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21.
Optical and Quantum Electronics - Numerical modelling of a Pr3+-doped chalcogenide glass fibre laser is presented in this paper. The spectroscopic parameters are extracted from in-house prepared...  相似文献   
22.

The article describes the syntheses and extraction properties of two p‐tert‐butylcalix[6]arene nitrile derivatives (3 and 4). The trinitrile derivative 3 has been synthesized from 5,11,17,23,29,35‐hexa‐tert‐butyl‐37,38,39,40,41,42‐hexahydroxycalix[6]arene 1. The compound 1 was directly converted to its hexanitrile derivative 4. In these syntheses, it was thought to explore the role of nitrile sites in the extraction of various metal cations and HCr2O7 ?/Cr2O7 2? anions. The liquid‐liquid extraction properties of 3 and 4 towards selected alkali/transition metal cations and HCr2O7 ?/Cr2O7 2? anions are reported. It has been observed that receptor 3 does not extract alkali/transition metal cations effectively, but shows affinity towards HCr2O7 ?/Cr2O7 2? anions at low pH. The compound 4 is an effective form for transferring Ni2+ selectively, while it shows poor transferring ability for HCr2O7 ?/Cr2O7 2? anions from an aqueous into a dichloromethane layer. It was observed that the cavity size of the calix[n]arenes and the cooperativity of the functionalities play important roles in two phase extraction systems.  相似文献   
23.
Crystalline films (thickness ~1 μm) of Prussian blue-based molecular magnets, synthesized using electrochemical method at two different reduction potentials ?0.5 and ?0.9 V, result into K0.1CrII 1.45[CrIII(CN)6]?·?mH2O (film 1) and K0.8CrII 1.1[CrIII(CN)6]?·?mH2O (film 2), respectively. The structural and magnetic properties of such films are investigated using atomic force microscopy (AFM), X-ray diffraction (XRD), infrared (IR) spectroscopy, and dc magnetization measurements. The film morphology, examined using AFM, shows uniformly distributed triangular crystallites over the substrate surface. The presence of CrIII–C≡N–CrII sequence, in the range of 1,900 to 2,300 cm?1 in IR spectra, confirms formation of Prussian blue analogues. The XRD results reveal information about the crystalline nature of the films and the relative intensities of the Bragg peaks change with the K+ ions. The exchange interaction between Cr ions through C≡N ligand confirms that the electron transfer from C≡N molecule to Cr ions is ferrimagnetic in nature. The high Curie temperatures (T C) are found to be ~195 and ~215 K for film 1 and film 2, respectively. The higher value of T C is attributed to the inclusion of more K+ ions for film 2, resulting decreases in the CrIII(C≡N)6 vacancies and increases in the number of nearest neighbors of CrII ions. The branching in the zero field-cooled and field-cooled magnetization data below Curie temperature is explained in terms of kinetic behavior of magnetic domains with different cooling conditions and the presence of water molecule vacancies in the lattice.  相似文献   
24.
