首页 | 本学科首页   官方微博 | 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   9164篇
  免费   865篇
  国内免费   783篇
化学   3408篇
晶体学   69篇
力学   2835篇
综合类   95篇
数学   2465篇
物理学   1940篇
  2024年   14篇
  2023年   99篇
  2022年   154篇
  2021年   172篇
  2020年   227篇
  2019年   200篇
  2018年   209篇
  2017年   285篇
  2016年   307篇
  2015年   258篇
  2014年   392篇
  2013年   648篇
  2012年   489篇
  2011年   543篇
  2010年   432篇
  2009年   533篇
  2008年   487篇
  2007年   509篇
  2006年   445篇
  2005年   508篇
  2004年   417篇
  2003年   403篇
  2002年   360篇
  2001年   284篇
  2000年   264篇
  1999年   253篇
  1998年   220篇
  1997年   226篇
  1996年   154篇
  1995年   183篇
  1994年   145篇
  1993年   125篇
  1992年   94篇
  1991年   108篇
  1990年   80篇
  1989年   60篇
  1988年   85篇
  1987年   74篇
  1986年   78篇
  1985年   56篇
  1984年   43篇
  1983年   18篇
  1982年   57篇
  1981年   21篇
  1980年   13篇
  1979年   21篇
  1978年   17篇
  1977年   10篇
  1976年   8篇
  1957年   4篇
排序方式: 共有10000条查询结果,搜索用时 15 毫秒
131.
This work describes an electroanalytical investigation of dopamine using cyclic voltammetry (CV) and the graphite–polyurethane composite electrode (GPU). In CV studies, well-defined redox peaks characterize the oxidation process at the GPU electrode, which is indicative of electrocatalytic effects associated with active sites on the GPU electrode surface. A new analytical methodology was developed using the GPU electrode and square wave voltammetry (SWV) in BR buffer solution (0.1 mol L–1; pH 7.4). Analytical curves were constructed under optimized conditions (f=60s–1, Ea=50 mV, EI=2 mV) and detection and quantification limits of 6.4×10–8 mol L–1 (12.1 g L–1) and 5.2×10–6 mol L–1 (0.9 mg L–1), respectively, were achieved. The precision of the method was checked by performing ten successive measurements for a 9.9×10–6 mol L–1 dopamine solution. For intra-assay and inter-assay precisions, the relative standard deviations were 1.9 and 2.3%, respectively. In order to evaluate the developed methodology, the determination of dopamine was performed with good sensitivity and selectivity, without the interference of ascorbic acid in synthetic cerebrospinal fluid, which indicates that the new methodology enables reliable analysis of dopamine.  相似文献   
132.
Supercritical fluid chromatography using flameless sulfur chemiluminescence detection has been investigated for the analysis of sulfur compounds in petroleum products. The chromatography and detection system was easy to implement and exhibited good precision, linearity, selectivity, and sensitivity. A minimum detectable limit of 0.3 pg sulfur/s was obtained, and response to sulfur in different sulfur species was nearly equimolar.  相似文献   
133.
陈祖兴  李焰 《应用化学》1997,14(4):111-113
混合高序铜法立体选择性合成(±)┐EpilitsenolideC2陈祖兴李焰*黄精美黄锦霞徐章煌(湖北大学化学系武汉430062)关键词烷叉基二氢羟基甲基(3H)呋喃酮,混合高序铜,立体选择性反应1996-08-28收稿,1997-05-06修回湖北...  相似文献   
134.
Diorganogallium Fluorides. The Crystal Structure of the Mixed Crystal [B(CH2Ph)3]0.92[Ga(CH2Ph)3]0.08 · NCMe The reaction of GaR3 with BF3 · OEt2 in diethylether leads to the diorganogallium fluorides R2GaF [R = i-Pr ( 1 ), CH2Ph ( 2 ), Mes ( 3 )]. Compound 1 is also available by the reaction of i-Pr2GaBr ( 6 ) with KF at ?20°C in acetonitrile. The by-product B(CH2Ph)3, formed together with 2 during the first reaction, crystallizes with ca. 8% Ga(CH2Ph)3 in acetonitrile as [B(CH2Ph)3]0.92[Ga(CH2Ph)3]0.08 · NCMe ( 4 ) in the space group P21/n with a = 1050.32(7) pm, b = 1159.5(2) pm, c = 1591.6(1) pm and β = 96.931(6)°.  相似文献   
135.
Supercritical fluid extraction of flumetralin in tobacco   总被引:2,自引:0,他引:2  
Summary This work evaluates the level of Flumetralin residues in real tobacco samples. Conventional extraction methods were compared with SFE methods in both static and dynamic modes using CO2 and CO2 with modifier. Additionally, in the dynamic SFE mode, different collection approaches, such as collection at room temperature without solvent, collection at room temperature in the presence of solvent (hexane) and collection in an ice bath, without solvent, were studied. SFE showed itself to be a promising extraction technique for pesticide residues in tobacco samples.  相似文献   
136.
