Activation of the Si–H bond of Et2SiH2 in photochemical reaction with W(CO)6: Spectroscopic characterization of intermediate W–Si compounds and the revisited crystal structure of the bis{(μ-η2-hydridodiethylsilyl)tetracarbonyltungsten(I)} complex [{W(μ-η2-H–SiEt2)(CO)4}2]

Gądek, Agnieszka; Kochel, Andrzej; Szymańska-Buzar, Teresa

doi:10.1016/j.jorganchem.2007.05.027

Cited by 16 publications

(10 citation statements)

References 49 publications

(118 reference statements)

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“…Such two reactions create new covalent bonds between the carbon atoms in PDMS and the oxygen atoms on RGO, thus greatly strengthening the interface and 131 improving the mechanical properties of the nano-carbon composites. These formations have also been shown in past work with photon-assisted [248][249][250]. Further, the XPS studies show direct correlation between bond formation and overall improvement in mechanical properties such as Young's modulus, strain energy density, toughness, and load transfer.…”

Section: Resultssupporting

confidence: 76%

Near infrared photon-assisted polymerization of advanced polymer composites.

Xu¹

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This dissertation describes a novel method to develop polymer composites using near infrared (NIR) photon-assisted polymerization and nanoscale reinforcement. We used multi-walled carbon nanotubes (MWNTs), reduced graphene oxide (RGO), and graphene nanoplatelets (GNPs) to make polymer composites, and explored in-situ NIR photon assisted heating of these nano carbons to enhance polymerization of the nanocarbon/polymer interface, thus achieving significant load transfer and improved vii mechanical properties. To specify, nano-carbon was dispersed into the polymer matrix by shear or evaporation mixing method to attain a uniform distribution in the prepared thin film composite. The thin film was exposed to NIR light during polymerization instead of conventional oven based heating. NIR was effectively absorbed by nano-carbons and also atoms from polymer molecule; the induced photo-thermal heat was transferred into the polymer matrix to induce polymerization of the composite and the covalent bonding between nano-carbons and polymer matrix at the interface. Scanning electron microscope (SEM), Raman spectroscopy, and RSA were used to evaluate the load transfer and mechanical strength of the polymerized composite samples. Investigating first the nanotube/polymer composites synergized by NIR photon-assisted polymerization, largeRaman shifts (20 cm -1 wavenumber for up to 80% strains) of the 2D band were recorded for the NIR light polymerized samples and an increase in Young's modulus by ~130%was measured for the 1 wt. MWNT/poly(dimethylsiloxane) (PDMS) composites. While at first it was thought that NIR radiation during polymerization heated the nano-carbons inside resulting in strengthening of the nano-carbon/polymer interface, it was seen after further experimentation with graphene reinforcements that other light induced bonding effects apart from heat were also responsible.Raman spectroscopy revealed that mixing graphene in polymer has a profound As a demonstration of applications, PDMS/RGO/PDMS sandwiched structure strain sensor, a demo application of the NIR photon-assisted polymerization was investigated. High sensitivity and high Gauge Factor (GF) are addressed. These results shown in this dissertation suggest that the NIR photon-assisted polymerization can be practically developed as a scalable nanomanufacturing technique to create large panels of advanced composites with strong interface and better mechanical properties compared to conventional oven based heating methods. It also suggests that it is possible to fabricate large-scale flexible smart device like high sensitivity strain sensors.xi

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Section: Resultssupporting

confidence: 76%

Near infrared photon-assisted polymerization of advanced polymer composites.

Xu¹

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“…The latter process is catalyzed by transition metal complexes, which are able to activate the H Si bond of silane and coordinate the organic substrate. The formation of 2 -silane complexes with photochemically generated M(CO) 5 moieties (M = Cr, Mo, W) has recently been observed by spectroscopic methods (IR, NMR) [75][76][77]. Similar 2 -silane complexes have been detected in photochemical reactions of [Mo(CO) 4 (nbd)] and Et 2 SiH 2 or Ph 2 SiH 2 [78].…”

Section: Hydrosilylation Of Alkenesmentioning

confidence: 74%

“…Carbonyl complexes of molybdenum are of great utility owing to their applications as precursors for the generation of true catalysts for such reactions as metathesis , metathesis polymerization and oligomerization [39][40][41][42][43][44][45][46][47][48][49][50][51][52][53][54][55][56], radical reactions [57][58][59][60][61][62][63][64][65], hydrogenation [66][67][68][69][70][71][72][73][74], hydrosilylation [75][76][77][78][79], hydrogermylation [80,81], hydrostannation [82][83][84][85][86][87]…”

