全文获取类型
收费全文 | 48885篇 |
免费 | 6553篇 |
国内免费 | 4797篇 |
专业分类
化学 | 13969篇 |
晶体学 | 1043篇 |
力学 | 11622篇 |
综合类 | 728篇 |
数学 | 16711篇 |
物理学 | 16162篇 |
出版年
2024年 | 56篇 |
2023年 | 488篇 |
2022年 | 799篇 |
2021年 | 1098篇 |
2020年 | 1468篇 |
2019年 | 1237篇 |
2018年 | 1274篇 |
2017年 | 1717篇 |
2016年 | 2021篇 |
2015年 | 1561篇 |
2014年 | 2403篇 |
2013年 | 3712篇 |
2012年 | 2947篇 |
2011年 | 3336篇 |
2010年 | 2811篇 |
2009年 | 3109篇 |
2008年 | 3040篇 |
2007年 | 3099篇 |
2006年 | 2875篇 |
2005年 | 2634篇 |
2004年 | 2329篇 |
2003年 | 2118篇 |
2002年 | 1874篇 |
2001年 | 1544篇 |
2000年 | 1403篇 |
1999年 | 1213篇 |
1998年 | 1121篇 |
1997年 | 944篇 |
1996年 | 822篇 |
1995年 | 776篇 |
1994年 | 718篇 |
1993年 | 580篇 |
1992年 | 576篇 |
1991年 | 442篇 |
1990年 | 357篇 |
1989年 | 267篇 |
1988年 | 251篇 |
1987年 | 179篇 |
1986年 | 133篇 |
1985年 | 172篇 |
1984年 | 164篇 |
1983年 | 68篇 |
1982年 | 105篇 |
1981年 | 78篇 |
1980年 | 42篇 |
1979年 | 50篇 |
1978年 | 49篇 |
1977年 | 57篇 |
1976年 | 30篇 |
1957年 | 25篇 |
排序方式: 共有10000条查询结果,搜索用时 15 毫秒
51.
Corinne Rondeau-Mouro Mireille Cambert Laurent Blondel Yves Diascorn Léo Mbaya Nor Nadiah Binti Ahmad Nazari Sarah Helary Tiphaine Lucas 《Magnetic resonance in chemistry : MRC》2022,60(7):678-691
A temperature control unit was implemented to vary the temperature of samples studied on a commercial Mobile Universal Surface Explorer nuclear magnetic resonance (MOUSE-NMR) apparatus. The device was miniaturized to fit the maximum MOUSE sampling depth (25 mm). It was constituted by a sample holder sandwiched between two heat exchangers placed below and above the sample. Air was chosen as the fluid to control the temperature at the bottom of the sample, at the interface between the NMR probe and the sample holder, in order to gain space. The upper surface of the sample was regulated by the circulation of water inside a second heat exchanger placed above the sample holder. The feasibility of using such a device was demonstrated first on pure water and then on several samples of bread dough with different water contents. For this, T1 relaxation times were measured at various temperatures and depths and were then compared with those acquired with a conventional compact closed-magnet spectrometer. Discussion of results was based on biochemical transformations in bread dough (starch gelatinization and gluten heat denaturation). It was demonstrated that, within a certain water level range, and because of the low magnetic field strength of the MOUSE, a linear relationship could be established between T1 relaxation times and the local temperature in the dough sample. 相似文献
52.
53.
移动加热器法(THM)生长碲锌镉晶体时,界面稳定性对晶体生长的质量有很大影响。本文基于多物理场有限元仿真软件Comsol建立了THM生长碲锌镉晶体的数值模拟模型,讨论了Te边界层与组分过冷区之间的关系,对不同生长阶段的物理场、Te边界层与组分过冷区进行仿真研究,最后讨论了微重力对物理场分布的影响,并对比了微重力与正常重力下的生长界面形貌。模拟结果表明,Te边界层与组分过冷区的分布趋势是一致的,在不同生长阶段,流场中次生涡旋的位置会发生移动,从而导致生长界面的形貌随着生长的进行发生变化,同时微重力条件下形成的生长界面形貌最有利于单晶生长。因此,在晶体生长的中前期,对次生涡旋位置的控制和对组分过冷的削弱,是THM生长高质量晶体的有效方案。 相似文献
54.
Mitra Talaee Bahareh Lorestani Majid Ramezani Mehrdad Cheraghi Saeed Jamehbozorgi 《Journal of separation science》2019,42(14):2418-2425
A simple and fast method named microfunnel‐filter‐based emulsification microextraction is introduced for an efficient determination of some organophosphorus pesticides including diazinon, malathion, and chlorpyrifos in the environmental samples including the river, sea, and well water. This method is based upon the dispersion of a low‐toxicity organic solvent (dihexyl ether), as the extractant, in a high volume of an aqueous sample solution (45 mL). It is implemented without a centrifugation step, and using a syringe filter and a micro‐funnel, the phase separation and transfer of the enriched analytes to the gas chromatograph are simply achieved. By filtration of the extractant phase, a suitable sample clean‐up is obtained, and the total extraction time is just a few minutes. The factors influencing the extraction efficiency are optimized, and under the optimal conditions, the proposed method provides a good linearity (in the range of 15–1500 ng/mL (R2 > 0.996). A high enrichment factor is obtained (in the range of 306–342), and the method provides low limits of detection and quantification (in the ranges of 4–8 and 15–25 ng/mL, respectively). 相似文献
55.
