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71.
The multiple melting behavior of poly(ethylene terephthalate) (PET) was investigated with differential scanning calorimetry (DSC) by examining PET samples having been subjected to special schemes of crystallization and annealing treatment at multiple descending temperatures. Upon such step-wise annealing in decreasing temperatures, the existence of doublet melting peaks in addition to a series of multiple minor peaks in the PET has been demonstrated using carefully designed thermal schemes. Using the Hoffman theory, multiple lamellae populations, might be suggested to be simultaneously present in the PET subjected to such thermal treatments. However, direct experimental evidence has yet to be provided. The low-temperature minor crystals simply melt during normal scanning without having time enough to reorganize into higher-melt crystals. Nevertheless, the effect of scanning on non-isothermal crystallization does exist but is primarily confined to the temperature range much below the main melting region where the crystallization of polymer chains can progress at a reasonable rate. At higher temperatures near the main melting region, annealing for extended times is required in order to result in relative changes of the melting endotherms of the upper and lower peaks in the main melting doublet. In all we have shown that interpretations of the multiple melting phenomenon in semicrystalline polymers can be better refined. 相似文献
72.
The effects of concentrations of surfactant (sodium lauryl sulfate [SLS]) and initiator (sodium persulfate [SPS]) on the polymerization of homogenized styrene emulsions, stabilized by SLS/lauryl methacrylate (LMA) or SLS/stearyl methacrylate (SMA), were studied. The rate of polymerization increases with increasing [SLS] or [SPS]. In addition to monomer droplet nucleation, the formation of particle nuclei in the aqueous phase (homogeneous nucleation) plays a crucial role in the polymerization kinetics. In comparison with the LMA containing polymerization system, monomer droplet nucleation becomes more important when the more hydrophobic SMA was used as the costabilizer. Furthermore, the degree of homogeneous nucleation increases with increasing [SPS]. 相似文献
73.
The thermodynamic properties of saturated aqueous lanthanide nitrate solutions were determined using recently published critically evaluated solubility and activity data. The variation of the thermodynamic functions and congruent melting points as a function of atomic number are interpreted in terms of changes in inner sphere coordination number in both the solid hexahydrates and in the aquo ions, and in terms of the double-double effect.Inconsistencies in experimental solubility data are generally caused by uncertainties in solid phase composition which is shown to be due to the very small Gibbs energies accompanying transitions from stable to metastable systems differing in the number of hydrating water molecules.Presentation to First International Symposium on Solubility Phenomena, University of Western Ontario, London, Ontario, August 21–23, 1984. 相似文献
74.
Summary The effect of extraction cell dimensions (i.d.: length) on supercritical fluid extraction (SFE) efficiencies of polychlorinated biphenyls (PCBs) is shown to be dependent on the type of sorbent used. For octadecylsilane (C18) sorbents, there is a significant increase in observed SFE recoveries of PCBs when the cell dimensions are made more broad (increased i.d.: length); whereas, no effect of cell geometry is observed when the common adsorbent, Florisil, is utilized. Additionally, recoveries decreased in proportion to the chlorine number, for the PCBs studied, for octadecylsilane sorbents, while no such effect was observed for Florisil. These results illustrate the magnitude of the matrix effect in SFE, which generally dominated observed recoveries, even in the simplest analyte/sorbent systems such as the one studied here. 相似文献
75.
Maria Grazia Bonicelli Gianfranco Ceccaroni Franco Gauzzi Giuseppe Mariano 《Thermochimica Acta》2005,430(1-2):95-99
Differential scanning calorimetry (DSC) and particle size measurements were carried out on disproportionation products of pure SnO to investigate the fusion and solidification behaviour of Sn droplets and their catalytic nucleation on Sn oxides. If disproportionation reaction takes place at T ≥ 798 K, the products are metallic Sn and SnO2; but for 523 < T < 798 K, SnO2 is replaced by an intermediate oxide (IO) SnxO(1+x). On melting, samples with IO show a drop of melting point of metallic tin due to Gibbs–Thomson effect; no lowering of melting point was observed in samples with SnO2. On the other hand, if solidification occurs in the presence of IO, Tin droplets always displayed three distinct exothermic solidification peaks, but if it takes place in the presence of SnO2, only one exothermic peak is observed. Undercooling values and contact angles were determined for each of the heterogeneous nucleation processes. The different behaviour of metallic Tin droplets was related to the different lattice symmetry of SnO2 and IO, which act as nucleation catalysts. 相似文献
76.
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78.
Min-zhi Chen Xiao-liang Wang Fang-fang Tao Qi Xue Ping-chuan 《高分子科学》2007,(1):107-111
The concept of entanglement provides the basis of our current understanding of the flow behavior of polymer melts, Current techniques developed to investigate the degree of interpenetration of polymer chains only provide indirectly the information of the degree of entanglement in a relatively large scale (several to tens of nanometer). In this article, we report ^1H-NMR spectroscopy with dipolar filters under fast magic angle spinning for probing chain interpenetration of polymer glasses at the molecular level. 相似文献
79.
The way to measure quantitatively full dissolution and crystallization of polyamides in water up to 200 °C and above by DSC is described. Stainless-steel high-pressure pans enable research on fully dissolving polyamides in water under vapor pressure. The results show clearly that polyamide 6 (PA6) is soluble in water under vapor pressure in the whole concentration range and that water acts as a crystallization and melting point suppressor. The maximum temperature depression is approximately 60 °C. This depression of the transitions is independent of concentration over a large range (10-70 mass% PA6 in water). When PA6 dissolves in water during heating, the polymer often sets to the sides of the DSC sample pan. Because of this the contact between the sample and the bottom of the pan reduces during measurement and therefore DSC heating curves are frequently curved. Adding steel wool to these stainless-steel high-pressure pans improves the measurements by increasing the thermal conductivity between the sample and pan bottom, and as a result the DSC curves become less curved. The interpretation of the measurements improves and the possibility of reproducible peak area calculations also in heating comes in sight. 相似文献
80.
Direct in situ determination of PGE1 in dioxane/water (1:1) at concentrations between 50 μg/ml and 1 mg/ml is described. HPTLC of PGE1 was carried out on HPTLC Kieselgel 60 o.F. plates; application (200 nl) was with a Nano-Appllcator and ethyl acetate/formic acid (400:5, v/v) served as mobile phase. The spots were located by dipping the plates into a 3% cupric acetate solution in 15% aqueous phosphoric acid, followed by heating at 120°C for 15 min. The plates were then evaluated directly at λ = 345 nm by chromatogram spectrometry. The coefficient of variation is 3.6%. 相似文献