Section: Introductionmentioning

confidence: 99%

“…In that way the coordinated alkene or alkyne can be transformed to a carbene ligand [8-25, 45, 46, 50]. The activation of a -bond (H H, H C, H Si, H Ge, H Sn) of a substrate such as dihydrogen [66][67][68][69], silane [75][76][77][78], germane [80][81], stannane [82], or aromatic hydrocarbon molecules is a key step in the catalytic transformation of such molecules. Recent investigations of molybdenum carbonyl complexes have revealed novel types of their reactivity toward unsaturated organic compounds, e.g.…”

Section: Introductionmentioning

confidence: 99%

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Carbonyl Complexes of Molybdenum and their Catalytic Activity

Szymańska-Buzar

2012

COC

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This is a review of the published papers that focus on the reactivity of carbonyl complexes of molybdenum in low oxidation states (usually zero or two) and possible applications of molybdenum complexes as precursors of catalysts in different reactions of unsaturated organic substrates such as alkenes and alkynes. The following reactions are analyzed: metathesis, metathesis polymerization, free radical reactions of alkenes, hydrogenation, hydrosilylation, hydrogermylation, hydrostannation, hydroarylation, asymmetric allylic alkylation, and epoxidation. In addition to the interesting practical aspects of these catalytic reactions, they provide additional insights into molybdenum chemistry.

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“…The problem of the activation of σ-bonds such as H−H, H−C, H−Si, and H−Ge is still an important research area. − Interest in the process of activation of the H−Ge bond of germanes by transition metals has been growing over the past decade due to its significance for the catalytic process known as hydrogermylation. − Recently we have found that photochemically activated Mo(CO) 6 and the norbornadiene (nbd) complex [Mo(CO) 4 (η 4 -nbd)] effectively initiate the hydrogermylation of norbornadiene by Et 3 GeH, which leads to the formation of triethylgermylnorbornene . In this paper, we present studies of the activation of the H−Ge bond of diethylgermane using photochemically activated Mo(CO) 6 .…”

Section: Introductionmentioning

confidence: 99%

Photochemical Reaction of Mo(CO)₆ with Et₂GeH₂: NMR and DFT Studies of Reaction Products; Crystal Structure of a Novel Complex [{Mo(μ-η²-H−GeEt₂)(CO)₄}₂]

et al. 2009

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The photochemical reaction of Mo(CO) 6 with the diethylgermane Et 2 GeH 2 leads to the formation of several new complexes, which were detected by IR and 1 H and 13 C NMR spectroscopy. From the mixture of compounds, a binuclear complex, [{Mo(μ-η 2 -H-GeEt 2 )(CO) 4 } 2 ], was isolated in crystalline form, and its molecular structure was established by single-crystal X-ray diffraction studies. The agostic hydride ligand of the Mo( μ-η 2 -H-GeEt 2 ) group was located in the structure at a chemically reasonable position between the Mo and Ge atoms of the Mo-Ge bond of the bridging germyl ligand, and its presence was confirmed by 1 H NMR spectroscopy due to a proton resonance at δ = -7.86. Two dihydride complexes were identified by 1 H and 13 C NMR spectroscopy, due to their differing thermal behavior. A DFT study of the structural properties of possible reaction products was performed.

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Activation of the Si–H bond of Et2SiH2 in photochemical reaction with W(CO)6: Spectroscopic characterization of intermediate W–Si compounds and the revisited crystal structure of the bis{(μ-η2-hydridodiethylsilyl)tetracarbonyltungsten(I)} complex [{W(μ-η2-H–SiEt2)(CO)4}2]

Cited by 16 publications

References 49 publications

Near infrared photon-assisted polymerization of advanced polymer composites.

Near infrared photon-assisted polymerization of advanced polymer composites.

Carbonyl Complexes of Molybdenum and their Catalytic Activity

Photochemical Reaction of Mo(CO)₆ with Et₂GeH₂: NMR and DFT Studies of Reaction Products; Crystal Structure of a Novel Complex [{Mo(μ-η²-H−GeEt₂)(CO)₄}₂]

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Activation of the Si–H bond of Et2SiH2 in photochemical reaction with W(CO)6: Spectroscopic characterization of intermediate W–Si compounds and the revisited crystal structure of the bis{(μ-η2-hydridodiethylsilyl)tetracarbonyltungsten(I)} complex [{W(μ-η2-H–SiEt2)(CO)4}2]

Cited by 16 publications

References 49 publications

Near infrared photon-assisted polymerization of advanced polymer composites.

Near infrared photon-assisted polymerization of advanced polymer composites.

Carbonyl Complexes of Molybdenum and their Catalytic Activity

Photochemical Reaction of Mo(CO)6 with Et2GeH2: NMR and DFT Studies of Reaction Products; Crystal Structure of a Novel Complex [{Mo(μ-η2-H−GeEt2)(CO)4}2]

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Photochemical Reaction of Mo(CO)₆ with Et₂GeH₂: NMR and DFT Studies of Reaction Products; Crystal Structure of a Novel Complex [{Mo(μ-η²-H−GeEt₂)(CO)₄}₂]