Leandro Augusto Gouvêa De Godoi Carla Eloísa Diniz Dos Santos Eugenio Foresti Marcelo Zaiat Márcia Helena Rissato Zamariolli Damianovic 《International journal of environmental analytical chemistry》2019,99(9):809-823
Recent developments in wastewater treatment have led to a renewed interest to obtain elemental sulphur (S°) as a by-product from bioreactors. However, practical studies are limited by the gap of adequate analytical techniques for its determination. This paper provides a statistical study and matrix effect evaluation of an adapted spectrophotometric method for routine S° analyses in aqueous samples, based on a methodology previously described by Hart (1961). Four complex matrices were tested: domestic sewage and effluent samples from three different bioreactors. Tested performance criteria included linearity, matrix effect, limit of detection and quantification and S° recovery. Results were linear (R2 = 0.99994) in the studied range (5 to 100 mg S° L?1) and no matrix effect was observed. The accuracy was based on recovery values that varied from 100% to 106%. The colloidal S° separation and extraction protocol was also considered suitable for aqueous samples, reaching more than 99.0% of S° recovery. 相似文献
56.
Reducing gas contaminants by affordable and effective adsorbents is a major challenge in the 21st century. In the present study, thorium metal organic framework (Th‐MOF) nanostructures are introduced as highly efficient adsorbents. These compounds were manufactured via a novel route resulting from the development of microwave assisted reverse micelle (MARM) and ultrasound assisted reverse micelle (UARM) methods. The products were characterized utilizing XRD, SEM, TGA/DSC, BET, and FT‐IR analyses. Based on the results, the samples synthesized by MARM had uniform size distribution, high thermal stability, and significant surface area. Calculations using DFT/B3LYP indicated that the compounds have a tendency to the polymeric form, which could theoretically confirm the formation of Th‐MOF. Results of analysis of variance (ANOVA) showed that synthesis parameters played a critical role in the manufacturing of products with distinctive properties. Response surface methodology (RSM) predicted the possibility of creating Th‐MOF adsorbents with the surface area of 2579 m2/g, which was a considerable value in comparison with the properties of other adsorbents. Adsorption studies showed that, in the optimum conditions, the Th‐MOF products had high adsorption capacity for CO and CH4. It is believed that the synthesis protocol developed in the present study and the systematic studies conducted on the samples which lead to products with ideal adsorption properties. 相似文献
57.
Yuying Qu Yingchun Li Xiaoli Tan Weixiang Zhai Dr. Guifang Han Dr. Jingli Hou Prof. Guoquan Liu Prof. Yuguang Song Prof. Yangping Liu 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(33):7888-7895
Tetrathiatriarylmethyl (TAM, trityl) radicals have found wide applications as spin probes/labels for EPR spectroscopy and imaging, and as polarizing agents for dynamic nuclear polarization. The high hydrophilicity of TAM radicals is essential for their biomedical applications. However, the synthesis of hydrophilic TAM radicals (e.g., OX063) is extremely challenging and has only been reported in the patent literature, to date. Herein, an efficient synthesis of a highly water-soluble TAM radical bis(8-carboxyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d′]bis([1,3]dithiol-4-yl)-mono-(8-carboxyl-2,2,6,6-tetrakis(2-hydroxyethyl)benzo[1,2-d:4,5-d′]bis([1,3]dithiol-4-yl)methyl (TFO), which contains four additional hydroxylethyl groups, relative to the Finland trityl radical CT-03, is reported. Similar to OX063, TFO exhibits excellent properties, including high water solubility in phosphate buffer, low log P, low pKa, long relaxation times, and negligible binding with bovine serum albumin. On the other hand, TFO has a sharper EPR line and higher O2 sensitivity than those of OX063. Therefore, in combination with its facile synthesis, TFO should find wide applications in magnetic resonance related fields and this synthetic approach would shed new light on the synthesis of other hydrophilic TAM radicals. 相似文献
58.
Tran Thu Ha Nguyen Hong Phong François-Xavier Le Dimet Hong Son Hoang 《Comptes Rendus Mecanique》2019,347(5):423-444
This article presents a correction method for a better resolution of the problem of estimating and predicting pollution, governed by Burgers' equations. The originality of the method consists in the introduction of an error function into the system's equations of state to model uncertainty in the model. The initial conditions and diffusion coefficients, present in the equations for pollution and concentration, and also those in the model error equations, are estimated by solving a data assimilation problem. The efficiency of the correction method is compared with that produced by the traditional method without introduction of an error function.Three test cases are presented in this study in order to compare the performances of the proposed methods. In the first two tests, the reference is the analytical solution and the last test is formulated as part of the “twin experiment”.The numerical results obtained confirm the important role of the model error equation for improving the prediction capability of the system, in terms of both accuracy and speed of convergence. 相似文献
59.
A high‐performance liquid chromatography–tandem mass spectrometry method was developed and validated for the simultaneous quantification of morphine, morphine's major metabolites morphine‐3‐glucuronide and morphine‐6‐glucuronide, and clonidine, to support the pharmacokinetic analysis of an ongoing double‐blinded randomized clinical trial that compares the use of morphine and clonidine in infants diagnosed with neonatal abstinence syndrome. Plasma samples were processed by solid‐phase extraction and separated on an Inertsil ODS‐3 (4 μm) column using an 0.1% formic acid in water–0.1% formic acid in methanol gradient. Detection of the analytes was conducted in the positive multiple reaction monitoring mode. The range of quantitation was 1–1000 ng/mL for morphine, morphine‐3‐glucuronide and morphine‐6‐glucuronide, and 0.25–100 ng/mL for clonidine. Intra‐day and inter‐day accuracy and precision were ≤15% for all analytes across the quantitation range. Extraction recovery rates were ≥94% for morphine, ≥90% for M3G, ≥87% for M6G and ≥ 79% for clonidine. Matrix effect ranged from 85–94% for clonidine to 101–106% for M3G. The method fulfilled all predetermined acceptance criteria and required only 100 μL of starting plasma volume. Furthermore, it was successfully applied to 30 clinical trial plasma samples. 相似文献
60.