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991.
Xing Chen Wenguang Zhao Feng Wang Jie Xu .Dalian National Laboratory for Clean Energy State 《天然气化学杂志》2012,(5):481-487
Preparation of dispersed transition metal oxides catalyst with low oxidation state still remains a challenging task in heterogeneous catalysis.In this study,vanadium oxides supported on zeolite SBA-15 have been prepared under hydrothermal condition using V 2 O 5 and oxalic acid as sources of vanadium and reductant,respectively.The structures of samples,especially the oxidation state of vanadium,and the surface distribution of vanadium oxide species,have been thoroughly characterized using various techniques,including N 2-physisorption,X-ray diffraction(XRD),transmission electron microscopy(TEM),X-ray photoelectron spectroscopy(XPS),UV-visible spectra(UV-Vis) and UV-visible-near infrared spectra(UV-Vis-NIR).It is found that the majority of supported vanadium was in the form of vanadium(IV) oxide species with the low valence of vanadium.By adjusting hydrothermal treatment time,the surface distribution of vanadium(IV) oxide species can be tuned from vanadium(IV) oxide cluster to crystallites.These materials have been tested in the hydroxylation of benzene to phenol in liquid-phase with molecular oxygen in the absence of reductant.The catalyst exhibits high selectivity for phenol(61%) at benzene conversion of 4.6%,which is a relatively good result in comparison with other studies employing molecular oxygen as the oxidant. 相似文献
992.
Chia-Wen Lu Yan Cao Hui Li Cathleen Webb Wei-Ping Pan 《Journal of Thermal Analysis and Calorimetry》2014,116(3):1241-1248
Titanium dioxide (TiO2), especially in its anatase form, is an effective photocatalyst under ultraviolet (UV) light. The particle size of TiO2 is a critical factor to determine its photoactivity based on its quantum effectiveness under light irradiations. Thus, nanocrystalline TiO2 has been widely accepted to significantly enhance this effect. The sol–gel method is generally used to synthesize the anatase form of nanocrystalline TiO2. In this study, we expanded the synthesis method of TiO2 to high pressures under direct heating (hydrothermal method) and indirect heating (microwave-assisted method). It was found that pH value is one of the major factors to control nano-sizes of TiO2 particles, and the neutral condition in all methods is preferable for controlling the sizes of the prepared TiO2 particles. The microwave-assisted method further improves quality of synthesized nano-size TiO2 below 10 nm. These results have been confirmed by both the direct size measurement using TEM images and indirect determination using XRD peaks. The collected samples are further analyzed using UV–Vis spectroscopy to identify the particle size-dependent photoreactivity and to confirm the effectiveness of microwave-assisting under neutral conditions. DSC is also a powerful tool to identify the crystalline transition of TiO2. 相似文献
993.
994.
995.
Xiaoji Cao Jingfang Qiao Liping Wang Xuemin Ye Lebin Zheng Nan Jiang Weimin Mo 《Rapid communications in mass spectrometry : RCM》2012,26(7):740-748
A powerful ionic liquid‐based ultrasonic‐assisted extraction (ILUAE) method combined with ultra‐performance liquid chromatography coupled to electrospray ionization quadrupole time‐of‐flight tandem mass spectrometry (UPLC/ESI‐QTOFMSn) was employed in the rapid simultaneous screening of iridoid glycosides, phenylethanoid glycosides, and cucurbitacin glycosides from P. scrophulariiflora. The ILUAE procedure was optimized over several ultrasonic parameters, including the ultrasonic power, concentration of the ionic liquid, and solid–liquid ratio. A comparison with conventional heat‐reflux extraction and regular UAE demonstrated that the optimized approach yielded a high extraction efficiency (Picroside I, 2.84%; Picroside II, 3.57%; 6‐O‐E‐feruloyl catalpol, 2.20%) within a short extraction time of 30 min. Negative ion mode ESI‐QTOFMS2 analysis of the fragmentation reactions of the [M–H]– ions was conducted to characterize the diagnostic ions related to the glycosyl moieties, aglycone units, and the type and substituted position of the ester groups. Interestingly, the positional isomers of the iridoid glycosides could be easily discriminated based on the characteristic ions. A total of 15 glycosides, including three groups of iridoid glycoside isomers and two groups of phenylethanoid glycoside isomers, were conveniently identified within 13.5 min. Moreover, 6'‐O‐vanilloyl catalpol was identified in P. scrophulariiflora for the first time. The method developed here was further validated by measuring the recovery, correlation coefficient (R2), and reproducibility (RSD, n = 5) of three iridoid glycosides: 89.60%–109.02%, 0.9991–0.9998, and 0.93%–1.44%, respectively. This study demonstrated the capabilities of ILUAE combined with UPLC/ESI‐QTOFMSn for the rapid screening of glycosides in P. scrophulariiflora. This method offers an approach to similar studies on other natural plants. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
996.
