NMR Study of the Crystallization Kinetics of Cis-Poly(Isoprene)s

1973 ◽  
Vol 46 (1) ◽  
pp. 22-29 ◽  
Author(s):  
R. C. Hirst ◽  
H. Y. Chen
Keyword(s):  
Room Temperature ◽  
Curve Shape ◽  
X Ray Diffraction ◽  
Rigid Lattice ◽  
X Ray ◽  
Nmr Study ◽  
Accurate Comparison ◽  
Dilatometric Studies ◽  
Kinetics Of ◽  
Good Agreement

Abstract The satisfactory agreement between our NMR results and X-ray diffraction results for the crystallinity in stark rubber at room temperature lead us to conclude that the NMR rigid lattice fraction, PRL, may be taken as equal to the fractional crystallinity obtained by other methods. Similarly, the good agreement between the time dependence of PRL at low temperature and the theoretical curve shape strongly suggest that the NMR crystallinity method works well down to at least −25° C for natural rubber and synthetic cis-poly (isoprene). It would be desirable to compare carefully the NMR crystallinity found for rubber crystallized at −25° C with X-ray diffraction results, but we have been unable to find any such X-ray diffraction studies at −25° C. Maximum values of ΔV/V≅0.025 from dilatometric studies appear to imply somewhat smaller crystallinities than those found by NMR, but an accurate comparison is not possible without having X-ray diffraction densities at −25° C. While the present experiments were carried out on unfilled, unstretched, unvulcanized samples, the NMR crystallinity method is equally applicable to samples which are filled, stretched, and vulcanized. Naturally any additive or impurity containing hydrogen is a possible source of interference, but there should be no difficulty in correcting for such interferences.

In situ high temperature X-ray diffraction study of the kinetics of phase separation in the uranium-plutonium mixed oxide (U0.55Pu0.45)O2-x

2014 ◽  
Vol 1645 ◽  
Author(s):  
Romain VAUCHY ◽  
Renaud.C. BELIN ◽  
Anne-Charlotte ROBISSON ◽  
Fiqiri HODAJ
Keyword(s):  
Phase Separation ◽  
Room Temperature ◽  
Mixed Oxides ◽  
Oxygen Stoichiometry ◽  
X Ray Diffraction ◽  
Fundamental Interest ◽  
X Ray ◽  
Uranium Plutonium ◽  
Kinetics Of

ABSTRACTUranium-plutonium mixed oxides incorporating high amounts of plutonium are considered for future nuclear reactors. For plutonium content higher than 20%, a phase separation occurs, depending on the temperature and on the oxygen stoichiometry. This phase separation phenomenon is still not precisely described, especially at high plutonium content. Here, using an original in situ fast X-ray diffraction device dedicated to radioactive materials, we evidenced a phase separation occurring during rapid cooling from 1773 K to room temperature at the rate of 0.05 and 2 K per second for a (U0.55Pu0.45)O2-x compound under a reducing atmosphere. The results show that the cooling rate does not impact the lattice parameters of the obtained phases at room temperature but their fraction. In addition to their obvious fundamental interest, these results are of utmost importance in the prospect of using uranium-plutonium mixed oxides with high plutonium content as nuclear fuels.

scholarly journals Compositional Dependence of Structural Properties of Prepared Alloys and Films

2011 ◽  
Vol 2011 ◽  
pp. 1-6
Author(s):  
M. F. A. Alias ◽  
A. A. J. Al-Douri ◽  
E. M. N. Al-Fawadi ◽  
A. A. Alnajjar
Keyword(s):  
Room Temperature ◽  
Thermal Evaporation ◽  
High Accuracy ◽  
Compositional Dependence ◽  
X Ray Diffraction ◽  
Thermal Evaporation Method ◽  
X Ray ◽  
Glass Substrates ◽  
Different Temperatures ◽  
Good Agreement

Results of a study of alloys and films with various Pb content have been reported and discussed. Films of of thickness 1.5 μm have been deposited on glass substrates by flash thermal evaporation method at room temperature, under vacuum at constant deposition rate. These films were annealed under vacuum around 10−6Torr at different temperatures up to 523 K. The composition of the elements in alloys was determined by standard surfaces techniques such as atomic absorption spectroscopy (AAS) and X-ray fluorescence (XRF), and the results were found of high accuracy and in very good agreement with the theoretical values. The structure for alloys and films is determined by using X-ray diffraction. This measurement reveals that the structure is polycrystalline with cubic structure and there are strong peaks at the direction (200) and (111). The effect of heat treatment on the crystalline orientation, relative intensity, and grain size of films is presented.

Solid-state and solution 117Sn NMR study of C2O4(SnPh3)2: a revision

2011 ◽  
Vol 34 (5-6) ◽  
pp. 153-153
Author(s):  
Libasse Diop
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Magnetic Resonance ◽  
State Structure ◽  
X Ray Diffraction ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Nmr Study ◽  
Tetrahedral Environment ◽  
Good Agreement

Abstract Solid-state and solution 117Sn nuclear magnetic resonance studies of C2O4(SnPh3)2 have been carried out and found to be in good agreement with the tetrahedral environment of the tin (IV) atom as found from the solid state structure, previously determined by a single crystal X-ray diffraction analysis.

