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41.
Lucica Viorica Ababei Angela Kriza Cristian Andronescu Adina Magdalena Musuc 《Journal of Thermal Analysis and Calorimetry》2012,107(2):573-584
Ten new mononuclear complexes having general formulae [ML2](ClO4)2, M = Cu(II), Co(II), Ni(II), Mn(II) and Zn(II), [ML2](SO4), M = Co(II), Ni(II) and [ML2(H2O)2](SO4), M = Cu(II), Mn(II) and Zn(II), L = 2-acetyl-pyridyl-isonicotinoylhydrazone have been synthesized and characterized based
on elemental analyses, IR spectroscopy, UV–Vis–NIR, EPR, as well as thermal analysis and determination of molar conductivity
and magnetic moments. The structures of [CoL2](ClO4)2 are accomplished by single crystal X-ray diffraction. The coordination sphere is formed by two N, N, O tridentates 2-acetyl-pyridyl-isonicotinoylhydrazone
ligands, or by two N, O bidentate 2-acetyl-pyridyl-isonicotinoylhydrazone and two water molecules. Biological activity studies
reveal a moderate activity of complexes against gram-negative and gram-positive bacteria. 相似文献
42.
C Tiseanu B Cojocaru VI Parvulescu M Sanchez-Dominguez PA Primus M Boutonnet 《Physical chemistry chemical physics : PCCP》2012,14(37):12970-12981
Pure and europium (Eu(3+)) doped ZrO(2) synthesized by an oil-in-water microemulsion reaction method were investigated by in situ and ex situ X-ray diffraction (XRD), ex situ Raman spectroscopy, high-resolution transmission electron microscopy (HRTEM), steady state and time-resolved photoluminescence (PL) spectroscopies. Based on the Raman spectra excited at three different wavelengths i.e. 488, 514 and 633 nm and measured in the spectral range of 150-4000 cm(-1) the correlation between the phonon spectra of ZrO(2) and luminescence of europium is clearly evidenced. The PL investigations span a variety of steady-state and time resolved measurements recorded either after direct excitation of the Eu(3+) f-f transitions or indirect excitation into UV charge-transfer bands. After annealing at 500 °C, the overall Eu(3+) emission is dominated by Eu(3+) located in tetragonal symmetry lattice sites with a crystal-field splitting of the (5)D(0)-(7)F(1) emission of 20 cm(-1). Annealing of ZrO(2) at 1000 °C leads to a superposition of Eu(3+) emissions from tetragonal and monoclinic lattice sites with monoclinic crystal-field splitting of 200 cm(-1) for the (5)D(0)-(7)F(1) transition. At all temperatures, a non-negligible amorphous/disordered content is also measured and determined to be of monoclinic nature. It was found that the evolutions with calcination temperature of the average PL lifetimes corresponding to europium emission in the tetragonal and monoclinic sites and the monoclinic phase content of the Eu(3+) doped ZrO(2) samples follow a similar trend. By use of specific excitation conditions, the distribution of europium on the amorphous/disordered surface or ordered/crystalline sites can be identified and related to the phase content of zirconia. The role of zirconia host as a sensitizer for the europium PL is also discussed in both tetragonal and monoclinic phases. 相似文献
43.
G. I. Rusu A. Airinei Viorica Hamciuc G. G. Rusu Petronela Râmbu Mihaela Diciu 《Journal of Macromolecular Science: Physics》2013,52(2):238-253
Polysulfone (PSF)-polydimethylsiloxane (PDMS) block copolymers (PSF-b-PDMS) with various compositions were prepared by condensing chloro-terminated polysulfone oligomers with α, ω -dihydrogensilyl-polydimethylsiloxane in refluxing chlorobenzene solution in the presence of urea as a hydrogen chloride acceptor. The temperature dependences of the electrical conductivity and thermoelectric power (Seebeck coefficient) of copolymers were studied using thin films deposited from a dimethylformamide solution (spin coating method) onto glass substrates. It was established that the various copolymers showed typical semiconducting properties. Some correlations between these properties (activation energy, ratio of carrier mobilities, etc) and molecular structure of the copolymers were found. A model based on band gap representation was found to be suitable for explanation of the electronic transport mechanism through the studied copolymers in thin films. The study of the transmission and absorption spectra (in the spectral range from 300 nm to 1400 nm) evidenced that the indirect allowed optical transitions were predominant. The values of the optical energy band gap (ranged between 1.50 eV and 1.70 eV) are in agreement with values of width of the forbidden band calculated from the temperature dependence of the electrical conductivity. 相似文献
44.
