A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface

Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract Ausführliche Beschreibung

Gespeichert in:

Autor*in:	Protsak, Iryna S. [verfasserIn] Morozov, Yevhenii M. [verfasserIn] Dong, Wen [verfasserIn] Le, Zichun [verfasserIn] Zhang, Dong [verfasserIn] Henderson, Ian M. [verfasserIn]

Format:	E-Artikel
Sprache:	Englisch

Erschienen:	2019

Schlagwörter:	Silicones Dialkyl carbonates H solid-state NMR spectroscopy Si solid-state NMR spectroscopy C solid-state NMR spectroscopy Surface modification Fumed nanosilica Bonding density

Übergeordnetes Werk:	Enthalten in: Nanoscale research letters - New York, NY [u.a.] : Springer, 2006, 14(2019), 1 vom: 14. Mai
Übergeordnetes Werk:	volume:14 ; year:2019 ; number:1 ; day:14 ; month:05

Links:	Volltext

DOI / URN:	10.1186/s11671-019-2982-2

Katalog-ID:	SPR022119558

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520			\|a Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract
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700	1		\|a Zhang, Dong \|e verfasserin \|4 aut
700	1		\|a Henderson, Ian M. \|e verfasserin \|4 aut
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allfields	10.1186/s11671-019-2982-2 doi (DE-627)SPR022119558 (SPR)s11671-019-2982-2-e DE-627 ger DE-627 rakwb eng 600 ASE Protsak, Iryna S. verfasserin aut A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface 2019 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract Silicones (dpeaa)DE-He213 Dialkyl carbonates (dpeaa)DE-He213 H solid-state NMR spectroscopy (dpeaa)DE-He213 Si solid-state NMR spectroscopy (dpeaa)DE-He213 C solid-state NMR spectroscopy (dpeaa)DE-He213 Surface modification (dpeaa)DE-He213 Fumed nanosilica (dpeaa)DE-He213 Bonding density (dpeaa)DE-He213 Morozov, Yevhenii M. verfasserin aut Dong, Wen verfasserin aut Le, Zichun verfasserin aut Zhang, Dong verfasserin aut Henderson, Ian M. verfasserin aut Enthalten in Nanoscale research letters New York, NY [u.a.] : Springer, 2006 14(2019), 1 vom: 14. Mai (DE-627)518632474 (DE-600)2253244-4 1556-276X nnns volume:14 year:2019 number:1 day:14 month:05 https://dx.doi.org/10.1186/s11671-019-2982-2 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_95 GBV_ILN_105 GBV_ILN_110 GBV_ILN_151 GBV_ILN_161 GBV_ILN_170 GBV_ILN_213 GBV_ILN_230 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_2014 GBV_ILN_2027 GBV_ILN_2055 GBV_ILN_4012 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4249 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4335 GBV_ILN_4338 GBV_ILN_4367 GBV_ILN_4700 AR 14 2019 1 14 05
spelling	10.1186/s11671-019-2982-2 doi (DE-627)SPR022119558 (SPR)s11671-019-2982-2-e DE-627 ger DE-627 rakwb eng 600 ASE Protsak, Iryna S. verfasserin aut A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface 2019 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract Silicones (dpeaa)DE-He213 Dialkyl carbonates (dpeaa)DE-He213 H solid-state NMR spectroscopy (dpeaa)DE-He213 Si solid-state NMR spectroscopy (dpeaa)DE-He213 C solid-state NMR spectroscopy (dpeaa)DE-He213 Surface modification (dpeaa)DE-He213 Fumed nanosilica (dpeaa)DE-He213 Bonding density (dpeaa)DE-He213 Morozov, Yevhenii M. verfasserin aut Dong, Wen verfasserin aut Le, Zichun verfasserin aut Zhang, Dong verfasserin aut Henderson, Ian M. verfasserin aut Enthalten in Nanoscale research letters New York, NY [u.a.] : Springer, 2006 14(2019), 1 vom: 14. Mai (DE-627)518632474 (DE-600)2253244-4 1556-276X nnns volume:14 year:2019 number:1 day:14 month:05 https://dx.doi.org/10.1186/s11671-019-2982-2 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_95 GBV_ILN_105 GBV_ILN_110 GBV_ILN_151 GBV_ILN_161 GBV_ILN_170 GBV_ILN_213 GBV_ILN_230 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_2014 GBV_ILN_2027 GBV_ILN_2055 GBV_ILN_4012 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4249 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4335 GBV_ILN_4338 GBV_ILN_4367 GBV_ILN_4700 AR 14 2019 1 14 05
