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51.
We report on the sol-gel synthesis of Zn1−xCrxO (x=0.0, 0.05, 0.10, 0.15 and 0.20) nanoparticles. These nanoparticles were characterized by using thermogravimetry/differential scanning calorimetry (TG/DSC), X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman and Photoluminescence (PL). Electronegativity of Cr ions (Cr3+) reduces the final decomposition temperature by 40 °C and activation energy of the reaction when Cr is doped into ZnO. Doping of higher Cr concentration (x≥0.10) into ZnO shows formation of secondary spinel (ZnCr2O4) phase along with the hexagonal (ZnO) and is revealed by XRD. Formation of secondary phase changes the activation energy of the reaction and thus the strain in ZnO lattice. In Raman spectra, additional Raman modes have been observed for Zn1−xCrxO nanoparticles, which can be assigned to the modes generated due to Cr doping. The Cr doping into ZnO is also supported by PL, in which vacancies are formed with Cr ion incorporation and emission band shifts towards higher wavelength. 相似文献
52.
Measurement of imidazoleacetic acid in urine by gas chromatography-mass spectrometry 总被引:1,自引:0,他引:1
Imidazoleacetic acid (IAA), a histamine and histidine metabolite, was quantified in human urine by gas chromatography-mass spectrometry (GC-MS). The acid was separated by ion-exchange chromatography, derivatized as the n-butyl ester with boron trifluoride-butanol and the derivative extracted with chloroform. GC-MS analysis was carried out by selected-ion monitoring of ions m/z 81 and m/z 83 corresponding, respectively, to IAA and [15N,15N']IAA used as internal standard. The mean IAA content in urine was about 8.02 nmol/mg of creatinine. The specificity of measurement was rigorously established by GC retention time, peak shape, ion abundance ratios, and recovery experiments. The method is capable of quantifying IAA in 0.05 ml of urine and in amounts as low as 0.20 nmol. 相似文献
53.
Summary Selenito manganese(III) complexes of the type MMn(SeO3)2 · × H2O (where M = H+, NH
4
+
, K+, Rb+ and Cs+) have been prepared, Magnetic measurements show all these complexes to be of high spin d4 type, On the basis of their i.r. and electronic spectral studies and other properties, a polymeric octahedral structure involving bridging oxygen atoms has been suggested. 相似文献
54.
Jos Luis Mata‐Mata J. Alfredo Gutirrez M. Angeles Paz‐Sandoval Amira R. Madrigal Antonio Martínez‐Richa 《Journal of polymer science. Part A, Polymer chemistry》2006,44(24):6926-6942
End‐functionalized polyesters have been synthesized by ring‐opening polymerization (ROP) of ?‐caprolactone (CL) initiated with five different ruthenium derivatives in the presence of a series of alcohols as transfer agents. Mechanistic studies were performed for ROP of CL with RuCl2(PPh3)3 ( I ), TpRuCl(PPh3)2 ( II ), and TpRuCl(PHPh2)(PPh3) ( III ) as catalysts in the presence or absence of benzyl alcohol (BzOH). Obtained molecular weights are proportional to CL/BzOH ratio, but there is not a direct relationship with CL/ruthenium complex ratios. 1H and 13C NMR spectroscopy revealed the existence of benzyl ester end‐groups. Catalysis involves (a) dissociation of ruthenium complexes, (b) coordination of the lactone CL, (c) coordination of the BzOH with the formation of a metal alkoxide, (d) transfer from the alkoxyl ligand to the coordinated lactone, and (e) ring‐opening of CL by oxygen‐acyl bond cleavage. The proposed mechanism is supported by 1H, 13C, and 31P NMR, gel permeation chromatography (GPC), and MALDI‐TOF analysis of the polymers. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 6926–6942, 2006 相似文献
55.
Karla A. Barrera‐Rivera Ángel Marcos‐Fernández Ricardo Vera‐Graziano Antonio Martínez‐Richa 《Journal of polymer science. Part A, Polymer chemistry》2009,47(21):5792-5805
Yarrowia lipolytica (YLL), Candida rugosa (CRL), and porcine pancreatic lipase (PPL) were employed successfully as catalysts in the enzymatic ring‐opening polymerization (ROP) of ε‐caprolactone in the presence of 1‐ethyl‐3‐methylimidazolium tetrafluoroborate ([EMIM][BF4]), 1‐butyl‐3‐methylimidazolium tetrafluoroborate ([BMIM][BF4]), 1‐butylpyridinium tetrafluoroborate ([BuPy][BF4]), 1‐butylpyridinium trifluoroacetate ([BuPy][CF3COO]), 1‐ethyl‐3‐methylimidazolium nitrate ([EMIM][NO3]) ionic liquids. Poly(ε‐caprolactone)s (PCLs) with molecular weights (Mn) in the range of 300–9000 Da were obtained. 1H‐ and 13C‐NMR analyses on PCLs formed by YLL, CRL, and PPL showed asymmetric telechelic α‐hydroxy‐ω‐carboxylic acid end groups. Differences between CP‐MAS and MAS spectra are observed and discussed in terms of morphology. MALDI‐TOF spectra show the formation of at least seven species. Differential scanning calorimetry (DSC) and Wide Angle X‐Ray Scattering (WAXS) results demonstrate the high degree of crystallinity present in all the polyesters. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 5792–5805, 2009 相似文献
56.
Fujiwara T Khandelwal P Akutsu H 《Journal of magnetic resonance (San Diego, Calif. : 1997)》2000,145(1):73-83
The maximum of the transferred magnetization in rotating powdered solids under the radiofrequency-driven recoupling (RFDR) pulse sequence is enhanced by reducing the orientation dependence of the effective recoupled homonuclear dipolar interaction. The compound RFDR (CRFDR) pulse sequence for this enhancement consists of RFDR pulse units (tau(i)-pi-tau(R)-pi-1171;tau(i)) with different tau(i), where tau(R) is the sample rotation period, tau(i) and 1171;tau(i) (=tau(R) - tau(i)) are delays, and pi is a 180 degrees pulse. The delay tau(i) modifies the zero-quantum spin operators and the sample rotation-angle dependence of the recoupled dipolar Hamiltonian. The CRFDR pulse sequences were optimized for mixing by varying tau(i). Numerical simulation for the two-spin system only with a dipolar interaction and isotropic chemical shifts indicates that the transfer efficiency of CRFDR averaged over the powder is about 70%, which is 30% higher than the efficiency of the RFDR pulse over a broad range of about 1/tau(R) in resonance frequency difference. The CRFDR sequences need about 60% longer mixing times to maximize the transferred magnetizaion in comparison with the original RFDR sequence. Chemical shift anisotropy, the other dipolar interactions, and relaxation generally reduce the enhancement by CRFDR. Experiments for fully (13)C-labeled alanine, however, show that the maximum of the magnetization transferred with CRFDR from the carboxyl to alpha carbon is about 15% greater than that with RFDR. Copyright 2000 Academic Press. 相似文献
57.
58.
IR absorption spectra of BeSO4.4H2O and its deuterated analogue are reported in the region 1200–250 cm−1 at 110 K. The half-widths and relative integrated intensities of the bands are also reported. The study largely confirms
the assignments for thev
3 andv
4 modes of SO
4
2−
ion and thev
3 mode of Be(aq)
4
2+
, complex as made by Diemet al. The assignments of the other modes of SO
4
2−
and Be(aq)
4
2+
, and the librational modes of water are given a more solid footing as result of the present investigation. 相似文献
59.
60.