全文获取类型
收费全文 | 3176篇 |
免费 | 454篇 |
国内免费 | 651篇 |
专业分类
化学 | 3538篇 |
晶体学 | 147篇 |
力学 | 21篇 |
综合类 | 32篇 |
数学 | 6篇 |
物理学 | 537篇 |
出版年
2024年 | 9篇 |
2023年 | 36篇 |
2022年 | 93篇 |
2021年 | 97篇 |
2020年 | 144篇 |
2019年 | 121篇 |
2018年 | 83篇 |
2017年 | 115篇 |
2016年 | 150篇 |
2015年 | 163篇 |
2014年 | 201篇 |
2013年 | 320篇 |
2012年 | 269篇 |
2011年 | 216篇 |
2010年 | 166篇 |
2009年 | 190篇 |
2008年 | 217篇 |
2007年 | 200篇 |
2006年 | 205篇 |
2005年 | 206篇 |
2004年 | 164篇 |
2003年 | 188篇 |
2002年 | 127篇 |
2001年 | 92篇 |
2000年 | 104篇 |
1999年 | 61篇 |
1998年 | 47篇 |
1997年 | 68篇 |
1996年 | 51篇 |
1995年 | 42篇 |
1994年 | 34篇 |
1993年 | 18篇 |
1992年 | 19篇 |
1991年 | 16篇 |
1990年 | 9篇 |
1989年 | 4篇 |
1988年 | 4篇 |
1987年 | 4篇 |
1986年 | 5篇 |
1985年 | 4篇 |
1984年 | 4篇 |
1983年 | 1篇 |
1982年 | 2篇 |
1981年 | 1篇 |
1980年 | 2篇 |
1979年 | 3篇 |
1978年 | 2篇 |
1976年 | 1篇 |
1975年 | 1篇 |
1972年 | 2篇 |
排序方式: 共有4281条查询结果,搜索用时 15 毫秒
171.
《Journal of separation science》2017,40(6):1403-1409
As a novel solid‐phase extraction material, zinc sulfide nanosheets were prepared by a simple method and were used to extract flavonoids. We used scanning electron microscopy to show its nanosheet morphology and energy dispersive X‐ray spectroscopy and powder X‐ray diffraction to confirm its chemical and phase compositions. Coupled to a high‐performance liquid chromatography, the zinc sulfide nanosheets were packed into a microcolumn and were used to extract four model flavonoids to examine their extraction ability. The parameters of sample loading and elution were investigated. Under optimized conditions, the analytical method for flavonoids was established. For the method, wide linearities from 1 to 250 μg/L and low limits of detection from 0.25 to 0.5 μg/L were obtained. The relative standard deviations for single column repeatability and column to column reproducibility were less than 7.7 and 10.4%, respectively. The established method was also used to analyze two real samples and the recoveries from 88.7 to 98.2% further proved the reliability of the method. Moreover, the zinc sulfide nanosheets have good stability and that in one column can be reused for more than 50 times. This work proves that the prepared zinc sulfide nanosheets are a good candidate as the flavonoids sorbent. 相似文献
172.
Shahla Mozaffari Marzieh Chaloosi Faten Divsar Ebrahim Abouzari-Lotf Samad T Bavili Ali Yousefi 《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):2439-2448
The complexation reactions between 7,10,13-triaza-1-thia-4,16-dioxa-20,24-dimethyl-2,3;17,18-dibenzo-cyclooctadecane-6,14-dione ( TTD ) and 7,10,13-triaza-1-sulfoxo-4,16-dioxa-20,24-dimethyl-2,3;17,18-dibenzo-cyclooctadecane-6,14-dione ( TSD ) macrocycles with Ag+, Cd2+, Cu2+, Pb2+, Sr2+, Tl+, and Zn2+ ions have been studied in ethanol and methanol solutions at 25°C. The complexes formed between macrocycles ( TTD ) and ( TSD ) with these metals cations had a stiochiometry of 1:1 and 1:2, respectively. The stability constants of the resulting complexes were determined and found to decrease in the order Cu2+ > Zn2+ > Ag+ > Tl+ > Cd2+ > Pb2+ > Sr2+ with macrocycle ( TTD ) and Tl+ > Zn2+ > Cd2+ > Pb2+ > Cu2+ > Ag+ > Sr2+ with macrocycle ( TSD ). 相似文献
173.
S. Gunesdogdu Sagdinc F. Kandemirli B. Köksoy S. Haman Bayari 《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):1243-1260
Abstract Zn(II) and Ni(II) complexes of 5-fluoroisatin-3-[-(N-cyclohexylthiosemicarbazone)] (H2FIC) have been prepared and characterized structurally by means of elemental analyses, FTIR, electronic, and 1H NMR spectra. The theoretical wavenumbers, IR intensities, and molecular parameters have been calculated by the ab-initio Hartree–Fock (HF) method with the LanL2DZ basis set. The theoretical wavenumbers show a good agreement with experimental data. The bond lengths, bond angles, the highest occupied molecular orbital energy (EHOMO), the lowest unoccupied molecular orbital energy (ELUMO), the energy gap between EHOMO and ELUMO (ΔEHOMO-LUMO), dipole moment, and charges on the atoms of H2FIC as monomer form were studied by the density functional theory/Becke-3-Lee-Yang-Parr (DFT/B3LYP) and ab-initio HF methods using 6-31G(d,p) basis set. The trimeric possible structure of H2FIC was also investigated using HF method. The observed IR wavenumbers of the H2FIC were analyzed in the light of the computed vibrational spectra of its monomer and trimer forms. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
174.