allfields_unstemmed	10.1186/s11671-019-2982-2 doi (DE-627)SPR022119558 (SPR)s11671-019-2982-2-e DE-627 ger DE-627 rakwb eng 600 ASE Protsak, Iryna S. verfasserin aut A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface 2019 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract Silicones (dpeaa)DE-He213 Dialkyl carbonates (dpeaa)DE-He213 H solid-state NMR spectroscopy (dpeaa)DE-He213 Si solid-state NMR spectroscopy (dpeaa)DE-He213 C solid-state NMR spectroscopy (dpeaa)DE-He213 Surface modification (dpeaa)DE-He213 Fumed nanosilica (dpeaa)DE-He213 Bonding density (dpeaa)DE-He213 Morozov, Yevhenii M. verfasserin aut Dong, Wen verfasserin aut Le, Zichun verfasserin aut Zhang, Dong verfasserin aut Henderson, Ian M. verfasserin aut Enthalten in Nanoscale research letters New York, NY [u.a.] : Springer, 2006 14(2019), 1 vom: 14. Mai (DE-627)518632474 (DE-600)2253244-4 1556-276X nnns volume:14 year:2019 number:1 day:14 month:05 https://dx.doi.org/10.1186/s11671-019-2982-2 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_95 GBV_ILN_105 GBV_ILN_110 GBV_ILN_151 GBV_ILN_161 GBV_ILN_170 GBV_ILN_213 GBV_ILN_230 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_2014 GBV_ILN_2027 GBV_ILN_2055 GBV_ILN_4012 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4249 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4335 GBV_ILN_4338 GBV_ILN_4367 GBV_ILN_4700 AR 14 2019 1 14 05
allfieldsGer	10.1186/s11671-019-2982-2 doi (DE-627)SPR022119558 (SPR)s11671-019-2982-2-e DE-627 ger DE-627 rakwb eng 600 ASE Protsak, Iryna S. verfasserin aut A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface 2019 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract Silicones (dpeaa)DE-He213 Dialkyl carbonates (dpeaa)DE-He213 H solid-state NMR spectroscopy (dpeaa)DE-He213 Si solid-state NMR spectroscopy (dpeaa)DE-He213 C solid-state NMR spectroscopy (dpeaa)DE-He213 Surface modification (dpeaa)DE-He213 Fumed nanosilica (dpeaa)DE-He213 Bonding density (dpeaa)DE-He213 Morozov, Yevhenii M. verfasserin aut Dong, Wen verfasserin aut Le, Zichun verfasserin aut Zhang, Dong verfasserin aut Henderson, Ian M. verfasserin aut Enthalten in Nanoscale research letters New York, NY [u.a.] : Springer, 2006 14(2019), 1 vom: 14. Mai (DE-627)518632474 (DE-600)2253244-4 1556-276X nnns volume:14 year:2019 number:1 day:14 month:05 https://dx.doi.org/10.1186/s11671-019-2982-2 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_95 GBV_ILN_105 GBV_ILN_110 GBV_ILN_151 GBV_ILN_161 GBV_ILN_170 GBV_ILN_213 GBV_ILN_230 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_2014 GBV_ILN_2027 GBV_ILN_2055 GBV_ILN_4012 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4249 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4335 GBV_ILN_4338 GBV_ILN_4367 GBV_ILN_4700 AR 14 2019 1 14 05
allfieldsSound	10.1186/s11671-019-2982-2 doi (DE-627)SPR022119558 (SPR)s11671-019-2982-2-e DE-627 ger DE-627 rakwb eng 600 ASE Protsak, Iryna S. verfasserin aut A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface 2019 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract Silicones (dpeaa)DE-He213 Dialkyl carbonates (dpeaa)DE-He213 H solid-state NMR spectroscopy (dpeaa)DE-He213 Si solid-state NMR spectroscopy (dpeaa)DE-He213 C solid-state NMR spectroscopy (dpeaa)DE-He213 Surface modification (dpeaa)DE-He213 Fumed nanosilica (dpeaa)DE-He213 Bonding density (dpeaa)DE-He213 Morozov, Yevhenii M. verfasserin aut Dong, Wen verfasserin aut Le, Zichun verfasserin aut Zhang, Dong verfasserin aut Henderson, Ian M. verfasserin aut Enthalten in Nanoscale research letters New York, NY [u.a.] : Springer, 2006 14(2019), 1 vom: 14. Mai (DE-627)518632474 (DE-600)2253244-4 1556-276X nnns volume:14 year:2019 number:1 day:14 month:05 https://dx.doi.org/10.1186/s11671-019-2982-2 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_95 GBV_ILN_105 GBV_ILN_110 GBV_ILN_151 GBV_ILN_161 GBV_ILN_170 GBV_ILN_213 GBV_ILN_230 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_2014 GBV_ILN_2027 GBV_ILN_2055 GBV_ILN_4012 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4249 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4335 GBV_ILN_4338 GBV_ILN_4367 GBV_ILN_4700 AR 14 2019 1 14 05
