全文获取类型
收费全文 | 31922篇 |
免费 | 2619篇 |
国内免费 | 4161篇 |
专业分类
化学 | 20855篇 |
晶体学 | 430篇 |
力学 | 2262篇 |
综合类 | 346篇 |
数学 | 4439篇 |
物理学 | 10370篇 |
出版年
2022年 | 526篇 |
2021年 | 607篇 |
2020年 | 735篇 |
2019年 | 770篇 |
2018年 | 842篇 |
2017年 | 862篇 |
2016年 | 1038篇 |
2015年 | 885篇 |
2014年 | 1262篇 |
2013年 | 1581篇 |
2012年 | 1614篇 |
2011年 | 1666篇 |
2010年 | 1552篇 |
2009年 | 1612篇 |
2008年 | 1642篇 |
2007年 | 1525篇 |
2006年 | 1407篇 |
2005年 | 1232篇 |
2004年 | 1136篇 |
2003年 | 963篇 |
2002年 | 1135篇 |
2001年 | 1020篇 |
2000年 | 908篇 |
1999年 | 693篇 |
1998年 | 486篇 |
1997年 | 416篇 |
1996年 | 393篇 |
1995年 | 358篇 |
1994年 | 301篇 |
1993年 | 343篇 |
1992年 | 341篇 |
1991年 | 326篇 |
1990年 | 351篇 |
1989年 | 333篇 |
1987年 | 294篇 |
1985年 | 312篇 |
1984年 | 321篇 |
1983年 | 290篇 |
1982年 | 292篇 |
1979年 | 311篇 |
1978年 | 334篇 |
1977年 | 321篇 |
1976年 | 405篇 |
1975年 | 360篇 |
1974年 | 388篇 |
1973年 | 396篇 |
1972年 | 369篇 |
1971年 | 333篇 |
1970年 | 314篇 |
1969年 | 298篇 |
排序方式: 共有10000条查询结果,搜索用时 15 毫秒
971.
通过熔融扩散法合成了一系列不同含硫量的有序介孔碳(CMK-3)/硫复合材料(C x Sy).使用X射线衍射(XRD)、拉曼光谱(Raman)、比表面积测定仪(BET)、扫描电镜(SEM)、透射电镜(TEM)分析、表征和观察样品.将复合材料组装成钠硫电池,室温下测试电化学性能.循环伏安(CV)曲线结果表明,室温钠硫电池在1.61 V处有一个还原峰,对应于Na2Sx(x=2~5)的形成;在1.82 V和1.95 V分别有一个氧化峰,对应于Na2Sx(x=2~5)的分解.50%(by mass,下同)硫含量(C1S1)电极0.05C(1C=558 mA·g-1)倍率首周放电容量500 mAh·g-1,50周期循环比容量为305.6 mAh·g-1.交流阻抗数据拟合计算其表观活化能为21.83 kJ·mol-1.本研究可为室温钠硫电池多孔电极材料的研究提供一定的指导作用. 相似文献
972.
Sha Zhu Ya Cao Zonghuang Ye Yongmei Yin Xiaoli Zhu 《Analytical and bioanalytical chemistry》2013,405(29):9593-9596
Breast cancer has become one of the most threatening diseases to women throughout the world. Emerging evidence implies that estrogen receptor (ER) and phosphatidylinositol 3-kinase (PI3K) pathways play central roles in both breast cancer progression and response to therapy. In this work, we have probed into ER expression related to the PI3K pathway at the protein level with an electrochemical technique based on the detection of ER proteins in nuclear extracts with an Exonuclease III protection-based strategy. Experimental results show that an increased number of ER proteins can be detected upon PI3K inhibition, demonstrating the reversal effect of the PI3K inhibitor on ER expression. Moreover, treatment with different concentrations of the PI3K inhibitor NVP-BEZ235 can result in a dose-dependent alteration of ER protein levels, implying an intimate link between ER and PI3K pathways. This work may be a great help to understand the mysteries underlying PI3K-related endocrine resistance and to evaluate the effect of therapeutic interventions in the future. 相似文献
973.
974.
Tangbin Zou Hongfu Wu Huawen Li Qing Jia Gang Song 《Journal of separation science》2013,36(20):3457-3462
Mangiferin is the main bioactive component in mango leaves, which possesses anti‐inflammatory, antioxidative, antidiabetic, immunomodulatory, and antitumor activities. In the present study, a microwave‐assisted extraction method was developed for the extraction of mangiferin from mango leaves. Some parameters such as ethanol concentration, liquid‐to‐solid ratio, microwave power, and extraction time were optimized by single‐factor experiments and response surface methodology. The optimal extraction conditions were 45% ethanol, liquid‐to‐solid ratio of 30:1 (mL/g), and extraction time of 123 s under microwave irradiation of 474 W. Under optimal conditions, the yield of mangiferin was 36.10 ± 0.72 mg/g, significantly higher than that of conventional extraction. The results obtained are beneficial for the full utilization of mango leaves and also indicate that microwave‐assisted extraction is a very useful method for extracting mangiferin from plant materials. 相似文献
975.
