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991.
The crystal structures of six members of the homologous series with general formula [BiQX]2[AgxBi1?xQ2?2xX2x?1]N+1 (Q = S, Se; X = Cl, Br; 1/2 ≤ x ≤ 1) and N = 4, 5, or 7 were determined by single‐crystal X‐ray diffraction. The series are characterized by the parameters N and x and are denoted (N, x)P. Ag3Bi4S6Cl3 (x = 0.60) (I) , Ag3.5Bi3.5S5Br4 (x = 0.70) (II) and Ag3.65Bi3.35Se4.70Br4.30 (x = 0.73) (III) belong to (4, x)P series Ag5xBi7?5xQ12?10xX10x?3 and adopt the AgBi6S9 structure type. The (5, x)P compound Ag3.66Bi4.34S6.68Br3.32 (IV) , which corresponds to x = 0.61 in Ag6xBi8?6xS14?12xBr12x?4, crystallizes isostructurally to AgBi3S5. The compounds Ag4.56Bi5.44Se8.88Br3.12 (x = 0.57) (V) and Ag5.14Bi4.86S7.76Br4.24 (x = 0.64) (VI) , which are members of (7, x)P series Ag8xBi10?8xQ18?16xBr16x?6, adopt the Ag3Bi7S12 structure type. In the monoclinic crystal structures (space group C2/m) two kinds of layered modules alternate along [001]. Modules of type A uniformly consist of paired rods of face‐sharing monocapped trigonal prisms around Bi atoms with octahedra around mixed occupied metal positions (M = Ag/Bi) between them. Modules of type B are composed of [MZ6] octahedra, which are arranged in NaCl‐type fragments of thickness N. All structures exhibit Ag/Bi disorder in octahedrally coordinated metal positions as well as Q/X mixed occupation of some anion positions. Corresponding to their black color, all compounds are narrow‐gap semiconductors (Eg = 0.35 eV for (II) ). General characteristics of the entire class of (N, x)P compounds are gathered in a catalogue. 相似文献
992.
993.
The hyphenation of CE with MS is nowadays accepted as a powerful analytical approach. Employing ESI, the most common interface, one challenge is to provide quantitative information, which is quite a difficult task, as it is linked, among other factors, to suction and dilution effects. In the coaxial ESI configuration, the suction effect has been presented in literature as stemming from nebulizing gas (NG) flow rate and drying gas temperature. But as this interface consists in three concentric capillaries, allowing for BGE, sheath liquid (SL) and NG mixing, it is demonstrated herein that other parameters are also involved in this suction effect: the CE capillary protrusion from the interface needle, SL flow rate, and overall BGE flow rate and velocity profile. Whereas NG flow rate is the parameter affecting suction to a greater extent, separation capillary protruding length, SL, and overall BGE flow rate have a significant additional impact on this phenomenon. It is shown that SL flow rate can affect suction differently according to the NG velocity, which may be explained by modification of the Taylor cone geometry. Furthermore, it appears that suction effect is noticeably favored by a parabolic velocity profile of the BGE, again probably due to the Taylor cone shape modification. Finally, the temperature gradient created by the contact between the heated NG and the separation capillary enhances this effect. 相似文献
994.
Philippini V Vercouter T Aupiais J Topin S Ambard C Chaussé A Vitorge P 《Electrophoresis》2008,29(10):2041-2050
The electrophoretic mobilities (mu ep,Ln) of twelve lanthanides (not Ce, Pr and Yb) were measured by CE-ICP-MS in 0.15 and 0.5 mol L(-1) Alk2 CO3 aqueous solutions for Alk+ = Li+, Na+, K+ and Cs+. In 0.5 mol L(-1) solutions, two different mu ep,Ln values were found for the light (La to Nd) and the heavy (Dy to Tm) lanthanides, which suggests two different stoichiometries for the carbonate limiting complexes. These results are consistent with a solubility study that attests the Ln(CO3)3(3-) and Ln(CO3)4(5-) stoichiometries for the heavy (small) and the light (big) lanthanides, respectively. The Alk+ counterions influence the mu ep,Ln Alk2 CO3 values, but not the overall shape of the mu ep,Ln Alk2 CO3 plots as a function of the lanthanide atomic numbers: the counterions do not modify the stoichiometries of the inner sphere complexes. The influence of the Alk+ counterions decreases in the Li+ > Na+ > K+ > Cs+ series. The K3,Ln stepwise formation constants of the Ln(CO3)3(3-) complexes slightly increase with the atomic numbers of the lanthanides while K4,Ln, the stepwise formation constants of Ln(CO3)4(5-) complexes, slightly decrease from La to Tb, and is no longer measurable for heavier lanthanides. 相似文献
995.
