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1.
The formation of silicon oxide precipitates from Czochralski grown silicon depends on the time and temperature of the heat treatment as well as on the initial content of interstitially dissolved oxygen. Samples containing between 5×1017 Oi/cm3 and 13×1017 Oi/cm3 have been heated at 750° C for 96 h. SiO2 precipitates of various shape and size have been obtained and investigated by means of small angle neutron scattering (SANS) in the Q-range 0.05 Å–1<Q<0.2 Å–1. The obtained SANS patterns reveal a typical anisotropy of their intensity distribution, which splits into a central peak at Q<0.1 Å–1 due to the shape of the individual particles and a number of weak intensities for large Q-values, originating from a correlation between defects, possibly between the precipitates. While these correlation peaks in the SANS patterns are seen best for rather low values of about (5–7)×1017 Oi/cm3 oxygen content, the central peak anisotropy is most pronounced for higher values of ca 10×1017 Oi/cm3. The integrated intensity of the central peak increases with increasing initial oxygen content. For comparison, untreated samples of the same initial oxygen content do not reveal any anisotropic SAN scattering or a broadened central peak beam.  相似文献   
2.
The complexes (RN=CH-CH=NR)Co(NO)(CO) with R = isopropyl, 2,6-diisopropylphenyl, or p-tolyl are chemically and electrochemically reducible to radical anions at potentials which strongly depend on R. The DFT calculated structure for the neutral compound with R = iPr agrees with the experiment, and the computed structure of the anion radical reveals changes according to a reduction of the R-DAB ligand. EPR results confirm an (R-DAB)-based singly occupied molecular orbital in [(RNCHCHNR)Co(NO)(CO)](.-), with minor but detectable contributions from NO as supported by IR spectroelectrochemistry and as quantified by DFT spin density calculations. The calculations indicate increasingly stabilized CO, NO, and RNCHCHNR pi* acceptor orbitals, in that order. On the basis of TD-DFT (time-dependent density functional theory) calculations, the lowest-lying excited states are assigned to metal-to-(R-DAB) charge transfer transitions while bands due to the metal-to-nitrosyl charge transfer occur at higher energies but still in the visible region. Resonance Raman studies were used to probe these assignments.  相似文献   
3.
The 27Al NMR spectra of calcium tungstate aluminate sodalite (CAW), Ca8[Al12O24](WO4)2, and the 23Na NMR spectra of sodium aluminosilicate sodalites of general composition Na9[Si6Al6O24]A2 with A = B(OH)4- (SBS), SCN- (SRS) and A2 = SO4(2-) (SSS), MoO4(2-) (SMS) have been measured using magic-angle spinning (MAS) and double-rotation (DOR) techniques. Rotor synchronized pulse excitation is applied in the DOR experiments. Dramatic line narrowing is observed in the DOR spectra of all samples. The 27Al DOR NMR spectra of CAW measured at 9.4 and 11.7 T and spinning rates of 800-1150 Hz of the outer and 5 kHz of the inner rotor show seven sharp central lines accompanied by a manifold of spinning sidebands. These lines correspond to the seven crystallographically inequivalent Al sites of the CAW framework derived from X-ray structure analysis. From the difference of the line positions in the 9.4 and 11.7 T spectra the quadrupole coupling constant, QCC, quadrupole induced shift, sigma qs, and isotropic chemical shift, delta cs, of each Al site have been calculated. QCC values in the range of 5 to 9 MHz are obtained which reflect the strong tetragonal distortion of the AlO4 tetrahedra in CAW. delta cs shows only small changes in the range between 74.4 and 77.2 ppm. A tentative assignment of all lines to the distinct Al sites is derived from the correlation between QCC and a "shear strain parameter" describing quantitatively the distortion of the AlO4 tetrahedra.(ABSTRACT TRUNCATED AT 250 WORDS)  相似文献   
4.
Czochralski grown silicon crystals contain interstitially dissolved oxygen which diffuses on heating to form precipitates of silica. We have examined these precipitates by small angle neutron scattering (SANS) in the Q-range 0.05 Å–1<Q<0.4 Å–1. The obtained SANS patterns reveal pronounced anisotropic intensity distributions which resemble the symmetry of the host crystal. The SANS spectra show an anisotropic central peak at Q<0.1 Å–1 due to the single particle shape and a number of weak intensities for larger Q-values. These weak side maxima are considered correlation peaks or quasi-elastic interference peaks. They show, however, an unexpected and distinct temperature dependence: with decreasing temperature below values of 220 K their intensity is lost slowly, but reversibly. At T = 50 K only the central peak from the single-particle scattering remains unchanged. Upon heating, the correlation peaks regain their former value of intensity and Q-position without any evidence of thermal hysteresis.  相似文献   
5.
The branching ratio, the photoemission intensity ratio of two spin-orbit-split components, has been applied for the first time as a means for obtaining a photoelectron holographic image. Angle-resolved photoemission from a monolayer of Bi adsorbed on Si(111) shows fine-structure oscillations in the branching ratio of the Bi 5d core level due to diffraction effects. These oscillations as a function of photon energy are recorded for a number of emission angles. Three-dimensional holographic inversion of the data yields an atomic image which shows that the Bi adatoms are arranged in a trimer structure.  相似文献   
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Several new zirconium phosphonates incorporating naphthalene and anthracene ring systems and having the general formula Zr(O3PR)1(O3PR')1 [R and R' = -C10H7, -C14H9, -OC4H9, and -OC2H5] have been synthesized. These compounds were chemically characterized using thermal gravimetric analysis (percentage of organic content), infrared spectroscopy (presence of the desired organic functional groups), and solid-state 31P NMR (phosphorus environments), while the structural parameters were determined using X-ray powder diffraction (interlayer d spacings). The d spacings of the zirconium bis(phosphonates) correlate well with a simple predictive model based on the effective length of the organic functional group. The zirconium mixed phosphonates examined are single-phase structures with random mixtures of the organic moieties within the interlayer and possess d spacings that are between those of the two parent zirconium bis(phosphonates).  相似文献   
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10.
The radical complex {(mu(4)-TCNQF4)[Re(CO)(3)(bpy)](4)}(PF(6))(3), as prepared and isolated from the reaction between TCNQF4 and [Re(CO)(3)(bpy)(MeOH)](PF(6)), was studied electrochemically and by IR vibrational spectroscopy, UV-Vis-NIR absorption spectroscopy, and by EPR at 9.5, 190 and 285 GHz. The isotropic g factor of 2.0058, the detectable g anisotropy, and the (185,187)Re EPR hyperfine coupling of 0.95 mT for four equivalent metal nuclei support predominant, but not exclusive, spin localisation at the bridging ligand. Nitrile and metal carbonyl stretching frequencies as well as the typically structured near infrared absorption band lend further support to (TCNQF4 (-))(Re(I))(4) as the most appropriate oxidation state formulation. In comparison to the non-radical complex {(mu(4)-TCNQ)[Re(CO)(3)(bpy)](4)}(PF(6))(4) an X-ray structure analysis of {(mu(4)-TCNQF4)[Re(CO)(3)(bpy)](4)}(PF(6))(3) shows a marginally more twisted (ReNCCCNRe)(C(6)X(4))(ReNCCCNRe) configuration and a different up/down arrangement of the [Re(CO)(3)(bpy)](+) groups. This first isolation, electrochemical, structural and spectroscopic characterisation of a discrete tetranuclear radical complex of a TCNQ-type ligand suggests a link between the stability of such materials and the rather small structural changes on ligand-based electron transfer.  相似文献   
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