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111.
Xiaoji Cao Jingfang Qiao Liping Wang Xuemin Ye Lebin Zheng Nan Jiang Weimin Mo 《Rapid communications in mass spectrometry : RCM》2012,26(7):740-748
A powerful ionic liquid‐based ultrasonic‐assisted extraction (ILUAE) method combined with ultra‐performance liquid chromatography coupled to electrospray ionization quadrupole time‐of‐flight tandem mass spectrometry (UPLC/ESI‐QTOFMSn) was employed in the rapid simultaneous screening of iridoid glycosides, phenylethanoid glycosides, and cucurbitacin glycosides from P. scrophulariiflora. The ILUAE procedure was optimized over several ultrasonic parameters, including the ultrasonic power, concentration of the ionic liquid, and solid–liquid ratio. A comparison with conventional heat‐reflux extraction and regular UAE demonstrated that the optimized approach yielded a high extraction efficiency (Picroside I, 2.84%; Picroside II, 3.57%; 6‐O‐E‐feruloyl catalpol, 2.20%) within a short extraction time of 30 min. Negative ion mode ESI‐QTOFMS2 analysis of the fragmentation reactions of the [M–H]– ions was conducted to characterize the diagnostic ions related to the glycosyl moieties, aglycone units, and the type and substituted position of the ester groups. Interestingly, the positional isomers of the iridoid glycosides could be easily discriminated based on the characteristic ions. A total of 15 glycosides, including three groups of iridoid glycoside isomers and two groups of phenylethanoid glycoside isomers, were conveniently identified within 13.5 min. Moreover, 6'‐O‐vanilloyl catalpol was identified in P. scrophulariiflora for the first time. The method developed here was further validated by measuring the recovery, correlation coefficient (R2), and reproducibility (RSD, n = 5) of three iridoid glycosides: 89.60%–109.02%, 0.9991–0.9998, and 0.93%–1.44%, respectively. This study demonstrated the capabilities of ILUAE combined with UPLC/ESI‐QTOFMSn for the rapid screening of glycosides in P. scrophulariiflora. This method offers an approach to similar studies on other natural plants. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
112.
Hui Mei Wenjia Han Jianglin Hu Se Xiao Yizhu Lei Rui Zhang Wanlin Mo Guangxing Li 《应用有机金属化学》2013,27(3):177-183
This work describes a highly efficient unstrained C(sp3)―N bond activation approach for synthesis of N,N‐dimethylacetamide (DMAc) via catalytic carbonylation of trimethylamine using a PdCl2/bipy (bipy = 2,2′‐bipyridine)/Me4NI catalyst system. A low Pd catalyst dosage (1.0 mol%) is sufficient for high selectivity (98.1%) and yield (90.8%), with a turnover number (TON) of 90.0 mmol of DMAc obtained per mmol of PdCl2 employed under mild reaction conditions. The influence of reaction parameters such as catalyst precursor dosage, ligand type and promoter on activity is investigated. This work also discusses in detail the halide promoter's role in the reaction, and provides a plausible mechanism based on the intermediates methyl iodide and acetyl iodide. Analyses indicate that the carbonylation of trimethylamine may proceed through an active intermediate acetyl iodide formed by carbonylation of methyl iodide generated from the decomposition of the promoter Me4NI under reaction conditions. The formation of acetyl iodide favors the cleaving efficiency of the inert unstrained C(sp3)―N bond of trimethylamine. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
113.
Alejandro Ortega Moñux Steve Greedy Ginés Lifante 《Optical and Quantum Electronics》2013,45(4):307-307
114.
Jia Mo Zhaofeng Ma Yixian Yang Xinxin Niu 《International Journal of Theoretical Physics》2013,52(11):3813-3819
This paper presents a Bell-dual-basis-based quantum watermarking protocol composed of three major algorithms: watermark embedding and extracting and the intercepting test. The first two are completed by using the entanglement swapping property of Bell dual basis and the test is accomplished through IBF protocol to guarantee its bottom security. The watermarking protocol is mainly designed for the protection of digital copyright in the existence of classical information. This design finds that the quality of digital contents is not damaged with its zero-watermark attributes when embedding watermarks. 相似文献
115.
