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211.
This study compares and evaluates the effect of various matrices on liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS) analysis. Permanent post-column infusion (PCI) was used to quantify matrix effects. In this way, the suppressed or enhanced signal of the target material resulting from different co-eluting matrix components could be assessed. Twenty-four biological samples from in vivo and in vitro experiments were selected for this study. In addition, 7 sample components were further analyzed after sample preparation by protein precipitation. Multiple regression analysis was used to investigate the collinear relationship between matrix effects and co-eluted components at different time intervals. We found that salt was the dominant factor which impacted changes in signal detection. In order to eliminate it, we used ammonium formate as a modifier of the mobile phase which resulted in charge-state redistribution profiles so that a homogeneous matrix formed. By employing pulse gradient chromatography in the presence of 5 mM ammonium formate, favorable improvements of enhanced signal intensity and reduced matrix effects were obtained. These experiments also indicated the feasibility of using analogue IS during bio-analysis which contributed to an overall faster assay that would be suitable for drug discovery and development purposes. 相似文献
212.
Meili Qu Qiying Lv Bing Yang Weide Zhang Jiaqi Zhang Shuzhong Zhan Jianshan Ye 《Electroanalysis》2010,22(4):375-378
Supported bilayer lipid membrane (s‐BLM) containing one‐dimensional compound 1, TCNQ‐based (TCNQ=7,7,8,8‐tetracyanoquinodimethane) organometallic compound {(Cu2(μ‐Cl)(μ‐dppm)2)(μ2‐TCNQ)}∞, was prepared and characterized on the self‐assembled monolayer (SAM) of 1‐octadecylmercaptan (C18H37SH) deposited onto Au electrode. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) results showed that the compound 1, dotted inside s‐BLM, can act as mediator for electron transfer across the membrane. Two redox peaks and the charge‐transfer resistance of 400 kΩ were observed for compound 1 inside s‐BLM. The mechanism of the electron transfer across s‐BLM by TCNQ is by electron hopping while TCNQ‐based organometallic compound is by conducting. Further conclusion drawn from this finding is that the TCNQ‐based organometallic compound embedded inside s‐BLM exhibits excellent electron transfer ability than that of free TCNQ. This opens a new path for the development of s‐BLM sensor and/or biosensor by incorporation with TCNQ‐based organometallic compounds. 相似文献
213.
The structural and magnetic properties of Ta-doped Ca4Mn3−xTaxO10 (0≤x≤0.3) compounds have been investigated. Structural refinement indicates that the Ta doping maintains the orthorhombic layered perovskite structure with space group Pbca as Ca4Mn3O10 but induces an increase in both unit cell volume and octahedral distortion. The magnetization measurements reveal that the magnetization first increases and reaches to maximum for the x=0.1 sample and then gradually decreases with the increase of Ta content. There appear short-range ferromagnetic (FM) clusters in all the doped samples, which are caused by the double-exchange interaction between Mn4+ and Mn3+ that is induced by the charge compensation effect. As x is higher than 0.1, the overall results show evidence for the gradual appearance of a cluster glass behavior. When x increases to 0.3, the long-range antiferromagnetic (AFM) ground state is melted into the short-range magnetically ordered regions due to the increase of Ta5+ and Mn3+ at the expense of Mn4+. The competition between AFM regions and FM clusters makes the short-range magnetic components frustrate when the temperature falls to a frustrating point, and thus cluster glass transition occurs. 相似文献
214.
A highly sensitive amperometric immunosensor has been developed for the detection of carcinoembryonic antigen (CEA). It is based on (a) Prussian Blue nanoparticles coated with poly(diallyldimethylammonium chloride) (P-PB) and (b) double-layer gold nanocrystals. The sensor was obtained by first electrodepositing porous gold nanocrystals on the glassy carbon electrode (GCE), and then by modifying the electrode with the coated P-PB. Subsequently, colloidal gold nanoparticles (nano-Au) were adsorbed onto the GCE by electrostatic interactions between the negatively charged nano-Au and the positively charged P-PB to immobilize CEA antibodies. Finally, bovine serum albumin was employed to block possible remaining active sites and to prevent the non-specific adsorption on the nano-Au. This immunosensor was characterized by cyclic voltammetry and scanning electron microscopy. The working range was adjusted to two concentration ranges, viz. from 0.5 to 10 ng.mL?1, and from 10 to 120 ng.mL?1 of CEA, with a detection limit of 0.2 ng.mL?1 at three times the background noise. 相似文献
215.
Meihua Wang Jin Cai Lei Huang Zhengbin Lv Yaozhou Zhang Zhinan Xu 《Applied biochemistry and biotechnology》2010,162(7):2027-2036
The bioactivity of swollenin is beneficial to cellulose decomposition by cellulase despite the lack of hydrolytic activity
itself. In order to improve the productivity of swollenin, the effects of culture conditions on the expression level in recombinant
Aspergillus oryzae were investigated systematically. With regard to the bioactivity of swollenin, glycerin and peanut meal were the optimal
carbon or nitrogen source, respectively. The highest level production of swollenin (50 mg L−1) was attained after 88 h cultivation with the initial pH of 5.6 in the culture medium. Then the soluble swollenin was effectively
purified from the cultural supernatant by ammonium sulfate precipitation and cationic exchange chromatography with recovery
yield of 53.2%. The purified swollenin was fully bioactive due to its strong synergistic activity with cellulose. 相似文献
216.
