Nmr Imaging of Silica-Silicone Composites

1989 ◽  
Vol 171 ◽  
Author(s):  
Leoncio Garrido ◽  
Jerome L. Ackerman ◽  
James E. Mark
Keyword(s):  
Imaging Techniques ◽  
Spin Echo ◽  
Sol Gel ◽  
Relaxation Times ◽  
Reaction Times ◽  
Silica Glasses ◽  
Spin Lattice ◽  
H Nmr ◽  
Hydrolysis Of

ABSTRACTPolydimethylsiloxane (PDMS) model networks reinforced by in situ precipitated SiO2, and polymer-modified silica glasses were obtained following the usual sol-gel methods. The conditions were chosen to increase the probability of observing inhomogeneities: (i) bulky samples, and (ii) limited reaction times. These composites were characterized by measuring bulk spin-lattice (T1) and spin-spin (T2) relaxation times and using 1H NMR two-dimensional Fourier transform (2DFT) spin echo imaging techniques. The T1 and T2 maps show clear and significant variations of NMR signal intensity throughout the sample due to nonuniform hydrolysis of the tetraethylorthosilicate (TEOS) in the specimens.

scholarly journals Rubber-Filler Interactions in Polyisoprene Filled with In Situ Generated Silica: A Solid State NMR Study

Polymers ◽  
2018 ◽  
Vol 10 (8) ◽  
pp. 822 ◽  
Author(s):  
Silvia Borsacchi ◽  
Umayal Sudhakaran ◽  
Lucia Calucci ◽  
Francesca Martini ◽  
Elisa Carignani ◽  
...  
Keyword(s):  
Solid State ◽  
Dynamic Properties ◽  
Sol Gel ◽  
Relaxation Times ◽  
Reaction Times ◽  
Rubber Matrix ◽  
Polymer Bulk ◽  
Nmr Study ◽  
Bound Rubber

In this paper we used high- and low-resolution solid state Nuclear Magnetic Resonance (NMR) techniques to investigate a series of polyisoprene samples filled with silica generated in situ from tetraethoxysilane by sol-gel process. In particular, 1H spin-lattice and spin-spin relaxation times allowed us to get insights into the dynamic properties of both the polymer bulk and the bound rubber, and to obtain a comparative estimate of the amount of bound rubber in samples prepared with different compositions and sol-gel reaction times. In all samples, three fractions with different mobility could be distinguished by 1H T2 and ascribed to loosely bound rubber, polymer bulk, and free chain ends. The amount of bound rubber was found to be dependent on sample preparation, and it resulted maximum in the sample showing the best dispersion of silica domains in the rubber matrix. The interpretation of the loosely bound rubber in terms of “glassy” behaviour was discussed, also on the basis of 1H T1 and T1ρ data.

Bonded Hydrogen and Trapped H2 in a-Si1−xGex:H Alloys

1989 ◽  
Vol 149 ◽  
Author(s):  
E. J. Vanderheiden ◽  
G. A. Williams ◽  
P. C. Taylor ◽  
F. Finger ◽  
W. Fuhs
Keyword(s):  
Temperature Dependence ◽  
Molecular Hydrogen ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
Spin Lattice Relaxation ◽  
Spin Lattice ◽  
H Nmr ◽  
Local Environments

ABSTRACT1H NMR has been employed to study the local environments of bonded hydrogen and trapped molecular hydrogen (H2) in a series of a-Si1−xGex:H alloys. There is a monotonic decrease of bonded hydrogen with increasing x from ≈ 10 at. % at x = 0 (a-Si:H) to ≈ 1 at. % at x = 1 (a-Ge:H). The amplitude of the broad 1H NMR line, which is attributed to clustered bonded hydrogen, decreases continuously across the system. The amplitude of the narrow 1H NMR line, which is attributed to bonded hydrogen essentially randomly distributed in the films, decreases as x increases from 0 to ≈ 0.2. From x = 0.2 to x ≈ 0.6 the amplitude of the narrow 1H NMR line is essentially constant, and for x ≥ 0.6 the amplitude decreases once again. The existence of trapped H2 molecules is inferred indirectly by their influence on the temperature dependence of the spin-lattice relaxation times, T1. Through T1, measurements it is determined that the trapped H2 concentration drops precipitously between x = 0.1 and x = 0.2, but is fairly constant for 0.2 ≤ x ≤ 0.6. For a-Si:H (x = 0) the H2 concentration is ≈ 0.1 at. %, while for x ≥ 0.2 the concentration of H2 is ≤ 0.02 at. %.