Qing Lv Qing Zhang Wentao Li Haiyu Li Pi Li Qiang Ma Xianshuang Meng Meiling Qi Hua Bai 《Journal of separation science》2013,36(21-22):3534-3549
This paper presents a method for the simultaneous determination of 48 fragrance allergens in four types of toys (plastic toys, play clays, plush toys, and paper toys) based on GC with ion trap MS/MS. Compared with single‐stage MS, MS/MS is superior in terms of the qualification and quantification of a large range of compounds in complicated matrices. Procedures for extraction and purification were optimized for each toy type. The method proved to be linear over a wide range of concentrations for all analytes with correlation coefficients between 0.9768 and 0.9999. Validation parameters, namely, LODs and LOQs, ranged from 0.005–5.0 and from 0.02–20 mg/kg, respectively. Average recoveries of target compounds (spiked at three concentration levels) were in the range of 79.5–109.1%. Intraday and interday repeatabilities of the proposed method varied from 0.7–10.5% and from 3.1–13.4%, respectively. The proposed method was used to monitor fragrance allergens in commercial toy products. Our findings indicate that this method is an accurate and effective technique for analyzing fragrance allergens in materials composed of complex components. 相似文献
976.
Qing Ye 《Journal of separation science》2013,36(12):2028-2034
In this work, microwave distillation assisted by Fe2O3 magnetic microspheres (FMMS) and headspace single‐drop microextraction were combined, and developed for determination of essential oil compounds in dried Zanthoxylum bungeanum Maxim (ZBM). The FMMS were used as microwave absorption solid medium for dry distillation of dried ZBM. Using the proposed method, isolation, extraction, and concentration of essential oil compounds can be carried out in a single step. The experimental parameters including extraction solvent, solvent volume, microwave power, irradiation time, and the amount of added FMMS, were studied. The optimal analytical conditions were: 2.0 μL decane as the extraction solvent, microwave power of 300 W, irradiation time of 2 min, and the addition of 0.1 g FMMS to ZBM. The method precision was from 4 to 10%. A total of 52 compounds were identified by the proposed method. The conventional steam distillation method was also used for the analysis of essential oil in dried ZBM and only 31 compounds were identified by steam distillation method. It was found that the proposed method is a simple, rapid, reliable, and solvent‐free technique for the determination of volatile compounds in Chinese herbs. 相似文献
977.
QING XiangDong WU HaiLong NIE ChongChong LI Yong YAN XiuFang ZHANG XiHua YIN XiaoLi YU RuQin 《中国科学:化学(英文版)》2013,56(11):1641-1650
This work presents a novel application of second-order calibration based on self-weighted alternating trilinear decomposition(SWATLD)algorithm for analyzing the HPLC-DAD data.The proposed method makes it possible to simultaneously determine teflubenzuron,hexaflumuron,flufenoxuron,chlorfluazuron,diflubenzuron and benzoylurea in different fruit samples,i.e.pear,apple and banana,in the selected time region of chromatogram.The concentration,elution time and spectral information of these benzoylurea insecticides are selectively extracted from complex matrices even in the presence of unknown interferences.The root-mean-square error of prediction(RMSEP)and figures of merit,including sensitivity(SEN),selectivity(SEL)and limit of detection(LOD)are employed to access the performance of the method.The LODs obtained for these insecticides are within the range 0.017–0.26 ppm in pears,0.039–0.33 ppm in apples,0.041–0.44 ppm in bananas,respectively.Such a chemometrics-based protocol holds great potential to be extended as a promising alternative for more practical applications in food safety and quality monitoring. 相似文献
978.
Dr. Shengliang Hu Ruixue Tian Lingling Wu Qing Zhao Prof. Jinlong Yang Prof. Jun Liu Shirui Cao 《化学:亚洲杂志》2013,8(5):1035-1041
Carbon quantum dots (CQDs) were synthesized by heating various carbon sources in HNO3 solution at reflux, and the effects of HNO3 concentration on the size of the CQDs were investigated. Furthermore, the oxygen‐containing surface groups of as‐prepared CQDs were selectively reduced by NaBH4, leading to new surface states. The experimental results show that the sizes of CQDs can be tuned by HNO3 concentration and then influence their photoluminescent behaviors; the photoluminescent properties are related to both the size and surface state of the CQDs, but the photocatalytic activities are determined by surface states alone. The different oxygen‐containing groups on the surface of the CQDs can induce different degrees of the band bending upward, which determine the separation and combination of the electron–hole pairs. The high upward band bending, which is induced by C?O and COOH groups, facilitates separation of the electron–hole pairs and then enhances high photocatalytic activity. In contrast, the low upward band bending induced by C? OH groups hardly prevents the electron–hole pairs from surface recombination and then exhibits strong photoluminescence. Therefore, both the photocatalytic activities and optical properties of CQDs can be tuned by their surface states. 相似文献
979.
Yu‐Long Wang Meng Feng Xian Tao Qing‐Yun Tang Ying‐Zhong Shen 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(1):25-28
The lanthanum(III) complexes tris(3,5‐diphenylpyrazolato‐κ2N,N′)tris(tetrahydrofuran‐κO)lanthanum(III) tetrahydrofuran monosolvate, [La(C15H11N2)3(C4H8O)3]·C4H8O, (I), and tris(3,5‐diphenyl‐1,2,4‐triazolato‐κ2N1,N2)tris(tetrahydrofuran‐κO)lanthanum(III), [La(C14H10N3)3(C4H8O)3], (II), both contain LaIII atoms coordinated by three heterocyclic ligands and three tetrahydrofuran ligands, but their coordination geometries differ. Complex (I) has a mer‐distorted octahedral geometry, while complex (II) has a fac‐distorted configuration. The difference in the coordination geometries and the existence of asymmetric La—N bonding in the two complexes is associated with intramolecular C—H...N/O interactions between the ligands. 相似文献
980.