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31.
The First Mitsunobu Protocol for Efficient Synthesis of α-Acyloxyphosphonates Using 4,4′-Azopyridine
Nasser Iranpoor Habib Firouzabadi Dariush Khalili 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):2166-2171
Abstract This is the first report on applying the Mitsunobu protocol for the synthesis of various α-acyloxyphosphonates using 4,4′-azopyridine and PPh3 with diverse aromatic and aliphatic carboxylic acids. Under these conditions, diethyl azodicarboxylate (DEAD) as the traditional reagent for Mitsunobu reaction is not efficient. The insoluble pyridine hydrazine byproduct can be simply isolated and recycled to its azopyridine by an oxidation reaction and reused again. [Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental resource: Characterization data of compounds 3a–3z2 and NMR spectra.] GRAPHICAL ABSTRACT 相似文献
32.
In this work, a vanillin complex is immobilized onto MCM-41 and characterized by FT-IR, X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, thermogravimetric analysis, and BET techniques. This supported Schiff base complex was found to be an efficient and recoverable catalyst for the chemoselective oxidation of sulfides into sulfoxides and thiols into their corresponding disulfides (using hydrogen peroxide as a green oxidant) and also a suitable catalyst for the preparation of 2,3-dihydroquinazolin-4(1H)-one derivatives in water at 90°C. Using this protocol, we show that a variety of disulfides, sulfoxides, and 2,3-dihydroquinazolin-4(1H)-one derivatives can be synthesized in green conditions. The catalyst can be recovered and recycled for further reactions without appreciable loss of catalytic performance. 相似文献
33.
Milad Kazemnejadi Seyyedeh Ameneh Alavi G. Zinat Rezazadeh Mohammad Ali Nasseri Ali Allahresani Mohsen Esmaeilpour 《应用有机金属化学》2020,34(2):e5388
Cu(II) Schiff base complex supported on Fe3O4@SiO2 nanoparticles was employed as a magnetic nanocatalyst (nanocomposite) with a phase transfer functionality for the one-pot preparation of α-aminonitriles (Strecker reaction). The desired α-aminonitriles were obtained from the reaction of aromatic or aliphatic aldehydes, aniline or benzyl amine, NaCN, and 1.6 mol% of the catalyst in water at room temperature and good to excellent yields were obtained for all substrates. The catalyst was characterized analytically and instrumentally including Fourier-transform infrared spectroscopy, X-ray diffraction, thermogravimetric, nuclear magnetic resonance, energy-dispersive X-ray spectroscopy, inductively coupled plasma spectroscopy, vibrating-sample magnetometry analysis, dynamic light scattering, Brunauer–Emmett–Teller surface area, field emission scanning electron microscopy, and transmission electron microscopy analyses. The reaction mechanism was investigated, in which the performance of the catalyst as a phase transition factor seems to be probable. The catalyst showed high activity, high turnover frequency (TOF)s, significant selectivity, and fast performance toward the Strecker synthesis. The nanocatalyst can be readily and quickly separated from the reaction mixture with an external magnet and can be reused for at least seven successive reaction cycles without significant reduction in efficiency. 相似文献
34.
Ben Salah M Vilminot S André G Richard-Plouet M Bourée-Vigneron F Mhiri T Kurmoo M 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(8):2048-2057
[Mn(3)(OH)(2)(SO(4))(2)(H(2)O)(2)] and its deuterated analogue were synthesized by a hydrothermal technique and characterized by differential thermal analysis, thermogravimetric analysis, and IR spectroscopy. Its nuclear structure, determined by single-crystal X-ray analysis and Rietveld analysis of neutron powder-diffraction data, consists of a 3D network of chains of edge-sharing Mn(1)O(6), running along the c axis, connected by the apices of Mn(2)O(6) and SO(4) units. It is isostructural to the nickel analogue. Determination of the magnetic structure and measurements of magnetization and heat capacity indicate the coexistence of both magnetic long-range ordering (LRO) and short-range ordering (SRO) below a Néel temperature of 26 K, while the SRO is retained at higher temperatures. The moments of the two independent Mn atoms lie in the bc plane, and that of Mn(1) rotates continuously by 54 degrees towards the c axis on decreasing the temperature from 25 to 1.4 K. While the SRO may be associated with frustration of the moments within a Mn(3) trimer, the LRO is achieved by antiparallel alignment of the four symmetry-related trimers within the magnetic unit cell. A spin-flop field, measured by dc and ac magnetization on a SQUID, is observed at 15 kOe. 相似文献
35.
Ben Salah M Vilminot S Richard-Plouet M André G Mhiri T Kurmoo M 《Chemical communications (Cambridge, England)》2004,(22):2548-2549
The synthetic mineral Co(II)5(OH)6(SO4)2(H2O)4 (1), obtained by hydrothermal reaction of CoSO4.7H2O and NaOH at 165 degrees C and consisting of brucite-like Co4(OH)6O2 layers pillared by OSO3-Co(H2O)4-O3SO, is a ferromagnet (T(Curie)= 12 K, Hc= 580 Oe). 相似文献
36.
