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51.
污泥和沉积物中微量大环内酯类、磺胺类抗生素、甲氧苄胺嘧啶和氯霉素的测定 总被引:7,自引:0,他引:7
利用超声波辅助萃取(USE)技术,联合固相萃取(SPE)净化浓缩以及液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)技术,建立了城市污泥和河流底泥中微量-痕量大环内酯类、磺胺类抗生素、甲氧苄胺嘧啶和氯霉素的多目标定量分析方法.样品经USE提取,SPE净化后,用LC-ESI-MS/MS检测.选择C18为分析柱,甲醇、5 mmol/L醋酸铵和0.1%甲酸混合溶液为流动相,选择在ESI正电离源下多反应监测(MRM)模式检测.对比了USE和加速溶剂萃取(ASE)对抗生素的萃取效率,优化了萃取条件.结果表明: USE和ASE对所选抗生素的萃取效率相当; 而50%甲醇溶液在酸性条件下(pH 2)萃取效率最好.抗生素的方法检出限为2.2~66.9 ng/g(干重,下同); 回收率介于74.7%~111.8%之间; 相对标准偏差小于10.6%.应用此方法在广州某污水处理厂脱水污泥及某河涌底泥中检测到磺胺二甲基嘧啶、克拉霉素、脱水红霉素及罗红霉素等多种抗生素,含量为6.8~125.6 ng/g. 相似文献
52.
Xincheng Xu Jianxin Li Hesheng Li Ying Cai Yuhe Cao Benqiao He Yuzhong Zhang 《Journal of membrane science》2009
Fouling is the most critical problem associated with membrane separations in liquid media. But it is difficult to control the inevitable membrane fouling because of its invisibility, especially on the inside surface of hollow fiber membranes. This study describes the extension of ultrasonic time-domain reflectometry (UTDR) for the real-time measurement of particle deposition in a single hollow fiber membrane. A transducer with a frequency of 10 MHz and polyethersulfone hollow fiber membranes with 0.8 mm inside diameter (ID) and 1.2 mm outside diameter (OD) were used in this study. The fouling experiments were carried out with 1.8 g/L kaolin suspension at flow rates 16.7 and 10.0 cm/s. The results show that UTDR technique is able to distinguish and recognize the acoustic response signals generated from the interfaces water/upper outside surface of the hollow fiber, lumen upside surface/water, water/lumen underside surface and lower outside surface/water in the single hollow fiber membrane module in pure water phase. The systemic changes of acoustic responses from the inside surfaces of the hollow fiber in the time- and amplitude-domain with operation time during the fouling experiments were detected by UTDR. It is associated with the deposition and formation of the kaolin layer on the inside surfaces. Further, the acoustic measurement indicates that the deposited fouling layer is denser on the lumen underside surface of the hollow fiber than that on the lumen upside surface as a result of weight. Moreover, it is found that the fouling layer grows faster on the inside surface of the hollow fiber at a flow rate of 10.0 cm/s than that at 16.7 cm/s due to the lower shear stress. The fouling layer formed is thicker at a flow rate of 10.0 cm/s than that at 16.7 cm/s. The flux decline data and SEM analysis corroborate the ultrasonic measurement. Overall, this study confirms that UTDR measurement will provide not only a new protocol for the observation of hollow fiber membrane fouling and cleaning, but also a quantitative approach to the optimization of the membrane bioreactor system. 相似文献
53.
超声波对制备Co-Fe/硅藻土选择加氢催化剂的影响 总被引:1,自引:0,他引:1
分别在有无超声条件下,采用分步浸渍法制备了负载型Co-Fe/硅藻土催化剂,以肉桂醛选择加氢为肉桂醇为探针反应,在固定床微分反应器上考察了催化剂的活性.采用热分析、红外、XRD及正电子寿命谱等技术分析了催化剂的催化性能及超声波对活性的影响.结果表明,经超声处理的催化剂对肉桂醛加氧为肉桂醇转化率、选择性和收率明显提高.超声处理没有改变催化剂载体的结构,但使主、助催化剂更好地分散在载体上,使催化剂表面的两类缺陷尺寸变小,同时增加第二类缺陷数量,有更好的催化活性. 相似文献
54.
55.
Zhi-Cai Wang Dan-Dan Zhao Guang-Yu Zhao Hu-Lin Li 《Journal of Solid State Electrochemistry》2009,13(3):371-376
A novel chemical method based on ultrasonic assisted polyol synthesis for the fabrication of highly dispersed Pt nanoparticles
on multi-walled carbon nanotubes (MWCNTs) was developed. The simple and green method took only about 10 min at ambient temperature.
