首页 | 官方网站   微博 | 高级检索  
文章检索
  按 检索   检索词:      
出版年份:   被引次数:   他引次数: 提示:输入*表示无穷大
  收费全文   19946篇
  免费   3771篇
  国内免费   2456篇
数理化   26173篇
  2024年   40篇
  2023年   381篇
  2022年   452篇
  2021年   673篇
  2020年   767篇
  2019年   827篇
  2018年   687篇
  2017年   627篇
  2016年   1009篇
  2015年   1049篇
  2014年   1133篇
  2013年   1483篇
  2012年   1777篇
  2011年   1879篇
  2010年   1330篇
  2009年   1319篇
  2008年   1359篇
  2007年   1137篇
  2006年   1035篇
  2005年   912篇
  2004年   772篇
  2003年   677篇
  2002年   761篇
  2001年   626篇
  2000年   478篇
  1999年   421篇
  1998年   394篇
  1997年   319篇
  1996年   263篇
  1995年   291篇
  1994年   248篇
  1993年   189篇
  1992年   155篇
  1991年   140篇
  1990年   123篇
  1989年   88篇
  1988年   63篇
  1987年   49篇
  1986年   45篇
  1985年   29篇
  1984年   31篇
  1983年   30篇
  1982年   16篇
  1981年   18篇
  1980年   16篇
  1979年   9篇
  1978年   8篇
  1975年   5篇
  1974年   7篇
  1957年   5篇
排序方式: 共有10000条查询结果,搜索用时 31 毫秒
991.
Ethynylferrocene was prepared in satisfactory yield by reaction of formylferrocene with triphenylphosphine and carbon tetrachloride followed by dehydrohalogenation in presence of n-butyllithum. The reaction condition is mild and the reaction time is much shorter. The method is convenient and economical.  相似文献   
992.
We report on a facile immunoassay for porcine circovirus type 2 (PCV2) based on surface enhanced Raman scattering (SERS) using multi-branched gold nanoparticles (mb-AuNPs) as substrates. The mb-AuNPs in the immunosensor act as Raman reporters and were prepared via Tris base-induced reduction and subsequent reaction with p-mercaptobenzoic acid (pMBA). They possess good stability and high SERS activity. Subsequently, the modified mb-AuNPs were covalently conjugated to the monoclonal antibody (McAb) against the PCV2 cap protein to form SERS immuno nanoprobes. These were captured in a microtiterplate via a immunoreaction in the presence of target antigens. The effects of antibody concentration, reaction time and temperature on the sensitivity of the immunoassay were investigated. Under optimized assay conditions, the Raman signal intensity at 1,076 cm?1 increases logarithmically with the concentrations of PCV2 in the concentration ranging from 8?×?102 to 8?×?106 copies per mL. The limit of detection is 8?×?102 copies per mL. Compared to conventional detecting methods such as those based on PCR, the method presented here is rapid, facile and very sensitive.
Figure
A simple and novel approach to detect porcine circovirus type 2 using surface enhanced Raman scattering (SERS) of multi-branched gold nanoparticles is demonstrated, it has a higher sensitivity than polymerase chain reaction and ELISA.  相似文献   
993.
We describe a molecularly imprinted polymer (MIP) for the solid-phase extraction of the skin protectant allantoin. The MIP was deposited on the surface of monodisperse silica microspheres possessing acroyl groups on the surface (MH-SiO2). The resulting MIP microspheres (MH-SiO2@MIP) showed a 3.4-fold higher adsorption capacity and a 1.9-fold better selectivity for allantoin than the respective non-imprinted polymer (MH-SiO2@NIP). The monolayer adsorption capacities of the MH-SiO2@MIP and the MH-SiO2@NIP were calculated with the help of the Langmuir model and found to be 6.8 and 1.9 mg?g?1, respectively. Adsorption kinetics fit a pseudo-second order rate mechanism, with an initial adsorption rate of 1.44 for the MH-SiO2@MIP, and of 0.07 mg?g?1?min?1 for the MH-SiO2@NIP. The material can be regenerated, and its adsorption capacity for allantoin remains stable for at least five regeneration cycles. It was successfully used as a sorbent for the selective solid-phase extraction of allantoin from Rhizoma dioscoreae.
Figure
A molecularly imprinted polymer for the selective separation of allantoin was developed. It was successfully used as a sorbent for the selective solid-phase extraction of allantoin from Rhizoma dioscoreae.  相似文献   
994.