A new monomer bearing N-trityl-l-serine methyl ester in structure, methacryloyloxyethyl carbamoyloxy–N-trityl methyl serine (MTS), was prepared to be further polymerized by atom transfer radical polymerization (ATRP) with pyrene-endcapped poly(methyl methacrylate) (Py–PMMA–Br) or poly(N-isopropylacrylamide) (Py–PNIPA–Br). The resulting block copolymers, poly(methyl methacrylate–block–methacryloyloxyethyl carbamoyloxy–N-trityl methyl serine) (Py–PMMA–b–PMTS) and poly(N-isopropylacrylamide–block–methacryloyloxyethyl carbamoyloxy–N-trityl methyl serine (Py–PNIPA–b–PMTS) were characterized by 1H (13C) NMR, ultraviolet, FTIR and fluorescence spectroscopy, thermal analysis, differential scanning calorimetry (DSC), atomic force microscopy (AFM), scanning electron microscopy (SEM), and gel permeation chromatography (GPC) measurements. The chemical composition in Py–PMMA–b–PMTS was estimated from the 1H NMR analysis that indicated a ratio of the repeating units of 46:19 (MMA:MTS). For the Py–PNIPA–b–PMTS the composition rate in the copolymer was 61:25 (NIPA:MTS). Quenching of the pyrene species with N,N-diethylaniline, nitrobenzene, nitrophenol, potassium iodide, p-nitrotoluene and tetracyanoquinodimethane (TCNQ) in DMF solution excited at 348 nm was evidenced, more efficiently being nitrophenol and TCNQ. In this case, the monomer emission at 388–409 nm underwent a significant decrease caused of an electron transfer from the electron-reach photoexcited pyrene molecule to the electron-deficient quenchers. 相似文献
45.
Simona M. Coman Anca Dobre Mircea D. Banciu Aurica Petride Valentin Cimpeanu Georges Poncelet Vasile I. Parvulescu 《Journal of molecular catalysis. A, Chemical》2004,220(2):257-265
Ru–BEA catalysts with 1.0–2.5 wt.% Ru were prepared by ion exchange. The acidic properties of these catalysts were investigated using deuterated acetonitrile, pyridine, and 2,6-di-tert-butyl-pyridine. The deposited Ru was studied by CO-FTIR spectroscopy. The materials were tested as catalysts in the hydrogenation of a conjugated cyclic keto–enol, namely, 5-hydroxymethylene-5H-6,7-dihydrodibenzo[a,c]cyclohepten-6-one. Beside hydrogenation, hydrogenolysis products were identified by GC–MS and 1H NMR techniques. Relations were sought between the selectivity and some physicochemical properties of the catalyst. 相似文献
46.
Yan Liu Viorica Lopez-Avila Marcela Alcaraz Werner F. Beckert 《Journal of separation science》1994,17(7):527-536
As part of a continuing evaluation of new analytical and sample preparation techniques conducted by the US Environmental Protection Agency (EPA), the use of capillary gas chromatography with atomic emission detection (GC-AED) for the simultaneous determination of organotin, organolead, and organomercury compounds in environmental samples was investigated. Pentylmagnesium bromide was used to pentylate ionic organotin, organolead, and organomercury compounds; the pentyl derivatives were then separated by GC and determined by AED. Several important GC-AED parameters, including the type of injector inlet, carrier gas flow rate, and helium make-up gas flow rate, were optimized for the simultaneous determination of these organometallic compounds. Their minimum detectable concentrations were approximately 1.0 to 2.5 ng/mL using a 0.5-μL on-column injection. The calibration curves exhibited good linearity between 2.5 and 2500 ng/mL for organotin and organolead compounds, and between 2.5 and 10000 ng/mL for organomercury compounds. 相似文献
47.
Supercritical fluid extraction of kava lactones from Piper methysticum Forst. herb is described here. The extraction was performed with supercritical carbon dioxide alone and supercritical carbon dioxide modified with 15% ethanol, and the extracts were analyzed by gas chromatography/mass spectrometry. Seven lactones including: 7,8-dihydrokavain; kavain; 5,6-dehydrokavain; 5, 6, 7, 8-tetrahydroyangonin; dihydromethysticin; yangonin; and methysticin were the major constituents in the SFE extract. 相似文献
48.