The influence of the flashlamp pump current pulse shape on Er:YAG laser efficiency and laser rod thermal focusing was studied theoretically and experimentally. Two pulse shapes, PFN (Pulse Forming Network) and VSP (Variable Square Pulse), were considered. Theoretical modeling and experimental measurements show that the pump pulse shape itself does not have a significant influence on the Er:YAG laser efficiency or thermal focusing. Instead, the major parameter influencing Er:YAG laser efficiency and thermal focusing was found to be the overall pulse duration. For PFN pulses, rise and fall times directly define the overall pulse duration, and therefore do have influence on thermal focusing. By contrast, VSP pulse duration is defined by the externally controlled on-time of the switching transistor. For square shaped pulses, short rise and fall times do not have a direct beneficial influence on thermal lensing. 相似文献
116.
117.
The study toward the total synthesis of (R)‐(+)‐harmicine is reported in this paper. The enantioselective synthesis of pyrrolidinone, the main backbone of of (R)‐(+)‐harmicine, has been completed by the methodology based on photo‐induced Wolff rearrangement of α‐diazo‐β‐carbonyl compounds. 相似文献
118.
The effect of WO3 on thermal behaviour and thermal stability of ZnO–P2O5–WO3 glasses prepared in compositional series (100 ? x)[0.5ZnO–0.5P2O5] ? xWO3 (x = 0–60) was investigated by heating microscopy and the results were correlated with the results determined by conventional thermodilatometry and differential thermal analysis. Thermoanalytical studies showed that the glass transformation temperature and dilatation softening temperature increase with increasing WO3 content while thermal expansion coefficient decreases. The highest stability towards crystallization possess glasses containing 20–30 mol% WO3. Major compounds formed by the crystallization of the glasses were Zn(PO3)2, WO3 and W18P2O59. The values of sphere temperature, hemisphere temperature and flow temperature obtained using heating microscopy were strongly influenced by the degree of crystallization process at the sintering. 相似文献
119.
Yu Mo Lei Zhao Chia-Lung Chen Giin Yu Amy Tan Jing-Yuan Wang 《Journal of Thermal Analysis and Calorimetry》2013,111(1):781-788
Pyrolysis is one important way to treat polystyrene waste and upcycle it into useful materials. A comparative pyrolysis study of virgin polystyrene (VPS) and two types of commonly used polystyrene products, expanded polystyrene (EPS) and polystyrene container (CPS) was carried out. Various values were found in the thermodynamic study and kinetic study of VPS, EPS, and CPS pyrolysis, suggesting distinct thermal degradation characteristics of these materials. The energy barrier order of the pyrolysis processes was EPS, CPS, VPS, showing activation energy of 230, 219, and 145 kJ mol?1, respectively. The order of amount of heat absorbed was EPS, CPS, VPS, with enthalpy of 224, 213, and 139 kJ mol?1, respectively. The reaction favorability order was EPS, CPS, and VPS with Gibbs free energy of 118, 132, and 210 kJ mol?1, respectively. Thermogravimetric analysis indicated the use of high heating rate would increase the reaction rate and shorten the reaction time. Product evolution profiles showed that VPS and CPS pyrolysis produced mainly aromatics, while EPS pyrolysis produced aromatics at the initial phase of the reaction and aliphatic hydrocarbon at the latter phase. The diverse pyrolysis behaviors of VPS, EPS, and CPS demonstrated that an examination on different polystyrene materials was desired to optimize the pyrolysis conditions and product distribution, and thus benefit the process of valuable materials recovery. 相似文献
120.
A series of self-healable polyurethane (SHPU)/modified graphene (MG) nanocomposites were synthesized from poly(tetramethylene glycol) (PTMG) and 4,4′-methylene diphenyl diisocyanate (MDI) with minute amounts (0–1 wt%) of MG which was chemically modified graphene oxide (GO) with phenyl isocyanate and reduced in the presence of phenylhydrazine. 相似文献