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1.
2.
C. Torres O. Alejos C. de Francisco J.M. Muñoz P. Hernández-Gómez 《Applied Physics A: Materials Science & Processing》2003,77(3-4):543-547
This paper describes a robust and fast fitting procedure applicable for relaxing processes that cannot be understood as a discrete sum of single processes but require an activation energy distribution. The method is based on a set of closed-form expressions that allow the computation of the relaxation parameters directly from the isochronal curves obtained experimentally. The usefulness of this method is checked by analyzing the isochronal curves given by a theoretical energy distribution and the magnetic disaccommodation spectra observed in yttrium iron garnet (YIG) samples. PACS 02.60.Ed; 75.60.Lr; 75.50.Gg 相似文献
3.
A. Paesano Jr. S. C. Zanatta S. N. De Medeiros L. F. CÓtica J. B. M. Da Cunha 《Hyperfine Interactions》2005,161(1-4):211-220
We have investigated the mechanosynthesis of gadolinium and yttrium iron garnets by high-energy ball-milling of α-Fe2O3 and Gd2O3 or α-Fe2O3 and Y2O3, respectively, followed by short thermal annealings conducted at moderate temperatures. The samples were characterized by X-ray diffraction and Mössbauer spectroscopy, in order to determine the influence of the milling time and annealing conditions on the final products. For as-milled samples of each rare-earth system, the results revealed the formation of perovskite phases, in relative amounts that depend on the milling time. The formation of garnet phases was observed in as-annealed samples treated at 1000°C for 2 h or 1100°C for 3 h, i.e., at very modest annealing requirements when compared with ordinary solid-state-reaction processes performed without previous high-energy milling. Also, the occurrence was verified of a milling time for which the relative amount of garnet phases formed by annealing was maximized. This time depends on the rare-earth composing the garnet phase and on the annealing temperature. 相似文献
4.
A. González Arias C. Torres C. de
Francisco J. M. Muñoz P. Hernández
Gómez O. Alejos O. Montero J. I. Iñiguez 《Journal of Thermal Analysis and Calorimetry》2006,86(1):195-198
The article discusses theory and experiment about the measurement of
defect concentration in Ti-substituted yttrium iron garnet by means of thermogravimetry
techniques. The two possible cases arising from oxygen interchange with atmosphere,
oxygen vacancies and interstitial cations, may be analyzed quantitatively
from the derived expressions. The possibility of another type of defects being
present in the samples, not associated to oxygen evolution, is not excluded.
Measurements were carried out in air and CO2 for different
Ti contents. The substitution tends to increase slightly the defect parameter
θ in YIG, while a CO2 reducing atmosphere is
much more effective than the Ti substitution for increasing θ. Calculations
for a given single-phased sample sintered in air show two possibilities: a
deficit of one oxygen atom for every 2.5 unit cells of 96 atoms, or one excess
cation for every 3.5 cells. Other samples show very similar results. The accuracy
involved in the measurements is about 2–3%. 相似文献
5.
Òscar Rubio-Pons Boris Minaev Oleksandr Loboda Hans Ågren 《Theoretical chemistry accounts》2005,113(1):15-27
The phosphorescence spectrum of p-dichlorobenzene has been calculated using multiconfiguration self-consistent-field wave functions and the quadratic response technique. Attention has been paid to the intensity distribution of the singlet–triplet (3B1u1Ag) transition through a number of vibronic subbands. The second order spin–orbit coupling (SOC) contribution to the spin splitting of the 3B1u (3*) state is found to be almost negligible, and the calculations therefore provide a good estimate for the zero-field splitting (ZFS) parameters based only on the electron spin–spin coupling expectation values. Nuclear quadrupole resonance constants for the different Cl isotopes are also calculated to accomplish the ZFS assignment. The electric dipole activity of the spin sublevels in the triplet–singlet transitions to the ground-state vibrational levels is estimated by calculations of derivatives using distorted geometries which are shifted from the equilibrium position along different vibrational modes. A vibrational analysis of the phosphorescence spectrum, based on the SOC-induced mixing of the singlet and triplet states calculated along different vibrational modes, provides reasonable agreement with experimental data.Acknowledgment O. R.-P. would like to thank the European MOLPROP network for support. The authors thank Alexander Baev for fruitful discussions. This work was supported by the Swedish Royal Academy of Science (KVA). 相似文献
6.