The structure and chemical nature of the resulting Pt/MWCNT composites were characterized by transmission electron microscopy
(TEM), X-ray diffraction (XRD), and energy dispersive X-ray spectrometry (EDS). The results showed that the prepared Pt nanoparticles
were uniformly dispersed on the MWCNT surface. The mean size of Pt nanoparticles was about 2.8 nm. Electrochemical properties
of Pt/MWCNT electrode for methanol oxidation were examined by cyclic voltammetry (CV) and excellent electrocatalytic activities
could be observed. The possible formation mechanism of Pt/MWCNTs was also discussed. 相似文献
56.
Shadpour Mallakpour Fariba Derakhshan 《International Journal of Polymer Analysis and Characterization》2014,19(8):750-764
In this study, the goal was the preparation, characterization, and surface morphology of poly(amide-imide)/TiO2-citric acid nanocomposites (PAI/TiO2-CA NCs). Owing to the high surface energy and tendency for agglomeration, the surface of TiO2 nanoparticles was modified with citric acid. Then poly(amide-imide) was synthesized by direct polycondensation reaction of N,N′-(pyromellitoyl)-bis-L-leucine diacid with 4,4′-diaminodiphenylmethane by triphenyl phosphite and tetra-n-butylammonium bromide as a green medium. The attained polymer and modified TiO2 nanoparticles were used to prepare PAI/TiO2-CA NCs through ultrasonic irradiation. The resulting PAI/TiO2-CA NC was characterized with FT-IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, and thermogravimetric analysis. 相似文献
57.
This paper presents a novel non-contact method for evaluating the resonant frequency of a microstructure, Firstly, the microstructure under test is excited by ultrasonic waves. This excitation method does not impose any undefined load on the specimen like the electrostatic excitation and also this is the first actual use of ultrasonic wave for exciting a microstructure in the literature. Secondly, the amplitudes of the microstructure are determined by image edge detection using a Mexican hat wavelet transform on the vibrating images of the microstructure. The vibrating images are captured by a CCD camera when the microstructure is vibrated by ultrasonic waves at a series of discrete high frequencies (〉30 kHz). Upon processing the vibrating images, the amplitudes at various excitation frequencies are obtained and an amplitude-frequency spectrum is obtained from which the resonant frequency is subsequently evaluated. A micro silicon structure consisting of a perforated plate (192 × 192 μm) and two cantilever beams (76 × 43 μm) which is about 4 μm thickness is tested. Since laser interferometry is not required, thermal effects on a test object can be avoided. Hence, the setup is relatively simple. Results show that the proposed method is a simple and effective approach for evaluating the dynamic characteristics of microstructures. 相似文献
58.
The isomorphic substitution of boron into ZSM‐5 zeolite under static hydrothermal condition was investigated. Evaluation of hydrothermal synthesis of BZSM‐5 was performed by treating the synthesis mixture by different aging processes, namely, ultrasonic, static, stirring, and microwave‐assisted aging prior to the conventional hydrothermal treatment. The synthetic processes with different techniques of aging prior to the onset of conventional hydrothermal crystallization were compared with a process without any prior aging. The obtained results showed that the ultrasonic and microwave assisted aging shortened the crystallization time and altered the crystal size and the morphology of the obtained products. The characteristics of the synthesized products were obtained by FT‐IR spectroscopic, XRD and SEM techniques. 相似文献
59.
Various empirical theories of ultrasonic velocity have been applied to three binary liquid mixtures, under pressures up to
200 MPa and their validity have been tested. A pressure dependent study of ultrasonic velocities has been made at 303.15 K.
The agreement between theory and experiment is found to be quite satisfactory. 相似文献
60.
E. Van Hoeck T. De Schaetzen C. Pacquet F. Bolle L. Boxus J. Van Loco 《Analytica chimica acta》2010,663(1):55-59
Benzophenone (BP) and 4-methylbenzophenone (4MBP) are photo-initiators that are generally used to cure ink on carton boards.In this contribution, a fast and reliable method for the determination of BP and 4MBP in breakfast cereals is described. The sample was extracted ultrasonically using a mixture of dichloromethane and acetonitrile (1:1), followed by a clean-up of the extract using solid phase extraction with a silica cartridge. Finally, the extract was analysed by GC-MSn. Benzophenone-d10 was used as internal standard. The presented method is validated in terms of linearity, recovery, repeatability and intra-laboratory reproducibility, specificity, limit of detection and limit of quantification. In conclusion, this method is able to detect both BP and 4MBP at very low concentrations (LOD = 2 μg kg−1) in breakfast cereals. 相似文献