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71.
New AP Wolff JC Crabtree S Freitas do Santos L Okafo G Lee J Divan K 《Journal of chromatography. A》2001,913(1-2):205-208
We have recently investigated the biodegradation of a number of acidic aromatic compounds that give excellent chromatography using trifluoroacetic acid (TFA) based HPLC methods. Unfortunately HPLC methods using TFA are not usually compatible with detection by negative ion mass spectrometry as TFA suppresses ionisation of the analyte during the electrospray process. We present a preliminary investigation of the use of an anion-exchange micro-membrane suppressor to remove TFA on-line post column with the aim of improvement of mass spectral data using an aromatic acid as an example, Thus LC-MS using a TFA based HPLC method with negative ion mass spectral detection is shown to be possible with good sensitivity. 相似文献
72.
Manuel J.S. Monte Sónia P. Pinto Ana I.M.C. Lobo Ferreira Luísa M.P.F. Amaral Vera L.S. Freitas Maria D.M.C. Ribeiro da Silva 《The Journal of chemical thermodynamics》2012,45(1):53-58
This work reports new experimental thermodynamic results on fluorene. Vapor pressures of both crystalline and liquid phases were measured using a pressure gauge (capacitance diaphragm manometer) and Knudsen effusion methods over a wide temperature range (292.20 to 412.16) K yielding accurate determination of enthalpy and entropy of sublimation and of vaporization. The enthalpy of sublimation was also determined using Calvet microcalorimetry. The enthalpy of fusion was derived from vapor pressure results and from d.s.c. experiments. Static bomb calorimetry was used to determine the enthalpy of combustion of fluorene from which the standard enthalpy of formation in the crystalline phase was calculated. The enthalpy of formation in the gaseous phase was calculated combining the result derived for the crystalline phase with the enthalpy of sublimation. 相似文献
73.
Fabio Rodrigues Gustavo M. do Nascimento Paulo S. Santos 《Macromolecular rapid communications》2007,28(5):666-669
Polyaniline is a model molecular system in the study of conductive polymers. Ionic liquids, on the other hand, are becoming more and more a very convenient alternative for conventional organic solvents. The dissolution of polyaniline‐emeraldine base (PANI‐EB) in imidazolium ILs leads to its doping, as indicated by optical and resonance Raman spectroscopies. In this study, it is proposed that the interaction of PANI‐EB and imidazolium ILs involves the specific interaction of the quinoid moiety of the former with the imidazolium ring of the latter, an interpretation that is also based on N K‐edge XANES measurements of neat PANI‐EB, neat ILs, and of their solutions.
74.
Polyanna Silveira Hornung Layse do Prado Cordoba Simone Rosa da Silveira Lazzarotto Egon Schnitzler Marcelo Lazzarotto Rosemary Hoffmann Ribani 《Journal of Thermal Analysis and Calorimetry》2017,127(3):1869-1877
Determination of the characteristics of native starches is crucial in order to select their best application in various industrial fields. Thus, two different types of non-traditional native starches from the Dioscoreaceas species (Dioscorea sp. and Dioscorea piperifolia Humb. var. Wild) were studied regarding their thermal, structural and rheological properties. The results were contrasted with traditional commercial starch sources (potato, cassava and corn). From the thermogravimetric results (TG/DTG), D. piperifolia starch obtained the highest thermal stability of the samples, except for potato starch. Furthermore, using differential scanning calorimetry and viscoamylograph profiles (RVA), it was found that the Dioscoreaceas starches presented a higher onset (T o) temperature and susceptibility to retrogradation. They also showed lower values in relation to relative crystallinity, which was calculated from their X-ray patterns and tendency to white (L*) colour. The shapes of the Discoreaceas starch granules were determined using electron microscopy; it was found that as the potato starch the Dioscoreaceas starches showed a wide range of particle size. 相似文献
75.
Soraa Bouattour Wannes Kallel Ana Maria Botelho do Rego L.F. Vieira Ferreira I. Ferreira Machado Sami Boufi 《应用有机金属化学》2010,24(10):692-699
This work reports on the synthesis of Li‐doped TiO2 nanoparticles using the sol–gel process and solid‐state sintering, and investigates their potential use as a photocatalyst for degradation under sunlight excitation of different organic model compounds in aqueous solution. The structure of the nanocrystals was examined by X‐ray diffraction, UV‐vis ground state diffuse reflectance absorption spectra and X‐ray photoelectron emission spectroscopy. Results showed that samples prepared by sol–gel process and calcined at 400 °C are composed of a mixture of anatase and rutile phases, in contrast to the one prepared by solid‐state sintering, which exhibits an anatase phase with Li being involved in a spinel phase. The photocatalytic degradation of aqueous solutions of different aromatic compounds was successfully achieved under sunlight excitation in presence of Li‐doped TiO2 prepared via sol–gel process. It was shown that the calcination temperature and the preparation mode greatly affect the photocatalytic efficiency. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
76.
