Microwave-Assisted Synthesis of Functional Polysilanes

Simionescu, Mihaela; Săcărescu, Liviu; Săcărescu, Gabriela

doi:10.1163/156855511x615010

Cited by 8 publications

(4 citation statements)

References 27 publications

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“…Changes in the reducing metal have also been studied, with interest in NaK alloys stabilized with crown ethers. These systems are soluble in THF and therefore provide a homogeneous platform instead of ultrasound, resulting in monomodal polymers with low dispersity (≈ 1.2) …”

Section: Chemistry and Synthesismentioning

confidence: 99%

“…These systems are soluble in THF and therefore provide a homogeneous platform instead of ultrasound, resulting in monomodal polymers with low dispersity (≈ 1.2). 141 Microwave-assisted Wurtz coupling represents a significant improvement and has been employed to synthesize polymethylphenylsilane with great success. Direct heating of the neat monomer melts the sodium, enabling rapid reaction times (∼3 min).…”

Section: Chemistry and Synthesismentioning

confidence: 99%

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Advances in the Synthesis of Preceramic Polymers for the Formation of Silicon-Based and Ultrahigh-Temperature Non-Oxide Ceramics

et al. 2023

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Preceramic polymers (PCPs) are a group of specialty macromolecules that serve as precursors for generating inorganics, including ceramic carbides, nitrides, and borides. PCPs represent interesting synthetic challenges for chemists due to the elements incorporated into their structure. This group of polymers is also of interest to engineers as PCPs enable the processing of polymer-derived ceramic products including high-performance ceramic fibers and composites. These finished ceramic materials are of growing significance for applications that experience extreme operating environments (e.g., aerospace propulsion and high-speed atmospheric flight). This Review provides an overview of advances in the synthesis and postpolymerization modification of macromolecules forming nonoxide ceramics. These PCPs include polycarbosilanes, polysilanes, polysilazanes, and precursors for ultrahigh-temperature ceramics. Following our review of PCP synthetic chemistry, we provide examples of the application and processing of these polymers, including their use in fiber spinning, composite fabrication, and additive manufacturing. The principal objective of this Review is to provide a resource that bridges the disciplines of synthetic chemistry and ceramic engineering while providing both insights and inspiration for future collaborative work that will ultimately drive the PCP field forward.

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Section: Chemistry and Synthesismentioning

confidence: 99%

Section: Chemistry and Synthesismentioning

confidence: 99%

Advances in the Synthesis of Preceramic Polymers for the Formation of Silicon-Based and Ultrahigh-Temperature Non-Oxide Ceramics

et al. 2023

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“…We are not the first to exploit this Si–H activation route to modified polysilanes, and Si–Ph cleavage strategies have also been reported . However, the parent polysilanes are notoriously sensitive to Si–Si bond cleavage under most conditions of modification, which can lead to reduced molecular weights (MWs) . For example, we found that previously reported radical, − titanocene, , and platinic acid mediated Si–H activation methods gave moderate to significant Si–Si bond scission at poly(phenylsilane) (H–[Si(H)Ph] n –H) and even at more robust 1,2-dihydrodisilanes such as sym -tetraphenyldisilane. , However, we have found that hydrosilation and heterodehydrocoupling reactions of disilanes mediated by B(C 6 F 5 ) 3 proceed under mild conditions with absolute chemoselectivity for Si–H versus Si–Si activation to give new Si–O- and Si–S-containing substituents. , In this communication we report the successful extension of this methodology to chemoselective postpolymerization modification of poly(phenylsilane) to introduce thiolato side chains.…”

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confidence: 99%

Borane-Catalyzed Si–H Activation Routes to Polysilanes Containing Thiolato Side Chains

2013

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Dehydrocoupling and hydrosilation reactions of the Si−H bonds in poly(phenylsilane) catalyzed by B(C 6 F 5 ) 3 allow the preparation of new polymers containing both Si−H and Si−SR side chains. This postpolymerization modification takes place without any observable competing Si−Si bond cleavage, unlike other Lewis acid, transition-metal, or radical mediated routes. The −SR-functionalized polymers have been characterized by GPC, IR, UV−vis, elemental analysis, and 1 H, 13 C, and 29 Si NMR.

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“…Poly [diphenyl-co-methyl(H)]silane was obtained following the Wurtz reductive coupling method, using methyl(H)dichlorosilane and diphenyldichlorosilane as reagents. The preparation process has been described in detail in two previous papers [ 21 , 60 ]. The molar ratio C 6 H 5 Si/CH 3 (H)Si groups Mr = 7/1 ensure polysilane functionality, along with very good solubility in the usual organic solvents (toluene, THF, dichloromethane, etc.…”

Section: Methodsmentioning

confidence: 99%

Cobalt Ferrite Particles Produced by Sol-Gel Autocombustion and Embedded in Polysilane: An Innovative Route to Magnetically-Induced Fluorescence Composites

Samoilă¹,

Cojocaru²,

Simionescu³

et al. 2022

Molecules

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Fluorescence detection is currently one of the commonly used techniques worldwide. Through this work, the preparation and optical properties of an interesting composite material are discussed. It is shown that encapsulating cobalt spinel ferrite (CoFe2O4), obtained by the sol-gel autocombustion method, into poly[diphenyl-co-methyl(H)]silane matrix leads to fluoromagnetic particles (PSCo) with intriguing optical properties. Transmission electron microscopy, combined with energy-dispersive X-ray analysis, showed 500 nm large spherical structures containing a core (around 400 nm in diameter) composed of magnetic ferrite particles, surrounded by a thin layer of semiconductive fluorescent polymer. The as-obtained material exhibited ferrimagnetic properties. The FTIR spectrum confirmed that the Si-H functionality of the polysilane was preserved. UV spectroscopy combined with molecular modeling studies indicated that the magnetic core had a strong influence on the intramolecular electron transitions characteristic of the σ-conjugated polysilane. Further analysis by steady-state fluorescence spectroscopy revealed that the internal magnetic field strongly enhances the polysilane emission. This property will be further investigated in the future in order to develop new detection devices.

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Microwave-Assisted Synthesis of Functional Polysilanes

Cited by 8 publications

References 27 publications

Advances in the Synthesis of Preceramic Polymers for the Formation of Silicon-Based and Ultrahigh-Temperature Non-Oxide Ceramics

Advances in the Synthesis of Preceramic Polymers for the Formation of Silicon-Based and Ultrahigh-Temperature Non-Oxide Ceramics

Borane-Catalyzed Si–H Activation Routes to Polysilanes Containing Thiolato Side Chains

Cobalt Ferrite Particles Produced by Sol-Gel Autocombustion and Embedded in Polysilane: An Innovative Route to Magnetically-Induced Fluorescence Composites

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