Le Wang Yong Ye Zhiyu Ju Shangbin Zhong Yufen Zhao 《Phosphorus, sulfur, and silicon and the related elements》2013,188(8):1958-1963
A modified method for preparing large-scale quantities of pure hexachlorocyclophosphazene (N3P3Cl6) and octachlorocyclotetraphosphazene (N4P4Cl8), phosphorus pentachloride with ammonium chloride, in the presence of zinc chloride, has been developed. The time of the reaction and the quantities of the catalyst are also studied. It is found that the optimum reaction time is 1.5 h and by-products are remarkably reduced by addition of 10% zinc chloride. As indicated by the 31 P NMR spectra, the synthesis and separation of cyclophosphazenes can be accomplished in moderate yield of tetramer (39%) and good yield of trimer (83%). 相似文献
175.
Maryam Zarei 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):865-870
AbstractNovel derivatives of diethyl (4-oxo-2-phenylchroman-3-yl) methyl phosphonate have been synthesized under optimal conditions using domino-Knoevenagel-phospha-Michael reaction catalyzed by nano-zinc oxide. The combination of recovery and reusability of catalyst, simple and applicable approach, good reaction time and good yields of products make this method as a suitable route for this purpose. The structures of the products were determined by FT-IR, 1H-, 13C- and 31P- Nuclear Magnetic Resonance spectroscopies, and elemental analysis. 相似文献
176.
Marie-Luise Lechner Roland Fischer Frank Uhlig 《Phosphorus, sulfur, and silicon and the related elements》2013,188(6):1341-1345
Abstract The reaction of dialkyltinhydrides with dialkylzinc results in a tin metal bond formation. Crystal structures of 1,1,1,2,3,3,3-hepta-phenyl-2-(ethylzincio)tristannane *TMEDA 1, 1,1,2,2,3,3,4,4-octaphenyl-1,4-(ethylzincio)tetrastannane*2TMEDA 2, and triphenyl(phenylzincio)stannane*TMEDA 3 could be obtained. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. GRAPHICAL ABSTRACT 相似文献
177.
Mojtaba Abbasian Nafiseh Khakpour Aali Solmaz Esmaeily Shoja 《高分子科学杂志,A辑:纯化学与应用化学》2013,50(9):966-975
A method to prepare zinc oxide (ZnO) nanoparticles with a covalently bonded poly(methyl methacrylate) (PMMA) shell by surface initiated atom transfer radical polymerization (ATRP) was reported. First, the initiator for ATRP was covalently bonded onto the surface of zinc oxide nanoparticles through our novel method. Firstly, the surface of ZnO nanoparticle was treated with 3-aminopropyl triethoxysilane, a silane coupling agent, and then this functionalization nanoparticle was reacted with α-chloro phenyl acetyl chloride to prepare atom transfer radical polymerization macroinitiator. The metal-catalyzed radical polymerization of MMA with ZnOmacroinitiator was performed using a copper catalyst system to give the ZnO-based nanoparticles hybrids linking PMMA segments (poly (methyl methacrylate)/zinc oxide nanocomposite). These hybrid nanoparticles had an exceptionally good dispersability in organic solvents and were subjected to detailed characterization using FTIR, TEM and TGA and DSC analyzed. 相似文献
178.
The photophysical and photochemical properties of tetraaminophthalocyanine complexes of lutetium and zinc covalently linked to polyacrylic acid were studied alongside those of unsubstituted zinc phthalocyanine within the same polymeric fiber matrix. All three phthalocyanines within the solid fiber matrices showed photoactivity by the generation of singlet oxygen as was observed in solution. The fluorescence behaviors of the composite fibers equally parallel those in solution. For the unsubstituted zinc phthalocyanine composite, the fiber showed fluorescence quenching on interaction with gaseous nitrogen dioxide similar to that in DMF and, thus could be a promising nanofabric material in developing optoelectronic devices that are responsive to the gas. 相似文献
179.
A new anti‐static agent was synthesized from zinc oxide‐adipic acid‐polyethylene glycol and caprolactam by three‐step reactions. The antistatic agent (called poly(ether ester amide zinc oxide) or PEEAZ) was analyzed by IR and DSC. The results showed that zinc oxide existed in the main chain of PEEAZ. The glass temperature and melt temperature of poly(ether ester amide zinc oxide) (referred to as PEEAZ in the following) decreased with increasing poly(ether ester zinc oxide) increasing in PEEAZ. Antistatic PA6 fiber was obtained by adding PEEAZ 2–8% (wt/wt) to PA6 during blend spinning. The specific resistance and the static half‐value period of PA6 fiber was less than 109Ω · cm and 60 sec, respectively. Excellent antistatic property remained after being washed 30 times. 相似文献