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81.
The attempted Baylis-Hillman reactions of N-tosyl aldimines and aryl aldehydes with 3-methylpenta-3,4-dien-2-one gave the corresponding Baylis-Hillman adducts 3 and 6 in moderate to good yields in the presence of DMAP in DMSO, respectively. In the case of the aza-Baylis-Hillman reactions of N-tosyl aldimines with 3-methylpenta-3,4-dien-2-one catalyzed by PBu3, the corresponding aza-Baylis-Hillman derivatives 4 and 5 were formed at the same time. 相似文献
82.
Jing-kun Xu Gao-quan Shi Feng-en Chen Xiao-yin Hong Department of Chemistry Bio-organic Phosphorous Chemistry Laboratory Tsinghua University Beijing China 《高分子科学》2002,(5):425-430
The Raman spectra of poly(3-methylthiophene) (PMeT) films with different thicknesses, which have beenelectrochemically deposited on a flat stainless steel electrode surface by direct oxidation of 3-methylthiophene in borontrifluoride diethyl etherate (BFEE) at a constant applied potential of 1.38 V (versus SCE), have been investigated byexcitation with a 633-nm laser beam. The spectroscopic results demonstrated that the doping level of PMeT film wasincreasing during film growth. This finding was also confirmed by electrochemical examination. Moreover, the Raman bandsassigned to radical cations and dications in doped PMeT films were found approximately at 1420 and 1400 cm~(-1),respectively. Radical cations and dications coexist on the backbone of PMeT as conductive species and their concentrationsincrease with the increase of doping level. Successive cyclic voltammetry was proved to be an effective approach toimproving the doping level of as-grown thin compact PMeT film. 相似文献
83.
Three modified procedures for the separation of cardiac myosin light chains are carefully compared. Ion-exchange chromatography gives a purified cardiac myosin light chain 1, whereas light chain 2 is always contaminated by light chain 1. Reversed-phase high-performance liquid chromatography gives the best resolution of these light chains and needs only 20 min for each run. However, it requires pure preparation of myosin light chains before separation. Isoelectric precipitation is the simplest procedure and suitable for large quantities of material. Although it gives the highest yield the separation is not adequate. A modified and rapid procedure for the isolation of cardiac and skeletal total myosin light chains is also presented. 相似文献
84.
A novel and practical procedure was developed for the abnormal Beckmann rearrangement of steroid 17-oximes. Treatment of the 17-oximes with TFA/CH(OMe)(3) in boiling THF for 2 h gives the corresponding 13,17-seco alkene nitrile products in unprecedented high yields (70-92%). Since the alkene nitriles can be subsequently converted into 18-norsteroids, this general method provides a highly efficient route to these biologically important compounds and, by extension, to other structurally related natural products. 相似文献
85.
Intramolecular proton transfer equilibria of acetamide and methyl carbamate have been studied by AMI MO calculations, and the results are compared with those of the MNDO method. It was found that the two semi- empirical methods predict essentially the same proton transfer mechanism, but MNDO tends to overestimate the activation barriers. Participation of one solvate vater in the proton transfer led to a considerable lovering of the activation barrier, by nearly the same amount, in both methods. One notable conflict between the two methods was that the methoxy-O-protonated form of methyl carbamate, in the gas phase, can be a local energy minimum with MNDO, whereas it leads to dissociation into two species Instead of an optimized structure with AM1. It was concluded that the MNDO method can be useful for this type of process, especially when one is interested in the relative activation barriers only. 相似文献
86.
The reaction of 1-alkynylcyclobutanols with aryl iodides in the presence of Pd(OAc)2 and Et3N in acetonitrile at 80°C for 24 h gives 2-disubstituted methylenecyclopentan-1-ones in modest to good yields. The tandem insertion-ring expansion process proceeds via the formation of an alkynyl π-complex, followed by migration of a carbon-carbon bond of the tert-alkanol to form the cyclopentanones stereoselectively. 相似文献
87.
88.
Ke Jian Liu Jin Jie Jiang Li Li Ji Xianglin Shi Harold M. Swartz 《Research on Chemical Intermediates》1996,22(5):499-509
Application of the spin trapping technique in intact animals requires an understanding of the stability and distribution of the spin traps and their spin adducts in vivo. We studied the stability of DMPO in vivo in mice using HPLC and the stability of spin adducts of DMPO by EPR in plasma, whole blood, peritoneal fluid, and homogenized heart tissue of the rat. At 15 minutes after intraperitoneal injection DMPO had similar concentrations in the liver, heart, and blood of the mice and 40% remained in the organs 2 hours after the injection. In contrast, the spin adduct DMPO-OH was short lived, with a half-life of 3.0 minutes in plasma, and was not detectable 1 minute after formation in whole blood and homogenized heart tissue. The carbon centered spin adduct DMPO-CH(OH)CH3 was more stable, having half-lives of 16, 11, 3.6, and 0.79 minutes in plasma, peritoneal fluid, whole blood, and homogenized heart tissue, respectively. The spin adduct DMPO-SO3 was sufficiently stable for the adduct to be observed directly from living mice. 相似文献
89.
Ke-Ming Wang Bo-Rong Shi Xiang-Dong Liu Tian-Bing Xu Pei-Ran Zhu Jun-Si Zhu Qing-Tai Zhao 《Applied Physics A: Materials Science & Processing》1992,55(4):332-334
The effect of 2.0 MeV Cu+ irradiation on Si(100) crystal has been studied by the Rutherford backscattering/channeling technique. Analysis of the lattice disorder distribution has been performed under 100 direction of tilting off from the target normal: 7°, 30°, and 45° as well as different doses. The lattice disorder distributions in Si(100) have been compared with TRIM'89 simulation. The results show that the lattice disorder distributions in Si(100) under different irradiation angles seem to be in good agreement with TRIM'89 simulation. When the dose increases up to 8.7×1014 ions/cm2, the defect concentration increases leading to the formation of an amorphous layer. 相似文献
90.