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Ahmad Al-Alousy Saad Alshehri John Burgess Maria del Mar Graciani Maria-Luisa Moya Ernestina Muñoz Amalia Rodriguez Francisco Sanchez 《Transition Metal Chemistry》1993,18(2):179-181
Summary Dependences of rate constants on pressure (up to 1 kbar) and on added salt concentration (up to 6.0 mol dm–3 LiNO3, NaNO3, NaCl, Na2SO4 or KNO3) have been established for dissociative substitution of pentacyanoferrates(II), [Fe(CN)5L]3– with L = 4-cyanopyridine, 4,4-bipyridyl, 4-phenylpyridine and 4-t-butylpyridine. Activation volumes derived directly from pressure effects, and indirectly from salt effects via surface tension dependences and derived surfaces of activation, are reported, compared and discussed. 相似文献
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Garcia EM Sanchez MD Tonetto G Volpe MA 《Journal of colloid and interface science》2005,292(1):179-185
The preparation of different samples of vanadia supported on ultrastable zeolite (VO(x)/USY) is discussed. The samples were prepared in order to obtain highly dispersed V-species, avoiding the formation of crystalline vanadia and the destruction of the zeolite framework. Two methods were employed for preparing VO(x)/USY samples: an organic route using V(AcAc)3 and an inorganic route using NH4VO3. The characterization of the samples was performed with XRD, TPR, NH3-TPD, and N2 isotherms. From these results it is concluded that when VO(x) is supported on the surface of USY from acidic aqueous solution of ammonium metavanadate, the destruction of the zeolite framework is accomplished. For higher pH values in the impregnating solution, undesired V2O5 is formed on the USY surface. On the other hand, VO(x)/USY prepared from the organic precursor shows no destruction of the USY structure. In addition, highly dispersed VO(x) are formed, though for relatively high V loadings (6%) an obstruction of the zeolite windows takes place. The samples are tested as catalysts for gas phase dehydrogenation of n-butane to olefins. The catalysts prepared from NH4VO3 are almost inactive for the reaction. On the other hand, both samples prepared from V(AcAc)3 present initial conversion levels in the 8-12% range. However, the selectivity depends on the V loading, the catalysts with 6% loading being the most selective (75%). The catalytic patterns of the samples (activity and selectivity) are in agreement with the physicochemical features of the VO(x)/USY surface. 相似文献
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Solid solutions of GeO2 in Fe2O3 were prepared by mechanically mixing the solids and firing at 1000°C in air, and from a gel obtained by the addition of an alcohol solution of germanium ethoxide to iron dissolved in HNO3. The dried gel was then heated at 1000°C. The solubility limit is 5 mole% GeO2, Fe1.95Ge0.05O3. Similar procedures were used to prepare solid solutions with Si and the solubility limit is greater than 4 mole% SiO2. Firing of mixtures or gels of Fe2O3 containing Mg produces a spinel phase even at the lowest detectable concentrations. The resistivity of pressed pellets of Fe2?xGexO3 varies from about 106 ohm-cm for x = 0 to about 10?1 ohm-cm for x = 0.05. The photoassisted electrolysis of water at Ge-doped Fe2O3 electrodes is demonstrated. The photoelectrochemical cell showed a 0.29-V open-circuit voltage, 1.2-mA/cm2 short-circuit current, 0.31 fill factor, and 0.06% power efficiency. 相似文献
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M. Chatry M. Henry M. In C. Sanchez J. Livage 《Journal of Sol-Gel Science and Technology》1994,1(3):233-240
The hydrolysis and condensation of zirconium n-propoxide in n-propanol have been chemically controlled via the complexation of the zirconium precursor with acetylacetone. The size of the zirconium oxide-based particles is mainly controlled by the complexation ratio x=[acac]/[Zr]. the mean size increases from nanometric to submicronic range when x decreases from 1 to 0.1. Amorphous colloidal particles are obtained at room temperature. They result from a competitive growth/termination mechanism of zirconium-oxo species in the presence of acac surface capping agents. However non-aggregated nanocrystalline particles of tetragonal zirconia, about 2 nm in diameter are formed upon aging at 60°C when hydrolysis is performed in the presence of paratoluene sulfonic acid (PTSA). 相似文献
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A multiresidue, automated and rapid method for the determination of pesticide residues in olive oil is presented. The method employs the through oven transfer adsorption-desorption interface for the on-line coupling of reversed-phase liquid chromatography and gas chromatography. In this fully automated system, olive oil is directly injected with no sample pre-treatment step other than filtration. Methanol-water is used as eluent in the liquid chromatography pre-separation step. The selected liquid chromatography fraction containing the pesticides is automatically transferred to the gas chromatography. The liquid chromatography column flow during elution is different from the flow during the transfer. Using a flame ionisation detector, pesticide detection limits varied from 0.1 to 0.3 mg/l. 相似文献
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Starting with 1,1-dimethoxy-2-propanone ( 1 ), 6-formyl-1,2-dihydro-2-oxo-3-pyridinecarboxylic acid ( 5a ) has been prepared in large quantities by a highly efficient, 4-step synthesis. This compound, along with its one carbon homologue, 6-acetyl-1,2-dihydro-2-oxo-3-pyridinecarboxylic acid ( 5b ) has been reacted with several carbonyl derivative forming reagents to provide a series of side chains for β-lactams. Among these carbonyl derivatives are styrylamides which were prepared from Wittig and Horner-Emmons reagents. The preparation of the phosphonium salts and phosphonate esters is also described. 相似文献