全文获取类型
收费全文 | 98649篇 |
免费 | 9640篇 |
国内免费 | 8376篇 |
专业分类
化学 | 37135篇 |
晶体学 | 1128篇 |
力学 | 12123篇 |
综合类 | 1750篇 |
数学 | 36593篇 |
物理学 | 27936篇 |
出版年
2024年 | 197篇 |
2023年 | 937篇 |
2022年 | 2859篇 |
2021年 | 2785篇 |
2020年 | 2396篇 |
2019年 | 2301篇 |
2018年 | 2092篇 |
2017年 | 2719篇 |
2016年 | 3194篇 |
2015年 | 2743篇 |
2014年 | 4327篇 |
2013年 | 6367篇 |
2012年 | 4920篇 |
2011年 | 5677篇 |
2010年 | 4965篇 |
2009年 | 5932篇 |
2008年 | 5924篇 |
2007年 | 6159篇 |
2006年 | 5302篇 |
2005年 | 4541篇 |
2004年 | 3851篇 |
2003年 | 3674篇 |
2002年 | 5887篇 |
2001年 | 3222篇 |
2000年 | 2666篇 |
1999年 | 2321篇 |
1998年 | 2177篇 |
1997年 | 1822篇 |
1996年 | 1613篇 |
1995年 | 1340篇 |
1994年 | 1281篇 |
1993年 | 1121篇 |
1992年 | 1090篇 |
1991年 | 781篇 |
1990年 | 711篇 |
1989年 | 555篇 |
1988年 | 549篇 |
1987年 | 398篇 |
1986年 | 358篇 |
1985年 | 525篇 |
1984年 | 411篇 |
1983年 | 254篇 |
1982年 | 422篇 |
1981年 | 576篇 |
1980年 | 485篇 |
1979年 | 544篇 |
1978年 | 437篇 |
1977年 | 338篇 |
1976年 | 279篇 |
1973年 | 211篇 |
排序方式: 共有10000条查询结果,搜索用时 0 毫秒
991.
Vanadium Doped Sol-Gel TiO2 Coatings 总被引:1,自引:0,他引:1
Maria Crisan Maria Zaharescu D. Crisan Rodica Ion Mihaela Manolache 《Journal of Sol-Gel Science and Technology》1998,13(1-3):775-778
A study of the experimental conditions required to obtain vanadium doped sol-gel TiO2 coatings is presented. Tetraethyl orthotitanate was employed as the TiO2 source and VCl3, VOSO4 · H2O and VOSO4 dissolved H2SO4 where employed as vanadium sources.Dip coating has been used to produce coatings on silicon wafers, spectral carbon electrodes and titanium electrodes. Both supported and unsupported films have been studied by UV-Vis spectra, IR spectroscopy and X-ray diffraction (XRD). The measurements have been made on samples as prepared and treated thermally at temperatures between 100°C and 300°C. The thermal treatment temperatures have been established from DTA/TGA measurements.The vanadium doped sol-gel TiO2 coatings have been tested as sensors for redox potential measurements in electrochemical processes. The influence of both the thickness of films and the nature of substrate has been investigated. 相似文献
992.
E. L. Anderson M. M. Thomason H. T. Mayfield W. Bertsch 《Journal of separation science》1979,2(6):335-342
A versatile two-dimensional gas chromatograph is described, consisting of 2 separate ovens, one intermediate trap, an auxiliary inlet, and the necessary hardware to effect off-line switching according to the principle of Deans. The unit has been designed for use with high resolution glass capillary columns. The performance of individual instrumental components was critically evaluated. Results showed that low dead volume glass to metal connections were required in the manifold and detector lines to minimize extra-column effects. The mass of the intermediate trap must be low to allow rapid heating. Operational parameters are discussed and examples of some applications are shown. 相似文献
993.
A capillary gas chromatographic method is described for the quantitative determination of liquid paraffin in blood. Paraffin is extracted from blood into n-heptane. After solvent evaporation and dissolution of the residue in 100–200 μl n-heptane one μl is injected into a gas chromatograph fitted with a fused silica capillary column (Permabond® OV-1-CB-0.1, 10 m × 0.32 mm i.d.) and flame ionization detector. Analysis is performed by using an oven program [50°C (3 min)?285°C (5 min), rise 10%min]. The sensitivity (1.5 ng hexadecane) and the reproducibility prove the applicability of the method for the determination of liquid paraffin in blood and for the study of the stability of the liquid paraffin hollow fiber membranes used in an extracorporeal liver support system. 相似文献
994.
聚酰胺修饰碳糊电极测定槲皮素的研究 总被引:10,自引:0,他引:10
用聚酰胺修饰碳糊电极在pH360的Briton-Robinson缓冲溶液中,将槲皮素开路富集一定时间后,从045V(vs.Ag/AgCl)向阴极化扫描至-055V获得I-E曲线。槲皮素的峰电位为018V。峰电流与槲皮素浓度在10~400μmol/L范围内呈良好的线性关系。所拟定方法用于芦丁水解产物测定,结果满意。 相似文献
995.