A thin film of poly(eriochrome black T) was deposited on the surface of glassy carbon electrode by cyclic voltammetry, and this system is shown to enable the sensitive determination of adenine (A) and guanine (G). Scanning electron microscopy, Fourier transform infrared spectroscopy and electrochemical impedance spectroscopy were carried out to characterize the film which exhibits excellent electrocatalytic activity toward the oxidation of A and G in 0.1 M phosphate buffer solution (pH 4.0). Square wave voltammetry reveals an oxidation peak at 1084 mV whose current is linearly related to the concentration of A in the range from 0.05 to 1.00 μM. The oxidation peak for G occurs at 788 mV, and its current is linearly related to the concentration of G in the range from 0.025 to 1.00 μM. The detection limits are 0.017 μM for A and 0.008 μM for G (at S/N?=?3), respectively. The modified electrode displays good reproducibility and selectivity for the determination of A and G. The sensor was applied to quantify A and G in fish sperm DNA with satisfactory results.
Figure
Square wave voltammograms of bare GCE (a), PEBT/GCE (b) in the presence of 1.00 μM adenine (A) and 1.00 μM guanine (G).  相似文献   
995.
Li-Hua Du  Xi-Ping Luo 《合成通讯》2013,43(19):2880-2886
A green, efficient method for the synthesis of various 2-aryl-benzimidazoles in the presence of hypervalent iodine as the oxidant at room temperature under solvent-free conditions is reported. The salient features of this method include mild conditions, short reaction times (3–5 min), excellent yields, and simple procedure.  相似文献   
996.
A novel, convenient, efficient, three‐step, one‐pot synthesis of 2‐oxazolidinones from phenyl 2‐hydroxyalkyl selenides was developed. Using this methodology, 2‐oxazolidinones are obtained in good yields (76–85%) by reaction of phenyl 2‐hydroxyalkyl selenides with benzoyl isocyanate and subsequent oxidation/cyclization, followed by hydrolysis with hydrochloric acid solution.  相似文献   
997.
J-AT nucleoside-based organogelators 1a and 1b were designed and synthesized. They were endowed with unparalleled superiority to natural nucleobase analogues 26 to gelate aromatic solvents due to their excellent self-assembly properties. The J-AT nucleoside-based organogelators showed a specific self-complementary base pair recognition characteristic. The gel stabilities of 1a and 1b were drastically influenced by adenine analogue 2, hardly affected by thymine analogue 3, uracil analogue 4, cytosine analogue 5, and mildly interrupted by guanine analogue 6.  相似文献   
998.
The self‐assembly of 4 ‐ MTPP [ 4 ‐ MTPP = 2‐(methylthio)‐4‐(pyridin‐4‐yl)pyrimidine] with Cu(NO3)2 and AgNO3 was structurally investigated. For Cu(NO3)2, a discrete mononuclear CuII coordination compound, [Cu( 4 ‐ MTPP )2(NO3)2] ( 1 ), resulted that is exclusively based on Cu–N coordination. For AgNO3, a unique one‐dimensional double‐chain structure ( 2 ) was obtained with the Ag–N distances varying from 2.181(9) to 2.223(9) Å, and the average Ag–S distance being 2.98 Å. Compared to zero‐dimensional 1 , the extension to one‐dimensional 2 is considered to result from the specific affinity between Ag+ and the ligand 4 ‐ MTPP that is attributed to the strong coordinating tendency of silver for aromatic nitrogen and thioether sulfur atoms.  相似文献   
999.
The cage‐like complex, Ag4L4(NO3)4 ( 1 ) [L = 1, 4‐bis(pyridine‐2‐ylmethoxy)benzene] was synthesized by the reaction of the flexible bidentate ligand and silver nitrate. It was characterized by elemental analysis, IR spectroscopy, TG, and single‐crystal X‐ray analysis. Complex 1 is reported as the first cage‐like cluster constructed by four nitrate anions bridging two [2+2] macrocycles. A blue luminescent emission and luminescent enhancement effect are observed in complex 1 .  相似文献   
1000.
Two new nickel(II) complexes, [Ni(4, 4′‐bpy)(H2O)4]n · n(cpp) · 0.5nH2O ( 1 ) and [Ni(cpp)(4, 4′‐bpy)(H2O)2]n ( 2 ) [4, 4′‐bpy = 4, 4′‐bipyridine, H2cpp = 3‐(4‐carboxyphenyl)propionic acid] were synthesized and characterized by single‐crystal X‐ray diffraction, elemental analysis, IR spectroscopy, and thermal analysis. In complex 1 , NiII ions are bridged by 4, 4′‐bpy into 1D chains, and cpp ligands are not involved in the coordination, whereas in complex 2 , cpp ligands adopt a bis(monodentate) mode and link NiII ions into 2D (4, 4) grids with the help of 4, 4′‐bpy ligands. Triple interpenetration occurs, which results in the formation of a complicated 3D network. The difference in the structures of the two complexes can be attributed to the different reaction temperatures and bases.  相似文献   
[首页] « 上一页 [95] [96] [97] [98] [99] 100 下一页 » 末  页»
设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司    京ICP备09084417号-23

京公网安备 11010802026262号