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171.
Small-angle X-ray scattering measurements using synchrotron radiation were carried out for poly(ethylene terephthalate) and poly(ethylene isophthalate-co-ethylene terephthalate)s. In addition, differential scanning calorimetric measurements were conducted. Measurements were made both on polymers undergoing isothermal crystallization and during subsequent remelting. The primary and secondary crystallization behaviors are examined. Isophthalate units were found to be excluded from the crystals into amorphous layers during crystallization. No crystal thickening was observed during isothermal crystallization, which may be due to the relatively high chain rigidity. Secondary crystallization, detected predominantly at the later stages of crystallization, causes densification and shrinkage of the amorphous layer. Considering the results, it is proposed that secondary crystallization involves the formation of short-range molecular order in the amorphous layers of a lamellar stack as well as in the amorphous regions between lamellar stacks. This short-range-ordered phase has a lower density than the lamellar crystal formed by primary crystallization. 相似文献
172.
Su Cao Bin Ma Davide Giassi Beth Anne V. Bennett Marshall B. Long 《Combustion Theory and Modelling》2018,22(2):316-337
In this study, the influence of pressure and fuel dilution on the structure and geometry of coflow laminar methane–air diffusion flames is examined. A series of methane-fuelled, nitrogen-diluted flames has been investigated both computationally and experimentally, with pressure ranging from 1.0 to 2.7 atm and CH4 mole fraction ranging from 0.50 to 0.65. Computationally, the MC-Smooth vorticity–velocity formulation was employed to describe the reactive gaseous mixture, and soot evolution was modelled by sectional aerosol equations. The governing equations and boundary conditions were discretised on a two-dimensional computational domain by finite differences, and the resulting set of fully coupled, strongly nonlinear equations was solved simultaneously at all points using a damped, modified Newton's method. Experimentally, chemiluminescence measurements of CH* were taken to determine its relative concentration profile and the structure of the flame front. A thin-filament ratio pyrometry method using a colour digital camera was employed to determine the temperature profiles of the non-sooty, atmospheric pressure flames, while soot volume fraction was quantified, after evaluation of soot temperature, through an absolute light calibration using a thermocouple. For a broad spectrum of flames in atmospheric and elevated pressures, the computed and measured flame quantities were examined to characterise the influence of pressure and fuel dilution, and the major conclusions were as follows: (1) maximum temperature increases with increasing pressure or CH4 concentration; (2) lift-off height decreases significantly with increasing pressure, modified flame length is roughly independent of pressure, and flame radius decreases with pressure approximately as P?1/2; and (3) pressure and fuel stream dilution significantly affect the spatial distribution and the peak value of the soot volume fraction. 相似文献
173.
Peter A. Beckmann Kendra S. Burbank Matty M. W. Lau Jessica N. Ree Tracy L. Weber 《Chemical physics》2003,290(2-3):241-250
We report and interpret the temperature dependence of the proton spin–lattice relaxation rate at 8.50 and 22.5 MHz in four polycrystalline solids composed of structurally related molecules: 2-ethylanthracene, 2-t-butylanthracene, 2-ethylanthraquinone, and 2-t-butylanthraquinone. We have been unable to grow single crystals and therefore do not know the crystal structures. Hence, we use the NMR relaxometry data to make predictions about the solid state structures. As expected, we are able to conclude that the ethyl groups do not reorient in the solid state but that the t-butyl groups do. The anthraquinones have a “simpler” structure than the anthracenes. The best dynamical models suggest that there is a unique crystallographic site for the t-butyl groups in 2-t-butylanthraquinone and two sites, each with half the molecules, for the ethyl groups in 2-ethylanthraquinone. There are also two sites in 2-ethylanthracene, but with unequal weights, suggesting four sites in the unit cell with lower symmetry than the two anthraquinones. Finally, the observed relaxation rate data in 2-t-butylanthracene is very complex and its interpretation demonstrates the uniqueness problem that arises in interpreting relaxometry data without the knowledge of the crystal structure. 相似文献
174.
An autoregressive-moving average model in which all roots of the autoregressive polynomial are reciprocals of roots of the moving average polynomial and vice versa is called an all-pass time series model. All-pass models generate uncorrelated (white noise) time series, but these series are not independent in the non-Gaussian case. An approximate likelihood for a causal all-pass model is given and used to establish asymptotic normality for maximum likelihood estimators under general conditions. Behavior of the estimators for finite samples is studied via simulation. A two-step procedure using all-pass models to identify and estimate noninvertible autoregressive-moving average models is developed and used in the deconvolution of a simulated water gun seismogram. 相似文献
175.
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177.
