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191.
192.
《Journal of Non》2001,279(2-3):97-109
The Raman spectra of binary xNa2S+(1−x)B2S3 glasses and polycrystals have been measured for the first time and are used to develop a structural model of the sodium thioborate glasses. The Raman spectra confirm our previous infrared (IR) experimental conclusions that the structure of vitreous (ν-B2S3) is comprised of B3(0) groups and six-membered rings. It was also found that as sodium sulfide is added to the glass in the low alkali (x<0.35) glass forming region, the B4 groups are formed at the expense of the B3(0) groups first and then from the six-membered ring groups. The Raman spectra are also consistent with the presence of a pyramidal structural arrangement of B4 groups with trigonally coordinated sulfur atoms. This structure could explain the existence of the super-stoichiometric amounts of B4 groups found using nuclear magnetic resonance (NMR). Glasses in the high alkali region (0.50<x<0.80) progressively change from being comprised of metathioborate rings to being comprised of B3(3) groups. The Raman spectra also confirms the IR spectra which saw no evidence of B3(2) groups in these sodium thioborate glasses.  相似文献   
193.
《Tetrahedron: Asymmetry》2001,12(8):1225-1233
Starting from (S)-1,1′-binaphthol, a series of ten novel enantiopure 1,1′-binaphthylazepine-based aminoalcohols and diamines 1a1j were efficiently prepared and fully characterized. These derivatives, having either only an atropisomeric bridged-binaphthyl backbone or an additional stereogenic carbon center, can be interesting ligands for asymmetric catalysis.  相似文献   
194.
《Solid State Sciences》2001,3(1-2):143-153
The hydrothermal synthesis, single crystal structure analysis, spectroscopic and thermal stability studies of the compounds Ba3(In1−xMx)2(HXO4)6 (0≤x≤1; M=Cr, Fe; X=P, As) are reported. The 3D framework of these new phosphates can be described as a pillared layered framework. The metal cations (In3+, Fe3+, and Cr3+) occupy two crystallographically independent octahedral sites, M(1) and M(2). The layers are formed of M(2)O6 octahedra and (HPO4) tetrahedra sharing corners, with M(1)O6 octahedra serving as pillars between adjacent layers. Single crystal study of Ba3(In0.5Fe0.5)(HPO4)6 shows that indium and iron segregate between the two metal sites with Fe occupying primarily the site M(1) and In located primarily in M(2) site. Interactions between the building units within the layers occur through hydrogen bonding. Barium cations are located between the pillars, in 8-membered ring tunnels and are coordinated by 12 oxides. The phases loose three water molecules through condensation of six HXO4 groups to form Ba2M2(X2O7)3 at temperatures between 480 and 600 °C. Mössbauer spectroscopy shows the presence of high-spin Fe3+ in octahedral coordination.  相似文献   
195.
The multivariate interference effects due to nitrates of sodium, potassium, magnesium and calcium on electrothermal atomization of manganese were modelled by using the multiple linear regression method in conjunction with a suitable experimental design. Since the model proved to be able to efficiently predict the simultaneous effects of the considered salts in a wide range of concentrations, it was applied to provide a computational correction of the matrix effects occurring in the ETAAS analysis of manganese in seawater, after preconcentration of the analyte on Chelex-100 resin and elution with nitric acid. Preliminary results showed that the matrix effects are significantly reduced, leading to an improvement in accuracy of the ETAAS analysis.  相似文献   
196.
197.
Progress in the features of three types of microwave plasmas is discussed, in view of the development of successful methods for atomic spectrometric element-specific detection in liquid chromatography. For the low-power microwave induced plasmas the development of the toroidal plasma in a TM010 cavity according to Beenakker is mentioned as the break-through for the introduction of wet aerosols. Capacitively coupled microwave plasmas (CMP), which can be operated with helium, argon and even air as working gases, are robust and allow obtaining of detection limits for Fe, Cr, Ni and Co in aqueous solutions in the 0.02 to 0.06 μg/ml range and in light oils, as an example of organic liquids, between 0.08 and 0.13 μg/ml. Special attention should be given to the microwave plasma torch (MPT) in which aerosols from aqueous as well as from organic solutions produced by a Légère nebulizer can be introduced without desolvation. Here, detection limits for Cd, Cr, Li and Pb range from 0.02 to 0.5 μg/ml. For the case of chromium dissolved as dithiocarbamate complex in an acetonitrile/H2O mixture (2:1), its detection limit is 0.12 μg/ml, being already below that obtained with UV spectrophotometry. The limits of detection achieved with the sources discussed in the case of atomic emission spectrometry show the prospective for further development.  相似文献   
198.
在溶剂热条件下,合成了2个碱土金属配位聚合物[Ca (tdc)(DMF)2]n(1)和[Ba (tdc)]n(2)(H2tdc=2,5-噻吩二甲酸),分别用元素分析、红外光谱、X射线单晶衍射、粉末衍射、热重分析和荧光光谱对它们进行了表征。结构分析表明,配合物1具有4,4连接的二维层状结构,拓扑符号为(44·62),而配合物2呈现三维网络结构。固体荧光测试表明配合物1比配合物2具有更显著的荧光性能。  相似文献   
199.
《Surface science》1996,364(1):L530-L539
In situ electrochemical scanning tunneling microscopy (ECSTM) has been employed to follow the renewal process of a graphite electrode accompanied by flavin adenine dinucleotide (FAD) electrochemical reaction which involves adsorption of the reduced form (FADH2) and desorption of the oxidized form (FAD). The renewal process initiates from steps or kinks on the electrode surface, which provide high active sites for adsorption. This renewal depends on the working electrode potential, especially in the range near the FAD redox potential. Our experiment suggests that delamination of the graphite surface is caused by interaction between the substrate and adsorbed molecules. A simple model is proposed to explain this phenomenon.  相似文献   
200.
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