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821.
Helio G. Bonacorso Liliane M.F. PorteJussara Navarini Gisele R. PaimFábio M. Luz Lenon M. OliveiraCarson W. Whietan Marcos A.P. MartinsNilo Zanatta 《Tetrahedron letters》2011,52(26):3333-3335
In this study, diethylaminosulfur trifluoride (DAST) was successfully applied in monofluorination reactions of some trifluoromethyl substituted 2-hydroxy-2H-chromenones, employing a general, mild, and efficient methodology. The fluorinated compounds (2-fluoro-2H-chromenones) were synthesized as unique products by a chemoselective reaction in 63-81% yield despite the presence of different reactive sites subjected to reactions with DAST. 相似文献
822.
Leandro J. Santos Ana S.P. Gonçalves Klaus Krambrock Maurício V.B. Pinheiro Marcos N. Eberlin Boniek G. Vaz Rossimiriam P. de Freitas Rosemeire B. Alves 《Journal of photochemistry and photobiology. A, Chemistry》2011,217(1):184-190
The preparation, characterization and photophysical properties of six new stable [6,6]-closed fullerene cycloadducts bearing five-membered heterocycles are described. The modified [60]fullerenes are obtained by a simple and rapid synthesis via a Bingel-type reaction with tetrazole and oxadiazole malonate derivatives. The photophysical kinetics of these new fullerene derivatives in toluene solution under ultraviolet illumination (375 nm, UVA) are studied by electron paramagnetic resonance and free-radical spin-trapping using α-phenyl-N-tert-butyl nitrone as a spin-trap. The results are compared with pure [60]fullerene and [6,6]-phenyl C61 butyric acid methyl ester (C60-PCBM). It is concluded that for all six new compounds as well as pure [60]fullerene and PCBM both superoxide and singlet oxygen are produced in the first stages of UVA illumination following the type I and II mechanisms, respectively. In all cases singlet oxygen is produced as the primary dominant species; however, the type I mechanism always occurs in parallel with type II. In the end, the superoxide is self-dismuted into hydroxyl radicals, thus yielding PBN-OH spin adducts (g = 2.007 and ahf (14N) = 1.54 mT). The kinetic reaction constants and their efficiencies in the production of reactive oxygen species at 375 nm and per mW of absorbed power are determined. The experimental results are consistent with an autocatalytic reaction model in which the system evolutes under UVA illumination, with superoxide catalyzing the conversion of singlet oxygen into more superoxide. 相似文献
823.
824.
Cristiane de A. Dias Henrique de Santana Marcos A. L. Nobre Mauro C. Lopes 《Journal of Solid State Electrochemistry》2013,17(7):1967-1976
A simple hybrid synthesis processing method was developed to synthesize γ-MnO2 nanocrystalline particles. The polyol method was modified by the addition of nitric acid in order to allow the synthesizing of single-phase Mn3O4 in a large scale. In the sequence, the acid digestion technique was used to transform Mn3O4 into γ-MnO2. Structural and morphological characterization was carried out by X-ray diffractometry, Infrared and Raman spectroscopy, thermogravimetric analysis, nitrogen adsorption isotherm, scanning electron microscopy, and transmission electron microscopy. The electrochemical properties were investigated by cyclic voltammetry and galvanostatic charge–discharge measurements. The synthesized material exhibits a specific capacitance of 125.1 F?g?1 at a mass loading of 0.98 mg?cm?2. The relation between structural features and electrochemical activity is discussed by comparing the synthesized material with commercial electrolytic manganese dioxide. 相似文献
825.
A procedure has been developed for the determination of bioavailable concentrations of selenium and arsenic in estuarine sediments employing inductively coupled plasma optical emission spectrometry (ICP OES) using a concomitant metals analyzer device to perform hydride generation. The optimization of hydride generation was done in two steps: using a two-level factorial design for preliminary evaluation of studied factors and a Doehlert design to assess the optimal experimental conditions for analysis. Interferences of transition metallic ions (Cd2+, Co2+, Cu2+, Fe3+ and Ni2+) to selenium and arsenic signals were minimized by using higher hydrochloric acid concentrations. In this way, the procedure allowed the determination of selenium and arsenic in sediments with a detection limit of 25 and 30 μg kg−1, respectively, assuming a 50-fold sample dilution (0.5 g sample extraction to 25 mL sample final volume). The precision, expressed as a relative standard deviation (% RSD, n = 10), was 0.2% for both selenium and arsenic in 200 μg L−1 solutions, which corresponds to 10 μg g−1 in sediment samples after acid extraction. Applying the proposed procedure, a linear range of 0.08-10 and 0.10-10 μg g−1 was obtained for selenium and arsenic, respectively. The developed procedure was validated by the analysis of two certified reference materials: industrial sludge (NIST 2782) and river sediment (NIST 8704). The results were in agreement with the certified values. The developed procedure was applied to evaluate the bioavailability of both elements in four sediment certified reference materials, in which there are not certified values for bioavailable fractions, and also in estuarine sediment samples collected in several sites of Guanabara Bay, an impacted environment in Rio de Janeiro, Brazil. 相似文献
826.