Grimalt S Pozo OJ Marín JM Sancho JV Hernández F 《Journal of the American Society for Mass Spectrometry》2005,16(10):1619-1630
The liquid chromatography tandem mass spectroscopy residue determination of compounds without any acidic or basic centers such as abamectin has been investigated. Several approaches regarding the interface used and adduct formation have been compared. The low acidity of the hydroxyl groups only made deprotonation feasible using the atmospheric pressure chemical ionization (APCI) interface. To obtain sufficient sensitivity for residue analysis, the Ion Sabre APCI interface was necessary. However, the sensitivity attained was lower than for monitoring adducts in positive ion mode. Using electrospray ionization, different adducts with Na+, NH4+, and Li+ were tested and compared. The best results were obtained for the ammoniated adduct in electrospray ionization (ESI) because of its high sensitivity and the presence of several product ions with similar abundance. The highest sensitivity was reached using an in-source fragment as precursor ion, leading to a limit of detection (LOD) of 2 microg/L with low relative standard deviation. The relatively high abundance of other transitions allowed abamectin confirmation at concentrations close to the LOD (6 microg/L). Alkali ions were found to be a suitable alternative to determine and confirm abamectin at residue levels. The [M + Na]+ also presented various product ions with similar abundance, which allowed confirmation at LOD levels. However, this LOD was found to be almost four times higher than with [M + NH4]+ because of the poor sensitivity of the transitions obtained. Although the use of Li+ facilitated the fragmentation of the adduct [M + Li]+, with similar sensitivity to [M + NH4]+, this fragmentation preferentially generated only one product ion, which did not allow confirmation at concentration levels lower than 15 microg/L. The use of APCI for monitoring adducts was also feasible, but with less sensitivity. The sensitivity increased with the Ion Sabre APCI, although it was still five times lower than with ESI. Other adduct formers such as Co2+ and Ni2+ also were tested with unsatisfactory results. 相似文献
7.
Óscar López 《Tetrahedron》2005,61(38):9058-9069
An efficient method for the preparation of urea-bridged cyclodextrins using triphosgene in the isocyanation step in an aqueous two-phase system is reported. Per-O-acetylated glycopyranosylamines and 2-amino-2-deoxy-α and β-d-glucose were also transformed into the corresponding isocyanates using either an aqueous two-phase or an anhydrous dichloromethane medium, and converted in situ into ureas. An alternative method for the preparation of sugar-derived ureas consisting of desulfurization of sugar thioureas with mercury oxide is also presented. 相似文献
8.
Inés Maya Óscar LópezSusana Maza José G. Fernández-BolañosJosé Fuentes 《Tetrahedron letters》2003,44(47):8539-8543
The preparation of a urea-bridged β-cyclodextrin dimer and of a 6-monodeoxy-6-mono[3-(β-d-glucopyranos-2-yl)ureido]-β-cyclodextrin has been developed, using triphosgene as the isocyanation agent in an aqueous two-phase system. Per-O-acetylated β-d-gluco and mannopyranosylamines and 2-amino-2-deoxy-α- and β-d-glucose were also transformed into the corresponding isocyanates and converted in situ into ureas by coupling with aromatic and aliphatic amines. 相似文献
9.
10.
Unexpected reactivity of pyridinium salts toward alkynyl Fischer complexes to produce oxo‐heterocycles
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María Inés Flores‐Conde Fabiola N. de la Cruz Julio López J. Óscar C. Jiménez‐Halla Eduardo Peña‐Cabrera Marcos Flores‐Álamo Francisco Delgado Miguel A. Vázquez 《应用有机金属化学》2018,32(3)
The unprecedented reaction of ketone‐containing aromatic pyridinium salts 3a ‐ e and alkynyl Fischer complexes 1a ‐ f proceeds via a mild domino process to provide 4,6‐disubstituted pyran‐2‐ones 5a ‐ k and 2,3,5‐trisubstituted furans 6a ‐ h (45‐97%). According of the results of isotopic labeling experiments, a mechanism involving an initial Michael addition appears to be the key step, obtaining a mesomeric structure responsible for the formation of both products. 相似文献