汪杰  涂永善  杨朝合 《催化学报》2003,24(6):452-456
 采用阳离子表面活性剂十六烷基三甲基溴化铵为模板剂,以正硅酸乙酯为硅源,以硫酸铝为铝源,水热合成了以催化油浆窄馏分为添加剂的高比表面积Al-MCM-41介孔分子筛,并利用XRD,HREM,TG-DTA及N2吸附-脱附等测试手段对合成样品进行了表征.合成的Al-MCM-41分子筛的比表面积和孔体积分别达到1295m2/g和1.5cm3/g,其平均孔径为4.3nm.重点研究了Al-MCM-41分子筛结晶度、晶胞参数、比表面积、孔体积及平均孔径等结构性质随催化油浆窄馏分添加量及其组成的变化规律,并从合成机理上进行了解释.  相似文献   
137.
In order to increase the biocompatibility and bioactivity of chitosan, hydroxyapatite had been in situ combined into chitosan scaffolds. The bioactivity of the composite scaffolds was studied by examining the apatite formed on the scaffolds by incubating in simulated body fluid and the activity of preosteoblasts cultured on them. The apatite layer was assessed using scanning electronic microscope (SEM), X-ray diffraction (XRD), Fourier-Transformed Infrared spectroscopy (FTIR) and weight measurement. Composite analysis showed that after incubation in simulated body fluid on both of the scaffolds carbonate hydroxyapatite was formed. With increasing nano-hydroxyapatite content in the composite, the quantity of the apatite formed on the scaffolds increased. Compared with pure chitosan, the composite with nano-hydroxyapatite could form apatite more readily during the biomimetic process, which suggests that the composite possessed better mineralization activity. Furthermore, preosteoblast cells cultured on the apatite-coated scaffolds showed different behavior. On the apatite-coated composite scaffolds cells presented better proliferation than on apatite-coated chitosan scaffolds. In addition, alkaline phosphatase activities of cells cultured on the scaffolds in conditioned medium were assessed. The cells on composite scaffolds showed a higher alkaline phosphatase activity which suggested a higher differentiation level. The results indicated that the addition of nano-hydroxyapatite improved the bioactivity of chitosan/nano-hydroxyapatite composite scaffolds. On the other hand, that is to say composition of substrates could affect the apatite formation on them, and pre-loaded hydroxyapatite can enhance the apatite-coating. It will also be significant in preparation of apatite-coating polymer scaffolds for bone tissue engineering.  相似文献   
138.
Zr0.5Ti0.5O2(ZT) and Zr0.25Ti0.25Al0.5O2(ZTA) mixed oxides were prepared by co-precipitation method and characterized by low temperature adsorption-desorption, XRD and NH3-TPD. The activity of Pt/Zr0.5Ti0.5O2 and Pt/ Zr0.5Ti0.5Al0.5O2 catalysts was evaluated using the simulated gases. The results show that ZTA samples exhibit higher specific surface area, larger pore volume and proper surface acidic amount and acidity in comparison with ZT. The results of the catalytic test indicate that Pt/ZT and Pt/ZTA catalysts exhibit excellent low-temperature catalytic activity and lower light-off temperatures of hydrocarbon, carbon monoxide and nitrogen oxides, especially better conversion for nitrogen oxides (NOx). The addition of Al2O3 into ZT enhanced the anti-aging property of Pt/ ZTA catalysts due to the excellent textural, structural, surface acidity and thermal stability.  相似文献   
139.
Organosols of NiS, PdS, and MnS in N,N-dimethylformamide were prepared by reaction of the metal acetate with H2S. Organosols of mixed-metal sulfides (Zn x Cd1–x S, Hg x Cd1–x S, Hg x Cu1–x S, Cd x Mn1–x S, Hg x Mn1–x S, Hg x Cd1–x S, and Mn x Zn1–x S) were similarly obtained by reaction of mixtures of the metal salts with H2S. The organosol of Zn0.5Cd0.5S contained particle with two particle size distributions centered at 6.5 nm and 29 nm, as revealed by Ar laser-scattering analysis. The metal sulfides are recovered by addition of Et2O to the organosols. Zn x Cd1–x S thus obtained shows magnetic susceptibility in the range 0.5×10–6–2.3×10–6 emug–1 depending on thex value. Addition of polymers to the organosols affords semiconducting films of metal sulfide-polymer composites.  相似文献   
140.
Complexes have been prepared by treatment ofn-decylammonium beidellite with mixtures ofn-decanol andn-tetradecanol with different concentrations. Measurements of the basal spacings of the obtained complexes have been performed in a wide range of temperatures. Three different bilayer phases have been established between (20 and 70°C: the i(C10) phases (=bilayers ofn-decyl chains); the i(C10/C14) phases (=mixed bilayers ofn-decyl andn-tetradecyl chains in molar ratio approximately 1:1) and the i(C14) phases (=bilayer ofn-tetradecy 1 chains with then-decylammonium ions included). In all bilayer phases the chains stand perpendicular to the silicate interfaces. In definite concentration ranges two of the phases coexist, i.e., miscibility gaps occur, which disappear at temperatures higher than the temperature of the i/ transition. The miscibility gaps are reversible with temperature. The composition of the intercalated bilayers has been studied by HPLC of the excess alkanol mixture separated from the beidellite complexes after the equilibrium has been reached. There is preferential adsorption of one of two alkanols from the mixture, which is in agreement with the observed miscibility gaps. The space filling problem as well as the structure of the three bilayer phases observed have been discussed.  相似文献   
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