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31.
Hisanori Yamane Ryouji Tanimura Junichi Takahashi Masahiko Shimada 《Journal of solid state chemistry》2006,179(1):289-295
New compounds CaY2Ge3O10 and CaY2Ge4O12 were prepared by heating mixtures of CaCO3, Y2O3 and GeO2 at 1200 °C. CaY2Ge3O10 is stable at 1300 °C, while CaY2Ge4O12 decomposes into a melt and CaY2Ge3O10 at approximately 1250 °C. We obtained single crystals of CaY2Ge3O10 by cooling a sample with an initial composition of Ca:Y:Ge=1:2:8 from 1300 °C with a rate of −6 °C/h. The crystal structure of CaY2Ge3O10 was determined by single crystal X-ray diffraction. CaY2Ge3O10 crystallizes in the monoclinic space group P21/c with a=6.0906(8), b=6.8329(8), and β=109.140(3)°, Z=4, and R1=0.029 for I>2σ(I). In the structure of CaY2Ge3O10, Ca and Y atoms are situated disorderly in three 7-fold coordination sites between isolated germanate groups of triple GeO4 tetrahedra, Ge3O10. The structural formula of CaY2Ge3O10 is expressed as (Ca0.45Y0.55)(Ca0.46Y0.54)(Ca0.09Y0.91)Ge3O10. The crystal structure of CaY2Ge4O12 was analyzed by the Rietveld method for the X-ray powder diffraction pattern. CaY2Ge4O12 is isotypic with SrNa2P4O12, crystallizing in the orthorhombic space group P4/nbm, a=9.99282(6), , Z=2, Rwp=0.092, Rp=0.067. CaY2Ge4O12 contains four-membered GeO4-tetrahedra rings, Ge4O12. Eight-fold coordinated square-anitiprism sites and 6-fold octahedral sites between the layers of the Ge4O12 rings are occupied by Y atom and Ca/Y atoms, respectively The structural formula is Y(Ca0.5Y0.5)2Ge4O12. 相似文献
32.
Hideyuki Yoshida Junichiro Sonoda Junichi Ishida Masatoshi Yamaguchi 《Analytica chimica acta》2005,534(2):177-183
A simple screening method of organic aciduria by spectrofluorometric measurement of total dicarboxylic acids in human urine is described. This method is based on an intramolecular excimer-forming fluorescence derivatization with a pyrene reagent, 4-(1-pyrene)butanoic acid hydrazide (PBH). Dicarboxylic acids in urine were converted to the corresponding dipyrene-labeled derivatives by reaction with PBH in the presence of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and pyridine, and the derivatives afforded intramolecular excimer fluorescence (420-540 nm) which can clearly be discriminated from the normal fluorescence (360-420 nm) emitted from reagent blanks. The technique is so selective that it permits spectrofluorometric measurement of total amount of dicarboxylic acids by the direct derivatization of diluted urine samples. The same reaction mixture has also served as a liquid chromatographic (LC) sample for the separative determination of individual dicarboxylic acids. The spectrofluorometric data did not contradict with the LC data. These methods were usefully applied to preliminary screening test of glutaric aciduria. In conclusion, the present derivatization method allows rapid and direct determination of total amount of dicarboxylic acids in human urine samples. 相似文献
33.
Contamination of the exterior surface of vials of cytostatic drugs by the drugs themselves is a potential hazard to human health. This study developed a validated method using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for the determination of contamination of the exteriors of vials of cisplatin and carboplatin. Large Alpha® sampling swabs were employed to wipe the vial exterior. Cisplatin or carboplatin and gold(III) as an internal standard were derivatized by N,N-diethyldithiocarbamate (DDTC). Pt(DDTC)3+ and Au(DDTC)2+ were monitored by the respective transitions of m/z 639.3-490.9 and 493.0-345.0, respectively. Each separation was completed within 9 min using a 3 μm particle ODS-column. Calibration curves for cisplatin and carboplatin were linear over concentration ranges of 30-10,000 and 30-30,000 pg vial−1, respectively. The accuracies and precisions were 96.1-102.5% and within 8.2% for intra-assay and 99.6-103.3% and within 7.6% for inter-assay, respectively. Their lower limit of quantification was 30 pg vial−1. Amounts of 0.17-17.0 ng vial−1 as cisplatin and 0.48-794 ng vial−1 as carboplatin were detected from the exterior surface of the vials. This validated method using LC-ESI-MS/MS for the determination of platinum anticancer drugs is helpful for monitoring contamination of the exterior surface of drug vials. 相似文献
34.
We consider the effect of a magnetic field for the asymptotic behavior of the trace of the heat kernel for the Schrödinger operator. We discuss the case where the operator has compact resolvents in spite of the fact that the electric potential is degenerate on some submanifold. According to the degree of the degeneracy, we obtain non-classical asymptotics. 相似文献
35.
