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J M Chezeau - One of the best experts on this subject based on the ideXlab platform.
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high resolution solid state nmr investigation of the filler Rubber Interaction part iii investigation on the structure and formation mechanism of carbon gel in the carbon black filled styrene butadiene Rubber
Rubber Chemistry and Technology, 2001Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This investigation describes the elastomer—filler Interaction and its formation mechanism using solid state high-resolution, high-speed 1H magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. Pulsed NMR measurements were carried out on pure styrene-butadiene Rubber (SBR), and solvent extracted carbon gels from freshly prepared and storage matured master batches. The effects of filler loading, storage maturation, severity of extraction and experimental temperature on the elastomer-filler Interaction were examined and discussed. High resolution in NMR was achieved by higher temperature/low spinning rate, room temperature/high spinning and combined rotation and multiple-pulse spectroscopy (CRAMPS) techniques. High-speed magic-angle spinning (MAS) was found to be the most suitable method to achieve high resolution. Proton spin—spin relaxation time, T2, was measured successfully for each of the principal resonance species present in the samples. These measurements reveal an insight into...
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high resolution solid state nmr investigation of the filler Rubber Interaction 2 high speed 1h magic angle spinning nmr spectroscopy in carbon black filled polybutadiene
Polymer International, 2001Co-Authors: Rachel Mansencal, Bassel Haidar, Alain Vidal, L Delmotte, J M ChezeauAbstract:This work investigates the behaviour of elastomeric chains (polybutadienes of identical molecular weight but different microstructures) in the close vicinity of carbon black surfaces in order to attain a better understanding of the structure and properties of interphases. Elastomer–filler Interactions are assessed through the study of the thermal properties and NMR relaxation characteristics of the corresponding materials. Three series of samples were compared: pure polymers, raw polymer–filler blends (filler loading ratio: 50 phr) and solvent-extracted blends (so as to get rid of any polymer which is not under the influence of the solid surface). While differential scanning calorimetry points to the existence of an elastomer fraction which is not detected as undergoing the glass transition, ie is strongly immobilized, [1H] high-resolution high-speed magic-angle spinning solid-state NMR provides information on the effect exerted by polymer–filler Interactions on the mobility of the various constitutive species of the macromolecular backbone. A systematic study of the evolution of the spectral lines yielded by the samples indicates that 1,2-polybutadiene moieties have a particular affinity towards the carbon black surface which suggests the occurrence of specific Interactions at the elastomer–filler interface. © 2001 Society of Chemical Industry
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high resolution solid state n m r investigation of the filler Rubber Interaction 1 high speed 1h magic angle spinning n m r spectroscopy in carbon black filled styrene butadiene Rubber
Polymer, 1994Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This present work, dealing with filler/Rubber Interactions, provides a new approach for investigating the behaviour of elastomeric chains (styrene-butadiene Rubber, SBR) in the close vicinity of carbon black surfaces. Pulsed nuclear magnetic resonance measurements have been carried out on pure SBR, and on carbon gels obtained by solvent extraction of the carbon black filled elastomers. The initial concentration of carbon black in the filler/Rubber mixtures was varied between 20 and 100 parts per hundred parts by weight (phr). The high resolution proton spin-spin relaxation time, T 2 , has been measured for each of the individual resonance species belonging to the SBR chain. High resolution was achieved by rapidly spinning the sample at the magic angle. It has been observed that a very high magic-angle spinning (MAS) rate (> 18 kHz) is necessary to achieve a fully resolved spectrum of SBR. However, at a spinning rate of ∼ 15 kHz it is possible to avoid all of the spinning side bands and to deconvolute, unambiguously, the different resonance peaks that are present in the spectrum. In the unfilled elastomer, at temperatures much higher than the T g , the chain segmental motions are anisotropic and deviate from true liquid-like behaviour. The adsorbed Rubber chains are found to consist of loosely and tightly immobilized segments. The relative immobilization of the different protons has evidenced the methine 1 H to be much more immobilized than the aromatic or methylene species. Therefore, the olefinic part of the butadiene segment of the elastomeric chain appears to be the most affected by the carbon black surface. Moreover, T 2 is found to be independent of the filler concentration in the 30–80 phr range, and the relative concentration of the tightly bound Rubber in the composite shows a maximum at a filler content of ∼ 50 phr, where maximum reinforcement is normally observed. As far as the molecular dynamics is concerned, highly filled systems (> 80 phr carbon black) behave differently from low and medium filled systems (
Bassel Haidar - One of the best experts on this subject based on the ideXlab platform.