Cristofor I. Simionescu Virgil BÎrboiu Bogdan C. Simionescu Viorica Talmaciu Corina Sava 《Journal of polymer science. Part A, Polymer chemistry》1986,24(5):851-860
Bulk radical copolymerization of methyl acrylate (MeA, M1) with styrene (St, M2) in presence and absence of ZnCl2 as complexing agent was studied. 1H-NMR spectra were used to establish copolymer composition and sequence distribution. The methoxy group signal was observed to be split due to pentads, but the analysis of sequence distribution is possible only at triad level. Both composition and sequence distribution data confirmed that bulk radical copolymerization respects quite well the terminal addition model; the values of r1 = 0.14 ± 0.02 (from composition data) and r1 = 0.25 ± 0.03 (from sequence distribution data) and r2 = 0.83 ± 0.10 (from composition data) were found. The presence of ZnCl2 increases the probability of alternating addition, e.g., for [ZnCl2]/[MeA] = 0.2, r1 = 0.03 ± 0.02 and r2 = 0.17 ± 0.03. The radical copolymer obtained in bulk in the absence of ZnCl2 presents a coisotactic configuration with σ = 0.75 ± 0.03, but the presence of the complexing agent reduces the probability of coisotactic addition, e.g., for [ZnCl2]/[MeA] = 0.2, σ = 0.52 ± 0.03. 相似文献
49.
Vasile I Parvulescu Viorica Parvulescu Uwe Endruschat Pascal Granger Ryan Richards 《Chemphyschem》2007,8(5):666-678
Sol‐gel synthesis of silica and silica–tantalum oxide embedded platinum nanoparticles is carried out using Pt colloids as templates. These colloids are prepared by reduction with Na[AlEt3H] and stabilized with different ligands (ammonium halide derivatives, non‐ionic surfactants with polyether chains, and 2‐hydroxy‐propionic acid). The aim of the present study is to prepare mesoporous silica embedded Pt colloids combining the “precursor concept” with the model of catalyst preparation using preformed spheres. Nanoparticles of Pt incorporated in high surface area mesoporous materials are formed after calcination. Further, it is observed that calcination of these catalysts causes partial aggregation and oxidation of the parent colloids, a process that is largely dependent on the nature of the stabilizing ligands. Several methods have been used for characterization of these materials: adsorption‐desorption isotherms at 77 K, H2 chemisorption, X‐ray diffraction(XRD), 29Si and 13C magic angle spinning (MAS) NMR, ammonia diffuse reflectance Fourier transform infrared spectroscopy (NH3‐DRIFT), transmission electron microscopy (TEM), and X‐ray photoelectron spectroscopy (XPS). It is found that both metal oxide systems exhibit Brønsted acidity (weaker for silica and quite strong for silica–tantalum oxide). In addition, NH3‐DRIFT experiments demonstrate the oxidative properties of the surface. Part of the adsorbed NH4+ species is oxidized to N2O. Testing these catalysts in the reduction of NO and NO2 with isopentane under lean conditions indicate that the activity of these catalysts is indeed dependent on the size of the platinum particles, with those of size 8–10 nm demonstrating the best results. The support likely contributes to this effect, particularly after Ta incorporation into silica. 相似文献
50.
In this study the electron beam (e-beam) radiation synthesis in “paste-like condition” and characterization of the network structure of acrylic acid (AA) sodium salt/xanthan gum (XG)/carboxymethylcellulose (CMC) superabsorbent hydrogels incorporating graphene oxide (GO) was investigated. The effects of the AA concentration on gel fraction, sol-gel analysis, swelling degree and network parameters, as well as the relationship between these parameters and radiation dose was also established.Gel fraction exceeds 90%, and the p0/q0 ratio shows a moderate degradation process. The swelling kinetic data were used to determine, first the swelling degree, second the diffusion characteristics, and third the average molecular weight between crosslinks (Mc), as well as. The diffusion data revealed a Fickian mechanism transport, for each hydrogel compositions. The network parameters (Mc and ξ) increased with absorbed dose, while cross-linking density and the radiation-chemical yields were decreased. 相似文献