Glancing Angle X-Ray Study of Crystallization of Amorphous Ge at the Ge-A1 Interface

1990 ◽  
Vol 202 ◽  
Author(s):  
S. M. Heald ◽  
J. K. D. Jayanetti ◽  
R. C. Budhani
Keyword(s):  
Initial Period ◽  
Time Characteristic ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffusion Limited ◽  
Glancing Angle ◽  
Lower Temperature ◽  
Kinetics Of ◽  
Diffusion Limited Reaction ◽  
Good Agreement

ABSTRACTThe amorphous to crystalline transformation of Ge in Al/Ge thin film couples has been studied using glancing angle EXAFS, x-ray reflectivity and diffraction. It was found that crystallization occurs at a much lower temperature (118-150 °C) than for bulk Ge, and initiates at the Al/Ge interface. X-ray diffraction studies were made at 152 °C to study the kinetics of the reaction. After an initial period we find good agreement with a square root dependence of the time, characteristic of a diffusion limited reaction.

1H NMR study of the solvolysis of the paramagnetic tetrachloro-bis(imidazole)ruthenium(III) anion in water, methanol, and dimethyl sulfoxide

1995 ◽  
Vol 73 (4) ◽  
pp. 471-482 ◽  
Author(s):  
Craig Anderson ◽  
André L. Beauchamp
Keyword(s):  
Dimethyl Sulfoxide ◽  
1H Nmr ◽  
Room Temperature ◽  
Single Species ◽  
X Ray Diffraction ◽  
Chloro Complexes ◽  
X Ray ◽  
H Nmr ◽  
Nmr Study ◽  
Nmr Signals

The 1H NMR signals of the Ru(III) species present in solution are considerably broadened and shifted by paramagnetism, but they can be used to follow chloride displacement in the trans-[RuCl4Im2]− ion. This anion remains predominant for several hours at room temperature in D2O, but its signals are progressively replaced by those of a monoaqua [RuCl3(D2O)Im2] complex. Over a period of days, two new sets of peaks appear, corresponding to two isomers of [RuCl2(D2O)2Im2]+. The same behaviour is observed for the 1-methyl-and 4-methylimidazole analogues. These reactions can be driven backwards by addition of KCl, but [RuCl4Im2]− is not quantitatively regenerated in solution even for 6 M NaCl. Within several months, the [RuCl2(D2O)2Im2]+ isomers further aquate to a single species [RuCl(D2O)3Im2]2+. In CD3OD, displacement of the first chloride of [RuCl4Im2]− takes place faster, over several hours, but substitution stops at the [RuCl3(CD3OD)Im2] stage. In DMSO, substitution occurs very slowly. The [RuCl3(DMSO)Im2]:[RuCl4Im2]−mixture (1:2) obtained after 12 days starts to show very slow reduction to two Ru(II) species, one of which precipitates as yellow crystals. From X-ray diffraction work (monoclinic, P21/n, a = 9.951, b = 8.564, c = 10.527 Å, β = 92.95°, R = 0.033), the compound was identified as [RuCl2(DMSO-d6)2Im2], where the metal has a trans-trans-trans coordination and the DMSO ligands are S-bonded. Keywords: paramagnetic ruthenium anion, solvolysis, chloro complexes.

Structures of Energetic Acetylene Derivatives HC≡CCH2ONO2, (NO2)3CCH2C≡CCH2C(NO2)3 and Trinitroethane, (NO2)3CCH3

2013 ◽  
Vol 68 (5-6) ◽  
pp. 719-731 ◽  
Author(s):  
Thomas M. Klapötke ◽  
Burkhard Krumm ◽  
Richard Moll ◽  
Alexander Penger ◽  
Stefan M. Sproll ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Gas Phase ◽  
Quantum Chemical ◽  
Room Temperature ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Polar Solvents ◽  
X Ray ◽  
Nmr Study ◽  
Acetylene Derivatives

The molecular structures and relative ratios of the two conformers (anti and gauche) of HCCCH2ONO2 detected in the gas phase at room temperature have been determined by electron diffraction. The results are discussed on the basis of quantum chemical calculations. The molecular structures of (NO2)3CCH2C≡CCH2C(NO2)3 and (NO2)3CCH3 have been determined by X-ray diffraction. A109Ag NMR study was performed for silver trinitromethanide Ag[C(NO2)3] in various polar solvents.

