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Formation of Higher Silanes in Low-Temperature Silane (Sih4) Ices † ‡ György Tarczay,*, Marko Förstel, Pavlo Maksyutenko, and Ralf I

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Formation of Higher Silanes in Low-Temperature Silane (Sih4) Ices † ‡ György Tarczay,*, Marko Förstel, Pavlo Maksyutenko, and Ralf I Article pubs.acs.org/IC Formation of Higher Silanes in Low-Temperature Silane (SiH4) Ices † ‡ György Tarczay,*, Marko Förstel, Pavlo Maksyutenko, and Ralf I. Kaiser* Department of Chemistry and W. M. Keck Research Laboratory in Astrochemistry, University of Hawaii at Manoa, Honolulu, Hawaii 96822, United States *S Supporting Information ABSTRACT: A novel approach for the synthesis and identification of higher silanes ≤ fi (SinH2n+2, where n 19) is presented. Thin lms of (d4-)silane deposited onto a cold surface were exposed under ultra-high-vacuum conditions to energetic electrons and sampled on line and in situ via infrared and ultraviolet−visible spectroscopy. Gas phase products released by fractional sublimation in the warm-up phase after the irradiation were probed via a reflectron time-of-flight mass spectrometer coupled with a tunable vacuum ultraviolet photon ionization source. The formation mechanisms of (higher) silanes were investigated by irradiating codeposited 1:1 − silane (SiH4)/d4-silane (SiD4) ices, suggesting that both radical radical recombina- tion and radical insertion pathways contribute to the formation of disilane along with higher silanes up to nonadecasilane (Si19H40). ́ ■ INTRODUCTION hydrolysis of magnesium silicide (Mg2Si). Feher and co- fi workers synthesized and characterized higher silanes up to Monosilane (SiH4) is exploited in signi cant quantities for the 11−14 production of amorphous silicon (α-Si:H) by sputtering and Si15H32. Recently, more sophisticated acidic hydrolysis methods were developed such as utilizing organic solvents or chemical vapor deposition (CVD) in semiconductor and solar fl 1 uorosilicic acid (H2SiF6), but these methods resulted in only cell industries. In contrast, higher silanes (SinH2n+2) have not 3,15,16 been employed in this manner because of their complex very low yields of a few percent. Higher silanes can also be prepared by coupling reaction of monosilane (SiH4) with the synthetic routes and their lack of availability on an industrial 3,17 scale. However, from an economical viewpoint, they may be help of transition metal catalysts. Further, the pyrolysis or preferential starting materials considering the higher efficiency photolysis of monosilane (SiH4) or disilane (Si2H6) leads to the of α-Si:H deposition coupled with lower energy consumption. formation of longer silane chains, but mostly, or solely, unsaturated subhydrides and amorphous silicon are the main Furthermore, silanes with more than 10 silicon atoms would 3,18 represent preferred starting materials because their boiling products. Since the early 1960s, electrical discharge reactors − points are above the temperature of the silicon deposition.2 4 were patented for the formation of higher silanes. In these Besides their importance in the semiconductor technology, reactors, mainly monosilane (SiH4) or mixtures with argon, neon, hydrogen, and nitrogen were used; these processes also higher silanes are considered as hydrogen storage materials, and 3,9 fuel with monosilane was successfully utilized as an ignition aid resulted mainly in unsaturated silanes. The newest methods in hypersonic NASA X-43A scramjet flights. From the suggest that tetrachlorosilane (SiCl4) and molecular hydrogen computational chemistry viewpoint, higher liquid silanes were can be converted in a plasma process to higher-order predicted to be usable as full-scale rocket fuels or fuel additives perhalogenated silanes, which can then be transformed to 5 saturated higher silanes by a treatment with lithium aluminum for liquid hydrocarbon-fueled scramjets. Monosilane (SiH4)is 19 also potentially relevant in astrochemistry and astrobiology.6,7 hydride (LiAlH4). In summary, although multiple processes As they are co-condensed on interstellar icy grains, the have been developed to synthesize higher-order silanes, these exposure of these astrophysical ices by ionizing radiation in are not suitable for a large-scale synthesis and/or easy laboratory applications, mainly because these processes do cold molecular clouds likely results in the formation of silicon- 3,9 bearing molecules. Popularized in the Star Trek episode The not result solely in the synthesis of saturated higher silanes. Devil in the Dark, speculation about silicon chain-based life This fact calls for the elucidation of alternative formation routes started in the mid-20th Century; these ideas were compiled in a of higher silanes. A thorough understanding of the physical and hypothesis paper of Bains.8 chemical properties of these compounds is crucial for such an Because of their potential role as reagents in the semi- undertaking. Earlier infrared spectroscopic studies of electron- conductor industry, novel formation and processing methods irradiated monosilane (SiH4) ices revealed that various silanes for higher silanes have been developed and patented in recent years.3,5,9,10 The classical, nearly half-a-century-old method of