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991.
An in situ reduction approach to synthesizing gold and silver nanoparticles by using a series of newly designed, redox-active amphiphiles at basic pH is described. These amphiphiles are the conjugates of a fatty acid (e.g., oleic acid, stearic acid, and lauric acid) and a redox-active amino acid (e.g., tryptophan or tyrosine). The amphiphile-coated nanoparticles are then efficiently transferred from water to different nonpolar organic media (such as benzene, toluene, xylene, cyclohexane, and hexane) simply by acid treatment. The phase-transfer process was monitored by UV/visible spectroscopy and transmission electron microscopy, and the results showed that the average particle size and size distribution remain almost unchanged after transferring to the organic media. The anchoring of the amphiphile to the nanoparticle surface was confirmed by FTIR spectroscopy and thermogravimetric analysis. A mechanism is proposed to describe the stability of colloidal Au and Ag nanoparticles formed in situ and their phase transfer to organic solvents. The presence of the amphiphile increases the thermal stability of the colloidal gold nanoparticle conjugates in organic solvents. 相似文献
992.
Suparna Guha Biswajit Ray Broja M. Mandal 《Journal of polymer science. Part A, Polymer chemistry》2001,39(19):3434-3442
Polyacrylamide prepared by dispersion (precipitation) polymerization in an aqueous t‐butyl alcohol (TBA) medium is only partially soluble when the TBA concentrations in the polymerization media are in the range 82 vol % < TBA < 95 vol %. Independent experiments with a soluble (linear) sample of polyacrylamide show that the polymer swells sufficiently in the aforementioned media to lower the glass‐transition temperature of the polymer below the polymerization temperature (50 °C). The anomalous solubility has been attributed to the crosslinking of polymer chains that occurs during the solid‐phase polymerization of acrylamide in the swollen polymer particles. It is postulated that some of the radical centers shift from the chain end to the chain backbone during solid‐phase polymerization by chain transfer to neighboring polymer molecules, and when pairs of such radicals come into close vicinity, crosslinking occurs. However, dispersion (precipitation) polymerization in other media such as aqueous methanol and aqueous acetone yields polymers that are soluble. This result has been attributed to the fact that the polymer radical undergoes a chain‐transfer reaction with these solvents at a much faster rate than with TBA, which overcomes the effect of the polymer‐transfer reaction. Even the addition of as little as 5% methanol to a TBA–water mixture (TBA:water = 85:10) gives rise to a soluble polymer. The chain‐transfer constants for acetone, methanol, and TBA have been determined to be 9.0 × 10?6, 6.9 × 10?6, and 1.48 × 10?6, respectively, at 50 °C. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 39: 3434–3442, 2001 相似文献
993.
Nanotechnology holds the prospective for pervasive and avant-garde changes to improve performance of materials. Mesua ferrea L. seed oil based highly thermostable and biodegradable polyester/clay nanocomposites have been prepared at different dose levels of nanoclay. The highly branched polyester resin was synthesized by condensation of 2,2-bis(hydroxymethyl) propionic acid with M. ferrea L. seed oil based carboxyl terminated pre-polymer. FTIR, rheometric, XRD, SEM and TEM studies unmasked well-dispersed partially exfoliated nanocomposites with good interfacial interaction. The results showed 2.6 and 6 times increase of tensile strength and elongation at break respectively, and about 150 °C increase of thermostability by the influence of nanoclay loading (1-5 weight %) compared to the pristine polymer. Two strains of Pseudomonas aeruginosa (PN8A1 and vs1) and one Bacillus subtilis strain (MTCC73) were used to study microbial degradation of pristine polymer and nanocomposite systems, with the revelation of enhanced degradation with increasing nanoclay loading. 相似文献
994.
Md. Obaidur Rahman Mridul Kanti Mandal Yasuo Shida Satoshi Ninomiya Lee Chuin Chen Hiroshi Nonami Kenzo Hiraoka 《Journal of mass spectrometry : JMS》2013,48(7):823-829
Probe electrospray ionization (PESI) uses a sharp solid needle as electrospray emitter. This method was found to be applicable to the analysis of real‐world samples with high concentrations of salts and detergents without sample pretreatment. Since PESI is only applicable to wet samples but not to dry samples, sheath‐flow PESI (SF‐PESI) has been developed. The metal needle was inserted into the fine plastic capillary with a protrusion of 0.1–0.2 mm from the capillary terminus. The solvent was supplied continuously through the capillary. At the lowest position of the probe, solvent flowing out from the capillary makes the sample wet and extracts the analytes from the surface. The extracted analytes were electrosprayed at the highest position of the needle. SF‐PESI was successfully applied to samples such as narcotics, tablets, bill, fruits, potatoes, etc. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
995.