The concentration quenching of photoluminescence in Eu3+-doped La2O3

2013 ◽  
Vol 37 (1) ◽  
pp. 47-54 ◽  
Author(s):  
V. Đorđević ◽  
Ž. Antić ◽  
M. G. Nikolić ◽  
M. D. Dramićanin
Keyword(s):  
Room Temperature ◽  
Hexagonal Phase ◽  
Average Particle Size ◽  
Average Particle ◽  
X Ray Diffraction ◽  
X Ray ◽  
Maximum Lifetime ◽  
Transmission Electron ◽  
Lifetime Value ◽  
Kinetics Of

Abstract This work explores the influence of dopant concentration on photoluminescent emission and kinetics of Eu3+-doped (0.2−10 at.%) nanocrystalline lanthanumoxide powders. The X-ray diffraction analysis confirmed that all samples crystallize in La2O3 hexagonal phase with space group P3¯ m1. Transmission electron microscopy showed particles with non-uniform shape and diverse size distribution with an average particle size of (95 ± 5) nm. The room temperature photoluminescence spectra of all samples contain characteristic Eu3+ luminescence lines with the most pronounced red 5D0 →7F2 emission at about 626 nm. The maximum intensity of red emission is observed for the sample containing 5at.% of Eu3+ ions. The emission kinetics was recorded in the temperature range from 10K to 300 K. The maximum lifetime value of 0.98 ms obtained for the sample with 0.5at.% Eu3+ at room temperature increases up to 1.3ms at 10 K.

scholarly journals Effect of lead salts on phase, morphologies and photoluminescence of nanocrystalline PbMoO4 and PbWO4 synthesized by microwave radiation

2016 ◽  
Vol 34 (3) ◽  
pp. 529-533 ◽  
Author(s):  
Anukorn Phuruangrat ◽  
Budsabong Kuntalue ◽  
Surachai Artkla ◽  
Surin Promnopas ◽  
Wonchai Promnopas ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Microwave Radiation ◽  
Room Temperature ◽  
Blue Emission ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lead Salts ◽  
Transmission Electron ◽  
Ft Ir ◽  
Kinetics Of

AbstractPbMoO4 and PbWO4 were successfully synthesized by microwave radiation using different lead salts (acetate, chloride, nitrate and sulfate) and Na2MO4 (M = Mo, W) in propylene glycol. The products were characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM, TEM), Fourier transform infrared (FT-IR), Raman spectroscopy and photoluminescence (PL) spectroscopy. In this research, morphologies, crystallization and photoluminescence of the products were influenced by the kinetics of anions, including the detection of M–O (M = Mo, W) stretching modes in the (MO4)2− tetrahedrons. Photoluminescence of PbMoO4 synthesized from Pb(NO3)2 and of PbWO4 synthesized from PbCl2 showed the strongest blue emission due to the electronic diffusion in tetrahedrons at room temperature.

scholarly journals Pressure-dependent X-ray diffraction of the multiferroics RMn2O5

2019 ◽  
Vol 75 (4) ◽  
pp. 687-696 ◽  
Author(s):  
Wei Peng ◽  
Victor Balédent ◽  
Marie-Bernadette Lepetit ◽  
Antoine Vaunat ◽  
Elisa Rebolini ◽  
...  
Keyword(s):  
Dft Calculations ◽  
Density Functional ◽  
Room Temperature ◽  
Exchange Interactions ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray ◽  
X Ray Scattering ◽  
Pressure Evolution ◽  
Good Agreement

The room-temperature structural properties of the RMn2O5 multiferroics have been investigated under pressure, using powder X-ray scattering and density functional theory (DFT) calculations. It was possible to determine the lattice parameters and the main atomic positions as a function of pressure. Good agreement was observed between the X-ray and DFT results for most of the determined crystallographic data. From the DFT calculations, it was possible to infer the pressure evolution of the exchange interactions, and this analysis led to the conclusion that the onset of the q = (½, 0, ½) magnetic structure under pressure is related to the increase in the J 1 super-exchange terms (due to the reduction in the Mn—O distances) compared with the Mn—R exchange interactions. In addition, the 1D antiferromagnetic character of the compounds should be reinforced under pressure.

Preparation and Characterization of Sr, Ba Filled Type-I Ge Clathrate Single Crystals

2007 ◽  
Vol 336-338 ◽  
pp. 896-899 ◽  
Author(s):  
Ke Feng Cai ◽  
L.C. Zhang ◽  
Q. Lei
Keyword(s):  
Single Crystals ◽  
Room Temperature ◽  
Nominal Composition ◽  
Type I ◽  
Vibrational Modes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Optimum Synthesis ◽  
Good Agreement

Sr or Ba filled type-I Ge clathrate single crystals were prepared using high pure elemental Ga, Ge, and Sr or Ba as the starting materials, and Ga as a flux. Powder X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), differential scanning calorimeter (DSC) were used to characterize the crystals, respectively. The results show that large and well-crystallized single crystals can be prepared under optimum synthesis condition. The composition of the crystals is in good agreement with the nominal composition (M8Ga16Ge30, M=Sr, Ba). Raman spectra of the single crystals were studied at room temperature and several of the Raman active vibrational modes in the crystals have been identified.

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