Received: June 3, 2016 synthesizing higher silanes is based on aqueous acidic Published: August 11, 2016 © 2016 American Chemical Society 8776 DOI: 10.1021/acs.inorgchem.6b01327 Inorg. Chem. 2016, 55, 8776−8785 Inorganic Chemistry Article and their radicals, e.g., SiH3,Si2H6,Si2H5,H3SiSiH, H2SiSiH2, was conducted to sublime the ice and any products by warming the 7,20 irradiated samples to 300 K at rates of 0.5 K min−1. During the and H2SiSiH, can be formed at 10 K. Hiraoka et al. also fi sublimation, the molecules were analyzed by a reflectron time-of-flight identi ed disilane (Si2H6)inhydrogenatom-irradiated monosilane (SiH ) ices at 10 K.21,22 In addition, the desorption mass spectrometer (Jordan TOF Products, Inc.) after photoionization 4 (PI-ReTOF-MS) at 118.2 nm (10.49 eV).25 The pulsed (30 Hz) products were investigated by electron impact (EI) ionization coherent vacuum ultraviolet (VUV) light was generated via four-wave coupled with a quadruple mass spectrometer (QMS). Although, mixing using xenon (Specialty Gases, 99.999%) as a nonlinear because of fragmentation, these studies could not reveal silicon- medium. The third harmonic (354.6 nm) of a high-power pulsed bearing molecules with mass-to-charge ratios (m/z) beyond m/ neodymium-doped yttrium aluminum garnet laser (Nd:YAG, Spectra z 90, on the basis of the temperature-programmed desorption Physics, PRO-250, 30 Hz) underwent a frequency-tripling process ω ω ∼ × 11 (TPD) curves of the fragment ions, the authors concluded that ( uv =3 1) to yield the 118.2 nm photons at levels of 4 10 VUV 31 trisilane (Si3H8), tetrasilane (Si4H10), and a small amount of photons per pulse. The xenon was pulsed into an evacuated mixing chamber at an operating pressure of ∼3 × 10−4 Torr. In separate pentasilane (Si5H12) sublime. experiments, 129.15 nm (9.60 eV) photons were generated by Here, to better characterize the products formed upon ω ω − ω × −4 resonant four-wave mixing ( uv =2 1 2) in Krypton (8 10 electron exposure of monosilane ices, we couple the TPD ω Torr). For this purpose, 202.3 nm (6.13 eV, 1) light was generated approach with tunable vacuum ultraviolet (VUV) photo- utilizing a dye laser (Sirah, Cobra-Stretch) containing a mixture of ionization (PI) of the subliming silanes followed by analysis Rhodamine 640 and Rhodamine 610 dyes (Exciton), which was of the ions in a reflectron time-of-flight mass spectrometer pumped by the second harmonic (532 nm, 2.33 eV) of the (ReTOF-MS). This methodology has been exploited previously fundamental of a Nd:YAG laser (1064 nm, 1.17 eV; Spectra Physics, to minimize fragmentation of the parent ions;23,24 therefore, it PRO-270-30) and frequency tripling of the dye laser output (606.9 β ° ° can aid the identification of higher silanes, which have a nm, 2.04 eV) using -BaB2O4 (BBO) crystals (44 and 77 ). Second, ω kinetically unstable Si−Si bond. Furthermore, the solid-state the 466.7 nm (2.66 eV, 2) light was produced by using the third reaction mechanisms were explored by exploiting a mixture of harmonic (354.6 nm, 3.49 eV) of the 1064 nm (1.17 eV) fundamental silane and d -silane. The results of this study are important both of a Nd:YAG laser (Spectra Physics, PRO-250-30) to pump a dye laser 4 (Sirah, Precision Scan) containing Coumarin 460 dye. The VUV light for the development of nontraditional production routes of was separated from the fundamental using a lithium fluoride (LiF) higher silanes and for understanding the mechanistical biconvex lens32 (ISP Optics) based on distinct refractive indices of the processes taking place in silane-containing astrophysical ices. lens material for different wavelengths and then directed 1 mm above the ice surface.31 The photoionized molecules were extracted to the ■ EXPERIMENTAL SECTION direction of the focusing regions by an extraction plate (−190 V). The experiments were performed in a contamination-free ultra-high- Mass-to-charge ratios were determined on the basis of the arrival time vacuum stainless steel chamber evacuated to an ultrahigh vacuum of a of the ions at a multichannel plate; the signal was amplified with a fast few 10−11 Torr, exploiting magnetically suspended turbomolecular preamplifier (Ortec 9306, 1 GHz, AC coupled) and recorded using a pumps coupled with oil-free scroll backing pumps.25,26 Briefly, a bin width of 4 ns, which was triggered at 30 Hz (Quantum rhodium-coated silver wafer is mounted onto a rotatable coldfinger Composers, 9518). made of oxygen-free high-conductivity copper (OFHC) cooled to 5.5 K by a closed-cycle helium refrigerator (Sumitomo Heavy Industries, ■ RESULTS AND DISCUSSION RDK-415E). The substrate can be freely rotated within the horizontal plane via a differential pumped rotational feedthrough (Thermoionics Infrared Spectroscopy. Pure silane ices exposed to Vacuum Products, RNN-600/FA/MCO) and also translated in the energetic electrons at 10 K were already investigated previously vertical axis through a UHV compatible bellows (McAllister, BLT106). via FTIR spectroscopy.7 Therefore, only a brief summary is Gas phase silane (SiH4, Linde, 99.999%) or d4-silane (SiD4, Linde, provided here, and we will concentrate on new information not ≥ 99% D) was condensed onto the substrate by introducing the gas published previously.
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