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991.
992.
Pérez-Sirvent C Martínez-Sánchez MJ García-Lorenzo M López-García I Hernández-Córdoba M 《Analytical and bioanalytical chemistry》2007,388(2):495-498
Use of small membrane pumps, instead of peristaltic pumps, to introduce sample and reagent solutions into the spectrometer
has several advantages in atomic fluorescence spectrometric determination of mercury. This simple modification results in
a substantial saving in the time required for the measurements and so 90% of reagent solution volumes and 95% of sample solution
volumes are saved, with a consequent decrease in the volume of waste generated. The sampling frequency is almost tripled,
with no deterioration in sensitivity, which is similar to that obtained by use of peristaltic pumps. The relative standard
deviation for ten consecutive measurements of a 1 μg L−1 mercury solution was approximately 2%.
Figure Small membrane pumps for the atomic fluorescene spectro metric determination of mercury 相似文献
993.
Sumit Saxena Archana Asokkumar K Bansi Lal 《Journal of Sol-Gel Science and Technology》2007,41(3):245-248
Terbium Aluminum Garnet (TAG) is an important optically active material and is one of the best materials known for the fabrication
of optical isolators. TAG has a large Verdet constant and has good transmission in the region of 350–1500 nm of the electromagnetic
spectrum. It is also known that TAG melts incongruently at 1840°C. This makes efficient synthesis of TAG important and challenging
and forms the motivation of the present work to develop techniques for the synthesis of TAG at lower temperatures. In the
present work we report the synthesis of TAG using sol-gel techniques following the citrate-nitrate route. The prepared sample
is sintered at various temperatures in presence of air and characterized using X-ray diffraction, FT-IR spectroscopy, energy
dispersive X-ray Analysis and the morphology is observed using the scanning electron microscopy. 相似文献
994.
Stéphanie Etienne C. Becker D. Ruch B. Grignard G. Cartigny C. Detrembleur C. Calberg R. Jerome 《Journal of Thermal Analysis and Calorimetry》2007,87(1):101-104
Silica nanoparticles of various sizes have
been incorporated by melt compounding in a poly(methyl methacrylate) (PMMA)
matrix to enhance its thermal and mechanical properties. In order to improve
nanoparticles dispersion, PMMA grafted particles have been prepared by atom
transfer radical polymerization (ATRP) from well-defined silica nanoparticles.
This strategy was expected to ensure compatibility between both components
of the PMMA nanocomposites. TEM analysis have been performed to evaluate the
nanosilica dispersion whereas modified and non-modified silica/PMMA nanocomposites
thermal stability and mechanical properties have been investigated by both
thermogravimetric and dynamical mechanical analysis. 相似文献
995.
Czesław Rudowicz Ireneusz Stefaniuk Roman Dziembaj Hitoshi Ohta Marcin Molenda Susumu Okubo Makoto Yoshida 《Research on Chemical Intermediates》2007,33(8):853-862
This paper deals with the analysis of the temperature dependence of high-frequency EMR (HF-EMR) spectra due to Mn3+ and Mn4+ ions in the lithium manganese spinel LiMn2O4. A range of powder samples obtained by the sol-gel method with calcinations in several temperature ranges were prepared for
this study. Based on the initial characterization carried out by a number of techniques, the physicochemical and structural
properties of the samples were earlier determined. Independently, temperature magnetization and HF-EMR measurements were carried
out. The EMR spectra vary strongly between samples, indicating possible structural or chemical changes. Quantitative analysis
of the temperature dependence of the HF-EMR spectra due to Mn3+ and Mn4+ ions in LiMn2O4 is presented in this paper. The spectral analysis concerns the line shape, linewidth, intensity and g-factors. Fittings using the Lorentzian spectral shape and, to a certain extent, the Gaussian spectral shape have been carried
out in order to parameterize the temperature dependence of the HF-EMR spectra. This parameterization of the HF-EMR experimental
data enables a deeper characterization of the samples. Subsequently, a better insight into the role of the Mn3+ and Mn4+ ions in accounting for the characteristics most suitable for application of LiMn2O4 as a cathode material may be gained. 相似文献
996.
Hanjiang Dong Zhengping Zhang Man-Ho Lee D. W. Mueller Richard F. Reidy 《Journal of Sol-Gel Science and Technology》2007,41(1):11-17
Sol-gel polymerization of methyltrimethoxysilane (MTMS) in ethanol using a two-step acid/base catalyzed procedure (B2) is
followed by 29Si NMR spectroscopy. Analysis of the structural evolution of the B2 system shows that esterification of monomeric and end
silicon species is rate-limited while that of linear and cyclic species is able to reach pseudoequilibrium in the second basic
step. Condensation reactivity is reduced with increasing network connectivity, however, to a much less degree under B2 conditions
than MTMS polymerization under acidic conditions. Steric effects as well as many other factors are attributed to this trend.
