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101.
The Ni-catalyzed cross-coupling of 2-bromo-3,3,3-trifluoropropene and aryl Grignard reagents was investigated. When NiCl2(PPh3)2 was used as a catalyst, the highest yield of α-trifluoromethylstyrene (89%) from 2-bromo-3,3,3-trifluoropropene and PhMgBr was obtained in 1,3-dimethyl-2-imidazolidinone at 50 °C for 30 min. Various α-trifluoromethylstyrene derivatives could be produced in satisfactory yields by NiCl2(PPh3)2-catalyzed coupling using aryl Grignard reagents. 相似文献
102.
A highly selective procedure is proposed for the determination of ultra-trace level concentrations of nickel in saline aqueous
matrices exploiting a micro-sequential injection Lab-On-Valve (μSI-LOV) sample pretreatment protocol comprising bead injection
separation/pre-concentration and detection by electrothermal atomic absorption spectrometry (ETAAS). Based on the dimethylglyoxime
(DMG) reaction used for nickel analysis, the sample, as contained in a pH 9.0 buffer, is, after on-line merging with the chelating
reagent, transported to a reaction coil attached to one of the external ports of the LOV to assure sufficient reaction time
for the formation of Ni(DMG)2 chelate. The non-ionic coordination compound is then collected in a renewable micro-column packed with a reversed-phase copolymeric
sorbent [namely, poly(divinylbenzene-co-N-vinylpyrrolidone)] containing a balanced ratio of hydrophilic and lipophilic monomers.
Following elution by a 50-μL methanol plug in an air-segmented modality, the nickel is finally quantified by ETAAS. Under
the optimized conditions and for a sample volume of 1.8 mL, a retention efficiency of 70 % and an enrichment factor of 25
were obtained. The proposed methodology showed a high tolerance to the commonly encountered alkaline earth matrix elements
in environmental waters, that is, calcium and magnesium, and was successfully applied for the determination of nickel in an
NIST standard reference material (NIST 1640-Trace elements in natural water), household tap water of high hardness and local
seawater. Satisfying recoveries were achieved for all spiked environmental water samples with maximum deviations of 6 %. The
experimental results for the standard reference material were not statistically different to the certified value at a significance
level of 0.05. 相似文献
103.
104.
We have described the first successful application of bidentate ligands in the asymmetric Ni-catalyzed trialkylaluminium addition to several aldehydes. The ligands are prepared from inexpensive d-(+)-xylose and d-(+)-glucose and have the advantage of carbohydrate and phosphite/phosphoroamidite moieties. After systematic variation of the position of the phosphoroamidite group at either C5 or C-3, the configuration of C-3 and the substituents in the biaryl phosphite/phosphoroamidite moieties, enantioselectivities up to 84% and high yields were obtained in the Ni-catalyzed trialkylaluminium addition to several aldehydes. 相似文献
105.
Jian‐Qiang Huang Chun‐Yu Ho 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2019,131(17):5758-5762
A cross‐hydroalkenylation/rearrangement cascade (HARC), using a cyclopropene and alkyne as substrate pairs, was achieved for the first time by using new [(NHC)Ni(allyl)]BArF catalysts (NHC=N‐heterocyclic carbenes). By controlling the (NHC)NiIIH relative insertion reactivity with cyclopropene and alkyne, a broad scope of cyclopentadienes was obtained with highly selectively. The structural features of the new (NHC)NiII catalyst were important for the success of the reaction. The mild reaction conditions employed may serve as an entry for exploring (NHC)NiII‐assisted vinylcyclopropane rearrangement reactivity. 相似文献
106.
Anastasia N. GeorgopoulouConstantinos G. Efthymiou Constantina PapatriantafyllopoulouVassilis Psycharis Catherine P. RaptopoulouManolis Manos Anastasios J. TasiopoulosAlbert Escuer Spyros P. Perlepes 《Polyhedron》2011,30(18):2978-2986
The synthetic investigation of the NiII/M(NO3)3·6H2O/di-2-pyridyl ketone [(py)2CO] tertiary reaction system in EtOH has yielded triangular Ni2M cationic complexes (M = lanthanide, Y). The reaction between Ln(NO3)3·6H2O, Ni(ClO4)2·6H2O, (py)2CO and base (1:3:3:3) in EtOH under gentle heating gave the isostructural complexes [Ni2Ln{(py)2C(OEt)(O)}3{(py)2C(OH)(O)}(NO3)(H2O)](ClO4)2 (Ln = Gd, 2; Ln = Tb, 3) in high yields. The ligands (py)2C(OEt)(O)− and (py)2C(OH)(O)− are the monoanions of the hemiketal and gem-diol derivatives of (py)2CO, respectively, formed in situ in the presence of the metal ions. The cations of 2 and 3 consist of one 8-coordinate LnIII and two distorted octahedral NiII atoms in an essentially isosceles, triangular arrangement capped by a central μ3-Ο− atom of the unique 3.3011 (Harris notation) (py)2C(OH)(O)− ligand. Each metal-metal edge is bridged by the deprotonated O atom of one 2.2011 (py)2C(OEt)(O)− ligand. The isostructural complexes [Ni2M{(py)2C(OEt)(O)}4(NO3)(H2O)]2[M(NO3)5](ClO4)2 (M = Y, 4 ; M = Tb, 5 ; M = Dy, 6) were prepared by the 1:1 reaction of the mononuclear “metalloligand” [Ni(O2CMe){(py)2CO}{(py)2C(OH)2}](ClO4) (1) and M(NO3)3·6H2O in EtOH under mild heating in moderate to good yields. The structures of the dications of 4-6 are similar to those in 2 and 3, the only difference being the replacement of the unique 3.3011 (py)2C(OH)(O)− ligand of the latter by one 3.3011 (py)2C(OEt)(O)− group in the former. The YIII, TbIII and DyIII atoms in [M(NO3)5]2− are coordinated by five bidentate chelating nitrato groups. Characteristic IR bands of the complexes are discussed in terms of the known structures and the coordination modes of the ligands. Variable temperature, solid-state direct current magnetic susceptibility and magnetization studies were carried out on dried samples of 2-4. The data indicate ferromagnetic Ni?Ni and Ni?Gd exchange interactions, and an ST = 11/2 ground state for 2. Complex 3 is characterized by a high-spin ground state while the ferromagnetic Ni?Ni interaction for 2 is independently supported by the study of 4. No out-of-phase, alternating current susceptibility signals have been detected for 3 that would be indicative of SMM behavior. 相似文献
107.