Ahmet Kocak  Sait Malkondu 《合成通讯》2013,43(21):3697-3708
General methods for the preparation of a variety of pyridone and oxypyridine derivatives are described. 2‐,3‐,4‐Hydroxy pyridine and 2‐pyridinemethanol were alkylated with ethylene‐, propylene‐, and stryrene‐oxide and epichlorohydrin in the presence of different Lewis acids as a catalyst. The best yield of 3a was achieved in the presence of CdI2/BF3 · OEt2. The corresponding pyridone derivatives (3ad, 7ad) were obtained from the reaction of 2‐and 4‐hydroxypyridine with oxiranes in good yields, whereas oxypyridine derivatives (5ad, 9a,b) were obtained from reactions of 3‐hydroxypyridine and 2‐pyridinemethanol with oxiranes. Chlorohydrines (3d, 5d, 7d) were easily converted to corresponding epoxy derivatives (10, 11, 12) in basic medium; then amino alcohols (1317) were obtained from the reaction of these epoxy derivatives with amines.  相似文献   
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To measure the gold content of a catalyst accurately, neutron activation analysis (NAA) is one of the methods of choice. NAA is preferred for such heterogeneous catalysts because: (1) it requires minimal sample preparation; (2) NAA provides consistent and accurate results; and (3) in most cases results are obtained much quicker than competing methods. NAA is also used as a referee for the other elemental techniques when results do not fall within expected statistical uncertainties. However, at very high gold concentrations, applying NAA to determine the gold in a heterogeneous catalyst is more challenging than a routine NAA procedure. On the one hand, the neutron absorption cross section for gold is very high, resulting in significant self-shielding related errors. On the other hand, gold exhibits low energy resonance neutron absorptions. In this application the self-shielding minimization effort was handled more rigorously than the classic suppression of neutron flux within a specimen. This non-routine approach was used because: (1) for most applications, high accuracy, <3 % relative, is desired, (2) the low energy resonances of gold make its neutron reaction rate complex and (3) the TRIGA reactor flux profile used in this study contains both thermal and significant epithermal neutron fluxes. Accuracy and precision, using this new approach, are expected to improve from 15 % to better than 3 % relative uncertainty. This has been accomplished through a rigorous assessment of the observed effects of low energy resonance on the neutron flux spectral shape within the sample and designing an experiment to minimize the effects.  相似文献   
27.
In-situ liquid-state 29Si nuclear magnetic resonance was used to investigate the temporal concentration changes during ammonia-catalyzed initial hydrolysis of tetraethyl orthosilicate in different solvents (methanol, ethanol, n-propanol, iso-propanol and n-butanol). Dynamic light scattering was employed to monitor simultaneous changes in the average diameter of silica particles and atomic force microscopy was used to image the particles within this time frame. Solvent effects on initial hydrolysis kinetics, size and polydispersity of silica particles were discussed in terms of polarity and hydrogen-bonding characteristics of the solvents. Initial hydrolysis rate and average particle size increased with molecular weight of the primary alcohols. In comparison, lower hydrolysis rate and larger particle size were obtained in the secondary alcohol. Exceptionally, reactions in methanol exhibited the highest hydrolysis rate and the smallest particle size. Ultimately, our investigation elaborated, and hence confirmed, the influences of chemical structure and nature of the solvent on the formation and growth of the silica particles under applied conditions.  相似文献   
28.
This paper describes a novel approach to detect Cd(II) using the combination of the differential pulse anodic stripping voltammetry and magnetic nanoparticle based dispersive solid phase microextraction as an efficient, green and accurate method. Currents of Cd(II) increased linearly in the range from 75 to 2000 ng L−1 Cd(II) with a detection limit of 21.6 ng L−1. The RSD values of 2.6 and 6.0 % for 1.00 and 0.10 μg L−1 respectively showed that proposed method has an acceptable repeatability. Recovery values between 92.3 and 98.6 % showed that this approach can be successfully used for determination of Cd(II) in water samples.  相似文献   
29.
The present research work describes the productive synthesis of novel bisbenzopyronopyran derivatives 4(a-h) and 5(a-h) via the photocyclization reactions of bischromones 3(a-h) under the inert conditions. The latter compounds have been realized efficiently through the O-alkylation reactions of the 3-hydroxychromone 2 with suitable dihalogenated aliphatic/aromatic/heteroaromatic reagents in the presence of dry acetone/anhydrous K2CO3/Bu4N+I (PTC). The cyclization reaction of chalcone 1 under the Algar-Flynn-Oyamada reaction conditions (KOH/H2O2) could results in the formation of compound 2 in the good yield. The structural scaffolds of the newly prepared bischromones and resultant bisbenzopyronopyrans have been certified from the meticulous analysis of their various spectroscopic parameters such as UV-Vis, IR, 1H/13C-NMR, and ESI-MS. It was found that o/m/p-xylene and pyridine-linked final symmetrical bistetracycles exhibited higher antimicrobial potencies as compared to alkyl chain-linked cyclized products. The bischromones 3(a-h) could be able to endow modest level of antimicrobial behavior.  相似文献   
30.
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