K

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