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   11792篇
  免费   2701篇
  国内免费   1121篇
化学   7746篇
晶体学   184篇
力学   1287篇
综合类   119篇
数学   452篇
物理学   5826篇
  2024年   33篇
  2023年   83篇
  2022年   343篇
  2021年   363篇
  2020年   487篇
  2019年   471篇
  2018年   496篇
  2017年   545篇
  2016年   644篇
  2015年   592篇
  2014年   730篇
  2013年   1190篇
  2012年   836篇
  2011年   775篇
  2010年   667篇
  2009年   655篇
  2008年   600篇
  2007年   639篇
  2006年   636篇
  2005年   550篇
  2004年   514篇
  2003年   433篇
  2002年   449篇
  2001年   381篇
  2000年   376篇
  1999年   318篇
  1998年   267篇
  1997年   252篇
  1996年   231篇
  1995年   190篇
  1994年   189篇
  1993年   136篇
  1992年   110篇
  1991年   71篇
  1990年   51篇
  1989年   59篇
  1988年   64篇
  1987年   40篇
  1986年   35篇
  1985年   16篇
  1984年   19篇
  1983年   5篇
  1982年   15篇
  1981年   19篇
  1980年   4篇
  1979年   9篇
  1978年   6篇
  1977年   4篇
  1974年   3篇
  1957年   2篇
排序方式: 共有10000条查询结果,搜索用时 218 毫秒
991.
介绍了目前可用于AlGaN半导体异质外延膜中Al组分含量测定的多种测试技术,包括高分辨X射线衍射技术、光致发光法、紫外-可见光透射光谱法、电子探针法、卢瑟福背散射法等,并对各种测试技术的原理和优缺点进行了概述。  相似文献   
992.
对畜禽肉中四环素类残留的检测方法进行改进,选用Na2EDTA-McIlvaine缓冲溶液作为提取液进行超声提取,经C18固相萃取小柱净化,脱溶剂后用流动相三氟乙酸-乙腈溶解,使用高效液相色谱-PDA检测器分段采集355 nm及270 nm波长下的色谱信息,对前处理方法及色谱条件进行优化。四环素、土霉素在0.01~1μg/g范围内,金霉素、多西环素在0.02~2μg/g范围内回收率为60%~85%,相对标准偏差小于5%,可以满足国家残留限量0.1~0.6μg/g的检测要求。  相似文献   
993.
This paper reports on the preparation and characterization of sulfonated poly(ether ether ketone) (sPEEK)-based mixed matrix membranes. The inorganic matrix consisted of silica: Aerosil®380, tetraethoxysilane (TEOS) or a combination of both to obtain an interconnected silica network. The behavior of these membranes in ethanol–water systems was studied for application in a direct ethanol fuel cell (DEFC). Uptake measurements showed that the converted TEOS content had a strong influence on the hydrophilicity of the membranes. Proton conductivity was strongly related to the water content in the membrane, but the proton diffusion coefficients of membranes with various Aerosil®380–TEOS combinations were similar. Dynamic measurements in liquid–liquid (L–L) and liquid–gas (L–G) systems were performed to study the ethanol transport through the membrane. No reduction in ethanol permeability was obtained in the L–L system, but a remarkable reduction was obtained in the L–G system when 2 M ethanol was applied. The reinforcing characteristic of the combined Aerosil®380–TEOS-system were best observed at 40 °C with 4 M ethanol. The fuel cell performance prediction based on the selectivity of proton diffusion coefficient to ethanol permeability coefficient showed for nearly all composite membranes an improvement with respect to the polymeric reference. The presence of an inorganic phase led to relatively constant proton diffusion coefficients and lower ethanol permeability coefficients in comparison with the polymeric reference.  相似文献   
994.
