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91.
The thermal decomposition of four commercial powders and of differently stored single crystals of sodium hydrogen carbonate is studied by power compensation DSC and by optical and FT-IR microscopy. Independently of manufacturer, specified purity and price, the thermal curves of all the commercial powders show a more or less pronounced low temperature peak preceding the one due to the main decomposition. Such small peak is not observed when samples of laboratory recrystallized material are used. However the thermal behaviour of the latter preparation differs remarkably depending on storage conditions: the material kept in closed glass containers decomposes at temperatures higher than those of the material stored in a dessiccator in the presence of concentrated H2SO4. The observation by optical microscopy of the behaviour of the surfaces of single crystals coming from different storage conditions when the temperature is raised in a Kofler heater helps the interpretation of the data collected. The mechanism of the decomposition is discussed and the relevant kinetic parameters reported. 相似文献
92.
93.
94.
95.
96.
A series of ferrocene‐containing liquid‐crystalline polyphosphonates with an even number of methylene groups are reported. All the polymers gave birefringent melts. The mesophase was identified as transparent with an increase in the spacer. The effects of pendant substitution and the spacer were studied with thermogravimetric analysis and differential scanning calorimetry. The effects of the phosphonate group in the spacer and the ferrocene ester group in the mesogen were examined. The presence of a steplike mesogenic structure and a pendant phenyl group in the spacer led to reductions in the glass‐transition and melting temperatures. The ferrocene moiety in the mesogen might be one of the reasons for the increased thermal stability and decreased liquid crystallinity. An energy‐minimized structure for the mesogenic and spacer segments was created with computer‐modeling programs, and it suggested the reason for the reductions in the glass‐transition and melting temperatures. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 2256–2263, 2002 相似文献
97.
B. T. Ibragimov S. A. Talipov T. F. Aripov 《Journal of inclusion phenomena and macrocyclic chemistry》1994,17(4):317-324
The structures of gossypol complexes are extremely sensitive to the halogenomethane present as the guest; e.g. changing the number of Cl atoms in chloromethane derivatives changes the structure of the gossypol complex. The crystals of C30H30O8·CH2Cl2 are monoclinic, space groupC2/c,a=21.320(4),b=19.199(6),c=15.765(2)Å, =113.05(2)o,V=5916(2)Å3,Z=8,D
x=1.35 g/cm3,T=295 K. The structure has been solved by direct methods and refined to the finalR value of 0.084 for 1828 reflections. In the structure H-bonded gossypol molecules form columns, generating channels in the structure which are filled by guest molecules. After decomposition (desolvation) monocrystals of the complexes are conserved without destruction, in which there are rather wide and empty channels though slightly smaller than in the complex. An attempt is made to explain some peculiarities of the behavior of the gossypol polymorph formed on the basis of its structure with empty channels.
Supplementary data relevant to this article have been deposited with the British Library Publication No. SUP 82165 (17 pages). 相似文献
98.
A. N. Chekhlov 《Journal of Structural Chemistry》2005,46(1):182-184
The crystal and molecular structure of tris(m-chlorophenyl)phosphine selenide, C18H12Cl3PSe (I), was investigated by X-ray diffraction (XRD) analysis. The trigonal rhombohedral structure of I (space group \(R\overline 3 c\), a = 14.110(2) Å, c = 32.360(4) Å, Z = 12) was solved by direct methods and refined by least squares in an anisotropic approximation (R = 0.029) for 1319 averaged measured reflections (CAD-4 automatic diffractometer, λCuKα). 相似文献
99.
Diamy A.-M. Hochard L. Legrand J.-C. Ricard A. 《Plasma Chemistry and Plasma Processing》1998,18(4):447-460
Measurements of nitrogen atom density, by means of NO chemical titration, along with an evaluation of the densities of some excited species N
2
(B, v=11), N
2
(B, v=2), N
2
(C, v=0), and N
2
+
(B,v=0), by means of a spectroscopic study of some bands of dinitrogen, are achieved along the flowing afterglow of a dinitrogen microwave plasma (2450 MHz) for several pressures. The concentrations obtained are in the following range: [N]10
+15
, [N
2
(B, 2)]10
+9
–10
+10
, [N
2
(B, 11)]10
+8
–10
+9
, [N
2
(C, 0)]10
+6
–10
+7
, [N
2
+
(B,0)]10
+6
-10
+8
(cm-3). From a kinetic study of the formation and decay of excited and charged species, an estimation of N
2
(A, v), N
2
(X, v, and N
2
+
(X) densities can be derived: [N
2
(A, v)]10
+12
, [N
2
(X, v6)]10
+15
–10
+16
, [N
2
(X, v12)]10
+14
–10
+15
, [N
2
+
(X)]10
+10
(cm
-3
). 相似文献
100.
Haishan Bu Erqiang Chen Shengyong Xu Kexin Guo Bernhard Wunderlich 《Journal of Polymer Science.Polymer Physics》1994,32(8):1351-1357
Single-molecule single crystals were grown from amorphous droplets of fractionated isotactic polystyrene. The crystals were analyzed by electron microscopy and electron diffraction. The molecular mass distribution could be matched with a statistical analysis of single-molecule particles (amorphous and crystals). Proof was brought that single molecules of isotactic polystyrene do not reach equilibrium dimensions on crystallization, rather assume the lamellar morphology with chain-folded macroconformation, also known from crystallization of polymolecular crystals. © 1994 John Wiley & Sons, Inc. 1 This article is a US Government work and, as such, is in the public domain in the United States of America. US Government contract No. DE-AC05-840R-21400. 相似文献