The concentration of cyclic and polycyclic species of the B2 system is nearly 3 times lower compared to the acid-catalyzed
system. The empirical degree of condensation at the gel point is determined to be 0.88. The effects of cyclization and phase
separation on MTMS gelation are discussed for both B2 and acid-catalyzed systems. Based on these results it is believed that
MTMS-based gels form for B2 and not acid-catalyzed conditions due to reduced cyclization, rapid hydrolysis and condensation,
effective use of functional groups, and effective contribution of branched and polycyclic species as crosslinking points to
connect polymeric chains in the B2 system. 相似文献
997.
A new protein molecularly imprinted polymer (MIP) was prepared with grafting polyvinyl alcohol as assistant recognition polymer chains (ARPCs). The ARPCs and acrylamide monomers were interpenetrated and then polymerized on the surface of macroporous acrylate adsorbent spheres. The template BSA was removed by treatment with 2.00 mol L-1 potassium chloride (KCl) solution and the adsorbed proteins were detected with sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). 0.150, 0.500, and 2.00 mo... 相似文献
998.
The aim of this work was to establish optimal conditions for the maximum production of endo-β-1,4 mannanases using cheaper
sources. Eight thermotolerant fungal strains were isolated from garden soil and compost samples collected in and around the
Gulbarga University campus, India. Two strains were selected based on their ability to produce considerable endo-β-1,4 mannanases
activity while growing in liquid medium at 37 °C with locust bean gum (LBG) as the only carbon source. They were identified
as Aspergillus niger gr and Aspergillus flavus gr. The experiment to evaluate the effect of different carbon sources, nitrogen sources, temperatures and initial pH of the
medium on maximal enzyme production was studied. Enzyme productivity was influenced by the type of polysaccharide used as
the carbon source. Copra meal defatted with n-hexane showed to be a better substrate than LBG and guar gum for endo-β-1,4 mannanases production by A. niger gr (40.011 U/ml), but for A. flavus gr (33.532 U/ml), the difference was not significant. Endo-β-1,4 mannanases produced from A. niger gr and A. flavus gr have high optimum temperature (65 and 60 °C) and good thermostability in the absence of any stabilizers (maintaining 50%
of residual activity for 8 and 6 h, respectively, at 60 °C) and are stable over in a wide pH range. These new strains offer
an attractive alternative source of enzymes for the food and feed processing industries. 相似文献
999.
The enantioresolution of zolmitriptan was performed using cyclodextrin (CD)-modified capillary zone electrophoresis (CZE)
with hydroxypropyl-β-CD (HP-β-CD) as the chiral selector. The influence of experimental conditions on the enantioseparation
of zolmitriptan, such as pH, temperature, applied voltage, and concentrations of running electrolyte and CD, was systematically
investigated, obtaining a baseline separation of two enantiomers by the use of a 25 mM sodium dihydrogen phosphate (SDPH)
running electrolyte (pH 2.4) containing 30 mM HP-β-CD at 15 °C. Binding constants for each enantiomer–HP-β-CD pair at different
temperatures, as well as thermodynamic parameters for binding, were calculated. A nonlinear van’t Hoff plot was obtained,
indicating that the thermodynamic parameters of complexation were temperature-dependent for zolmitriptan enantiomers. The
significant contribution of the enthalpy difference to the Gibbs free energy change suggested a stereomeric barrier mechanism
for chiral recognition.
Figure Resolution of zolmitriptan enantiomers was achieved by using CD-modified CZE
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
1000.
Wang F Weidt S Xu J Mackay CL Langridge-Smith PR Sadler PJ 《Journal of the American Society for Mass Spectrometry》2008,19(4):544-549
Reactions of the anticancer complex [(eta(6)-bip)Ru(en)Cl](+) (where bip is biphenyl and en is ethylenediamine) with the tripeptide glutathione (gamma-L-Glu-L-Cys-Gly; GSH), the abundant intracellular thiol, in aqueous solution give rise to two ruthenium cluster complexes, which could not be identified by electrospray mass spectrometry (ESI-MS) using a quadrupole mass analyzer. Here we use Fourier transform ion cyclotron mass spectrometry (nanoLC-FT-ICR MS) to identify the clusters separated by nanoscale liquid chromatography as the tetranuclear complex [{(eta(6)-bip)Ru(GSO(2))}(4)](2-) (2) and dinuclear complex [{(eta(6)-bip)Ru(GSO(2))(2)}(2)](8-) (3) containing glutathione sulfinate (GSO(2)) ligands. Use of (18)OH(2) showed that oxygen from water can readily be incorporated into the oxidized glutathione ligands. These data illustrate the power of high-resolution MS for identifying highly charged multinuclear complexes and elucidating novel reaction pathways for metallodrugs, including ligand-based redox reactions. 相似文献