An automated on-line method for the determination of the substituted aniline compounds was developed using in-tube solid-phase microextraction coupling to high-performance liquid chromatography (HPLC). In this work, oxidized multiwalled carbon nanotubes (MWCNTs-COOH) coated on the outer surface of the fused-silica tube and inserted in the polyether ether ketone (PEEK) tubing, which was fixed directly on the six-port injection valve to substitute for the sample loop. The extraction procedure was performed by a constant flow pump frequently driving the sample solution through the PEEK tubing and the analytes were adsorbed onto MWCNTs-COOH materials when the six-port valve set to load position. After extraction, the valve switched to inject position and the extracted analytes were desorbed by mobile phase in dynamic mode. High extraction capacity was achieved for the investigated analytes and great improvement of the limits of detection was obtained in comparison with other methods. The calibration plots were linear (r(2)> or =0.9949) over the concentration range of 1.04-104ngmL(-1) for 4-nitroaniline, 1.02-102ngmL(-1) for 2-nitroaniline, 1.68-168ngmL(-1) for 2-chloroaniline and 1.09-109ngmL(-1) for 2,4-dichloroaniline. The detection limit ranged from 0.04ngmL(-1) to 0.13ngmL(-1) (at S/N=3). The possibility of applying the established method to water samples analysis was also studied. 相似文献
996.
1-Decyl-2,3-dimethylimidazolium bromide (ddmimBr) has been synthesized by the reaction of 1,2-dimethylimidazole and 1-bromodecane. Micellization of ddmimBr surfactant in water (W) and water-ethanolamine (W-EA) with the weight percent of EA changing within the range 0-39.79%, has been investigated at 298.15 K. Information about the influence of the added EA on the critical micelle concentration (CMC) was obtained through density and surface tension measurements. This last provides information about the dependence of the surface excess concentration, the minimum area per surfactant molecule and the surface pressure at the CMC on the added weight percentage of organic solvent. The effect of binary aqueous mixtures of W-EA on the apparent molar volume (phi V) of the ddmimBr has been investigated. The apparent molar volume upon aggregation (Delta phi V) shows a maximum at about 15 wt% of EA, this behavior is discussed in terms of the changes of the solvent structure. Partial specific volume data, obtained by density measurements, indicate that the fraction of solvent molecules interact with the surfactant remained roughly constant. 相似文献
997.
Thierry Brunin Benoît Rigo Jean‐Pierre Hénichart 《Journal of heterocyclic chemistry》2008,45(5):1525-1528
A new ring‐switching reaction of enaminoesters behaving as bisnucleophiles towards other enaminoesters behaving as biselectrophiles is described. By starting from pyroglutamic derivatives, this reaction provided easy access to methyl 5‐oxo‐1,2,3,5‐tetrahydro‐3‐indolizinecarboxylates substituted by an aminoester side chain in position 6. 相似文献
998.
Karine Scarpellini‐Charras Gérard Boyer Nathalie Filloux Jean‐Pierre Galy 《Journal of heterocyclic chemistry》2008,45(1):67-70
The preparation of symmetric 2,2′‐dimethoxy‐10,10′‐biacridinyl‐9,9′‐dione atropisomers were obtained by the oxidative coupling of 9(10H)‐acridinone with 1,3‐dibromo‐5,5‐dimethyl‐imidazolidine‐2,4‐dione 相似文献
999.
Arno Behr Thomas Beckmann Pierre Schwach 《Journal of organometallic chemistry》2008,693(18):3097-3102
Two different routes to acetoxyoctadiene are presented. The first one uses the well-known telomerisation of butadiene with acetic acid operating in a multiphase semi-batch mode. The second reaction involves the cleavage of acetic anhydride, hydrogen transfer via ketene formation and thus a telomerisation as well. 相似文献
1000.
Frédéric Clabau Pierre Bonville Thierry Le Mercier Stéphane Jobic 《Journal of solid state chemistry》2008,181(6):1456-1461
The fluorescence and phosphorescence properties of Europium-doped MAl2Si2O8 (M=Ca, Sr, Ba) are reinvestigated and discussed on the basis of the propensity of an activator to agglomerate with an oxygen vacancy. Due to a stronger attraction of the anion vacancy towards Eu2+ cations going from BaAl2Si2O8 to SrAl2Si2O8 and CaAl2Si2O8 host lattices, the interpretation of the fluorescence spectra turns out to be less trivial in the Ca and Sr host lattices than in the Ba one and requests the account for Eu2+ cations lying at alkaline-earth sites with or without vacancy in their neighborhood. Phosphorescence in these compounds is highlighted. 相似文献