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21.
The interaction between oppositely charged polyelectrolytes, in this study poly(diallyldimethylammonium chloride) (PDADMAC)
and copolymers of acrylamide and sodium-acrylate differing in their chain length and charge density parameter (ξ) was investigated
in relation to the molar charge ratio of anionic to cationic charges (n
−/n
+). The molecular weights of the polyelectrolytes used were 2.9·105 g/mol for PDADMAC and for the polyacrylamide copolymers 14 ·106 g/mol as well as 5·105 g/mol obtained by ultrasonic degradation of the high molecular weight copolymers. The charge density parameters of the polyanions
used (ξ
PR
) varied between 0.14 and 0.64. Complexation between PDADMAC and high molecular weight polyanions leads mainly to macroscopic
phase separation whereas the degraded polyanions and PDADMAC formed soluble complexes as well as stable dispersions, if charge
excess was available. Precipitates and dispersions were characterized by several methods such as element analysis, thermogravimetry,
pyrolysis-GC/MS, PEL titration, ζ-potential measurements, determination of turbidity, particle size measurements and determination
of carbon content (TOC).
All precipitated complexes include about 20% water and are of 1:1 stoichiometry concerning ionic binding. Investigations
of dispersions confirm 1:1 stoichiometry of complex particles stabilized by excess polyelectrolyte and soluble complexes.
It was also found that the particle size can be varied via the charge density parameter of the polyanions used in the range
of negative charge excess.
Received: 21 June 2001 Accepted: 9 October 2001 相似文献
22.
Rainer Niewa Andreas Czulucki Gudrun Auffermann Martin Meven Frank Steglich 《Journal of solid state chemistry》2010,183(6):1309-1313
Large single crystals of ZrAsxSey (x>y, x+y≤2, PbFCl type of structure, space group P4/nmm) were grown by Chemical Transport. Structural details were studied by single crystal neutron diffraction techniques at various temperatures. One single crystal specimen with chemical composition ZrAs1.595(3)Se0.393(1) was studied at ambient temperature (R1=5.10 %, wR2=13.18 %), and a second crystal with composition ZrAs1.420(3)Se0.560(1) was investigated at 25 K (R1=2.70%, wR2=5.70 %) and 2.3 K (R1=2.30 %, wR2=4.70 %), respectively. The chemical compositions of the crystals under investigation were determined by wavelength dispersive X-ray spectroscopy. The quantification of trace elements was carried out by Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry. According to the crystal structure refinements the crystallographic 2a site is occupied by As, together with a significant amount of vacancies. One of the 2c sites is fully occupied by As and Se (random distribution). With respect to the fractional coordinates of the atoms, the crystal structure determinations based on the data obtained at 25.0 K and 2.3 K did not show significant deviations from ambient temperature results. The temperature dependence of the displacement parameters indicates a static displacement of As on the 2a sites (located on the (0 0 1) planes) for all temperatures. No indications for any occupation of interstitial sites or the presence of vacancies on the Zr (2a) site were found. 相似文献
23.
Dr. Thomas Lunkenbein Dr. Frank Girgsdies Anna Wernbacher Dr. Johannes Noack Dr. Gudrun Auffermann Akira Yasuhara Achim Klein‐Hoffmann Prof. Wataru Ueda Dr. Maik Eichelbaum Dr. Annette Trunschke Prof. Robert Schlögl Dr. Marc G. Willinger 《Angewandte Chemie (International ed. in English)》2015,54(23):6828-6831
Complex Mo,V‐based mixed oxides that crystallize in the orthorhombic M1‐type structure are promising candidates for the selective oxidation of small alkanes. The oxygen sublattice of such a complex oxide has been studied by annular bright field scanning transmission electron microscopy. The recorded micrographs directly display the local distortion in the metal oxygen octahedra. From the degree of distortion we are able to draw conclusions on the distribution of oxidation states in the cation columns at different sites. The results are supported by X‐ray diffraction and electron paramagnetic resonance measurements that provide integral details about the crystal structure and spin coupling, respectively. 相似文献
24.
Selective Template Removal by Thermal Depolymerization to Obtain Mesostructured Molybdenum Oxycarbide
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Martin Schieder Thomas Lunkenbein Carina Bojer Martin Dulle Julia vom Stein Gudrun Auffermann Tina Löbling Judith Schöbel Holger Schmalz Josef Breu 《无机化学与普通化学杂志》2015,641(10):1829-1834
The carbon content of mesostructured organic‐inorganic hybrid material of a cylindrical block copolymer template of poly(2‐vinylpyridine)‐block‐poly(allyl methacrylate) (P2VP‐b‐PAMA) and ammonium paramolybdate (APM) could be reduced by thermal depolymerization. By calcination in vacuo at 320 °C the PAMA core can be completely removed while the remaining P2VP brush preserves the mesostructure. The P2VP‐APM composite can then be carburized in‐situ to MoOxCy in a second pyrolysis step without any additional carbon source but P2VP. The molybdenum oxycarbide nanotubes obtained, form hierarchically porous non‐woven structures, which were tested as catalyst in the decomposition of NH3. They proved to be catalytically active at temperatures above 450 °C. The activation energy was estimated from an Arrhenius Plot to be 127 kJ · mol–1. 相似文献
25.
Hermann P Hermelink A Lausch V Holland G Möller L Bannert N Naumann D 《The Analyst》2011,136(6):1148-1152
Tip-enhanced Raman spectroscopy (TERS) is a highly sensitive spectroscopic technique which combines the advantages of optical spectroscopy with the requirements needed for the characterization of biological nano-structures. In this study, TERS was used to investigate the applicability of this spectroscopic technique for the detection of different virus strains like avipoxvirus and adeno-associated virus. TERS spectra obtained from different particles of the same virus strain show variations in relative peak intensities and positions of most spectral features observed. These spectral variations were higher for the larger avipoxvirus particles (?≈350 nm) than for the smaller adeno-associated virus particles (?≈26 nm). 相似文献
26.
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28.
Gudrun Freitag 《Journal of multivariate analysis》2005,94(1):123-158
Semiparametric models to describe the functional relationship between k groups of observations are broadly applied in statistical analysis, ranging from nonparametric ANOVA to proportional hazard (ph) rate models in survival analysis. In this paper we deal with the empirical assessment of the validity of such a model, which will be denoted as a “structural relationship model”. To this end Hadamard differentiability of a suitable goodness-of-fit measure in the k-sample case is proved. This yields asymptotic limit laws which are applied to construct tests for various semiparametric models, including the Cox ph model. Two types of asymptotics are obtained, first when the hypothesis of the semiparametric model under investigation holds true, and second for the case when a fixed alternative is present. The latter result can be used to validate the presence of a semiparametric model instead of simply checking the null hypothesis “the model holds true”. Finally, various bootstrap approximations are numerically investigated and a data example is analyzed. 相似文献
29.
Lutz Grotjahn Ronald Frank Gudrun Heisterberg-Moutsis Helmut Blöcker 《Tetrahedron letters》1984,25(47):5373-5376
Negative ion FAB-MS is recommended for the rapid routine identification of monomeric as well as oligomeric building blocks used in the phosphotriester synthesis of DNA fragments. 相似文献
30.