Influence of temperature and residence time on thermal decomposition of monosilane

Wyller, Guro Marie; Mongstad, Trygve; Lindholm, Dag; Klette, H.; Nordseth, Ørnulf; Filtvedt, W.O.; Marstein, Erik Stensrud

doi:10.1016/j.egypro.2017.09.352

Cited by 5 publications

(4 citation statements)

References 27 publications

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“…The experiments shown in this section discuss silane and water reactivity at higher gas temperatures up to 700 °C. According to literature, monosilane thermally decomposes at temperatures between 300 and 550 °C depending on the presence of a catalytic surface, the remaining hydrogen content inside the atmosphere, and the residence time inside the reactor chamber. , Perhaps it is possible to force a hydrolysis between water and silicon radicals formed during the thermal decomposition of silane, thus reducing the water content in the gas phase. To test this hypothesis and the temperature behavior of the silane water reactivity, silane was passed through a quartz glass tube inside a tube furnace and afterwards into the QMS and FTIR, respectively.…”

Section: Resultsmentioning

confidence: 99%

Gas Phase Reaction of Silane with Water at Different Temperatures and Supported by Plasma

et al. 2023

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The interaction of silane and water is discussed controversially in literature: some authors suggest monosilane and water react kinetically and sufficiently fast enough to remove water, while others state the reaction occurs only at elevated temperatures. This question is of technological interest for the removal of unavoidable water residues in Ar gases. Thermodynamic calculations show that virtually complete removal of water is expected with superstoichiometric silane addition. However, mass spectrometric and infrared spectroscopic experiments give evidence that the addition of monosilane to such an Ar gas at room temperature is unable to remove residual water, which disagrees with some current hypotheses in the literature. This holds even for very high SiH4 concentrations up to 2 vol.-%. Silane reacts with water above temperatures of 555 °C, initiated by the thermal decomposition of silane. A cold dielectric barrier discharge-plasma used for silane and water dissociation enhances reactivity similar to elevated temperatures. Fourier-transformed infrared spectroscopy points toward silanol generation at temperatures between 400 and 550 °C, while quadrupole mass spectrometry indicates the creation of SiOH+, SiHOH+, SiH2OH+, and SiH3OH+. Cold plasmas generate smaller amounts of SiOH+, SiHOH+, and SiH2OH+ compared to elevated temperatures. Reaction products are hydrogen and nanoscaled particles of non-stoichiometric silicon oxides. The silicon-oxide particles produced differ in elemental composition and shape depending on the prevailing water content during decomposition: SiO x generated with residual water appears with relatively smooth surfaces, while the addition of water supports the formation of significantly rougher particle surfaces. Higher initial water contents correlate with higher oxygen contents of the particles.

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Section: Resultsmentioning

confidence: 99%

Gas Phase Reaction of Silane with Water at Different Temperatures and Supported by Plasma

et al. 2023

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“…Typical total flow rates are about 4 slm (standard liter per minute), resulting in residence times about 1-5 s, depending on the number of active heating zones. Further details about the reactor can be found in our previous work [17].…”

Section: Silane Pyrolysis Reactormentioning

confidence: 99%

“…We have previously shown [17] that our GC-MS technique can be used for monitoring the presence of silanes from different silane families as function of reactor conditions. With our improved understanding of the mass spectra of separate isomers, we are now able to track concentrations of separate isomers rather than whole silane families.…”

Section: Application To Silane Reactor Monitoringmentioning

confidence: 99%

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Identification of higher order silanes during monosilane pyrolysis using gas chromatography-mass spectrometry

Wyller

Klette

Mongstad

et al. 2018

Journal of Crystal Growth

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a b s t r a c tThere is a deficit of ways to detect higher order silane isomers during silane pyrolysis. Thus, a novel instrument utilizing gas chromatography-mass spectrometry (GC-MS) for detection of higher order silanes has been developed. The instrument enables us to separate higher order silane species using gas chromatography before they are introduced to the mass spectrometer, thereby obtaining spectra of separate isomers, rather than overlaid spectra. In this contribution we describe the details of the GC-MS system. We compare our GC-separated mass spectra of mono-, di-and trisilane to mass spectra of these species available in the literature. Further, we present mass spectra of the tetrasilane isomers n-tetrasilane (n-Si 4 H 10 ), silyltrisilane (i-Si 4 H 10 ) and cyclotetrasilane (cyclo-Si 4 H 8 ) and of the pentasilane isomers n-pentasilane (n-Si 5 H 12 ), silyltetrasilane (i-Si 5 H 12 ) disilyltrisilane (neo-Si 5 H 12 ) and cyclopentasilane (cyclo-Si 5 H 10 ). Six of these mass spectra are previously unpublished. Based on the fragmentation pattern in the tetra-and pentasilane mass spectra, we are able to acquire mass spectra of silanes with up to eight silicon atoms. Finally, we apply the novel detection technique to a silane pyrolysis reactor to track the outlet concentration of higher order silanes as function of reactor temperature. We believe that the detection technique that we present here may open the door for validation of monosilane pyrolysis models, and thus constitute a roadmap for future research in this field.

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Combination of a millimeter scale reactor and gas chromatography-mass spectrometry for mapping higher order silane formation during monosilane pyrolysis

Wyller

Anjitha

Skare

et al. 2020

Journal of Crystal Growth

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Influence of temperature and residence time on thermal decomposition of monosilane

Cited by 5 publications

References 27 publications

Gas Phase Reaction of Silane with Water at Different Temperatures and Supported by Plasma

Gas Phase Reaction of Silane with Water at Different Temperatures and Supported by Plasma

Identification of higher order silanes during monosilane pyrolysis using gas chromatography-mass spectrometry

Combination of a millimeter scale reactor and gas chromatography-mass spectrometry for mapping higher order silane formation during monosilane pyrolysis

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