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Investigation of network heterogeneities in filled, trimodal, highly functional PDMS networks by 1H Multiple Quantum NMR

Description: The segmental order and dynamics of polymer network chains in a filled, tri-modal silicone network have been studied by static 1H Multiple Quantum (MQ) NMR methods to gain insight into the structure property relationships. The materials were synthesized with two different types of crosslinks, with functionalities of 4 and near 60. The network chains were composed of distributions of high, low, and medium molecular weight chains. Crosslinking was accomplished by standard acid catalyzed reactions. MQ NMR methods have detected domains with residual dipolar couplings (<{Omega}{sub d}>) of near 4 kRad/s and 1 kRad/s assigned to (a) the shorter polymer chains and chains near the multifunctional ({phi}=60) crosslinking sites and to (b) the longer polymer chains far from these sites. Three structural variables were systematically varied and the mechanical properties and distributions of residual dipolar couplings measured in order to gain insight in to the network structural motifs that contribute significantly to the composite properties. The partitioning of and the average values of the residual dipolar couplings for the two domains were observed to be dependent on formulation variable and provided increased insight into the mechanical properties of these materials which are unavailable from swelling and spin-echo methods. The results of this study suggest that the domains with high crosslink density contribute significantly to the high strain modulus, while the low crosslink density domains do not. This is in agreement with theories and experimental studies on silicone bimodal networks over the last 20 years. In-situ MQ-NMR of swollen sample suggests that the networks deform non-affinely, in agreement with theory. The NMR experiments shown here provide increased ability to characterize multimodal networks of typical engineering silicone materials and to gain significant insight into structure-property relationships.
Date: September 6, 2006
Creator: Gjersing, E; Chinn, S; Maxwell, R S; Herberg, J; Eastwood, E; Bowen, D et al.
Partner: UNT Libraries Government Documents Department

Multiple Quantum NMR Investigations of Structure- Property Relationships in Synthetic and Aged Silicone Elastomers

Description: Complex engineering elastomeric materials are often characterized by a complex network structure obtained by crosslinking network chains with multiple chain lengths. Further, these networks are commonly filled with thixotropic reinforcing agents such as SiO{sub 2} or carbon black. Degradation of such materials often occurs via mechanisms that alter the fundamental network structure. In order to understand the effects of modifications of network structure and filler-polymer interaction on component performance, a series of model compounds have been studied by {sup 1}H multiple quantum NMR analysis and traditional mechanical property assessments. The {sup 1}H NMR data provides insight into the distribution of segmental dynamics that reveals insight into the changes in mechanical properties.
Date: September 27, 2006
Creator: Maxwell, R; Gjersing, E; Chinn, S; Herberg, J; Eastwood, E; Bowen, D et al.
Partner: UNT Libraries Government Documents Department

Probing Structure Property Relationships in Complex Engineering Silicones by 1H NMR

Description: It is generally accepted that the properties of polymeric materials are controlled by the network structure and the reactions by which they have been constructed. These properties include the bulk moduli at creation, but also the properties as a function of age during use. In order to interpret mechanical properties and predict the time dependent changes in these properties, detailed knowledge of the effect of structural changes must be obtained. The degree and type of crosslinking, the molecular weight between crosslinks, the number of elastically ineffective chains (loops, dangling chain ends, sol-fraction) must be characterized. A number of theoretical and experimental efforts have been reported in the last few years on model networks prepared by endlinking reactions and the relationships of those structures with the ultimate mechanical properties. A range of experimental methods have been used to investigate structure including rheometric, scattering, infrared, {sup 29}Si MAS and CPMAS, {sup 1}H relaxation measurements, and recently {sup 1}H multiple quantum methods. Characterization of the growth of multiple quantum coherences have recently been shown to provide detailed insight into silicone network structure by the ability to selective probe the individual components of the polymer network, such as the polymer-filler interface or network chains. We have employed recently developed MQ methods to investigate the structure-property relationships in a series of complex, endlinked filled-PDMS blends. Here, a systematic study of the relationship between the molecular formulation, as dictated by the amount and type of crosslinks present and by the remaining network chains, and the segmental dynamics as observed by MQ NMR was performed.
Date: July 14, 2006
Creator: Chinn, S C; Gjersing, E L; Maxwell, R S; Eastwood, E; Bowen, D & Stephens, T
Partner: UNT Libraries Government Documents Department

Investigation of network heterogeneities in filled, trimodal, highly functional PDMS networks by 1H Multiple Quantum NMR

