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911.
Oxide ceramic masses react to simple shearing with hardening (peptisation: increase in the shear stress with the shear deformation).
In the present study the correlation between the increase in the shear stress and the porosity, agglomeration processes and
the type of flow are analysed. For this purpose oxide ceramic masses are tested in a shear device especially developed for
pastes and analysed by rheometric experiments, NMR methods and particle size analysis. The results support the hypothesis
that structural changes (hardening, increase in the mean porosity) of the material during the peptisation mainly depend on
the magnitude and not on the kind of the energy input and thus of the type of flow. The fraction of bound (more generally,
the immobilised) water increases with the shear displacement. Also crushing of primary particles could be observed. Both the
crushing of solid particles causing an increased solid surface and the formation of a three-dimensional gel structure are
microscopic effects capable of resulting in the binding or retaining water. On a macroscopic scale these phenomena cause hardening.
Magnetic resonance imaging visualises flow-induced agglomerates, which form owing to the shear flow and increase the porosity
averaged over the whole sample. After the shear experiment rolls of paste can be seen which indicate that the general assumption
of a plane shear flow in the shear device is not warrantable.
Received: 19 July 2001 Accepted: 25 October 2001 相似文献
912.
Summary A method is reported for the determination of dibutyltin (DBT), diphenyltin (DPhT), tributyltin (TBT), and triphenyltin (TPhT)
species at the nanogram per litre concentration level in natural water samples. Analytes were isolated from samples by solid-phase
extraction and analysed both off-line and on-line by reversed-phase high-performance liquid chromatography with post-column
derivatization and fluorimetric detection. Several SPE cartridges and eluents were evaluated; C18 enrichment and elution with a mixture of methanol, acetic acid, and water was found most suitable. Preconcentration factors
up to 250 can be achieved when a 500-mL sample is processed. Detection limits, recovery rates, and the precision of the whole
process have been determined. The method has been applied to the determination of organotin species in spiked natural water
samples collected on the NW Mediterranean coast. Recovery rates range from 75 to 110% and detection limits are at the low
ng L−1 level (1–3 ng Sn L−1 for DPhT, DBT, and PhT and 40 ng Sn L−1 for TBT when 250 mL spiked sea water is processed.) 相似文献
913.
914.
The introduction of a 5-trimethylsilyl group on the least hindered face of the diene thebaine was anticipated to favor attack by dienophiles from the alternate face, but only gave rise to a rearrangement product when treated with 3-butene-2-one at 110 °C. Reaction with the more reactive benzoquinone at lower temperature gave rise to a very slow reaction from the same face as the silyl group, indicating that a trimethylsilyl group does not sufficiently hinder this face to achieve reaction at the other face. 相似文献
915.
John D. Van Dyke Kim L. Kasperski 《Journal of polymer science. Part A, Polymer chemistry》1993,31(7):1807-1823
Dried samples of polyacrylamide in an He atmosphere have been subjected to thermogravimetric analysis in the 30–600°C range, and the evolved gases were monitored by FTIR. Water, ammonia, and small quantities of carbon dioxide are released in the first stages of decomposition (220–340°C), where the polymer chains remain intact and the reaction occurs on the pendant amide groups. In the second stage of decomposition (340–440°C), the majority of the weight loss occurs, and main chain breakdown occurs, releasing carbon dioxide, water, nitrile compounds, and imides. Trapping of the gases in this stage and analysis by GC–FTIR and GC–MS reveals the presence of more than 20 decomposition products, and confirms that a large proportion of these can be assigned to glutarimide and its substituted analogs. Imidization and dehydration reactions on the amide groups, as well as free radical breakdown of the main chains, with inter- and intramolecular hydrogen transfer, can account for many of the products of the decomposition. © 1993 John Wiley & Sons, Inc. 相似文献
916.
917.
It is proved that the simplified Navier--Stokes (SNS) equations presented by Gao Zhi,Davis and Golowachof--Kuzbmin--Popof (GKP) are respectively regular and singular neara separation point for a two--dimensional laminar flow over a flat plate. The order of thealgebraic singularity of Davis and GKP equation near the separation point is indicated.A comparison among the classical boundary layer (CBL) equations, Davis and GKP equations,Gao Zhi equations and the complete Navier--Stokes (NS) equations near the separationpoint is given. 相似文献
918.
Development and validation of a stability-indicating HPLC method for the determination of degradation products in dipyridamole injection 总被引:1,自引:0,他引:1
Summary The development and subsequent validation of an isocratic high-performance liquid chromatographic (HPLC) procedure employing
ultraviolet (UV) detection for the determination of degradation products in Dipyridamole Injection is reported. The development
of this assay involved the evaluation of several factors including buffer type, ionic strength, pH, organic composition, and
column type. The described method is simple, reproducible, accurate, and selective. The precision, relative standard deviation
(RSD), amongst five sample preparations for total degradation products was not more than (NMT) 10.2 %, while the individual
degradation products were NMT 12.1%. Intermediate precision, as determined from fifteen sample preparations, generated by
two Analysts on different HPLC systems over three days, exhibited an RSD for total and individual degradation products of
8.2 % and NMT 27.5 %, respectively. The mean absolute recovery of dipyridamole using the described method is 102.1±1. 9%,
(mean±SD, n=12) over the concentration range of 0.03 % to 5.0 % of its label claim of 5 mg mL−1. The limit of detection and limit of quantitation were 0.1 and 0.3 μg mL−1, respectively. The linearity of the peak response was verified with respect to dipyridamole concentration over a range of
0.3 and 50 μg mL−1 (0.03 % to 5.0 % label claim). The Standard and Assay Preparations are stable for up to 48 hours at room temperature. The
selectivity was evaluated by subjecting the finished product (Dipyridamole Injection) to thermal, acidic, basic, oxidative
and fluorescent radiation stress conditions. No interference in the analysis of degradation products was observed, showing
the method is stability-indicating. 相似文献
919.
920.