Wen-Jia Zhou Shu-Juan Bao Yan-Yu Liang Ben-Lin He Hu-Lin Li 《Journal of Solid State Electrochemistry》2006,10(5):277-282
Pure-phase and well-crystallized spinel LiMn2O4 powders were successfully synthesized by a simple rheological phase method. The thermal behavior and structure properties
of the powders prepared by the rheological phase method compared with the solid-state reaction were investigated by thermogravimetry,
powder X-ray diffraction , scanning electron microscopy and transmission electron microscopy. According to the results of
the electrochemical tests, it is obvious that the sample resulting from the rheological phase method shows higher discharge
capacity and better cycling stability than one formed in the solid-state reaction. The cyclic voltammogram and columbic efficiency
curves also confirm that the product by the rheological phase method has a good cycling performance due to its fine cubic
spinel structure and morphology. 相似文献
996.
An automated on-line method for the determination of the isoflavones, daidzein and genistein, was developed using in-tube solid-phase microextraction coupled to high-performance liquid chromatography (in-tube SPME-HPLC). In-tube SPME is a new extraction technique for organic compounds in aqueous samples, in which analytes are extracted from the sample directly into an open tubular capillary by repeated draw/eject cycles of sample solution. Daidzein, genistein and their glucosides tested in this study were clearly separated within 8 min by HPLC using an XDB-C8 column with diode array detection. In order to optimize the extraction of these compounds, several in-tube SPME parameters were examined. The glucosides daidzin and genistin were analyzed as aglycones after hydrolysis because the glucosides were not concentrated by in-tube SPME. The optimum extraction conditions for daidzein and genistein were obtained with 20 draw/eject cycles of 40 microl of sample using a Supel-Q porous layer open tubular capillary column. The extracted compounds were easily desorbed from the capillary by mobile phase flow, and carryover was not observed. Using the in-tube SPME-HPLC method, the calibration curves of these compounds were linear in the range 5-200 ng/ml, with a correlation coefficient above 0.9999 (n = 18), and the detection limits (S/N = 3) were 0.4-0.5 ng/ml. This method was successfully applied to the analysis of soybean foods without interference peaks. The recoveries of aglycones and glucosides spiked into food samples were above 97%. 相似文献
997.
The adverse effects of injection solvent strength on microbore packed column SFC band broadening are demonstrated and a solventless injection system that eliminates these effects is introduced. The injection system removes solvent in a GC-like manner using a retention gap and an on-column capillary GC syringe. The analyte is delivered to the analytical column in a solvent-free plug of supercritical fluid mobile phase. 相似文献
998.
G. Yu. Ishmuratov M. P. Yakovleva R. Ya. Kharisov G. I. Kunafina E. V. Gorobets A. V. Kuchin G. A. Tolstikov 《Russian Chemical Bulletin》1997,46(8):1465-1467
A convergent synthesis of octadeca-2E, 13Z-dienyl acetate, a pheromone component ofSynanthedon tipuliformis C., has been developed. The synthesis is based on cross-coupling of 8-iodooct-2E-en-I-ol THP ether with dec-5Z-enyl bromide catalyzed by CuBr.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1529–1531, August, 1997. 相似文献
999.
Single nucleotide polymorphism (SNP) arrays were used to detect chromosomal regions with DNA copy number alterations. Current statistical methods for microarray-based comparative genomic hybridization (array-CGH) analysis generally assume certain relationships among adjacent markers on the same chromosome, and these assumptions may be questionable. For an SNP-array-based CGH study, multiple normal reference SNP arrays were collected. In order to utilize these normal reference SNP arrays, we derived an empirical distribution of signal ratios for each SNP marker. With an assumed threshold value for the overall error rate control and the defined signal ratio ranges for chromosomal amplification and deletion, we proposed a procedure to identify chromosomal alteration regions based on several bootstrapped one-sample t-tests and the false discovery rate control. When we have multiple arrays for different individuals with the same disease, our method can also be used to detect SNP markers for chromosomal alteration regions that are common among these individuals. We applied our method to a published SNP array data set for breast carcinoma cell lines. For an individual with breast cancer, numerous chromosomal alteration regions were identified. Compared to results of previous studies, our method identified more chromosomal alteration regions, with some being implicated in the literature to harbor genes associated with breast cancer. For multiple cancer arrays, our results suggested the existence of common chromosomal alteration regions. However, a high proportion of false positives also indicated that genetic variations among different individuals with breast cancer can be present. 相似文献
1000.
F. M. Bautista J. M. Campelo A. Garcia D. Luna J. M. Marinas A. A. Romero M. R. Urbano 《Reaction Kinetics and Catalysis Letters》1997,62(1):47-54
The vapor-phase catalytic alkylation of phenol with methanol and dimethyl carbonate on a series of differently prepared CrPO4 (Cr/P=1) and CrPO4-AlPO4 (CrAIP) catalysts, has been studied at different temperatures (473–673 K). The reaction is first order in phenol, giving
a mixture of O- and C-alkylated products (C-alkylation taking place preferentially at theortho-position). Moreover, dimethyl carbonate is a better methylating agent than methanol. 相似文献