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141.
Recent studies in ultrafast electron crystallography (UEC) using a reflection diffraction geometry have enabled the investigation of a wide range of phenomena on the femtosecond and picosecond time scales. In all these studies, the analysis of the diffraction patterns and their temporal change after excitation was performed within the kinematical scattering theory. In this contribution, we address the question, to what extent dynamical scattering effects have to be included in order to obtain quantitative information about structural dynamics. We discuss different scattering regimes and provide diffraction maps that describe all essential features of scatterings and observables. The effects are quantified by dynamical scattering simulations and examined by direct comparison to the results of ultrafast electron diffraction experiments on an in situ prepared Ni(100) surface, for which structural dynamics can be well described by a two-temperature model. We also report calculations for graphite surfaces. The theoretical framework provided here allows for further UEC studies of surfaces especially at larger penetration depths and for those of heavy-atom materials. 相似文献
142.
143.
Florian Modicom Ellen M. G. Jamieson Elise Rochette Stephen M. Goldup 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2019,131(12):3915-3919
We report the unexpected discovery of a tandem active template CuAAC‐rearrangement process, in which N2 is extruded on the way to the 1,2,3‐triazole product to give instead acrylamide rotaxanes. Mechanistic investigations suggest this process is dictated by the mechanical bond, which stabilizes the CuI‐triazolide intermediate of the CuAAC reaction and diverts it down the rearrangement pathway; when no mechanical bond is formed, the CuAAC product is isolated. 相似文献
144.
A high-performance liquid chromatography (HPLC) method was established using an analytical reversed-phase column and gradient
elution to achieve chromatographic separation of typical compounds in essential oils. For detection, a diode array detector
monitoring different wavelengths simultaneously as well as a mass spectrometer (MS) were used. Atmospheric pressure chemical
ionization operating in the positive mode turned out to be a suitable tool to detect volatiles of different chemical classes
and to identify them in essential oil matrices. Characteristic fingerprints of eucalyptus, lavender, may chang, pine, rosemary,
thyme, and turpentine essential oils monitored at a representative wavelength (220 nm) demonstrated the suitability of HPLC
in essential oil analysis. Additional monitoring wavelengths (210, 250, and 280 nm) provided useful information about the
identity of the specific component and opened the possibility to differentiate presumably coeluting compounds by means of
their distinct absorption behavior. Finally, peak assignment in seven essential oils was performed on the basis of characteristic
retention times and UV and MS data of a broad set of reference volatiles. 相似文献
145.
Calcium carbonate (vaterite) nanoparticles of 20-60 nm size were obtained without stabilizing tensides by heating a dispersion of calcium bicarbonate (CaHCO(3)) in ethylene glycol for 30 minutes at 40 to 100 °C. 相似文献
146.
The four epimeric azido alcohols of estra-1,3,5(10)-trien-3-methyl ether with nitrogen at C-16 and oxygen at C-17 were prepared by the following reactions: cleavage of the 16α,17α-epoxide 1 with sodium azide affords the 16β,17α-azido alcohol 2a. The analogous reaction of the 16β,17β-epoxide 4 gives the 17α,16β-azido alcohol 5a and the desired 16α,17β-azido alcohol 6a in low yield. 6a is obtained in a smooth reaction by substitution of the 16β,17β-bromohydrine 8 with sodium azide. Sodium borohydride reduction of the 16β-azido-17-ketone 9 yields the 16β,17β-azido alcohol 10a, reduction of 16α-azido-17-ketone 13 with lithium borohydride gives the 16α,17α-azido alcohol 14a. From the azido alcohols the corresponding amino alcohols 3a, 7a, 11a and 15a are prepared with hydrazine hydrate/Raney nickel. The amino alcohols give the acetic anhydride the corresponding acetylamino alcohols. The cis-amino alcohols 11a and 15a react with acetone to the corresponding oxazolidines 12 and 16. 相似文献
147.
Zusammenfassung Es wurde ein Mikroverfahren zur Bestimmung von organisch gebundenem Fluor ausgearbeitet. Die Substanz wird mit Kalium im Glasröhrchen aufgeschlossen. Die Röhrchen werden vorher durch Auskochen mit Salzsäure blindwertfrei gemacht. Die Titration des Fluoridions kann durch geeignete Maßnahmen direkt in der Aufschlußlösung erfolgen, so daß die zeitraubende Abdestillation des Fluorids erspart wird. Die Titration selbst wird in bekannter Weise mittels Thoriumnitrat durchgeführt. Als Indikatoren dienen Alizarinrot S, dem Wasserblau oder Chinablau zugesetzt ist. ZurpH-Einstellung dient ein Glycin-Perchlorsäure-Puffer.
