Controlled Mesoporosity in SiOC via Chemically Bonded Polymeric "Spacers"

Silicon oxycarbides with controlled porosity in the mesopore range have been obtained through high‐temperature pyrolysis of newly developed reactive siloxane formulations. The starting gels have been synthesized via Pt catalyzed hydrosilylation reaction between polyhydromethylsiloxane (PHMS) and vin...

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Published in	Journal of the American Ceramic Society Vol. 96; no. 9; pp. 2785 - 2792
Main Authors	Blum, Yigal, Sorarù, Gian Domenico, Ramaswamy, Aravind Parakkulam, Hui, David, Carturan, Sara Maria
Format	Journal Article
Language	English
Published	Columbus Blackwell Publishing Ltd 01.09.2013 Wiley Subscription Services, Inc
Subjects	Chemical bonds Chemically bonded Gels High temperature Hydrosilylation Molecular weight Porosity Pyrolysis Silicon Silicone resins Spacers Thermogravimetric analysis
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Abstract	Silicon oxycarbides with controlled porosity in the mesopore range have been obtained through high‐temperature pyrolysis of newly developed reactive siloxane formulations. The starting gels have been synthesized via Pt catalyzed hydrosilylation reaction between polyhydromethylsiloxane (PHMS) and vinyl‐terminated polydimethylsiloxane (PDMS) of different molecular weights in the presence of tetravinyltetramethylcyclotetrasiloxane as a crosslinking enhancer. In our approach, the PDMS serves the double purpose of size‐controlling templating agent as well as solvent at the early stages of the synthesis. During the curing step, the vinyl‐terminated PDMS is chemically bonded to the preceramic network through the extremely efficient hydrosilylation reaction and “solidify.” Accordingly, its removal during pyrolysis occurs through decomposition of a solid phase with retention of the formed porosity. The structural and morphological evolution of the preceramic gels containing the molecular spacers have been investigated as a function of the thermal treatment temperature by N2 physisorption measurements, thermogravimetry, and SEM analyses. The results show that the pore size distribution of the resulting SiOCs depends on the molecular weight of the PDMS and is directly related to the molecular volume assumimg that the PDMS chains are entangled into spheroidal shapes. The total pore volume is related to the initial amount of templating PDMS assuming its complete decomposition during pyrolysis.
AbstractList	Silicon oxycarbides with controlled porosity in the mesopore range have been obtained through high-temperature pyrolysis of newly developed reactive siloxane formulations. The starting gels have been synthesized via Pt catalyzed hydrosilylation reaction between polyhydromethylsiloxane (PHMS) and vinyl-terminated polydimethylsiloxane (PDMS) of different molecular weights in the presence of tetravinyltetramethylcyclotetrasiloxane as a crosslinking enhancer. In our approach, the PDMS serves the double purpose of size-controlling templating agent as well as solvent at the early stages of the synthesis. During the curing step, the vinyl-terminated PDMS is chemically bonded to the preceramic network through the extremely efficient hydrosilylation reaction and "solidify." Accordingly, its removal during pyrolysis occurs through decomposition of a solid phase with retention of the formed porosity. The structural and morphological evolution of the preceramic gels containing the molecular spacers have been investigated as a function of the thermal treatment temperature by N2 physisorption measurements, thermogravimetry, and SEM analyses. The results show that the pore size distribution of the resulting SiOCs depends on the molecular weight of the PDMS and is directly related to the molecular volume assumimg that the PDMS chains are entangled into spheroidal shapes. The total pore volume is related to the initial amount of templating PDMS assuming its complete decomposition during pyrolysis. [PUBLICATION ABSTRACT] Silicon oxycarbides with controlled porosity in the mesopore range have been obtained through high‐temperature pyrolysis of newly developed reactive siloxane formulations. The starting gels have been synthesized via Pt catalyzed hydrosilylation reaction between polyhydromethylsiloxane ( PHMS ) and vinyl‐terminated polydimethylsiloxane ( PDMS ) of different molecular weights in the presence of tetravinyltetramethylcyclotetrasiloxane as a crosslinking enhancer. In our approach, the PDMS serves the double purpose of size‐controlling templating agent as well as solvent at the early stages of the synthesis. During the curing step, the vinyl‐terminated PDMS is chemically bonded to the preceramic network through the extremely efficient hydrosilylation reaction and “solidify.” Accordingly, its removal during pyrolysis occurs