A simple, reproducible, and efficient liquid chromatographic method was developed with UV detection. Water (0.05% TFA):acetonitrile
(0.05% TFA) was used as the mobile phase in a gradient system for the determination of procyanidin B2 (PB2) and epicatechin
(EC) in the bark of Guazuma ulmifolia Lam. The analysis was performed using a Phenomenex Gemini RP C18 column (5 μm) as stationary phase, at 30 °C, with a flow rate of 0.8 mL min−1, at a wavelength of 210 nm for detection and determination. The main validation parameters of the method were also determined.
Calibration curves were found to be linear, with ranges of 20.00–150.00 (PB2) and 10.00–110.00 μg mL−1 (EC). The correlation coefficients of linear regression analysis were between 0.9981 and 0.9988, and the detection limits
were between 2.89 and 2.54 μg mL−1. The contents of PB2 and EC were successfully determined, with satisfactory reproducibility and recovery. Recoveries of the
PB2 and EC were 103.00 and 104.01%, respectively. The method was successfully applied to the determination of procyanidins
in the bark of G. ulmifolia. 相似文献
827.
On the effect of heat on the chemical composition and dimensions of thermally-modified wood 总被引:1,自引:0,他引:1
Marcos M. González-Peña Simon F. Curling Michael D.C. Hale 《Polymer Degradation and Stability》2009,94(12):2184-2193
Heat-induced weight loss (WL) and chemical and dimensional changes of small specimens of beech (Fagus sylvatica L.), Scots pine (Pinus sylvestris L.) and Norway spruce (Picea abies L.) wood were examined after thermal modification in the 190-245 °C temperature range. Treated specimens exhibited reductions in their oven-dry weight in line with the severity of the treatment, with the effect of increasing the temperature of exposure being greater than extending the period of treatment. Wood polysaccharides were found to be distinctly more labile than the lignin constituent; the latter increased possibly as a result of repolymerisation reactions trapping some degradation products in the process. Specimens shrank in the transversal plane in a tangential to radial ratio of 2:1 regardless of the treatment regime, while their length increased marginally for WL < 10-12%. It is proposed that the thermal modification leaves the cell wall material in a permanent strained state. 相似文献
828.
Marcos F.S. Teixeira Bruno H. Freitas Patricia M. Seraphim Leandra O. Salmazo Marcos A. Nobre Silvania Lanfredi 《Procedia Chemistry》2009,1(1):293-296
In the work described by this paper, we studied the development of a selective potassium ion sensor constituted of a carbon paste electrode modified (CPEM) with a novel KSr2Nb2O15. The material KSr2Nb2O15 is an oxide with the tetragonal tungsten bronze structure (TTB) type are in forefront both in the area of research as well as in industrial applications. The sensor response to potassium ions was linear in the concentration range 1.26 x 10-5 at 1.62 x 10-3 mol L-1 (E (mV) = 32.7 + 51.1 log [K+]). The sensor based KSr2Nb2O15, of the TTB-type presented very good potentiometric response, with a slope of 51.1 mV/dec (at 25 °C) and detection limit for the potassium ions of 7.27 x 10-5 mol.L-1. 相似文献
829.
830.
Wagna Piler Carvalho Santos Jacira Teixeira Castro Marcos Almeida Bezerra Andréa Pires Fernandes Sérgio Luis Costa Ferreira Maria Graças Andrade Korn 《Microchemical Journal》2009,91(2):153-158
In this paper, multivariate optimization was applied for the development of an ultrasound-assisted multielemental extraction procedure for analysis of bean samples by inductively coupled plasma optical emission spectrometry. For this procedure, powdered samples were treated with an acid mixture and submitted to ultrasound energy for extracting the target elements (Ba, Ca, Cu, Fe, K, Mg, Mn, Sr and Zn). Centroid simplex mixture design was used for optimize the acid proportions (nitric, acetic and chloride acid) and Box Behnken design was applied for optimize the process variables (particle size, final concentration of extracting solution and sonication time) after mixture optimization. Iron had not presented quantitative extractions and it was excluded from final samples analysis. The developed method presents the follow limits of quantification in μg g− 1: Ba (0.90); Ca (5.2); Cu (4.0); K (0.90); Mg (1.4); Mn (0.22); Sr (0.25) and Zn (4.0). Accuracy was accessed by comparison of determined concentration with the values obtained by the microwave digestion procedure. The proposed method was applied toward the determination of elemental composition in bean samples collected in the country zone from Jequié city located on the Bahia State, Brazil. The trace elements content ranged from 0.21 to 3.04, 3.84 to 10.8, 0.60 to 5.23, 31.0 to 46.5 and 10.8 to 19.6 μg g− 1 Ba, Cu, Sr, Zn, Mn, respectively. The major elements content ranged from 0.0418 to 0.0877, 0.109 to 0.153 and 1.30 to 1.56% (w/w) Ca, Mg and K, respectively. 相似文献