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   1374篇
  免费   72篇
  国内免费   26篇
化学   1022篇
晶体学   5篇
力学   72篇
数学   154篇
物理学   219篇
  2024年   4篇
  2023年   9篇
  2022年   34篇
  2021年   61篇
  2020年   83篇
  2019年   69篇
  2018年   113篇
  2017年   63篇
  2016年   111篇
  2015年   83篇
  2014年   92篇
  2013年   187篇
  2012年   103篇
  2011年   116篇
  2010年   72篇
  2009年   74篇
  2008年   61篇
  2007年   41篇
  2006年   20篇
  2005年   22篇
  2004年   7篇
  2003年   14篇
  2002年   10篇
  2001年   4篇
  1999年   4篇
  1994年   3篇
  1993年   2篇
  1992年   1篇
  1991年   1篇
  1989年   1篇
  1986年   1篇
  1985年   3篇
  1984年   2篇
  1976年   1篇
排序方式: 共有1472条查询结果,搜索用时 31 毫秒
201.
Journal of Thermal Analysis and Calorimetry - The natural gas entering the liquefaction cycle usually consists of nitrogen, ethane, propane and also heavier hydrocarbons which are economically...  相似文献   
202.
In this study a new series of magnetic and heat resistant nanocomposites were prepared based on a highly soluble poly(imide-ether) (PIE) reinforced with two different types of magnetic nanoparticles via a solution intercalation technique. New PIE with good solubility and desired molar mass containing bulky xanthene rings and amide groups in the side chains was synthesized via thermal cyclization of the poly(amic acid) precursor, obtained from the reaction of a new diamine derived from 9H-xanthene and 4,4′-oxydiphthalic dianhydride (ODPA). Improved solubility was attributed to the presence of xanthene group and flexible ether linkage in the polyimide backbones that reduce the chain-chain interaction and enhance solubility by penetrating solvent molecules into the polyimide chains. Fe3O4 nanoparticles (MNPs) which synthesized from chemical co-precipitation route were coated with silica (SiO2), sequentially with (3-aminopropyl)triethoxysilane and poly-melamine-terephthaldehyde (MNPs-PMT), and then separately dispersed in the poly(amic acid) solutions and thermally imidized to form PIE/Fe3O4 and PIE/MNPs-PMT nanocomposites. The nanostructures and properties of the resultant materials were investigated using FTIR spectroscopy, X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). The properties of the nanocomposites were strongly related to the dispersion and interaction between the nanoparticles and PIE matrix. The thermogravimetric analysis (TGA) results showed that the addition of MNPs-PMT nanoparticles resulted in a substantial increase in the thermal stability of the corresponding PIEN. The temperature at 10% weight loss (T10) was increased from 416 °C to 428 °C for PIEN containing 3 wt% MNPs-PMT as compared to neat PIE, as well the char yield enhanced. Furthermore, the MNPs-PMT nanoparticles had better dispersion in the polymer matrix due to the strong intermolecular hydrogen bond interactions between the NH and C=N groups of surface-modified nanoparticles and the PIE matrix than the uncoated Fe3O4 nanoparticles, and exhibited a better intercalated morphology and improved thermal properties. Also, the PIEN nanocomposites under applied magnetic field exhibited the hysteretic loops of the superparamagnetic nature.  相似文献   
203.
Research on Chemical Intermediates - Fe3O4@SiO2–TiCl3 NPs, a novel core shell catalyst, was synthesized via preparing Fe3O4@SiO2 as a magnetic support followed by treatment with titanium...  相似文献   
204.
A new class of 2-arylamino-dihydroxyindenopyrroles were prepared by the one-pot multicomponent reaction of ninhydrin, N-methyl-1-(methylthio)-2-nitroethenamine and aromatic amines in EtOH at room temperature. The advantages of this procedure are short reaction times, good to high yields, easy separation of products and good functional group tolerance.  相似文献   
205.
Journal of Radioanalytical and Nuclear Chemistry - In this study, we introduce a new 99mTc-radiolabeled bombesin derivative for imaging of prostate cancer (PC). We used 6-hydrazinonicotinamide...  相似文献   
206.
A solid-phase microextraction fiber was prepared by polyaniline/graphene oxide nanocomposite as sorbent on the surface of a platinized stainless steel wire using electrospinning technique. The nanocomposite structure was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The polyaniline/graphene oxide nanocomposite fiber was used for the determination of nicotine from tobacco samples using headspace solid-phase microextraction method and gas chromatography–flame ionization detection. Influential experimental variables on the extraction efficiency of nicotine, such as extraction time and temperature, humidity and desorption conditions, were evaluated and optimized. Under the optimal experimental conditions? the limit of detection, linear dynamic range, intraday and inter-days precisions were found to be 0.01 μg g?1, 0.05–700 µg g?1 (R2?=?0.996), 6.9 and 8.1%, respectively. Comparison of the polyaniline/graphene oxide nanocomposite sorbent with polyaniline and commercial fibers shows longer durability, larger capacity and higher extraction efficiency. The polyaniline/graphene oxide nanocomposite fiber was successfully applied for the determination of nicotine in tobacco samples.  相似文献   
207.