以大黄酸为原料,γ-氨丙基三乙氧基硅烷(KH-550)为偶联剂,简便制备了一种新型羧基键合硅胶固定相(RBSP),并用红外光谱、热重分析及元素分析对其结构进行表征.考察了流动相中甲醇含量对键合固定相色谱性能的影响,并以含酸性、中性和碱性化合物的混合物为溶质,评价了RBSP的色谱性能.以甲醇-水为流动相,用C18柱作参比,研究了该键合硅胶作为HPLC固定相对两种大豆异黄酮化合物和几种生物碱基的分离,并对其色谱分离机理进行了初步探讨.实验结果表明,该固定相(RBSP)具有较好的反相色谱性能,同时由于键合相中含有酚羟基及酰胺基团,能为多种溶质提供作用位点,对极性化合物的分离具有明显优势,且分离速度快,可有效用于极性化合物的分离分析.  相似文献   
995.
The acetyl esterified calixarene (CA) derivatives were prepared from calix[4]resorcinarene (CRA), and ptert‐butylcalixarene (BCA[n], n = 4, 6, 8), respectively. Using these CA derivatives as curing agents, the thermal curing reactions of two multifunctional epoxy resins (jER 828, 186 g/equiv., and ESCN, 193.7 g/equiv.) were investigated. The temperatures of glass transition (Tg) and decomposition (T) were measured by DSC and TGA, respectively. Based on the yields, Tgs, and Tds of the thermal cured jER 828 epoxy resin with CRA‐E100, the curing conditions were optimized to be tetrabutylphosphonium bromide (TBPB) as catalyst in NMP at 160 °C for 15 h. Under this curing condition, the cured materials of jER 828 or ESCN using various CA derivatives as curing agents were prepared. Except for BCA4 derivatives, the yields of thermal curing reaction were higher than 90%. Tgs and Ts of the resultant cured materials were in the range of 113–248 °C and 363–404 °C, respectively. These results mean that the cured epoxy resins with excellent Tgs were successfully formed by using CA derivatives as curing agents. It was also found that the Tgs of cured epoxy resins were strongly affected by the degree of esterification of CA derivatives. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 1931–1942, 2010  相似文献   
996.
Functional nucleic acids, such as aptamers and allosteric ribozymes, can sense their ligands specifically, thereby undergoing structural alterations that can be converted into a detectable signal. The direct coupling of molecular recognition to signal generation enables the production of versatile reporters that can be applied as molecular probes for various purposes, including high‐throughput screening. Here we describe an unprecedented type of a nucleic acid‐based sensor system and show that it is amenable to high‐throughput screening (HTS) applications. The approach detects the displacement of an aptamer from its bound protein partner by means of luminescent oxygen channeling. In a proof‐of‐principle study we demonstrate that the format is feasible for efficient identification of small drug‐like molecules that bind to a protein target, in this case to the Sec7 domain of cytohesin. We extended the approach to a new cytohesin‐specific single chain DNA aptamer, C10.41, which exhibits a similar binding behavior to cytohesins but has the advantage of being more stable and easier to synthesize and to modify than the RNA‐aptamer M69. The results obtained with both aptamers indicate the general suitability of the aptamer‐displacement assay based on luminescent oxygen channelling (ADLOC) for HTS. We also analyzed the potential for false positive hits and identified from a library of 18 000 drug‐like small molecules two compounds as strong singlet‐oxygen quenchers. With full automation and the use of commercially available plate readers, we estimate that the ADLOC‐based assay described here could be used to screen at least 100 000 compounds per day.  相似文献   
997.