Summary A method was developed for the determination of organically bound fluorine. The sample is decomposed by heating with potassium in a small glass tube. The tubes are treated ahead of time with hot hydrochloric acid to render them blank-free. The titration of the fluoride ion can be conducted directly in the decomposition solution if proper precautions are taken. The time-consuming distilling off of the fluoride is thus avoided. The titration itself is made in the usual manner by thorium nitrate. The indicator is alizarin red S, to which is-added water blue or China blue. A glycerol-perchloric acid buffer is used to-adjust the ph.
Résumé Mise au point d'un procédé de microdosage du fluor dans les composés-organiques. La substance est attaquée par le potassium dans de petits tubes de verre. Ceux-ci sont préalablement traités dans l'acide chlorhydrique bouillant pour éviter toute correction d'essai à blanc. Le titrage de l'ion fluorure peut être exécuté directement dans la solution provenant de l'attaque sous réserve de respecter des conditions appropriées; on évite ainsi la longue séparation du fluorure par distillation. Le titrage proprement dit est effectué de la façon habituelle à l'aide de nitrate de thorium en présence d'un indicateur constitué par du rouge d'alizarine S auquel on a ajouté du bleu soluble (Wasserblau ou Chinablau). On opère àpH constant à l'aide du tampon glycocolle — acide perchlorique.相似文献
148.
149.
Zusammenfassung 2,4,5-substituierte 4-Alkylamino-2H-imidazole entstehen mit guten Ausbeuten aus 2-Methyl-2,4-diaryl-imidazolin-3-thionen-(5) durch Umsetzung mit prim. bzw. sek. aliphatischen oder heterocyclischen Aminen in Benzol bei Rückflußtemperatur.
55. Mitt.:F. Asinger, E.-Chr. Witte undW. Schäfer, Ann. Chem., im Druck.
Teil der DissertationG. Kriebel, Techn. Hochschule Aachen, 1965. 相似文献
2.4.5-substituted 4-alkylamino-2H-imidazoles are formed in good yields by the reaction of 2-methyl-2.4-diaryl-3-imidazoline-5-thiones with prim. or sec. aliphatic or heterocyclic amines in boiling benzene.
55. Mitt.:F. Asinger, E.-Chr. Witte undW. Schäfer, Ann. Chem., im Druck.
Teil der DissertationG. Kriebel, Techn. Hochschule Aachen, 1965. 相似文献
150.
F. Asinger W. Schäfer H. Meisel H. Kersten A. Saus 《Monatshefte für Chemie / Chemical Monthly》1967,98(2):338-352
Zusammenfassung 2,2,5-Trisubstituierte Imidazolidin-thione-(4) lassen sich mittels Schwefels mit guten Ausbeuten zu Imidazolin-(3)-thionen-(5) dehydrieren. Hierüber sowie über einige Verbesserungen der bisher bekannten Synthesen für insbesondere 2,2,5-trisubstituierte Imidazolidin-thione-(4) wird berichtet.
Mitt.:F. Asinger, W. Schäfer undH. Triem, Mh. Chem.97, 1510 (1966).
Teil der Dissertation vonH. Meisel, Techn. Hochschule Aachen, 1963.
Teil der Dipl.-Arbeit vonHilde Kersten, Techn. Hochschule Aachen, 1963, und Teil der Dissertation vonHilde Kersten, Techn. Hochschule Aachen, 1965. 相似文献
Dehydration of 2.2.5-trisubstituted imidazolidine-(4)-thiones with elementary sulfur gives in good yields 3-imidazoline-(5)-thiones. This reaction and improved methods of the well known syntheses of especially 2.2.5-trisubstituted imidazolidine-(4)-thiones are described.
Mitt.:F. Asinger, W. Schäfer undH. Triem, Mh. Chem.97, 1510 (1966).
Teil der Dissertation vonH. Meisel, Techn. Hochschule Aachen, 1963.
Teil der Dipl.-Arbeit vonHilde Kersten, Techn. Hochschule Aachen, 1963, und Teil der Dissertation vonHilde Kersten, Techn. Hochschule Aachen, 1965. 相似文献