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1.
When dealing with simple phenols such as caffeic acid (CA) and ferulic acid (FA), found in a variety of plants, it is very important to have control over the most important factors that accelerate their degradation reactions. This is the first report in which the stabilities of these two compounds have been systematically tested by exposure to various different factors. Forced degradation studies were performed on pure standards (trans-CA and trans-FA), dissolved in different solvents and exposed to different oxidative, photolytic and thermal stress conditions. Additionally, a rapid, sensitive, and selective stability-indicating gas chromatographic-mass spectrometric method was developed and validated for determination of trans-CA and trans-FA in the presence of their degradation products. Cis-CA and cis-FA were confirmed as the only degradation products in all the experiments performed. All the compounds were perfectly separated by gas chromatography (GC) and identified using mass spectrometry (MS), a method that additionally elucidated their structures. In general, more protic solvents, higher temperatures, UV radiation and longer storage times led to more significant degradation (isomerization) of both trans-isomers. The most progressive isomerization of both compounds (up to 43%) was observed when the polar solutions were exposed to daylight at room temperature for 1 month. The method was validated for linearity, precision as repeatability, limit of detection (LOD) and limit of quantitation (LOQ). The method was confirmed as linear over tested concentration ranges from 1−100 mg L−1 (r2s were above 0.999). The LOD and LOQ for trans-FA were 0.15 mg L−1 and 0.50 mg L−1, respectively. The LOD and LOQ for trans-CA were 0.23 mg L−1 and 0.77 mg L−1, respectively. 相似文献
2.
乐毅 《宁波大学学报(理工版)》2004,17(4):437-440
从正交各向异性三维弹性动力学的控制方程出发,在求得四边简支矩形板自由振动频率和位移振型的基础上,构造了受迫振动的位移函数;利用自由振动位移振型的正交性,将控制方程的空间变量和时间变量分离,得到了广义质量、广义力和频率表示的关于时间的2阶常微分方程,从而得到了正交各向异性弹性矩形板在受迫振动下的位移场和应力场.给出了本文方法与薄板理论的算例. 相似文献
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不良导体导热系数测定实验中仪表风扇对实验结果的影响 总被引:1,自引:0,他引:1
根据对物体冷却规律的分析,并从实验结果比较,指出稳态法测不良导体导热系数实验中,设置散热盘的冷却过程应与其在稳态过程时的强迫对流散热方式保持一致. 相似文献
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P. G. Royall D. Q. M. Craig M. Reading T. J. Lever 《Journal of Thermal Analysis and Calorimetry》2000,60(3):795-805
The purpose of this study was to investigate the feasibility of modulating the temperature programme of a conventional DSC
by use of an alternating gas-flow system. Modulated temperature differential scanning calorimetry (MTDSC) is an important
thermal analysis technique but suffers from a limited applicable frequency range due to the mass of the sample and DSC cell
leading to the impingement of thermal conductivity effects. We suggest that the frequency limit can be increased by replacing
the cell as the source of temperature modulation with an external gaseous source, directed towards the sample and reference
pans. In this evaluation, an alternating gas-flow was passed through a line to a forced gas-flow accessory (FGFA). The FGFA
consisted of two matched cylinders containing chambers that allowed pre-temperature-equilibration of the stream of gas before
it was passed over the sample and reference pans. The development of this device revealed the essential practical requirements
of gas-flow modulation for high-frequency temperature modulation. These include the following: an appropriately sealed tunable
gas supply to both sample and reference pans, an effective method for high-frequency cycling of the gas-flow rate, a small
aperture to deliver the flowing gas directly over the pan and a temperature equilibration chamber. The results from samples
of quenched PET and amorphous Saquinavir indicate that gas-flow modulation is indeed feasible, with the FGFA able to raise
the attainable temperature modulation frequency by an order of magnitude compared to conventional MTDSC.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
10.
Khaleel AA 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(4):925-932
Pure maghemite, gamma-Fe(2)O(3), was prepared as ultra fine particles in the nanometer-sized range via the forced precipitation method in an organic solvent. The precipitation of iron(III) ions, from iron(III) chloride in 2-propanol led selectively to highly dispersed particles of ferrihydrite, which upon treatment with temperatures higher than 200 degrees C under dynamic vacuum resulted in high-surface-area particles of gamma-Fe(2)O(3). Precipitation in water also led to ferrihydrite, but the final product, after heating at 300 degrees C, contained a mixture of gamma-Fe(2)O(3) and alpha-Fe(2)O(3) (hematite). The precipitation from iron(III) nitrate in water resulted in goethite which was converted to hematite upon heating. On the other hand, the final product in 2-propanol was a mixture of maghemite and hematite. The products were characterized by FTIR, TGA, XRD, and gas sorption analysis. Nitrogen gas adsorption studies for the pure gamma-Fe(2)O(3) samples revealed mesoporous particles with high surface areas in the range of 70-120 m(2) g(-1) after heat treatment at 300 degrees C. The gamma-Fe(2)O(3) particles retained their gamma-phase as well as their mesoporous structure at relatively high temperatures, as high as 400 degrees C. 相似文献