through decomposition of a solid phase with retention of the formed porosity. The structural and morphological evolution of the preceramic gels containing the molecular spacers have been investigated as a function of the thermal treatment temperature by N 2 physisorption measurements, thermogravimetry, and SEM analyses. The results show that the pore size distribution of the resulting SiOC s depends on the molecular weight of the PDMS and is directly related to the molecular volume assumimg that the PDMS chains are entangled into spheroidal shapes. The total pore volume is related to the initial amount of templating PDMS assuming its complete decomposition during pyrolysis. Silicon oxycarbides with controlled porosity in the mesopore range have been obtained through high-temperature pyrolysis of newly developed reactive siloxane formulations. The starting gels have been synthesized via Pt catalyzed hydrosilylation reaction between polyhydromethylsiloxane (PHMS) and vinyl-terminated polydimethylsiloxane (PDMS) of different molecular weights in the presence of tetravinyltetramethylcyclotetrasiloxane as a crosslinking enhancer. In our approach, the PDMS serves the double purpose of size-controlling templating agent as well as solvent at the early stages of the synthesis. During the curing step, the vinyl-terminated PDMS is chemically bonded to the preceramic network through the extremely efficient hydrosilylation reaction and "solidify." Accordingly, its removal during pyrolysis occurs through decomposition of a solid phase with retention of the formed porosity. The structural and morphological evolution of the preceramic gels containing the molecular spacers have been investigated as a function of the thermal treatment temperature by N2 physisorption measurements, thermogravimetry, and SEM analyses. The results show that the pore size distribution of the resulting SiOCs depends on the molecular weight of the PDMS and is directly related to the molecular volume assumimg that the PDMS chains are entangled into spheroidal shapes. The total pore volume is related to the initial amount of templating PDMS assuming its complete decomposition during pyrolysis. Micro-mesoporous ceramics are used in a wide range of applications, including catalyst supports, chemical reactors, electrodes for supercapacitors, gas storage and drug delivery. Silicon oxycarbides with controlled porosity in the mesopore range were obtained through high-temperature pyrolysis of newly developed reactive siloxane formulations. The starting gels were synthesised via Pt catalysed hydrosilylation between polyhydromethylsiloxane (PHMS) and vinyl-terminated polydimethylsiloxane (PDMS) of different molecular weights in the presence of tetravinyltetramethylcyclotetrasiloxane as a crosslinking enhancer. The PDMS served the double purpose of size-controlling templating agent as well as solvent at the early stages of the synthesis. During the curing step, the vinyl-terminated PDMS was chemically bonded to the preceramic network through the extremely efficient hydrosilylation reaction and solidification. Accordingly, its removal during pyrolysis occurred through decomposition of a solid phase with retention of the formed porosity. The structural and morphological evolution of the preceramic gels containing the molecular spacers were investigated as a function of the thermal treatment temperature by N2 physisorption measurements, thermogravimetry, and SEM analyses. The results showed that the pore size distribution of the resulting SiOCs depended on the molecular weight of the PDMS and was directly related to the molecular volume, assuming that the PDMS chains were entangled into spheroidal shapes. The total pore volume was related to the initial amount of templating PDMS, assuming its complete decomposition during pyrolysis.
Author	Ramaswamy, Aravind Parakkulam Sorarù, Gian Domenico Blum, Yigal Carturan, Sara Maria Hui, David
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Snippet	Silicon oxycarbides with controlled porosity in the mesopore range have been obtained through high‐temperature pyrolysis of newly developed reactive siloxane... Silicon oxycarbides with controlled porosity in the mesopore range have been obtained through high-temperature pyrolysis of newly developed reactive siloxane... Micro-mesoporous ceramics are used in a wide range of applications, including catalyst supports, chemical reactors, electrodes for supercapacitors, gas storage...
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StartPage	2785
SubjectTerms	Chemical bonds Chemically bonded Gels High temperature Hydrosilylation Molecular weight Porosity Pyrolysis Silicon Silicone resins Spacers Thermogravimetric analysis
Title	Controlled Mesoporosity in SiOC via Chemically Bonded Polymeric "Spacers"
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