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121.
Icbudak H. Heren Z. Kose D. Ali Necefoglu H. 《Journal of Thermal Analysis and Calorimetry》2004,76(3):837-851
The mixed-ligand p-hydroxybenzoate complexes of Ni(II), Cu(II) and Zn(II) with nicotinamide and N,N-diethylnicotinamide were synthesized and
characterized by elemental analysis, magnetic susceptibility measurements and mass spectrometry. The thermal behavior of the
complexes was studied by simultaneous TG, DTG and DTA methods in static air atmosphere. The infrared spectral characteristics
of the complexes are also discussed. The complexes contain two water molecules, two p-hydroxybenzoato (p-hba) and two nicotinamide (na) (or diethylnicotinamide (dena)) ligands per formula unit. In these complexes,
all ligands are coordinated to the metal ion as monodendate ligands. In Zn(II)-na and Cu(II)-dena complexes, thep-hydroxybenzoate behaves as bidentate chelating ligand through carboxylic oxygen atoms. The decomposition pathways and the
stability of the complexes are interpreted in the terms of the structural data. The final decomposition products were found
to be the respective metal oxides.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
122.
The surface area of kaolinite-benzamide (K-Bz)6.62 m2 g–1, whichis noticeably lower than that of kaolinite-dimethyl sulphoxide (K-DMSO) 14.61m2 g–1, the co-perturbationof the inner-surface hydroxyl features at 3697 and 3650 cm–1,and the increase of d(001) value by 7.44 Å are all related to the benzamidespecies inserted into the kaolinite structure through the replacement of theK-DMSO composites. Disappearance of the DMSO reflections and emergence ofwell-defined features at 6.04(2θ) and 11.16(2θ), 001 and 002 reflectionswith d values of 14.62 and 7.92 Å, respectively point out that the DMSOspecies were substituted efficiently by benzamide molecules. The thermal stabilityof the K-Bz derivative up to 300°C can be attributed to the slightly tiltedaromatic ring keying into the gibbsitic sheets via the –NH2groups. 相似文献
123.
Kotaro Hidea Hiroshi Maezawa Atsushi Ito Katsumi Kobayashi Yoshiya Furusawa Takashi Ito 《Photochemistry and photobiology》1986,44(3):417-419
The spectral throughput of a vacuum-ultraviolet irradiation system at the SOR-RING facility was examined with various combinations of aluminum-and gold-coated optical elements in a 2.2-m modified Wadsworth monochromator. We found that the optimum was a combination of an aluminum-coated collimating mirror, concave grating, and plane deflecting mirror, and a combination of a gold-coated collimating mirror, concave grating and an aluminum-coated plane deflecting mirror in the wavelength regions 190-110 nm and 110-50 nm, respectively. 相似文献
124.
Direct synthesis of phenol by hydroxylation of benzene with H2O2 over the vanadium-substituted heteropolymolybdic acid catalyst was investigated at 70 °C. H2O2 was used as an oxidant while 36 wt.% MeCO2H was employed as the solvent. After 100 min the selectivity for phenol was 93% and the yield of PhOH was 10.1%. The catalyst
was characterized by elemental analysis, thermal gravimetric analysis, infrared spectroscopy, u.v.–vis spectroscopy, X-ray
diffraction, and 31P-n.m.r. and 51V-n.m.r. techniques. The experimental conditions such as reaction temperature, the amounts of H2O2 and catalyst were explored. The as-prepared phenol could be separated by column chromatography and was characterized by infrared
and mass spectrometry. 相似文献
125.
Tarek A. Salama Abdel-Aziz S. El-Ahl Abdel-Galil M. Khalil Margret M. Girges Bernd Lackner Christian Steindl Saad S. Elmorsy 《Monatshefte für Chemie / Chemical Monthly》2003,20(5):1241-1252
Several new 1-aryl-, aralkyl-, and heteroaryl-5-(4-phenylbuta-1,3-dienyl)tetrazole derivatives and annulated tetrazole derivatives were efficiently and regiospecifically prepared in nearly quantitative yield via a facile one step reaction of dienones with a combination of tetrachlorosilane and sodium azide in acetonitrile under mild conditions. A complete structure assignment of three representative examples of the tetrazoles was achieved by advanced 2D NMR measurements including COSY, TOCSY, HSQC, HMBC, NOESY, and ROESY experiments. 相似文献
126.