997.
Mei Tian Huan Huan Sun Xiao Wei Tian Zhi Xin Xu Feng Qiao Wang Dan Shu Yao 《Liquid crystals》2013,40(3):298-308
A series of side-chain liquid crystal (LC) polysiloxanes were synthesised with Poly(methylhydrogeno)siloxane, 4?-(undec-10-enoyloxy) biphenyl – 4 – yl 4- (trifluoromethyl) benzoate (Mth) and a chiral nematic (N*) LC monomer 1-allyl 10-(cholesteryl)-decanedioate (Mch). The chemical structures and LC properties of the monomers and polymers were characterised by FTIR, 1H-NMR, differential scanning calorimetry, thermogravimetric analysis, POM and X-ray diffractometer. Mch is monotropic N* LC. The homopolymer derived from monomer Mch is enantiotropic N* LC. Monomer Mth is a smectic A liquid crystal. The copolymers derived from Mch and Mth are N* LCs. The temperatures at which 5% weight loss occurred are greater than 300°C for all the fluoro-containing polymers, and the residue weights of the samples at 600°C increased slightly as the content of trifluoromethyl mesogens increased in the polymers. The glass transition temperatures of the polymers increased as trifluoromethyl mesogens increased, too. The N*–I phase transition temperatures show a negative deviate from ideal or linear behaviour. The values of the enthalpy changes for the cholesteryl containing polymers are rather low and this is attributed to the biaxiality of cholesteryl moiety which tends to reduce the change in the orientational order at the N*–I transition. Compared to the monomers, the polymers show wider mesophase region. 相似文献
998.
999.
Dr. Chun-Xiao Li Qian Ning Wenxuan Zhao Hou-Ji Cao Yi-Ping Wang Prof. Dr. Hong Yan Prof. Dr. Chang-Sheng Lu Prof. Dr. Yong Liang 《Chemistry (Weinheim an der Bergstrasse, Germany)》2021,27(8):2699-2706
The convenient cross-coupling of sp2 or sp3 carbons with a specific boron vertex on carborane cage represents significant synthetic values and insurmountable challenges. In this work, we report an Rh-catalyzed reaction between o-carborane and N-acyl-glutarimides to construct various Bcage−C bonds. Under the optimized condition, the removable imine directing group (DG) leads to B(3)− or B(3,6)−C couplings, while the pyridyl DG leads to B(3,5)−Ar coupling. In particular, an unexpected rearrangement of amide reagent is observed in pyridyl directed B(4)−C(sp3) formation. This scalable protocol has many advantages, including easy access, the use of cheap and widely available coupling agents, no requirement of an external ligand, base or oxidant, high efficiency, and a broad substrate scope. Leveraging the RhI dimer and twisted amides, this method enables straightforward access to diversely substituted and therapeutically important carborane derivatives at boron site, and provides a highly valuable vista for carborane-based drug screening. 相似文献
1000.
The first total synthesis of isoquinolinone alkaloid marinamide 1 and its methyl ester 2 was described. The key steps involved a regioselective Frieclel-Crafts reaction of 1-benzyl-1H-pyrrole to form the intermediate 8. 相似文献