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   2121篇
  免费   115篇
  国内免费   18篇
化学   1339篇
晶体学   30篇
力学   87篇
数学   330篇
物理学   468篇
  2024年   9篇
  2023年   21篇
  2022年   44篇
  2021年   139篇
  2020年   80篇
  2019年   86篇
  2018年   81篇
  2017年   85篇
  2016年   134篇
  2015年   114篇
  2014年   122篇
  2013年   187篇
  2012年   184篇
  2011年   161篇
  2010年   112篇
  2009年   91篇
  2008年   106篇
  2007年   90篇
  2006年   62篇
  2005年   60篇
  2004年   61篇
  2003年   33篇
  2002年   35篇
  2001年   14篇
  2000年   15篇
  1999年   7篇
  1998年   8篇
  1997年   6篇
  1996年   9篇
  1995年   8篇
  1994年   11篇
  1993年   6篇
  1992年   6篇
  1991年   7篇
  1990年   11篇
  1989年   2篇
  1988年   4篇
  1986年   2篇
  1985年   5篇
  1984年   3篇
  1983年   3篇
  1982年   4篇
  1981年   5篇
  1980年   4篇
  1979年   3篇
  1977年   2篇
  1976年   4篇
  1972年   2篇
  1965年   2篇
  1907年   1篇
排序方式: 共有2254条查询结果,搜索用时 15 毫秒
81.
Conductive polythiophene (PTh)/poly(ethylene terephthalate) (PET) composite fibers were prepared by polymerization of thiophene in the presence of PET fibers in acetonitrile medium using FeCl3. The effects of polymerization conditions such as oxidant/monomer mol ratio and polymerization temperature and time on PTh content and surface electrical resistivity of PTh/PET composite fiber were investigated in detail. It was observed that the usage of preswelled PET fibers in dichloromethane increased the PTh content and decreased surface resistivity of composite fiber. Composite fiber having the highest PTh content (5.7%) and the lowest surface resistivity (80 kΩ) was obtained at 20°C with 1.25 M FeCl3 and 0.42 M thiophene concentrations. The washing effects of laundering detergent and dry cleaning liquid on surface resistivity of composite fibers were investigated. The electromagnetic shielding effectiveness (EMSE) and relative shielding efficiency by absorption and reflection of composite fibers were measured in the radio and microwave frequency range. The results show that the EMSE values decreased with increasing frequency from radio waves to microwaves with an attenuation of 21 dB to 4 dB.  相似文献   
82.
In this study, for the first time a model electrochemical kit was constructed for the detection of a functional polymorphism in catechol‐O‐methyl transferase (COMT) gene which is important for diagnosis of neuropsychiatric disorders as Alzheimer disease. The disposable pencil graphite electrode (PGE) is designed as a “kit” and the probe DNA covered PGE can detect single nucleotide polymorphisms (SNPs) from real samples based on the guanine oxidation signal even after 5 months of kit preparation (150 days durability).The detection limit (S/N=3) of the biosensor was calculated as 1.18 pmol of synthetic target sequence and 6.09×105 molecules of real samples in 30 min detection time.  相似文献   
83.
In this study graphite electrodes modified by a thin DNA‐imprinted polypyrrole layer, which was able to bind specific target‐DNA, are reported. For this aim, electrochemical synthesis of polypyrrole was performed on a pencil graphite electrode by cyclic voltammetry (CV) or by potential pulse sequences (PPS). The modified electrode surface was used for electrochemical determination of target‐DNA by differential pulse voltammetry. According to our best knowledge this is a first report on the application of DNA‐imprinted polymer for the determination of target‐DNA. The results showed that the molecularly imprinted polypyrrole (MIPPy) layer that formed on the carbon electrode surface was sensitive for target‐DNA, while the nonimprinted polypyrrole layer was not sensitive to the same target‐DNA. Comparison of electrodes modified using PPS and CV techniques is presented.  相似文献   
84.
Kurbanoglu  Sevinc  Gumustas  Mehmet  Uslu  Bengi  Ozkan  Sibel A. 《Chromatographia》2013,76(21):1477-1485

A RP-LC method is presented, which is sensitive and selective for the simultaneous determination of enalapril–lercanidipine and enalapril–nitrendipine binary mixtures in their pharmaceutical dosage forms. The analyte peaks were detected using the LC method with the mobile phase ratio of methanol: water (70:30 v/v, pH 3.0) and a 1.0 mL min−1 flow rate. The detection wavelength was selected at 210 nm using photo diode array detector and column temperature was optimized to 30 °C. Linearity was obtained at different concentration ranges for all working pharmaceutically active compounds between 0.5 and 25 μg mL−1. The proposed methods were extensively validated according to USP 27 requirements and ICH guidelines. The methods were applied to the analysis of pharmaceutical dosage forms containing binary mixtures of enalapril–lercanidipine and enalapril–nitrendipine. Moreover, the proposed methods were applied for the degradation studies of the selected compounds. Degradation studies were conducted using stress conditions such as UV light, acidic and alkaline hydrolysis, oxidation and heat in oven, to evaluate the ability of the separation of the response of standard compounds from their degradation products.