A new method for the quantification of butenafine hydrochloride (BTF) present in the main skin layers was validated and a study conducted with the aim of analyzing the penetration and/or the permeation of the drug. The quantification was performed by liquid chromatography. To evaluate the specificity of the method, the influence of the components of the skin was analyzed, as well as the skin in contact with the excipient ingredients. Linearity was assessed with concentrations in the range of 0.1–10 μg/mL (r 2 = 0.9999) and ANOVA showed non‐significant linear deviation (p > 0.05). Adequate results were obtained for repeatability, intra‐day precision and accuracy. The obtained values for the limit of quantification and the limit of detection were 68.4 and 17.7 ng/mL, respectively. Also, a comparative study of BTF cutaneous penetration through porcine skin was performed applying two different formulations: Tefin, present in the Brazilian market, and Lotrimin Ultra®, available in the American market. No statistical difference was found in the skin (epidermis plus dermis) and in the epidermis (p > 0.05), although in the dermis the difference was significant (p < 0.05). During the experimental period (8 h), no drug permeation from either formulation was detected in the receptor fluid. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
178.
Liu HF McCooey B Duarte T Myers DE Hudson T Amanullah A van Reis R Kelley BD 《Journal of chromatography. A》2011,1218(39):6943-6952
Cation exchange chromatography using conventional resins, having either diffusive or perfusive flow paths, operated in bind-elute mode has been commonly employed in monoclonal antibody (MAb) purification processes. In this study, the performance of diffusive and perfusive cation exchange resins (SP-Sepharose FF (SPSFF) and Poros 50HS) and a convective cation exchange membrane (Mustang S) and monolith (SO(3) Monolith) were compared. All matrices were utilized in an isocratic state under typical binding conditions with an antibody load of up to 1000 g/L of chromatographic matrix. The dynamic binding capacity of the cation exchange resins is typically below 100 g/L resin, so they were loaded beyond the point of anticipated MAb break through. All of the matrices performed similarly in that they effectively retained host cell protein and DNA during the loading and wash steps, while antibody flowed through each matrix after its dynamic binding capacity was reached. The matrices differed, though, in that conventional diffusive and perfusive chromatographic resins (SPSFF and Poros 50HS) demonstrated a higher binding capacity for high molecular weight species (HMW) than convective flow matrices (membrane and monolith); Poros 50HS displayed the highest HMW binding capacity. Further exploration of the conventional chromatographic resins in an isocratic overloaded mode demonstrated that the impurity binding capacity was well maintained on Poros 50HS, but not on SPSFF, when the operating flow rate was as high as 36 column volumes per hour. Host cell protein and HMW removal by Poros 50HS was affected by altering the loading conductivity. A higher percentage of host cell protein removal was achieved at a low conductivity of 3 mS/cm. HMW binding capacity was optimized at 5 mS/cm. Our data from runs on Poros 50HS resin also showed that leached protein A and cell culture additive such as gentamicin were able to be removed under the isocratic overloaded condition. Lastly, a MAb purification process employing protein A affinity chromatography, isocratic overloaded cation exchange chromatography using Poros 50HS and anion exchange chromatography using QSFF in flow through mode was compared with the MAb's commercial manufacturing process, which consisted of protein A affinity chromatography, cation exchange chromatography using SPSFF in bind-elute mode and anion exchange chromatography using QSFF in flow through mode. Comparable step yield and impurity clearance were obtained by the two processes. 相似文献
179.
Zebra finches produce a learned song that is rich in harmonic structure and highly stereotyped. More is generally known about how birds learn and produce this song than how they perceive it. Here, zebra finches were trained with operant techniques to discriminate changes in natural and synthetic song motifs. Results show that zebra finches are quite insensitive to changes to the overall envelope of the motif since they were unable to discriminate more than a doubling in inter-syllable interval durations. By contrast, they were quite sensitive to changes in individual syllables. A series of tests with synthetic song syllables, including some made of frozen noise and Schroeder harmonic complexes, showed that birds used a suite of acoustic cues in normal listening but they could also distinguish among syllables simply on the basis of the temporal fine structure in the waveform. Thus, while syllable perception is maintained by multiple redundant cues, temporal fine structure features alone are sufficient for syllable discrimination and may be more important for communication than previously thought. 相似文献
180.
Yanling Ma Shu Yan Zhang Chris Goodway Robert Done Beth Evans Oleg Kirichek 《高压研究》2013,33(3):364-375
Positions of elastic plastic interfaces play a vital role in safe design and safe use of high pressure vessels. The ENGIN-X neutron diffractometer at the ISIS facility was used to measure the residual strain profiles in a series of aluminium vessels which had been subjected to different pressure levels. The positions of elastic plastic interfaces of the autofrettaged pressure vessels were identified. The results revealed that the residual strain magnitude and the depth of the plastic region will increase with increasing autofrettage pressure level. When autofrettage pressure produces an elastic-plastic boundary at a greater depth than the geometric mean position of the vessel wall, reverse yielding will occur, hence the loss of the vessels’ elastic ability to its subsequent loading. The neutron experimental results agreed well with both the suggestions from existing literatures and the results from FE simulations. 相似文献