language	English
source	Enthalten in Nanoscale research letters 14(2019), 1 vom: 14. Mai volume:14 year:2019 number:1 day:14 month:05
sourceStr	Enthalten in Nanoscale research letters 14(2019), 1 vom: 14. Mai volume:14 year:2019 number:1 day:14 month:05
format_phy_str_mv	Article
institution	findex.gbv.de
topic_facet	Silicones Dialkyl carbonates H solid-state NMR spectroscopy Si solid-state NMR spectroscopy C solid-state NMR spectroscopy Surface modification Fumed nanosilica Bonding density
dewey-raw	600
isfreeaccess_bool	true
container_title	Nanoscale research letters
authorswithroles_txt_mv	Protsak, Iryna S. @@aut@@ Morozov, Yevhenii M. @@aut@@ Dong, Wen @@aut@@ Le, Zichun @@aut@@ Zhang, Dong @@aut@@ Henderson, Ian M. @@aut@@
publishDateDaySort_date	2019-05-14T00:00:00Z
hierarchy_top_id	518632474
dewey-sort	3600
id	SPR022119558
language_de	englisch
fullrecord	<?xml version="1.0" encoding="UTF-8"?><collection xmlns="http://www.loc.gov/MARC21/slim"><record><leader>01000caa a22002652 4500</leader><controlfield tag="001">SPR022119558</controlfield><controlfield tag="003">DE-627</controlfield><controlfield tag="005">20220111084949.0</controlfield><controlfield tag="007">cr uuu---uuuuu</controlfield><controlfield tag="008">201006s2019 xx \|\|\|\|\|o 00\| \|\|eng c</controlfield><datafield tag="024" ind1="7" ind2=" "><subfield code="a">10.1186/s11671-019-2982-2</subfield><subfield code="2">doi</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(DE-627)SPR022119558</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(SPR)s11671-019-2982-2-e</subfield></datafield><datafield tag="040" ind1=" " ind2=" "><subfield code="a">DE-627</subfield><subfield code="b">ger</subfield><subfield code="c">DE-627</subfield><subfield code="e">rakwb</subfield></datafield><datafield tag="041" ind1=" " ind2=" "><subfield code="a">eng</subfield></datafield><datafield tag="082" ind1="0" ind2="4"><subfield code="a">600</subfield><subfield code="q">ASE</subfield></datafield><datafield tag="100" ind1="1" ind2=" "><subfield code="a">Protsak, Iryna S.</subfield><subfield code="e">verfasserin</subfield><subfield code="4">aut</subfield></datafield><datafield tag="245" ind1="1" ind2="2"><subfield code="a">A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface</subfield></datafield><datafield tag="264" ind1=" " ind2="1"><subfield code="c">2019</subfield></datafield><datafield tag="336" ind1=" " ind2=" "><subfield code="a">Text</subfield><subfield code="b">txt</subfield><subfield code="2">rdacontent</subfield></datafield><datafield tag="337" ind1=" " ind2=" "><subfield code="a">Computermedien</subfield><subfield code="b">c</subfield><subfield code="2">rdamedia</subfield></datafield><datafield tag="338" ind1=" " ind2=" "><subfield code="a">Online-Ressource</subfield><subfield code="b">cr</subfield><subfield code="2">rdacarrier</subfield></datafield><datafield tag="520" ind1=" " ind2=" "><subfield code="a">Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. 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author	Protsak, Iryna S.
spellingShingle	Protsak, Iryna S. ddc 600 misc Silicones misc Dialkyl carbonates misc H solid-state NMR spectroscopy misc Si solid-state NMR spectroscopy misc C solid-state NMR spectroscopy misc Surface modification misc Fumed nanosilica misc Bonding density A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface
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topic_title	600 ASE A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface Silicones (dpeaa)DE-He213 Dialkyl carbonates (dpeaa)DE-He213 H solid-state NMR spectroscopy (dpeaa)DE-He213 Si solid-state NMR spectroscopy (dpeaa)DE-He213 C solid-state NMR spectroscopy (dpeaa)DE-He213 Surface modification (dpeaa)DE-He213 Fumed nanosilica (dpeaa)DE-He213 Bonding density (dpeaa)DE-He213
topic	ddc 600 misc Silicones misc Dialkyl carbonates misc H solid-state NMR spectroscopy misc Si solid-state NMR spectroscopy misc C solid-state NMR spectroscopy misc Surface modification misc Fumed nanosilica misc Bonding density