  相似文献   
85.
We have obtained dihydrofurans 3aj in the radical cyclization of 4‐hydroxycoumarin 1a and 2‐hydroxy‐1,4‐naphtoquinone 1b with electron rich alkenes 2ai by manganese(III) acetate. Methods A and B, which have different molar ratios were studied comparatively in these reactions, and we observed that method B (molar ratio 2:1:3) gave the best results. Treatment of 4‐hydroxycoumarin 1a and electron rich alkenes 2ae gave 2,3‐dihydro‐4H‐furo[3,2‐c]chromen‐4‐ones 3ae in 36–86% yields by the method B. Under the same conditions, the reactions of 2‐hydroxy‐1,4‐naphtaquinone 1b with conjugated alkenes 2b and 2fi afforded 2,3‐dihydronaphtho[2,3‐b]furan‐4,9‐diones 3fj in an excellent yields.  相似文献   
86.
A series of β-amino alcohols derivatives were synthesized from (R)-2-amino-1-butanol and (S)-1,2-propanediol, and they have been used as organocatalaysts in the racemic ring opening of epoxide in good yields with high enantiomeric excess (up to 97%).  相似文献   
87.
88.
In this study, the solid-state reaction mechanism and kinetics were investigated for production of anhydrous sodium metaborate (NaBO2), an industrially and technologically important boron compound. To assess the kinetics of solid-state production of NaBO2, the chemical reaction between borax (Na2B4O7) and sodium hydroxide (NaOH) was investigated by use of the thermal analysis techniques thermogravimetry (TG) and differential thermal analysis (DTA). DTA curves obtained under non-isothermal conditions at different heating rates (5, 10 and 20 °C/min), revealed five endothermic peaks corresponding to five solid-state reactions occurring at 70, 130, 295, 463, and 595 °C. The stages of the solid-state reaction used for production NaBO2 were also analyzed by XRD, which showed that at 70 and 130 °C, Na2B4O7 and NaOH particles contacted between the grains, and diffusion was initiated at the interface. However, there was not yet any observable formation of NaBO2. Formation of NaBO2 was initiated and sustained from 295 to 463 °C, and then completed at 595 °C; the product was anhydrous NaBO2. Activation energies (E a) of the solid-state reactions were calculated from the weight loss based on the Arrhenius model; it was found that in the initial stages of the solid-state reaction E a values were lower than in the last three steps.  相似文献   
89.
Nano tetrapod based on conducting polythiophene (PTh) and tin-phosphate (SnP) were synthesized by in situ chemical oxidative polymerization. The morphology of the resulting polythiophene tinphosphate composite was characterized by elemental analysis, fourier transform infrared spectroscopy, thermogravimetric analysis, powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The physico-chemical characterization carried out on the composite showed that SnP was modified by conducting PTh with an enhancement of various properties. On the basis of highest distribution coefficient values for Hg(II), the composite was also used for the preparation of Hg(II) selective membrane electrode. The electrode showed working concentration range of 1 × 10?1 to 1 × 10?7 with Nernstian slope of 29.29 mV per decade change in concentration and the electrode may be used for wide working pH range of 4–8 having quick response time about 23 s. The life of electrode is 4 months without any notable drift in potential.  相似文献   
90.
Various types of crystalline cellulose consisting of group I (cell I, IIII, IVI) and group II (cell II, IIIII, IVII) prepared from cotton linter were adjusted for their degree of polymerization (DP) as starting materials. These celluloses were then treated by semi-flow hot-compressed water (HCW) at 230–270 °C/10 MPa/2–15 min to study their decomposition behaviors. The treatments performed resulted in residues of celluloses and water-soluble (WS) portions. Consequently, the crystallinity of the residues was found to remain the same, but the DP was reduced as the temperature increased. Additionally, X-ray diffractometry and Fourier transform-infrared analyses demonstrated that crystallographic changes occurred for residues of cell IIII, IVI and IIIII. Despite these changes, the overall results of the residues showed that group I has higher resistance to decomposing than group II. As for the WS portions, the yields of the hydrolyzed and degraded products were higher in group II than group I, indicating that group II is less resistant to decomposition by HCW treatment. Results for both the residues and WS portions are in agreement with each other, showing that the degree of difficulty of decomposition was higher in group I than group II. Therefore, the decomposition behaviors of the celluloses are due to differences in the crystalline forms.  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