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high resolution solid state nmr investigation of the filler Rubber Interaction part iii investigation on the structure and formation mechanism of carbon gel in the carbon black filled styrene butadiene Rubber
Rubber Chemistry and Technology, 2001Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This investigation describes the elastomer—filler Interaction and its formation mechanism using solid state high-resolution, high-speed 1H magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. Pulsed NMR measurements were carried out on pure styrene-butadiene Rubber (SBR), and solvent extracted carbon gels from freshly prepared and storage matured master batches. The effects of filler loading, storage maturation, severity of extraction and experimental temperature on the elastomer-filler Interaction were examined and discussed. High resolution in NMR was achieved by higher temperature/low spinning rate, room temperature/high spinning and combined rotation and multiple-pulse spectroscopy (CRAMPS) techniques. High-speed magic-angle spinning (MAS) was found to be the most suitable method to achieve high resolution. Proton spin—spin relaxation time, T2, was measured successfully for each of the principal resonance species present in the samples. These measurements reveal an insight into...
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high resolution solid state nmr investigation of the filler Rubber Interaction 2 high speed 1h magic angle spinning nmr spectroscopy in carbon black filled polybutadiene
Polymer International, 2001Co-Authors: Rachel Mansencal, Bassel Haidar, Alain Vidal, L Delmotte, J M ChezeauAbstract:This work investigates the behaviour of elastomeric chains (polybutadienes of identical molecular weight but different microstructures) in the close vicinity of carbon black surfaces in order to attain a better understanding of the structure and properties of interphases. Elastomer–filler Interactions are assessed through the study of the thermal properties and NMR relaxation characteristics of the corresponding materials. Three series of samples were compared: pure polymers, raw polymer–filler blends (filler loading ratio: 50 phr) and solvent-extracted blends (so as to get rid of any polymer which is not under the influence of the solid surface). While differential scanning calorimetry points to the existence of an elastomer fraction which is not detected as undergoing the glass transition, ie is strongly immobilized, [1H] high-resolution high-speed magic-angle spinning solid-state NMR provides information on the effect exerted by polymer–filler Interactions on the mobility of the various constitutive species of the macromolecular backbone. A systematic study of the evolution of the spectral lines yielded by the samples indicates that 1,2-polybutadiene moieties have a particular affinity towards the carbon black surface which suggests the occurrence of specific Interactions at the elastomer–filler interface. © 2001 Society of Chemical Industry
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high resolution solid state n m r investigation of the filler Rubber Interaction 1 high speed 1h magic angle spinning n m r spectroscopy in carbon black filled styrene butadiene Rubber
Polymer, 1994Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This present work, dealing with filler/Rubber Interactions, provides a new approach for investigating the behaviour of elastomeric chains (styrene-butadiene Rubber, SBR) in the close vicinity of carbon black surfaces. Pulsed nuclear magnetic resonance measurements have been carried out on pure SBR, and on carbon gels obtained by solvent extraction of the carbon black filled elastomers. The initial concentration of carbon black in the filler/Rubber mixtures was varied between 20 and 100 parts per hundred parts by weight (phr). The high resolution proton spin-spin relaxation time, T 2 , has been measured for each of the individual resonance species belonging to the SBR chain. High resolution was achieved by rapidly spinning the sample at the magic angle. It has been observed that a very high magic-angle spinning (MAS) rate (> 18 kHz) is necessary to achieve a fully resolved spectrum of SBR. However, at a spinning rate of ∼ 15 kHz it is possible to avoid all of the spinning side bands and to deconvolute, unambiguously, the different resonance peaks that are present in the spectrum. In the unfilled elastomer, at temperatures much higher than the T g , the chain segmental motions are anisotropic and deviate from true liquid-like behaviour. The adsorbed Rubber chains are found to consist of loosely and tightly immobilized segments. The relative immobilization of the different protons has evidenced the methine 1 H to be much more immobilized than the aromatic or methylene species. Therefore, the olefinic part of the butadiene segment of the elastomeric chain appears to be the most affected by the carbon black surface. Moreover, T 2 is found to be independent of the filler concentration in the 30–80 phr range, and the relative concentration of the tightly bound Rubber in the composite shows a maximum at a filler content of ∼ 50 phr, where maximum reinforcement is normally observed. As far as the molecular dynamics is concerned, highly filled systems (> 80 phr carbon black) behave differently from low and medium filled systems (
Alain Vidal - One of the best experts on this subject based on the ideXlab platform.
