Abstract:A one-pot facile synthesis of cyclosiloxane-based hybrid polymers based on hydrosilylation reaction and their network polymer film formation via self-crosslinking by hydrolysis/condensation reactions are reported.
“…appear to exhibit a two‐step mass loss event. The first, lower temperature event is assigned to Si—C and C—C bond cleavage, whereas the second event is attributed to the redistribution of the siloxane network . With the exception of SiCE‐H41 and SiCE‐H25, the onset of degradation ( T d ) and char yields appear to increase as the amount of siloxane component is increased.…”
Section: Resultsmentioning
confidence: 99%
“…The SiCE‐MTDMSS and SiCE‐PTDMSS elastomers also had the lowest char yields at approximately 25%. Upon thermal decomposition, these elastomers would produce mostly silicon dioxide (SiO 2 ) and silicon oxycarbide (Si x O y C z ) char . Being of lowest content of siloxane, the char yields should be reduced with respect to those elastomers containing the siloxane pre‐polymers.…”
Section: Resultsmentioning
confidence: 99%
“…The first, lower temperature event is assigned to Si-C and C-C bond cleavage, whereas the second event is attributed to the redistribution of the siloxane network. 37,38 With the exception of SiCE-H41 and SiCE-H25, the onset of degradation (T d ) and char yields appear to increase as the amount of siloxane component is increased. Furthermore, by crosslinking the pre-polymers with TAC, the T d values are shifted upwards by between 40 and 250 ∘ C depending on the pre-polymer employed.…”
Section: Characterization Of Sice Elastomersmentioning
confidence: 98%
“…Upon thermal decomposition, these elastomers would produce mostly silicon dioxide (SiO 2 ) and silicon 544 www.soci.org AR Jennings et al oxycarbide (Si x O y C z ) char. 38,41 Being of lowest content of siloxane, the char yields should be reduced with respect to those elastomers containing the siloxane pre-polymers. In transitioning to the formulation prepared using the lowest molecular weight siloxane pre-polymer (1000-1100 g mol −1 ), SiCE-H11, T d is shifted upwards by nearly 100 ∘ C and is assigned to the increased thermochemical stability arising from the incorporation of the siloxane pre-polymer.…”
Section: Characterization Of Sice Elastomersmentioning
A number of siloxane‐based cyanate ester (SiCE) elastomers were prepared from commercially available starting reagents employing a hydrosilylation reaction. Each elastomer was designed to utilize 2,4,6‐tris(allyloxy)‐1,3,5‐triazine as a crosslinker and multifunctional vinyl component in the hydrosilylation reaction, ensuring that the triazine rings were completely formed, and thus the elastomers resemble fully cured cyanate ester networks. The hydride‐terminated siloxane components used were varied from small‐molecule siloxanes to pre‐polymers of different molecular weights. Attenuated total reflectance Fourier transform infrared analysis confirmed the successful hydrosilylation reaction and complete curing of the SiCE elastomers via functional group analysis. Thermal characterization by thermogravimetric analysis and differential scanning calorimetry demonstrated that thermal properties of the elastomers could be tailored depending on the type of siloxane component that was utilized. The gel content of the elastomers was also determined. Investigations into the effects of a platinum catalyst on the elastomers determined that the presence of the catalyst affected the thermochemical stability of the SiCE elastomers. Published 2016. This article is a U.S. Government work and is in the public domain in the USA.