Guangyuan Teng Lijing Gao Guomin Xiao Hu Liu Jianhua Lv 《Applied biochemistry and biotechnology》2010,162(6):1725-1736
This paper discusses the synthesis of biodiesel catalyzed by solid base of K2CO3/HT using Jatropha curcas oil as feedstock. Mg–Al hydrotalcite was prepared using co-precipitation methods, in which the molar ratio of Mg to Al was 3:1. After calcined at 600 °C for 3 h, the Mg–Al hydrotalcite and K2CO3 were grinded and mixed according to certain mass ratios, in which some water was added. The mixture was dried at 65 °C, and after that it was calcined at 600 °C for 3 h. Then, this Mg–Al hydrotalcite loaded with potassium carbonate was obtained and used as catalyst in the experiments. Analyses of XRD and SEM characterizations for catalyst showed the metal oxides formed in the process of calcination brought about excellent catalysis effect. In order to achieve the optimal technical reaction condition, five impact factors were also investigated in the experiments, which were mass ratio, molar ratio, reaction temperature, catalyst amount and reaction time. Under the best condition, the biodiesel yield could reach up to 96%. 相似文献
217.
A novel photoelectrochemical cells (PEC) based on quantum dots (QDs) sensitized graphene for light harvesting and energy conversion was described in this work. QDs sensitized graphene was prepared by in situ growth of QDs on noncovalently functionalized graphene. QDs sensitized graphene photoelectrodes showed enhanced photocurrent generation capability and incident photon-to-electron conversion efficiency (IPCE) at visible light, and could also be an efficient platform for other optoelectronic applications. 相似文献
218.
Xiao-Tao Wang Ying-Kui Yang Zhi-Fang Yang Xing-Ping Zhou Yong-Gui Liao Chen-Chen Lv Feng-Chih Chang Xiao-Lin Xie 《Journal of Thermal Analysis and Calorimetry》2010,102(2):739-744
Vinylated polyhedral oligomeric silsesquioxane (POSS-M) was prepared by the reaction of POSS containing amine groups with
acrylic acid. Azobenzene liquid crystalline copolymer (LCP-POSS) was then synthesized with 6.0 mol% POSS-M and 94.0 mol% acrylate
monomer containing azobenzene liquid crystalline moiety (Azo-M) by free-radical copolymerization. Homopolymer of Azo-M (LCP)
was also synthesized under the same conditions. Their thermal properties and liquid crystallinity were characterized by Thermal
gravimetric analysis (TG), differential scanning calorimetry (DSC), Wide-angle X-ray diffraction experiments (XRD) and polarized
optical micrographs (POM). The results showed that LCP-POSS has higher thermal stability and glass transition temperature
than pure LCP due to the incorporation of the rigid cage-like POSS. Especially, LCP-POSS exhibits enantiotropic smectic and
nematic liquid crystalline behaviors, its smectic-nematic transition temperature (T
SN) and nematic-isotropic transition temperature (T
NI) are higher than those of pure LCP, which may promote and extend its applications on stimuli-responsive materials and devices. 相似文献
219.
Molecularly imprinted microspheres (MIMs) were prepared by suspension polymerization for the binding and recognition of dibutyl phthalate (DBP). DBP was used as the template molecule, methacrylic acid as the functional monomer, ethylene dimethacrylate (EDMA) as the linking agent, PVA as the dispersing agent, and Span 60 as the surfactant. The MIMs were characterized with electron microscope scanning and rebinding experiments. The Scatchard plot revealed that the template‐polymer system has a two‐site binding behavior with dissociation constants of 4.05 and 0.515 mmol/L. The MIMs exhibited the highest selective rebinding to DBP at 736.85 μg/g. The recoveries of the MIM‐SPE column for DBP extraction was 94.75–101.9% with the RSD of 1.5–7.3%, indicating the feasibility of the prepared MIMs for DBP extraction. Finally, the method developed was used to analyze the trace levels of phthalate in aqueous environment samples. 相似文献
220.
Hongyuan Yan Jingjing Du Xiguo Zhang Gengliang Yang Kyung Ho Row Yunkai Lv 《Journal of separation science》2010,33(12):1829-1835
A simple and rapid ultrasound‐assisted dispersive liquid–liquid microextraction method coupled with GC‐flame ionization detection was developed for simultaneous determination of nine pyrethroids in domestic wastewater samples. An ultrasound‐assisted process was applied to accelerate the formation of the fine cloudy solution using small volume of disperser solvent, which markedly increased the extraction efficiency and reduced the equilibrium time. Various parameters affecting the extraction efficiency were investigated, including the type and volume of extraction solvent and disperser solvent, extraction and ultrasonic time. Good linearity was obtained for all analytes in the range of 0.8–100 μg/L with the correlation coefficient (r2)≥0.998. The recoveries at three spiking levels ranged from 75.3 to 101.2% with the RSD less than 8.7% (n=5). Under the optimum condition, the enrichment factors for the nine pyrethroids ranged from 728‐ to 1725‐fold. This method offered a good alternative for routine analysis due to its simplicity and reliability. 相似文献