Ehsan A. H. Gomaa H. Schut A. Van Veen M. Mohsen U. Fromm P. Morshuis 《Journal of Radioanalytical and Nuclear Chemistry》1996,211(1):77-83
Using the positron annihilation lifetime technique, the annihilation parameters have been measured for epoxy and high density polyethylene (HDPE) as a function of AC electric field strength and the exposure time. The lifetime spectra have been resolved into three components, the longest component (I33) is attributed to the pick-off annihilation of o-Ps in the amorphous regions. The intermediate one (I22) is due to the annihilation of free positrons, while the shorter component (I11) stems from self annihilation of p-Ps. In HDPE, the o-Ps parameters 3 andI
3 are measured as a function of electric field strengths in the range from 10 to 100 kV/cm exposed for 24 hours. A decrease inI
3 of 8% is observed from zero to 50 kV/cm followed by an increase of the same order from 50 to 100 kV/cm. By investigating the effect of the exposure time from 2 to 24 hours at 16 and 50 kV/cm, the effect is confirmed and is attributed to the inhibition of o-Ps formation at lower field strength. In epoxy, the effect or exposure time onI
3 at 166 and 133 kV/cm shows a similar behavior as in HDPE. At 133 kV/cmI
3 decreases by only 2.5%. On the other hand, the changes in 3 occur at short exposure times. Again at large times the saturation is obtained. These effects are attributed to the expansion of free volume (increase of 3) competing at longer exposure times with other phenomena, such as liberation of free radicals, which reduce the o-Ps intensityI
3 through the conversion to p-Ps. The reactions between o-Ps and free radicals might also lead to free positrons, which could explain the increase ofI
2 and the decrease of 3 at longer exposure times. 相似文献
37.
Kamyabi Mohammad Ali Alipour Zahra Moharramnezhad Mohsen 《Journal of Solid State Electrochemistry》2021,25(2):445-456
Journal of Solid State Electrochemistry - Here is reported a new feasible and facile method for the determination of amoxicillin by the electrochemiluminescence (ECL) method. The ECL signal was... 相似文献
38.
Noha M. Soliman Faiyaz Shakeel Nazrul Haq Fars K. Alanazi Sultan Alshehri Mohsen Bayomi Ahmed S. M. Alenazi Ibrahim A. Alsarra 《Molecules (Basel, Switzerland)》2022,27(14)
Various chitosan (CS)-based nanoparticles (CS-NPs) of ciprofloxacin hydrochloride (CHCl) have been investigated for therapeutic delivery and to enhance antimicrobial efficacy. However, the Box–Behnken design (BBD)-supported statistical optimization of NPs of CHCl has not been performed in the literature. As a result, the goal of this study was to look into the key interactions and quadratic impacts of formulation variables on the performance of CHCl-CS-NPs in a systematic way. To optimize CHCl-loaded CS-NPs generated by the ionic gelation process, the response surface methodology (RSM) was used. The BBD was used with three factors on three levels and three replicas at the central point. Tripolyphosphate, CS concentrations, and ultrasonication energy were chosen as independent variables after preliminary screening. Particle size (PS), polydispersity index (PDI), zeta potential (ZP), encapsulation efficiency (EE), and in vitro release were the dependent factors (responses). Prepared NPs were found in the PS range of 198–304 nm with a ZP of 27–42 mV. EE and drug release were in the range of 23–45% and 36–61%, respectively. All of the responses were optimized at the same time using a desirability function based on Design Expert® modeling and a desirability factor of 95%. The minimum inhibitory concentration (MIC) of the improved formula against two bacterial strains, Pseudomonas aeruginosa and Staphylococcus aureus, was determined. The MIC of the optimized NPs was found to be decreased 4-fold compared with pure CHCl. The predicted and observed values for the optimized formulation were nearly identical. The BBD aided in a better understanding of the intrinsic relationship between formulation variables and responses, as well as the optimization of CHCl-loaded CS-NPs in a time- and labor-efficient manner. 相似文献
39.
Ranjbar-Azad Mohammad Behpour Mohsen Keyhanian Fereshteh 《Journal of Solid State Electrochemistry》2022,26(11):2541-2553
Journal of Solid State Electrochemistry - The development of safe, fast charging, and long-lasting Li-ion batteries has been taking major steps forward through novel combinations of nanomaterials.... 相似文献
40.
The comparative electrochemical behavior of self-assembled monolayers of two Schiff's bases, 2-{[(Z)-1-(3-furyl)methylidene]amino}-1-benzenethiol (FMAB) and 2-{[(2-sulfanylphenyl)imino]methyl}phenol (SIMP) on a bare gold electrode (Au FMAB SAM-modified electrode and Au SIMP SAM-modified electrode, respectively), was investigated by means of cyclic voltammetry and electrochemical impedance spectroscopy in a 0.1 mol L(-1) KCl solution that contains 5.0 × 10(-3) mol L(-1) [Fe(CN)(6)](3-/4-). The results revealed that the modified electrodes showed an electrocatalytic activity toward the anodic oxidation of dopamine by a marked enhancement in the current response and lower overpotential (60 and 90 mV for the Au FMAB and Au SIMP SAM-modified electrodes, respectively) in phosphate buffer solution at pH 6.0. The Au SIMP SAM-modified electrode was applied successfully to the determination of dopamine in the presence of a high concentration of ascorbic acid. Selective detection was realized in total elimination of ascorbic acid response-a method different from the ones based on the potential separations. The detection limit of dopamine was 5.0 × 10(-8) mol L(-1) in a linear range from 1.0 × 10(-6) to 1.2 × 10(-4) mol L(-1) in the presence of 1.0 × 10(-3) mol L(-1) ascorbic acid. The interference studies also showed that the Au SIMP SAM-modified electrode exhibited good selectivity in the presence of a large excess of uric acid and could be employed for the determination of dopamine in pharmaceutical formulations, plasma samples and human urine with adequate selectivity and precision. 相似文献