A method for one-step synthesis of ultrafine agarose-coated superparamagnetic iron oxide nanoparticles (AC-SPIONs) was developed. The method is facile and fast and requires no organic solvent or surfactant. The average particle size of the prepared AC-SPIONs was only 20–40 nm with a narrow size distribution and with large saturation magnetization at room temperature. The obtained ultrafine nanogel particles were characterized by scanning electron microscopy, energy-dispersive X-ray analysis, Fourier transform infrared spectroscopy, transmission electron microscopy and vibrating sample magnetometer techniques. The AC-SPIONs were epoxy-activated by epichlorohydrin and aminated by ammonium hydroxide. The amination of the particles was investigated by the Kaiser test. The adsorption of two model compounds (gallic acid and ellagic acid) on the functionalized nanoparticles and their releases from them were investigated spectrophotometrically in three different pH values under biological conditions. The functionalized AC-SPIONs displayed good adsorption and in vitro drug release in a phosphate-buffered saline (pH 7.4). The ultrafine AC-SPIONs can be potentially used in magnetic solid-phase extraction, drug delivery, protein purification and enzyme immobilization methods.  相似文献   
208.
In a successful fortification program, the stability of micronutrients added to the food is one of the most important factors. The added vitamin D3 is known to sometimes decline during storage of fortified milks, and oxidation through fatty acid lipoxidation could be suspected as the likely cause. Identification of vitamin D3 oxidation products (VDOPs) in natural foods is a challenge due to the low amount of their contents and their possible transformation to other compounds during analysis. The main objective of this study was to find a method to extract VDOPs in simulated whole milk powder and to identify these products using LTQ-ion trap, Q-Exactive Orbitrap and triple quadrupole mass spectrometry. The multistage mass spectrometry (MSn) spectra can help to propose plausible schemes for unknown compounds and their fragmentations. With the growth of combinatorial libraries, mass spectrometry (MS) has become an important analytical technique because of its speed of analysis, sensitivity, and accuracy. This study was focused on identifying the fragmentation rules for some VDOPs by incorporating MS data with in silico calculated MS fragmentation pathways. Diels–Alder derivatization was used to enhance the sensitivity and selectivity for the VDOPs’ identification. Finally, the confirmed PTAD-derivatized target compounds were separated and analyzed using ESI(+)-UHPLC-MS/MS in multiple reaction monitoring (MRM) mode.
Graphical Abstract ?
  相似文献   
209.
In the present study, two new zinc complexes with the chemical formulas of [Zn(2-Ampy)(Acac)2] (I) and [Zn(p-Van)2(H2O)2] (II) were synthesized and characterized by FT-IR, 1H NMR, and UV-Vis spectroscopy. Moreover, the crystal structures of the complexes were determined by X-ray diffraction technique. Single-crystal X-ray diffraction analyses (CIF files CCDC nos. 1513672 (I) and 1513673 (II)) revealed that complex I has a distorted square pyramid environment, and complex II has a distorted octahedral geometry. The complexes were also screened for in vitro antibacterial activities against some bacteria. The results show that complexes have the effective antibacterial activities. The complexes were employed to prepare ZnO nanoparticles by the combustion synthesis method at 700°C for 8 h. The nanoparticles were characterized, using powder X-ray diffraction analysis (PXRD), scanning electron microscopy and transmission electron microscope. PXRD analysis showed the presence of pure phase in both samples. Furthermore, the crystallite size was approximately 37 and 42 nm for ZnO prepared from complexes I and II, respectively.  相似文献   
210.
In this work, phenol reacted with 4-aminoantipyrine (4-AAP) reagent in presence of potassium hexacyanoferrate(III) and then was extracted using ultrasound-assisted emulsification microextraction via 1-hexyl-3-methyl imidazolium hexafluorophosphate as an environmentally friendly solvent. Effects of the main experimental variables were investigated and optimized by central composite design. Under the optimum conditions (pH 9.5, 100 mg/L 4-AAP, 100 μL of ionic liquid as extraction solvent, 0.2 g/L K3Fe(CN)6 and 0.2 M NH4Cl) the dynamic linear range, limit of detection and relative standard deviation were obtained as 0.2?25 μg/L, 0.07 μg/L and 2.6%, respectively. Finally, the applicability of the proposed ultrasoundassisted emulsification microextraction was examined and very good results were obtained. The results confirmed the applicability of the proposed method as a versatile, low cost and sensitive preconcentration method for determination of very low concentrations of phenol in aqueous solutions.  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