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high resolution solid state nmr investigation of the filler Rubber Interaction part iii investigation on the structure and formation mechanism of carbon gel in the carbon black filled styrene butadiene Rubber
Rubber Chemistry and Technology, 2001Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This investigation describes the elastomer—filler Interaction and its formation mechanism using solid state high-resolution, high-speed 1H magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. Pulsed NMR measurements were carried out on pure styrene-butadiene Rubber (SBR), and solvent extracted carbon gels from freshly prepared and storage matured master batches. The effects of filler loading, storage maturation, severity of extraction and experimental temperature on the elastomer-filler Interaction were examined and discussed. High resolution in NMR was achieved by higher temperature/low spinning rate, room temperature/high spinning and combined rotation and multiple-pulse spectroscopy (CRAMPS) techniques. High-speed magic-angle spinning (MAS) was found to be the most suitable method to achieve high resolution. Proton spin—spin relaxation time, T2, was measured successfully for each of the principal resonance species present in the samples. These measurements reveal an insight into...
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high resolution solid state nmr investigation of the filler Rubber Interaction 2 high speed 1h magic angle spinning nmr spectroscopy in carbon black filled polybutadiene
Polymer International, 2001Co-Authors: Rachel Mansencal, Bassel Haidar, Alain Vidal, L Delmotte, J M ChezeauAbstract:This work investigates the behaviour of elastomeric chains (polybutadienes of identical molecular weight but different microstructures) in the close vicinity of carbon black surfaces in order to attain a better understanding of the structure and properties of interphases. Elastomer–filler Interactions are assessed through the study of the thermal properties and NMR relaxation characteristics of the corresponding materials. Three series of samples were compared: pure polymers, raw polymer–filler blends (filler loading ratio: 50 phr) and solvent-extracted blends (so as to get rid of any polymer which is not under the influence of the solid surface). While differential scanning calorimetry points to the existence of an elastomer fraction which is not detected as undergoing the glass transition, ie is strongly immobilized, [1H] high-resolution high-speed magic-angle spinning solid-state NMR provides information on the effect exerted by polymer–filler Interactions on the mobility of the various constitutive species of the macromolecular backbone. A systematic study of the evolution of the spectral lines yielded by the samples indicates that 1,2-polybutadiene moieties have a particular affinity towards the carbon black surface which suggests the occurrence of specific Interactions at the elastomer–filler interface. © 2001 Society of Chemical Industry
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high resolution solid state n m r investigation of the filler Rubber Interaction 1 high speed 1h magic angle spinning n m r spectroscopy in carbon black filled styrene butadiene Rubber
Polymer, 1994Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This present work, dealing with filler/Rubber Interactions, provides a new approach for investigating the behaviour of elastomeric chains (styrene-butadiene Rubber, SBR) in the close vicinity of carbon black surfaces. Pulsed nuclear magnetic resonance measurements have been carried out on pure SBR, and on carbon gels obtained by solvent extraction of the carbon black filled elastomers. The initial concentration of carbon black in the filler/Rubber mixtures was varied between 20 and 100 parts per hundred parts by weight (phr). The high resolution proton spin-spin relaxation time, T 2 , has been measured for each of the individual resonance species belonging to the SBR chain. High resolution was achieved by rapidly spinning the sample at the magic angle. It has been observed that a very high magic-angle spinning (MAS) rate (> 18 kHz) is necessary to achieve a fully resolved spectrum of SBR. However, at a spinning rate of ∼ 15 kHz it is possible to avoid all of the spinning side bands and to deconvolute, unambiguously, the different resonance peaks that are present in the spectrum. In the unfilled elastomer, at temperatures much higher than the T g , the chain segmental motions are anisotropic and deviate from true liquid-like behaviour. The adsorbed Rubber chains are found to consist of loosely and tightly immobilized segments. The relative immobilization of the different protons has evidenced the methine 1 H to be much more immobilized than the aromatic or methylene species. Therefore, the olefinic part of the butadiene segment of the elastomeric chain appears to be the most affected by the carbon black surface. Moreover, T 2 is found to be independent of the filler concentration in the 30–80 phr range, and the relative concentration of the tightly bound Rubber in the composite shows a maximum at a filler content of ∼ 50 phr, where maximum reinforcement is normally observed. As far as the molecular dynamics is concerned, highly filled systems (> 80 phr carbon black) behave differently from low and medium filled systems (
L Delmotte - One of the best experts on this subject based on the ideXlab platform.