Description: The segmental order and dynamics of polymer network chains in a filled, tri-modal silicone foam network have been studied by static 1H Multiple Quantum (MQ) NMR methods to gain insight into the structure property relationships. The foam materials were synthesized with two different types of crosslinks, with functionalities, {phi}, of 4 and near 60. The network chains were composed of distributions of high, low, and medium molecular weight chains. Crosslinking was accomplished by standard acid catalyzed reactions. MQ NMR methods have detected domains with residual dipolar couplings (<{Omega}{sub d}>) of near 4 kRad/s and 1 kRad/s assigned to (a) the shorter polymer chains and chains near the multifunctional (f=60) crosslinking sites and to (b) the longer polymer chains far from these sites. Three structural variables were systematically varied and the mechanical properties via compression and distributions of residual dipolar couplings measured in order to gain insight in to the network structural motifs that contribute significantly to the composite properties. The partitioning of and the average values of the residual dipolar couplings for the two domains were observed to be dependent on formulation variable and provided increased insight into the network structure of these materials which are unavailable from swelling and spin-echo methods. The results of this study suggest that the domains with high crosslink density contribute significantly to the high strain modulus, while the low crosslink density domains do not. This is in agreement with theories and experimental studies on silicone bimodal networks over the last 20 years. In-situ MQ-NMR of swollen sample suggests that the networks deform heterogeneously and non-affinely. The heterogeneity of the deformation process was observed to depend on the amount of the high functionality crosslinking site PMHS. The NMR experiments shown here provide increased ability to characterize multimodal networks of typical engineering silicone foam materials and ...
Date: March 20, 2007
Creator: Maxwell, R.; Gjersing, E.; Chinn, S.; Giuliani, J.; Herberg, J.; Eastwood, E. et al.
Partner: UNT Libraries Government Documents Department

Proposal to study multiparticle-peripheral hadron physics at NAL

Description: We propose to build a large wire chamber magnetic spectrometer at NAL to measure multi-body forward-going hadronic systems produced by {pi}'s, K's and protons up to 80 GeV/c. Specific reactions will be isolated in order to study the s and t dependencies of the cross sections for peripheral processes, search for new resonant states and attempt to measure {pi}{pi} and K{pi} inelastic scattering. We propose a physics program for the spectrometer which is initially limited to those processes easiest to measure and which nevertheless spans a large range of strong interaction problems. Technically, the proposed spectrometer is a relatively modest extension of presently operating systems in the 10-20 GeV/c region, and does not present a challenge of uncertain magnitude to construct.
Date: February 1, 1971
Creator: Dzierba, A.; Gomez, R.; Nagashima, Y.; Pine, J.; /Caltech; Malamud, E. et al.
Partner: UNT Libraries Government Documents Department

Comparison of synchrotron x-ray microanalysis with electron and proton microscopy for individual particle analysis

Description: This paper is concerned with the evaluation of the use of synchrotron/radiation induced x-ray fluorescences ({mu}-SRXRF) as implemented at two existing X-ray microprobes for the analysis of individual particles. As representative environmental particulates, National Institutes of Science and Technology (NIST) K227, K309, K441 and K961 glass microspheres were analyzed using two types of X-ray micro probes: the white light microprobe at beamline X26A of the monochromatic (15 keV) X-ray microprobe at station 7.6 of the SRS. For reference, the particles were also analyzed with microanalytical techniques more commonly employed for individual particles analysis such as EPMA and micro-PIXE.
Date: December 31, 1991
Creator: Janssens, K. H.; van Langevelde, F.; Adams, F. C.; Vis, R. D.; Sutton, S. R.; Rivers, M. L. et al.
Partner: UNT Libraries Government Documents Department

Comparison of synchrotron x-ray microanalysis with electron and proton microscopy for individual particle analysis

Description: This paper is concerned with the evaluation of the use of synchrotron/radiation induced x-ray fluorescences ({mu}-SRXRF) as implemented at two existing X-ray microprobes for the analysis of individual particles. As representative environmental particulates, National Institutes of Science and Technology (NIST) K227, K309, K441 and K961 glass microspheres were analyzed using two types of X-ray micro probes: the white light microprobe at beamline X26A of the monochromatic (15 keV) X-ray microprobe at station 7.6 of the SRS. For reference, the particles were also analyzed with microanalytical techniques more commonly employed for individual particles analysis such as EPMA and micro-PIXE.
Date: January 1, 1991
Creator: Janssens, K.H.; van Langevelde, F.; Adams, F.C. (Universitaire Instelling Antwerpen, Antwerp (Belgium)); Vis, R.D. (Vrije Univ., Amsterdam (Netherlands)); Sutton, S.R.; Rivers, M.L. (Chicago Univ., IL (United States)) et al.
Partner: UNT Libraries Government Documents Department