Padmini Ramaswamy Sukhendu Mandal Srinivasan Natarajan 《Journal of solid state chemistry》2009,182(9):2491-2496
A novel manganese phosphite-oxalate, [C2N2H10][Mn2II(OH2)2(HPO3)2(C2O4)] has been hydothermally synthesized and its structure determined by single-crystal X-ray diffraction. The structure consists of neutral manganese phosphite layers, [Mn(HPO3)]∞, formed by MnO6 octahedra and HPO3 units, cross-linked by the oxalate moieties. The organic cations occupy the middle of the 8-membered one-dimensional channels. Magnetic studies indicate weak antiferromagnetic interactions between the Mn2+ ions. 相似文献
996.
Samik Gupta Bijan Kumar Paul Anil Kumar Barik Tarak Nath Mandal Somnath Roy Nikhil Guchhait Ray J. Butcher Susanta Kumar Kar 《Polyhedron》2009,28(16):3577-3585
Dioxomolybdenum(VI) complexes [MoO2(B1)H2O] (1), [MoO2(B2)EtOH] (2), [MoO2(B3)EtOH] (3) and [MoO2(B4)EtOH] (4) were synthesized using the Schiff base ligands H2B1(previously reported), H2B2, H2B3 and H2B4, respectively. These ligands were prepared by condensation of 1-(2-pyridyl) 5-methyl 3-pyrazole carbohydrazide with salicylaldehyde, o-hydroxy acetophenone, 5-bromo salicylaldehyde and 5-nitro salicylaldehyde respectively. Due to the presence of a substituted 1-(2-pyridyl) pyrazole unit, ligands H2B1, H2B2 and H2B3 exhibit fluorescent emissions, and the most intense emission was obtained for H2B3. H2B4 is incapable of showing fluorescence emission. As the ligands are capable of using different binding modes, according to the demands of the guest metal ions, their emission properties also change accordingly. The dioxomolybdenum(VI) complex of the ligand H2B1, i.e. complex 1, shows quenched emission compared to H2B1. Again when Cu2+, Co2+ or Ni2+ ions are added to a solution of 1, in each case a new complex of Cu2+ Co2+ or Ni2+ is formed in solution and further quenching was observed. However, with Zn2+ input to a solution of 1, fluorescence recovery was observed up to the level of the free ligand. The copper(II) complex of H2B1 (complex 5), produced by adding equivalent amount of Cu2+ salt to a solution of 1, was isolated and characterized. One of the dioxomolybdenum(VI) complexes, 3, when subjected to an oxo-transfer reaction with PPh3 produces complex [MoO(B3)CH3CN] (6). Complex 6 shows reduced fluorescence emissions compared to 3 in the solid phase. These observations open up the possibilities for these ligands to work as fluorescent signaling system with different metal ion inputs. All the complexes are characterized by elemental analyses, electronic spectra, IR, 1H NMR, magnetic measurements, EPR and by cyclic voltammetry. Complexes 1 and 5, as well as the ligands H2B2 and H2B3, have been crystallographically characterized. 相似文献
997.
Hassan NM Murimboh JD Sekaly AL Mandal R Chakrabarti CL Grégoire DC 《Analytical and bioanalytical chemistry》2006,384(7-8):1558-1566
Kinetic speciation of nickel, aluminium, and iron in fresh water has been investigated by cascade ultrafiltration followed by competing ligand exchange of the ultrafiltered fractions. Graphite furnace atomic absorption spectrometry was used to measure the kinetics of metal complex dissociation. Dissolved metal species were fractionated by cascade ultrafiltration. Metal speciation in each ultrafiltered fraction was then characterized as free metal ions, “labile” metal complexes (with dissociation rate constants ≥10−3 s−1), “slowly labile” metal complexes (with dissociation rate constants >10−6 s−1), and “inert” metal complexes (with dissociation rate constants <10−6 s−1). The experimental results were compared with the predictions of a computer-based equilibrium speciation model, the Windermere humic aqueous model (WHAM) V. Cascade ultrafiltration coupled with kinetic speciation of the metal species in each molecular weight cut-off (MWCO) fraction provided a more comprehensive picture and insight into the physical and the chemical characteristics of the metal species than either ultrafiltration or measurement of dissociation kinetics alone. 相似文献
998.