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high resolution solid state nmr investigation of the filler Rubber Interaction part iii investigation on the structure and formation mechanism of carbon gel in the carbon black filled styrene butadiene Rubber
Rubber Chemistry and Technology, 2001Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This investigation describes the elastomer—filler Interaction and its formation mechanism using solid state high-resolution, high-speed 1H magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. Pulsed NMR measurements were carried out on pure styrene-butadiene Rubber (SBR), and solvent extracted carbon gels from freshly prepared and storage matured master batches. The effects of filler loading, storage maturation, severity of extraction and experimental temperature on the elastomer-filler Interaction were examined and discussed. High resolution in NMR was achieved by higher temperature/low spinning rate, room temperature/high spinning and combined rotation and multiple-pulse spectroscopy (CRAMPS) techniques. High-speed magic-angle spinning (MAS) was found to be the most suitable method to achieve high resolution. Proton spin—spin relaxation time, T2, was measured successfully for each of the principal resonance species present in the samples. These measurements reveal an insight into...
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high resolution solid state nmr investigation of the filler Rubber Interaction 2 high speed 1h magic angle spinning nmr spectroscopy in carbon black filled polybutadiene
Polymer International, 2001Co-Authors: Rachel Mansencal, Bassel Haidar, Alain Vidal, L Delmotte, J M ChezeauAbstract:This work investigates the behaviour of elastomeric chains (polybutadienes of identical molecular weight but different microstructures) in the close vicinity of carbon black surfaces in order to attain a better understanding of the structure and properties of interphases. Elastomer–filler Interactions are assessed through the study of the thermal properties and NMR relaxation characteristics of the corresponding materials. Three series of samples were compared: pure polymers, raw polymer–filler blends (filler loading ratio: 50 phr) and solvent-extracted blends (so as to get rid of any polymer which is not under the influence of the solid surface). While differential scanning calorimetry points to the existence of an elastomer fraction which is not detected as undergoing the glass transition, ie is strongly immobilized, [1H] high-resolution high-speed magic-angle spinning solid-state NMR provides information on the effect exerted by polymer–filler Interactions on the mobility of the various constitutive species of the macromolecular backbone. A systematic study of the evolution of the spectral lines yielded by the samples indicates that 1,2-polybutadiene moieties have a particular affinity towards the carbon black surface which suggests the occurrence of specific Interactions at the elastomer–filler interface. © 2001 Society of Chemical Industry
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high resolution solid state n m r investigation of the filler Rubber Interaction 1 high speed 1h magic angle spinning n m r spectroscopy in carbon black filled styrene butadiene Rubber
Polymer, 1994Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This present work, dealing with filler/Rubber Interactions, provides a new approach for investigating the behaviour of elastomeric chains (styrene-butadiene Rubber, SBR) in the close vicinity of carbon black surfaces. Pulsed nuclear magnetic resonance measurements have been carried out on pure SBR, and on carbon gels obtained by solvent extraction of the carbon black filled elastomers. The initial concentration of carbon black in the filler/Rubber mixtures was varied between 20 and 100 parts per hundred parts by weight (phr). The high resolution proton spin-spin relaxation time, T 2 , has been measured for each of the individual resonance species belonging to the SBR chain. High resolution was achieved by rapidly spinning the sample at the magic angle. It has been observed that a very high magic-angle spinning (MAS) rate (> 18 kHz) is necessary to achieve a fully resolved spectrum of SBR. However, at a spinning rate of ∼ 15 kHz it is possible to avoid all of the spinning side bands and to deconvolute, unambiguously, the different resonance peaks that are present in the spectrum. In the unfilled elastomer, at temperatures much higher than the T g , the chain segmental motions are anisotropic and deviate from true liquid-like behaviour. The adsorbed Rubber chains are found to consist of loosely and tightly immobilized segments. The relative immobilization of the different protons has evidenced the methine 1 H to be much more immobilized than the aromatic or methylene species. Therefore, the olefinic part of the butadiene segment of the elastomeric chain appears to be the most affected by the carbon black surface. Moreover, T 2 is found to be independent of the filler concentration in the 30–80 phr range, and the relative concentration of the tightly bound Rubber in the composite shows a maximum at a filler content of ∼ 50 phr, where maximum reinforcement is normally observed. As far as the molecular dynamics is concerned, highly filled systems (> 80 phr carbon black) behave differently from low and medium filled systems (
Naba K Dutta - One of the best experts on this subject based on the ideXlab platform.