U. Çevik A. I. Kopya H. Karal Y. Sahin 《Journal of Radioanalytical and Nuclear Chemistry》1995,201(3):241-249
Sea-bed sediments from Eastern Black Sea have been analyzed for their Fe, Ba and Sr contents using the methods of standard addition and energy dispersive X-ray fluorescence (EDXRF). Samples were prepared from powder sifted by a 200 mesh sieve. An annular 100 mCi241Am radioactive source emitting 59.543 keV photons was used for excitation and a Ge(Li) detector, which has a 190 eV FWHM for 5.9 keV photons was used for intensity measurements. 2048 channels of the MCA are employed for 20 or 30 min. Dried and ground sea-bed sediments are found to contain 2.95–7.50% Fe, 0.032–0.268% Ba and about 73–273 ppm Sr. These results agree with those obtained via atomic absorption methods. 相似文献
127.
In this study, a rapid pre-concentration procedure, which employs powdered activated carbon as a clean-up and pre-concentration material, is described for the gas chromatographic analysis of N-nitrosodiethylamine (NDEA) and N-nitrosodimethylamine (NDMA) in aqueous solutions. It was found that powdered activated carbon is suitable for the adsorption of volatile N-nitrosamine compounds from aqueous solutions. Adsorption efficiency with spiked beer samples (alcohol content 5% v/v) was found to be 80.5% (NDMA) and 89.4% (NDEA) and recovery of extraction from activated carbon was calculated as 82.1% (NDMA) and 89.7% (NDEA), respectively. The effect of 100µgmL–1 of tannic acid on the adsorption was also studied, and no significant effect on the adsorption and extraction of volatile N-nitrosamine compounds was found. 相似文献
128.
Two synthetic routes have been introduced and evaluated for the preparation of hydrophilic silica-based monoliths possessing surface-bound cyano functions. In one synthetic scheme, the silica monolith was reacted in a single step with 3-cyanopropyldimethylchlorosilane to yield a cyano phase referred to as CN-monolith. In a second synthetic route, the silica monolith was first reacted with gamma-glycidoxypropyltrimethoxysilane (gamma-GPTS), followed by a reaction with 3-hydroxypropionitrile (3-HPN) to give a stationary phase denoted CN-OH-monolith. Although the gamma-GPTS was intended to play the role of a spacer arm to link the 3-HPN to the silica surface, this spacer arm became an integral part of the hydrophilic stationary phase. Thus, the CN-OH-monolith can be viewed as a double-layered stationary phase (i.e., stratified phase) with a hydroxy sub-layer and a cyano top layer. Due to its stronger hydrophilic character, the CN-OH-monolith yielded higher retention and better selectivity than the CN-monolith. The CN-OH-monolith was demonstrated in the normal-phase capillary electrochromatography (CEC) of various polar compounds including phenols and chloro-substituted phenols, nucleic acid bases, nucleosides, and nitrophenyl derivatives of mono- and oligosaccharides. The CN-OH-monolith yielded a relatively strong electroosmotic flow over a wide range of mobile phase composition, thus allowing rapid separation of the polar compounds studied. 相似文献
129.
Tojino M Uenoyama Y Fukuyama T Ryu I 《Chemical communications (Cambridge, England)》2004,(21):2482-2483
Free-radical carbonylation of omega-alkynylamines with tributyltin hydride gives a mixture of alpha-methylene lactams and alpha-stannylmethylene lactams. Nucleophilic addition of an internal amino group to the carbonyl group of alpha-ketenyl radicals is proposed as the cyclization step. The subsequent unusual 1,4-H shift from the resulting 1-hydroxyallyl radical, followed by elimination of the beta-tributyltin radical leads to the formation of alpha-methylene lactams. 相似文献
130.
Atom transfer radical polymerization conditions with copper(I) bromide/2,2′-bipyridine (Cu/2,2′-bpy) as the catalyst system were employed for the homopolymerization and random copolymerization of 1-phenoxycarbonyl ethyl methacrylate (PCMA) with methyl methacrylate (MMA). Temperature studies indicated that the polymerizations occurred smoothly in bulk at 110 °C. Poly(PCMA)(polydispersity index=1.27) homopolymer was characterized and then used as macroinitiator for increasing its molecular weight. The homopolymerization of PCMA was also carried out under free radical conditions using 2,2′-azobisisobutyronitrile as an initiator.The monomer and polymers were characterized by FT-IR and 1H and 13C-NMR techniques. The glass transition temperatures, the solubility parameters and average-molecular weights of the polymers were determined. Thermal stabilities of the polymers were given as compared with each other by using TGA curves. Thermal degradation products of poly(PCMA)s obtained by ATRP and free radical polymerization were compared with each other by using 1H-NMR technique. 相似文献