Nuclear magnetic resonance spin–lattice relaxation and the rotation of adamantane and hexamethylenetetramine in solution

1977 ◽  
Vol 55 (13) ◽  
pp. 2564-2569 ◽  
Author(s):  
Roderick E. Wasylishen ◽  
Brian A. Pettitt
Keyword(s):  
Variable Temperature ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
Spin Lattice Relaxation ◽  
Hard Sphere Model ◽  
Correlation Times ◽  
Spin Lattice ◽  
H Nmr ◽  
Large Step ◽  
Resonance Spin

Deuterium nmr spin–lattice relaxation times have been measured for dilute solutions of adamantane-d16 in CH2I2, CHBr3, CCl4, CHCl3, and CH2Cl2. The reorientation correlation times, τ2, calculated from the experimental data are used to calculate τJ, the angular momentum correlation times, assuming both the J-diffusion and Hubbard relations. The derived τJ values suggest that adamantane executes small step diffusion in CH2I2 and CHBr3, and large step diffusion in CCl4, CHCl3, and CH2Cl2. The calculated τJ values do not appear to be related to the mean times between collisions calculated using a hard sphere model. Both variable solvent and variable temperature experiments indicate 1 ps/cP for the viscosity dependence of the adamantane reorientation time, about 1/36th the value predicted using the familiar Stokes–Einstein equation.Carbon-13 and 1H nmr T1 data indicate that reorientation of hexamethylenetetramine in H2O (28 ps/cP), CHCl3 (27 ps/cP), and CHBr3 (18 ps/cP) is severely hindered because of inter-molecular hydrogen bonding.

Surface Rotational Dynamics of Liquids Confined in Nanopores

1996 ◽  
Vol 464 ◽  
Author(s):  
J.-P. Korb ◽  
L. Malier ◽  
F. Cros ◽  
Shu Xu ◽  
J. Jonas
Keyword(s):  
Relaxation Times ◽  
Nmr Relaxation ◽  
Rotational Dynamics ◽  
Surface Relaxation ◽  
Nanoporous Silica ◽  
Silica Glasses ◽  
H Nmr ◽  
Fast Exchange ◽  
Nmr Relaxation Times ◽  
Different Time Scales

ABSTRACT2H NMR relaxation times of selectively deuterated polar molecules confined to a set of calibrated nanoporous silica glasses are reported. These experiments, combined with the consideration of different time scales in the theory of surface relaxation, show how confinement effects can provide detailed information on the rotational dynamics of temporarily adsorbed liquid layers in presence of biphasic fast exchange.

Molecular Motions in Halogen-Bridged One-Dimensional Pt Complexes, [PtII(en)2][PtIVX2(en)2](ClO4)4 (X = Cl, Br) Studied by 2H and 1H NMR

2002 ◽  
Vol 57 (6-7) ◽  
pp. 413-418 ◽  
Author(s):  
Noriyoshi Kimura ◽  
Toru Hachisuka ◽  
Yukitaka Nakano ◽  
Ryuichi Ikeda
Keyword(s):  
Relaxation Times ◽  
Lattice Relaxation ◽  
Energy Difference ◽  
Spin Lattice Relaxation ◽  
X Ray Diffraction ◽  
Potential Wells ◽  
One Dimensional ◽  
X Ray ◽  
Spin Lattice ◽  
H Nmr

2H and 1H NMR measurements were performed on crystalline [Pt(en)2][PtX2(en)2](ClO4)4 (X = Cl, Br), where the protonated and partially deuterated ethylenediamines (en’s), NH2(CH2)2NH2, NH2(CD2)2NH2 and ND2(CH2)2ND2 were used as ligands. Measurements of 2H and 1H NMR spin-lattice relaxation times showed the presence of motions of en chelate rings at the temperatures near the phase transitions, whereas broad 2H NMR spectra and the reported X-ray diffraction data showed no marked motions. These results were consistently explained by introducing the en puckering motion between highly asymmetric potential wells with an energy difference of 10 - 13 kJ mol-1. This difference was shown to be much larger than 2 - 5 kJ mol-1, reported for the iodo-complex, [Pt(en)2][PtI2(en)2](ClO4)4

Characterization of Biomaterials with NMR

1990 ◽  
Vol 217 ◽  
Author(s):  
Leoncio Garrido ◽  
Bettina Pfleiderer ◽  
Jerome L. Ackerman ◽  
John Moore
Keyword(s):  
Chemical Shift ◽  
Mechanical Stress ◽  
Imaging Techniques ◽  
Relaxation Times ◽  
Nmr Imaging ◽  
Spin Lattice ◽  
Model Networks ◽  
Crosslink Densities

ABSTRACTSilicone based biomaterials are characterized with NMR. Bulk spin-lattice (T1) and spin-spin (T2) relaxation times are measured in polydimethylsiloxane (PDMS) model networks and various types of implants. The T2 results seem to indicate that crosslink densities of these biomaterials are lower than those of the PDMS model networks studied. 1H chemical shift NMR imaging techniques are developed to investigate the aging (e.g., migration of free polymer, rupture due to mechanical stress, etc.) of biomaterials in vivo.