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high resolution solid state nmr investigation of the filler Rubber Interaction part iii investigation on the structure and formation mechanism of carbon gel in the carbon black filled styrene butadiene Rubber
Rubber Chemistry and Technology, 2001Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This investigation describes the elastomer—filler Interaction and its formation mechanism using solid state high-resolution, high-speed 1H magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. Pulsed NMR measurements were carried out on pure styrene-butadiene Rubber (SBR), and solvent extracted carbon gels from freshly prepared and storage matured master batches. The effects of filler loading, storage maturation, severity of extraction and experimental temperature on the elastomer-filler Interaction were examined and discussed. High resolution in NMR was achieved by higher temperature/low spinning rate, room temperature/high spinning and combined rotation and multiple-pulse spectroscopy (CRAMPS) techniques. High-speed magic-angle spinning (MAS) was found to be the most suitable method to achieve high resolution. Proton spin—spin relaxation time, T2, was measured successfully for each of the principal resonance species present in the samples. These measurements reveal an insight into...
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high resolution solid state n m r investigation of the filler Rubber Interaction 1 high speed 1h magic angle spinning n m r spectroscopy in carbon black filled styrene butadiene Rubber
Polymer, 1994Co-Authors: Naba K Dutta, Roy N Choudhury, Bassel Haidar, Alain Vidal, J B Donnet, L Delmotte, J M ChezeauAbstract:Abstract This present work, dealing with filler/Rubber Interactions, provides a new approach for investigating the behaviour of elastomeric chains (styrene-butadiene Rubber, SBR) in the close vicinity of carbon black surfaces. Pulsed nuclear magnetic resonance measurements have been carried out on pure SBR, and on carbon gels obtained by solvent extraction of the carbon black filled elastomers. The initial concentration of carbon black in the filler/Rubber mixtures was varied between 20 and 100 parts per hundred parts by weight (phr). The high resolution proton spin-spin relaxation time, T 2 , has been measured for each of the individual resonance species belonging to the SBR chain. High resolution was achieved by rapidly spinning the sample at the magic angle. It has been observed that a very high magic-angle spinning (MAS) rate (> 18 kHz) is necessary to achieve a fully resolved spectrum of SBR. However, at a spinning rate of ∼ 15 kHz it is possible to avoid all of the spinning side bands and to deconvolute, unambiguously, the different resonance peaks that are present in the spectrum. In the unfilled elastomer, at temperatures much higher than the T g , the chain segmental motions are anisotropic and deviate from true liquid-like behaviour. The adsorbed Rubber chains are found to consist of loosely and tightly immobilized segments. The relative immobilization of the different protons has evidenced the methine 1 H to be much more immobilized than the aromatic or methylene species. Therefore, the olefinic part of the butadiene segment of the elastomeric chain appears to be the most affected by the carbon black surface. Moreover, T 2 is found to be independent of the filler concentration in the 30–80 phr range, and the relative concentration of the tightly bound Rubber in the composite shows a maximum at a filler content of ∼ 50 phr, where maximum reinforcement is normally observed. As far as the molecular dynamics is concerned, highly filled systems (> 80 phr carbon black) behave differently from low and medium filled systems (