topic_unstemmed	ddc 600 misc Silicones misc Dialkyl carbonates misc H solid-state NMR spectroscopy misc Si solid-state NMR spectroscopy misc C solid-state NMR spectroscopy misc Surface modification misc Fumed nanosilica misc Bonding density
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title	A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface
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title_full	A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface
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author_browse	Protsak, Iryna S. Morozov, Yevhenii M. Dong, Wen Le, Zichun Zhang, Dong Henderson, Ian M.
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author-letter	Protsak, Iryna S.
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title_sort	29si, 1h, and 13c solid-state nmr study on the surface species of various depolymerized organosiloxanes at silica surface
title_auth	A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface
abstract	Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract
abstractGer	Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract
abstract_unstemmed	Abstract Three poly(organosiloxanes) (hydromethyl-, dimethyl-, and epoxymethylsiloxane) of different chain lengths and pendant groups and their mixtures of dimethyl (DMC) or diethyl carbonates (DEC) were applied in the modification of fumed silica nanoparticles (FSNs). The resulting modified silicas were studied in depth using 29Si, 1H, and 13C solid-state NMR spectroscopy, elemental analysis, and nitrogen adsorption-desorption (BET) analysis. The obtained results reveal that the type of grafting, grafting density, and structure of the grafted species at the silica surface depend strongly on the length of organosiloxane polymer and on the nature of the “green” additive, DMC or DEC. The spectral changes observed by solid-state NMR spectroscopy suggest that the major products of the reaction of various organosiloxanes and their DMC or DEC mixtures with the surface are D (RR’Si($ O_{0.5} $)2) and T (RSi($ O_{0.5} $)3) organosiloxane units. It was found that shorter methylhydro (PMHS) and dimethylsiloxane (PDMS) and their mixtures with DMC or DEC form a denser coverage at the silica surface since SBET diminution is larger and grafting density is higher than the longest epoxymethylsiloxane (CPDMS) used for FSNs modification. Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. Graphical abstract
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title_short	A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface
url	https://dx.doi.org/10.1186/s11671-019-2982-2
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author2	Morozov, Yevhenii M. Dong, Wen Le, Zichun Zhang, Dong Henderson, Ian M.
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Additionally, for FSNs modified with short organosiloxane PMHS/DEC and also medium organosiloxane PDMS/DMC, the dense coverage formation is accompanied by a greater reduction of isolated silanols, as shown by solid-state 29Si NMR spectroscopy, in contrast to reactions with neat organosiloxanes. The surface coverage at FSNs with the longest siloxane (CPDMS) greatly improves with the addition of DMC or DEC. The data on grafting density suggest that molecules in the attached layers of FSNs modified with short PMHS and its mixture of DMC or DEC and medium PDMS and its mixture of DMC form a “vertical” orientation of the grafted methylhydrosiloxane and dimethylsiloxane chains, in contrast to the reaction with PDMS/DEC and epoxide methylsiloxane in the presence of DMC or DEC, which indicates a “horizontal” chain orientation of the grafted methyl and epoxysiloxane molecules. This study highlights the major role of solid-state NMR spectroscopy for comprehensive characterization of solid surfaces. 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A 29Si, 1H, and 13C Solid-State NMR Study on the Surface Species of Various Depolymerized Organosiloxanes at Silica Surface

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