Ping Tong  Lan Zhang  Yu He  Jintian Cheng 《Talanta》2010,82(4):1101-1106
In this paper, a rapid and effective method based on capillary zone electrophoresis (CZE) coupled with electrospray ionization mass spectrometry (ESI-MS) was established for the trace analysis of microcystin (MC) isomers in crude algae sample. The experimental conditions including the composition, acidity and concentration of buffer, separation voltage, injection time, and MS detection parameters were investigated in detail. A capillary separation system was as follows: a uncoated fused-silica capillary tube (50 μm i.d. × 90 cm), 40 mmol L−1 ammonium acetate solution (pH 9.86) as running buffer, 25 kV as separation voltage, 20 kV × 3 s water first and 20 kV × 20 s for sample injection. Mass analysis was performed in ESI source, with sheath gas temperature 150 °C, sheath gas pressure 10 psi, and sheath gas flow 6 L min−1. And sheath liquid was 7.5 mmol L−1 acetic acid in 50% isopropanol-water (3 μL min−1). Protonation and ammonium adduct molecular ions m/z 506.9 (MC-LR) and 532.0 (MC-YR) were used for the quantification of MCs. Under these conditions, two MCs were baseline separated within 9 min, the calibration curves were obtained in the range of 0.11-10.0 μg mL−1 and 0.16-10.5 μg mL−1 for MC-LR and MC-YR, respectively. Meanwhile, limits of detection were 0.05 and 0.08 μg mL−1 for MC-LR and MC-YR, respectively. The recoveries for the two MCs were in the range of 95.8-108%. The developed approach had been successfully applied to the analysis of MCs in crude algae samples.  相似文献   
998.
The thermoelectric properties of Pb0.5Sn0.5Te doped with In at 1.0, 2.0, and 3.0×1019/cm3 and sintered at a high pressure and high temperature (HPHT) of 4.0 GPa and 800 or 900 °C, respectively, have been studied. All samples show p-type semiconducting behavior with positive thermopower. We find that HPHT sintering of conventionally synthesized materials improves their thermoelectric properties. The highest power factor is obtained for In doping of 2.0×1019/cm3 with 13.5 μW/cm K2 at 230 °C. The corresponding figure of merit is 1.43×10−3/K. This represents a twofold improvement in thermoelectric figure of merit, compared to the conventionally sintered materials reported in the literature. When exposed to 400 °C for 10 days, samples sintered at 900 °C exhibit more stable thermoelectric properties, while the properties of those sintered at 800 °C deteriorated. These results demonstrate that HPHT sintering is a viable and controllable way of tuning the thermoelectric properties of PbTe-based materials.  相似文献   
999.
Boron reacted with ball milled boron oxide under pressures between 1 and 5 GPa and at temperatures between 1300 and 1700 °C to afford boron suboxide (B6O). Icosahedral B6O grains with diameters ranging from 100 nm to 1.3 μm were prepared. The factors that affect the synthesis of B6O are investigated. The best sample with crystal size up to 1.3 μm is obtained at 2 GPa and 1400 °C for 6 h. The indentation experiment gave an average Vickers hardness of 32.3 GPa for bulk B6O sample, which is consistent with previous reports. Bulk B6O sample exhibits oxidation resistance in air up to 1000 °C and mild oxidation in the temperatures of 1000-1200 °C, which is more oxidation resistant than diamond. It is possible that B6O could be used as a substitute for diamond in industry because of its relatively mild synthesis conditions, high thermal stability and high hardness.  相似文献   
1000.
Serum is a typical sample for non-invasive studies in clinical research. Its proteome characterization is challenging, since requires extensive protein depletion. Methods used nowadays for removal of high-abundance proteins are expensive or show quite often a low loading capacity, which has strong repercussions on the number of samples and replicates per analysis.In order to deplete immunoglobulins (Igs) and albumin (HSA) from 1 mL serum samples, we have developed a protocol based on a combination of thiophilic chromatography, not previously used in clinical proteomics, and a HSA-specific resin. Ig/HSA-depleted samples, immunoglobulinome and albuminone were analyzed by 2-DE. Thiophilic chromatography, coupled with HSA-depletion, allows a good 2-DE resolution as well as the visualization of new spots. Moreover, it yields enough protein to evaluate technical variability and facilitate subsequent protein identification. To validate the protocol, we carried out a preliminary comparative study between triplicate Igs/HSA-depleted serum samples from healthy control individuals and recently diagnosed/untreated rheumatoid arthritis (RA) patients. RA patients showed several acute phase proteins, as well as additional serum proteins, differentially and significantly regulated.Therefore, thiophilic chromatography can be used as an efficient and economical method in 2-DE to deplete immunoglobulins from large human serum samples before a more extensive fractioning.  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