scholarly journals Titanium Dioxide Nanofibers and Microparticles Containing Nickel Nanoparticles

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Faheem A. Sheikh ◽  
Javier Macossay ◽  
Muzafar A. Kanjwal ◽  
Abdalla Abdal-hay ◽  
Mudasir A. Tantry ◽  
...  
Keyword(s):  
Hydrogen Production ◽  
Production Systems ◽  
Sol Gel ◽  
Titanium Isopropoxide ◽  
Electrospinning Process ◽  
Internal Morphology ◽  
Hydrolysis Of ◽  
Potential Use ◽  
Sem Analyses

The present study reports on the introduction of various nanocatalysts containing nickel (Ni) nanoparticles (NPs) embedded within TiO2 nanofibers and TiO2 microparticles. Typically, a sol-gel consisting of titanium isopropoxide and Ni NPs was prepared to produce TiO2 nanofibers by the electrospinning process. Similarly, TiO2 microparticles containing Ni were prepared using a sol-gel syntheses process. The resultant structures were studied by SEM analyses, which confirmed well-obtained nanofibers and microparticles. Further, the XRD results demonstrated the crystalline feature of both TiO2 and Ni in the obtained composites. Internal morphology of prepared nanofibers and microparticles containing Ni NPs was characterized by TEM, which demonstrated characteristic structures with good dispersion of Ni NPs. In addition, the prepared structures were studied as a model for hydrogen production applications. The catalytic activity of the prepared materials was studied by in situ hydrolysis of NaBH4, which indicated that the nanofibers containing Ni NPs can lead to produce higher amounts of hydrogen when compared to other microparticles, also reported in this paper. Overall, these results confirm the potential use of these materials in hydrogen production systems.

Solitons, polarons and their dynamics in mixed-valence halogen-bridged MX-chains

2007 ◽  
Vol 366 (1862) ◽  
pp. 93-100 ◽  
Author(s):  
Shinya Takaishi ◽  
Masahiro Yamashita
Keyword(s):  
Mixed Valence ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
Spin Lattice Relaxation ◽  
Relaxation Processes ◽  
Spin Lattice ◽  
H Nmr ◽  
Spin Resonance ◽  
1D Chain ◽  
The One

This article describes the photo-generation processes of elementary excitations such as solitons and polarons, and their dynamics in the one-dimensional (1D) halogen-bridged Pt compound [Pt(en) 2 Br](ClO 4 ) 2 . Spin-solitons were photo-generated via relaxation processes of CT excitons and self-trapped excitons, made evident by photo-induced absorption and photo-induced electron spin resonance spectra. Polarons were not generated from CT excitons. Diffusion of spin-solitons on the 1D chain was studied quantitatively by analysing 1 H NMR spin-lattice relaxation times ( T 1 ).

High Pressure NMR Studies of Confined Liquids

1992 ◽  
Vol 290 ◽  
Author(s):  
J. Jonas ◽  
Jing Zhang ◽  
Shu Xu
Keyword(s):  
Surface Layer ◽  
Rotational Diffusion ◽  
Relaxation Times ◽  
Porous Silica ◽  
Lattice Relaxation ◽  
Spin Lattice Relaxation ◽  
Nmr Studies ◽  
Silica Glasses ◽  
Spin Lattice ◽  
Confined Liquids

AbstractThe main goal of our novel NMR experiments on confined liquids was to determine the effects of pressure on the dynamics of liquids in the surface layer by using the twostate, fast exchange model and compare them to the pressure effects observed for bulk liquids. With this goal in mind, the deuteron NMR spin-lattice relaxation times, T1, in liquid pyridine-d5, nitrobenzene-d5, and methylcyclohexape-d confined to sol-gel porous silica glasses with pore radii in the range from 18Å to 49˚A were measured as a function of pressure up to 5 kbar at 300 K. In another set of high resolution natural abundance 13C NMR experiments, the 13C relaxation behavior of each carbon in 2- ethylhexyl benzoate model lubricant was measured as a function of pressure in porous silica glasses. In fact, the described experimental approach which allows investigation of the effects of pressure on the dynamic behavior of surface-layer liquids, may provide a new tool in studies of model liquid lubricants at extreme conditions of pressure and temperature. In addition selected results of a recent study of acetonitrile-d3 are reviewed. The 2H and 14N spin-lattice relaxation times of acetonitrile-d3 in porous silica glasses were measured in order to study the confinement effects on the anisotropic reorientation characterized by rotational diffusion constants, D⊥ and D‖, of this symmetric-top molecule.

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