The transient absorption properties of several commercially available TiO2 photocatalysts were investigated by femtosecond diffuse-reflectance spectroscopy. Using femtosecond diffuse-reflectance spectroscopy, the quantities and rates of the initial trapping processes of holes and electrons generated by the photoexcitation of TiO2 photocatalysts were investigated. It was found that the total amounts of trapped electrons for the pure-anatase and pure-rutile TiO2 became smaller with increasing particle size, but increased again when the particles’ diameters were larger than 50 nm. The anatase–rutile mixed TiO2 photocatalysts were found to have smaller amounts of trapped electrons compared with pure-anatase and pure-rutile TiO2 photocatalysts. The lifetimes of trapped holes of various TiO2 photocatalysts were also investigated, and it was found that the lifetimes were proportional to the anatase–rutile mixed ratios. 相似文献
36.
曝光系统离焦对平面全息光栅衍射波前的影响 总被引:1,自引:0,他引:1
波前像差是衍射光栅的重要技术指标,它直接影响光栅的分辨率。由光致刻蚀剂记录两束相干光干涉条纹是制作全息光栅的关键步骤。为了提高全息光栅曝光系统调整精度、减小离焦、降低光栅的衍射波前像差,从离焦对反射球面准直镜的准直光平行度的影响程度出发,分析了准直光平行度对全息光栅衍射波前像差的影响。理论分析和数值模拟结果表明,准直镜调整误差直接决定全息光栅衍射波前像差大小。以3种不同刻线密度光栅为例,得出了准直镜调整误差的允许变化范围。 相似文献
37.
Ramesh P Okazaki T Taniguchi R Kimura J Sugai T Sato K Ozeki Y Shinohara H 《The journal of physical chemistry. B》2005,109(3):1141-1147
Double-wall carbon nanotubes (DWNTs) have been selectively synthesized over Fe/Co loaded mesoporous silica by catalytic chemical vapor deposition of alcohol. Several silica materials with desired pore diameter and morphology have been investigated for the DWNT growth. The diameter distribution and selectivity of the DWNT are found to depend on the reaction temperature, pore size, and thermal stability of the support material. A high-yield synthesis of DWNTs has been achieved at 900 degrees C over high-temperature stable mesoporous silica. The outer diameter of DWNTs is found to be in the range of 1.5-5.4 nm with a "d" spacing of 0.38 +/- 0.02 nm between inner and outer layers, which is much larger than those of multiwall carbon nanotubes. 相似文献
38.
We report a simple preparation of Pd particles dispersed mesoporous carbons. The carbons were prepared by steam activation of carbonized vinylidene chloride/methyl acrylate copolymer (poly(VDC/MA)) containing yttrium acetylacetonate (Y(acac)(3)) and palladium acetylacetonate (Pd(acac)(2)). The resulting carbons consist of high contents of mesopore and uniformly dispersed fine Pd particles. We measured the catalytic activities of the carbons obtained for hydrogenation of methyl linoleate. The Pd particles dispersed in mesoporous activated carbons obtained from poly(VDC/MA) containing both Y(acac)(3) and Pd(acac)(2) showed high catalytic activities, compared with the microporous activated carbon obtained from poly(VDC/MA) containing only Pd(acac)(2). Especially Pd particles dispersed in mesoporous carbons exhibited excellent selectivity for hydrogenation of diene (methyl linoleate) to monoene (methyl oleate). 相似文献
39.
40.
Akiyama H Sakata K Makiyma D Nakamura K Teshima R Nakashima A Ogawa A Yamagishi T Futo S Oguchi T Mano J Kitta K 《Journal of AOAC International》2011,94(5):1540-1547
In many countries, the labeling of grains, feed, and foodstuff is mandatory if the genetically modified (GM) organism content exceeds a certain level of approved GM varieties. We previously developed an individual kernel detection system consisting of grinding individual kernels, DNA extraction from the individually ground kernels, GM detection using multiplex real-time PCR, and GM event detection using multiplex qualitative PCR to analyze the precise commingling level and varieties of GM maize in real sample grains. We performed the interlaboratory study of the DNA extraction with multiple ground samples, multiplex real-time PCR detection, and multiplex qualitative PCR detection to evaluate its applicability, practicality, and ruggedness for the individual kernel detection system of GM maize. DNA extraction with multiple ground samples, multiplex real-time PCR, and multiplex qualitative PCR were evaluated by five laboratories in Japan, and all results from these laboratories were consistent with the expected results in terms of the commingling level and event analysis. Thus, the DNA extraction with multiple ground samples, multiplex real-time PCR, and multiplex qualitative PCR for the individual kernel detection system is applicable and practicable in a laboratory to regulate the commingling level of GM maize grain for GM samples, including stacked GM maize. 相似文献