A sensitive procedure is presented for the voltammetric determination of nickel. The procedure involves an adsorptive accumulation of nickel 1-nitroso-2-napthol (NN) complex on a bismuth film electrode prepared ex situ by electrodeposition. The most suitable operating conditions and parameters such as pH, ligand concentration (CNN), adsorptive potential (Eads), adsorptive time (tads), scan rate and others were selected and the determination of nickel in aqueous solutions using the standard addition method was possible. The adsorbed Ni-NN complex gives a well defined cathodic stripping peak current at −0.70 V, which was used for the determination of nickel in the concentration range of 10.0-70.0 μg L−1 (pH 7.5; CNN 6.5 μmol L−1; Eads −0.30 V; tads 60 s) with a detection limit of 0.1 μg L−1. The relative standard deviation for a solution containing 10.0 μg L−1 of Ni(II) was 3.5% (n = 4). The proposed method was validated determining Ni(II) in certified reference waste water (SPS-WW1) and Certified Reference Water for Trace Elements (TMDA 51.3) with satisfactory results. Then lake water samples were analyzed. 相似文献
108.
Oracio Serrano 《Journal of organometallic chemistry》2011,696(10):2217-2219
The nickel (0) compound Ni(COD)(GaAr′)2 (Ar′ = C6H3-2,6-(C6H3-2,6-i-Pr2)2), 1, was synthesized by the reaction of Ni(COD)2 (COD = 1,5-cyclooctadiene) with (GaAr′)2. Compound 1 reacted with ethylene at 25 °C and at 1 atm pressure to give the bimetallic cluster [Ni2(GaAr′)2(η1:η1-μ2-C2H4)], 2, through the incorporation of one molecule of ethylene and displacement of COD. The structure of 2 featured an unusual Ni2Ga2C2 core bicyclic structure in which the C2H4 moiety bridges the Ga···Ga edge of a Ga2Ni2 tetrahedron. The galliums each carry an η1-bonded Ar′ substituent which complexes the nickel atom by an η6-π interaction with one of its flanking Ar’ rings. 相似文献
109.
Copper(II) complex with
-piperidine-3-carboxylic acid (
-Hpipe-3):[Cu(
-pipe-3)2(H2O)] and cobalt(II) and nickel(II) complexes with piperidine-4-carboxylic acid (Hpipe-4):[M(Hpipe-4)2(H2O)4]Cl2 (M: Co, Ni) have been prepared and characterized by means of IR and powder diffuse reflection spectra, thermal analysis, and magnetic susceptibility. The crystal structures of these complexes have been determined by X-ray diffraction. The crystal of [Cu(
-pipe-3)2(H2O)] is orthorhombic with the space group Pbcn. The copper atom is in a square pyramidal geometry, ligated by two carboxylato oxygen atoms, two nitrogen atoms, and a water molecule. One molecule of this complex consists of either
-piperidine-3-carboxylic acid or
-piperidine-3-carboxylic acid. The crystals of [M(Hpipe-4)2(H2O)4]Cl2 are monoclinic with space group P21/n. In these complexes the metal atom is in an octahedral geometry ligated by two carboxylato oxygen atoms and four water molecules. 相似文献
110.
Hierarchical flower-like architectures of[Ni3(BTC)2·12H2O](BTC3=benzene-1,3,5-tricarboxylate) were successfully prepared by a simple solution-phase method under mild conditions without any template or surfactant.Phase-pure porous NiO nanocrystals were obtained by annealing the Ni-BTC complex without significant alteration in morphology.The product was characterized by X-ray diffraction techniques,field-emission scanning electron microscopy(FESEM).transmission electron microscopy(TEM) and high-resolution TEM(HRTEM).The catalytic effect of the NiO product was investigated on the thermal decomposition of ammonium perchlorate(AP) and it was found that the annealed NiO product has higher catalytic activity than the commercial NiO. 相似文献