Prakash GK Panja C Vaghoo H Surampudi V Kultyshev R Mandal M Rasul G Mathew T Olah GA 《The Journal of organic chemistry》2006,71(18):6806-6813
Organofluorine compounds are becoming increasingly important in different fields, such as material science, agro chemistry, and the pharmaceutical industry. Nucleophilic trifluoromethylation is one of the widely used methods to incorporate a trifluoromethyl moiety into organic molecules. We have carried out extensive studies to develop varieties of easily accessible nucleophilic catalysts to promote such reactions. TMS-protected trifluoromethylated alcohols were prepared from both aldehydes and ketones in excellent yields using catalytic amount of amine N-oxide. Carbonate and phosphate salts also showed efficient catalytic activity toward this reaction. These reactions were highly solvent dependent, and DMF was found to be the most suitable one among the various solvents studied. All these reactions proceeded under very mild conditions, giving clean products and avoiding the use of any fluoride initiators or expensive catalysts, and extremely water-free conditions. The mechanism for the reaction is discussed in detail. DFT calculations were performed on the possible reaction intermediates using the Gaussian 03 program at B3LYP/6-311+G* level to support the proposed mechanism. 相似文献
999.
First VLF detections of ionospheric disturbances due to Soft Gamma Ray Repeater SGR J1550-5418 and Gamma Ray Burst GRB 090424 总被引:1,自引:0,他引:1
Sandip K. Chakrabarti Sushanta K. Mandal Sudipta Sasmal Debashis Bhowmick Asit K. Choudhury Narendra N. Patra 《Indian Journal of Physics》2010,84(11):1461-1466
We present the first report of the detection of sudden ionospheric disturbances (SIDs) due to a Soft Gamma Ray Repeater (SGR)
SGR J1550-5418 and a Gamma Ray Burst (GRB) GRB 090424. These detections were made with receiving stations of Indian Centre
for Space Physics which were monitoring Very Low Frequency signals (VLFs) from the VTX transmitter located at the southern
tip of Indian sub-continent. These positive detections add to the list of a handful of similar detections of other GRBs and
SGRs throughout the world. 相似文献
1000.
Uttam Mandal Amlan Kanti Sarkar Kadagi Veeran Gowda Sangita Agarwal Anirbandeep Bose Uttam Bhaumik Debotri Ghosh Tapan Kumar Pal 《Chromatographia》2008,67(3-4):237-243
A bioanalytical method has been developed and validated for determination of pregabalin in human plasma. The analytical method
consists in the precipitation of plasma sample with trichloro acetic acid (20% v/v solution in water), followed by the determination of pregabalin by an LC-MS-MS method using gabapentin as internal standard.
Separation was achieved on a Gemini C18 50 mm × 2.0 mm (3 μm) column with an isocratic mobile phase consisting of methanol–water (98:2, v/v) with 0.5% v/v formic acid. Protonated ions formed by a turbo ionspray in positive mode were used to detect analyte and internal standard.
The MS-MS detection was by monitoring the fragmentation of 160.2→55.1 (m/z) for pregabalin and 172.2→67.1 (m/z) for gabapentin on a triple quadrupole mass spectrometer. The assay was calibrated over the range 0.1–15.0 μg mL−1 with correlation coefficient of 0.9998. Validation data showed intra-batch (n = 6) CV% ≤ 6.89 and RE (%) between −4.17 and +3.08 and inter-batch (n = 18) CV% < 9.09 and RE (%) between −3.0 and +10.00. Mean extraction recovery were 80.45–89.12% for three QC samples and 87.56%
for IS. Plasma samples were stable for three freeze–thaw cycles, or 24 h ambient storage, or 1 and 3 months storage at −20 °C.
Processed sample (ready for injection) were stable up to 72 h at autosampler (4 °C). This method has been used for analyzing
plasma samples from a bioequivalence study with 18 volunteers. 相似文献