“…appear to exhibit a two‐step mass loss event. The first, lower temperature event is assigned to Si—C and C—C bond cleavage, whereas the second event is attributed to the redistribution of the siloxane network . With the exception of SiCE‐H41 and SiCE‐H25, the onset of degradation ( T d ) and char yields appear to increase as the amount of siloxane component is increased.…”
Section: Resultsmentioning
confidence: 99%
“…The SiCE‐MTDMSS and SiCE‐PTDMSS elastomers also had the lowest char yields at approximately 25%. Upon thermal decomposition, these elastomers would produce mostly silicon dioxide (SiO 2 ) and silicon oxycarbide (Si x O y C z ) char . Being of lowest content of siloxane, the char yields should be reduced with respect to those elastomers containing the siloxane pre‐polymers.…”
Section: Resultsmentioning
confidence: 99%
“…The first, lower temperature event is assigned to Si-C and C-C bond cleavage, whereas the second event is attributed to the redistribution of the siloxane network. 37,38 With the exception of SiCE-H41 and SiCE-H25, the onset of degradation (T d ) and char yields appear to increase as the amount of siloxane component is increased. Furthermore, by crosslinking the pre-polymers with TAC, the T d values are shifted upwards by between 40 and 250 ∘ C depending on the pre-polymer employed.…”
Section: Characterization Of Sice Elastomersmentioning
confidence: 98%
“…Upon thermal decomposition, these elastomers would produce mostly silicon dioxide (SiO 2 ) and silicon 544 www.soci.org AR Jennings et al oxycarbide (Si x O y C z ) char. 38,41 Being of lowest content of siloxane, the char yields should be reduced with respect to those elastomers containing the siloxane pre-polymers. In transitioning to the formulation prepared using the lowest molecular weight siloxane pre-polymer (1000-1100 g mol −1 ), SiCE-H11, T d is shifted upwards by nearly 100 ∘ C and is assigned to the increased thermochemical stability arising from the incorporation of the siloxane pre-polymer.…”
Section: Characterization Of Sice Elastomersmentioning
A number of siloxane‐based cyanate ester (SiCE) elastomers were prepared from commercially available starting reagents employing a hydrosilylation reaction. Each elastomer was designed to utilize 2,4,6‐tris(allyloxy)‐1,3,5‐triazine as a crosslinker and multifunctional vinyl component in the hydrosilylation reaction, ensuring that the triazine rings were completely formed, and thus the elastomers resemble fully cured cyanate ester networks. The hydride‐terminated siloxane components used were varied from small‐molecule siloxanes to pre‐polymers of different molecular weights. Attenuated total reflectance Fourier transform infrared analysis confirmed the successful hydrosilylation reaction and complete curing of the SiCE elastomers via functional group analysis. Thermal characterization by thermogravimetric analysis and differential scanning calorimetry demonstrated that thermal properties of the elastomers could be tailored depending on the type of siloxane component that was utilized. The gel content of the elastomers was also determined. Investigations into the effects of a platinum catalyst on the elastomers determined that the presence of the catalyst affected the thermochemical stability of the SiCE elastomers. Published 2016. This article is a U.S. Government work and is in the public domain in the USA.
“…[1][2][3][4] The physical properties and performance of siloxane-based materials depend substantially on their structures.I nt he design of siloxane-based materials on the molecular scale to the mesoscale, ab uilding-block approachu sing oligosiloxanes with specific structures exhibits potential. [5] Until now,o ligosiloxanes with linear, [6] branched, [7,8] ladder-like, [9,10] cyclic, [11][12][13][14][15][16] or cage structures [17,18] have been used as building blockst op roduce soluble polymers with organic or siloxane linkers, [11,16,19,20] three-dimensionally crosslinked microporous materials, [12,17,[21][22][23][24] ordered mesostructured materials, [6-8, 14, 18, 25, 26] and crystalline zeolitic materials. [27,28] Oligosiloxanes with polycyclic and cage structures are of particular interest because they are the basic structural units of crystalline silica materials, such as layered silicate and zeolites.…”
The controlled synthesis of oligosiloxanes with well‐defined structures is important for the bottom‐up design of siloxane‐based nanomaterials. This work reports the synthesis of various polycyclic and cage siloxanes by the hydrolysis and intramolecular condensation of monocyclic tetra‐ and hexasiloxanes functionalized with various alkoxysilyl groups. An investigation of monoalkoxysilylated cyclosiloxanes revealed that intramolecular condensation occurred preferentially between adjacent alkoxysilyl groups to form new tetrasiloxane rings. The study of dialkoxy‐ and trialkoxysilylated cyclotetrasiloxanes revealed multistep intramolecular condensation reactions to form cubic octasiloxanes in relatively high yields. Unlike conventional methods starting from organosilane monomers, intramolecular condensation enables the introduction of different organic substituents in controlled arrangements. So‐called Janus cubes have been successfully obtained, that is, Ph4R4Si8O12, in which R=Me, OSiMe3, and OSiMe2Vi (Vi=vinyl). These findings will enable the creation of siloxane‐based materials with diverse functions.
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