Affolder T Akimoto H Akopian A Albrow MG Amaral P Amidei D Anikeev K Antos J Apollinari G Arisawa T Artikov A Asakawa T Ashmanskas W Azfar F Azzi-Bacchetta P Bacchetta N Bachacou H Bailey S de Barbaro P Barbaro-Galtieri A Barnes VE Barnett BA Baroiant S Barone M Battle C Bauer G Bedeschi F Belforte S Bell WH Bellettini G Bellinger J Benjamin D Bensinger J Beretvas A Berge JP Berryhill J Bhatti A Binkley M Bisello D Bishai M Blair RE Blocker C Bloom K Blumenfeld B Blusk SR Bocci A Bodek A 《Physical review letters》2002,88(7):071806
We present the first general search for new heavy particles, X, which decay via X --> WZ0 --> e(nu)+jj as a function of M(X) and Gamma(X) in pp collisions at square root[s] = 1.8 TeV. No evidence is found for production of X in 110 pb(-1) of data collected by the Collider Detector at Fermilab. General cross section limits are set at the 95% C.L. as a function of mass and width of the new particle. The results are further interpreted as mass limits on the production of new heavy charged vector bosons which decay via W' --> WZ0 in an extended gauge model as a function of the width, Gamma(W'), and mixing factor between the W' and the standard model W bosons. 相似文献
77.
José R. B. Gomes Luísa M. P. F. Amaral Manuel A. V. Ribeiro da Silva 《Journal of Physical Organic Chemistry》2008,21(5):365-371
The standard (p0 = 0.1 MPa) molar enthalpy of formation of 3,4‐dimethylbenzophenone was derived from the standard molar energy of combustion, in oxygen, at T = 298.15 K, measured by static bomb combustion calorimetry. The Calvet high temperature vacuum sublimation technique was used to measure the enthalpy of sublimation of the compound. From these experimental parameters, the standard molar enthalpy of formation of 3,4‐dimethylbenzophenone, in the gaseous phase and at T = 298.15 K, was derived as ?(17.1 ± 2.9) kJ mol?1. Density functional theory was used to investigate the gas‐phase molecular energetics of the 12 dimethylbenzophenones. Molecular geometries and vibrational frequencies were computed at the B3LYP/6‐31G(d) level of theory. The larger 6‐311+G(2d,2p) basis set was used to compute the energy of all dimethylbenzophenones and of the other compounds that were considered for the estimation of the standard molar enthalpies of formation at T = 298.15 K. The calculations show that the 2,2′‐ and 4,4′‐dimethylbenzophenones are the least and most stable isomers, respectively. Finally, the calculated enthalpy of formation of the benzophenone that was also studied experimentally, 3,4‐dimethylbenzophenone, is ?16.7 kJ mol?1, which is in excellent agreement with the experimental result. Copyright © 2008 John Wiley & Sons, Ltd. 相似文献
78.
Sol-Gel Synthesis of Transparent Alumina Gel and Pure Gamma Alumina by Urea Hydrolysis of Aluminum Nitrate 总被引:2,自引:0,他引:2
Maria I. F. Macêdo Carla C. Osawa Celso A. Bertran 《Journal of Sol-Gel Science and Technology》2004,30(3):135-140
-Alumina was synthesized by a sol-gel method with the aluminum ion hydrolysis control performed by urea. The initial saturated Al3+/urea solution presented urea coordinated with the aluminum ion, as shown in the 13C NMR and 27Al NMR spectra and longitudinal relaxation times, T
1, from the latter. The substitution of water molecules in the Al3+ coordination shell by urea controlled the hydrolysis process and provided an extensive nucleation during the initial steps of the aluminum hydroxide formation due to urea thermolysis at 90°C. The resulting sol, composed of Al(OH)3 nanoparticles, coalesced and became a transparent gel permeated by a solution of urea and the polycation ion [Al13O4(OH)24(H2O)12]7+. The freshly prepared gel was transformed, under heating at 300°C, directly to -alumina, characterized by FTIR, 27Al-MAS-NMR and SBET techniques, without - or -phases, as a consequence of the high degree of homogeneity of the -alumina precursor. 相似文献
79.
Arnaldo Simal do Nascimento 《Journal of Differential Equations》2003,190(1):16-38
We prove existence and establish the asymptotic behavior, as ε→0, of stable stationary solutions to the equation ut=ε∇·[d(x)∇u]+(1−u2)[u−a(x)], for , where , N?2, with Neumann boundary condition. The function a(x)∈C0,ν(Ω) satisfies −1<a(x)<1 and vanishes on some hypersurfaces. The results generalize to N-dimensional domains and to variable diffusivity earlier paper by Angenent et al. (J. Differential Equations 67 (1987) 212). 相似文献
80.
In this paper, we obtain some rigidity theorems for compact Riemannian manifolds Ω with boundary M and nonnegative Ricci curvature; for instance, we prove that the existence of certain functions on M together with a lower bound c > 0 on the principal curvtures of M imply that Ω is an euclidean ball of radius $ {1\over c} $ . 相似文献