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951.
Xi-Dan Han Xian-Li Tian Wen-Hao Yu Shi-Kai Xiang Ping Hu Bi-Qin Wang 《Liquid crystals》2017,44(11):1727-1738
A comparative study of our established synthetic approaches to hexasubsituted triphenylenes 2,3-dicarboxylic esters containing four identical β-alkoxy and two adjacent β-alkoxycarbonyl side chains shows that the phase behaviours of small-sized discotic liquid crystals can be tailored over a wide range by simply varying the length of the peripheral alkyl chains. All the prepared esters in two series were observed to form a single hexagonal columnar phase, except for Tp4-1 having four β-butyloxy and two adjacent β-methoxycarbonyl chains which displays two columnar mesophase behaviours with a transition from the columnar plastic phase to hexagonal columnar phase. A significant difference between the two mesophase was observed in the variable temperature X-ray diffraction studies, and the mesophase assignment was also confirmed by polarising optical microscopy and differential scanning calorimetry. Moreover, the prepared esters in each series display the general trend of decreasing clearing temperature upon increasing alkoxy or alkoxycarbonyl chains length. The intermediate triphenylene 2,3-dicarboxylic acids were also found not only to exhibit columnar hexagonal mesophase over a narrower temperature range by maintaining high melting and clearing points but also to form organogel on mixing with toluene or dichloromethane with the assistance of hydrogen bonding. 相似文献
952.
Five saturated α-branched fatty acids, also known as Guerbet acids, including α-propylhexyl acid (G 1 ), α-butylhexyl acid (G 2 ), α-propyloctyl acid (G 3 ), α-butyloctyl acid (G 4 ), and α-hexyloctyl acid (G 5 ), were synthesized in high yields by four-step reaction. Colorless, almost odorless, and oily products were obtained with high purity, whose structures were confirmed by GC, 1H/13C NMR, and ESI–MS characterization. G 1 , G 3 , and G 4 had pour points lower than ?60 °C, while G 2 and G 5 showed higher pour points (?42 °C and 6 °C, respectively) because of their molecular symmetry. Considering the low-temperature properties, G 1 , G 3 , G 4 , and even G 2 held great potential applications in the lubricant and oilfield. 相似文献
953.
A sensitive and accurate LC method was developed and further validated for the determination of enantiomeric purity of GSK962040. Before separation, a pre-column derivatization procedure was performed. Baseline separation with a resolution higher than 1.9 was accomplished within 15 min using a Chiralpak AD-H (250 × 4.6 mm; particle size 5 μm) column, with n-hexane: 2-propanol (85:15 v/v) as mobile phase at a flow rate of 1 mL min?1. The eluted analytes were subsequently detected with a UV detector at 260 nm. The effects of mobile phase components and temperature on enantiomeric selectivity as well as resolution of enantiomers were thoroughly investigated. The calibration curves were plotted within the concentration range between 4 and 200 μg mL?1 (n = 8), and recoveries between 98.15 and 101.48% were obtained, with relative standard deviation (RSD) lower than 1.42%. The LOD and LOQ for the Boc-GSK962040 were 1.23 and 4.15 μg mL?1 and for its enantiomer were 1.38 and 4.76 μg mL?1, respectively. The developed method was also evaluated and validated by analyzing bulk samples with different enantiomeric ratios of GSK962040. It was demonstrated that the method was accurate, robust and sensitive, and also had practical utilities for real analysis. 相似文献
954.
Catalytic Asymmetric Functionalization of Aromatic CH Bonds by Electrophilic Trapping of Metal‐Carbene‐Induced Zwitterionic Intermediates 下载免费PDF全文
Shikun Jia Dr. Dong Xing Dan Zhang Prof. Dr. Wenhao Hu 《Angewandte Chemie (International ed. in English)》2014,53(48):13098-13101
Asymmetric functionalization of aromatic C? H bonds of N,N‐disubstituted anilines with diazo compounds and imines is reported for the efficient construction of α,α‐diaryl benzylic quaternary stereocenters in good yields with high diastereoselectivities and excellent enantioselectivities. This RhII/chiral phosphoric acid cocatalyzed transformation is proposed to proceed through a metal‐carbene‐induced zwitterionic intermediate which undergoes electrophilic trapping. To the best of our knowledge, this is the first asymmetric example of metal carbene‐induced intermolecular functionalization of aryl C? H bonds. 相似文献
955.
An Ylide Transformation of Rhodium(I) Carbene: Enantioselective Three‐Component Reaction through Trapping of Rhodium(I)‐Associated Ammonium Ylides by β‐Nitroacrylates 下载免费PDF全文
Xiaochu Ma Dr. Jun Jiang Siying Lv Wenfeng Yao Yang Yang Dr. Shunying Liu Dr. Fei Xia Prof. Dr. Wenhao Hu 《Angewandte Chemie (International ed. in English)》2014,53(48):13136-13139
The chiral RhI–diene‐catalyzed asymmetric three‐component reaction of aryldiazoacetates, aromatic amines, and β‐nitroacrylates was achieved to obtain γ‐nitro‐α‐amino‐succinates in good yields and with high diastereo‐ and enantioselectivity. This reaction is proposed to proceed through the enantioselective trapping of RhI‐associated ammonium ylides by nitroacrylates. This new transformation represents the first example of RhI‐carbene‐induced ylide transformation. 相似文献
956.
The structural properties, phase stability, electronic structure, elastic properties, and optical properties of Ca5(PO3)4F (FA), Ca5(PO3)4Cl (ClA) and Ca5(PO3)4Br (BrA) are studied by DFT calculations with the generalized gradient approximation. 相似文献
957.
High resolution capillary electrophoresis of carbon nanotubes 总被引:2,自引:0,他引:2
Doorn SK Fields RE Hu H Hamon MA Haddon RC Selegue JP Majidi V 《Journal of the American Chemical Society》2002,124(12):3169-3174
Purification of single-walled carbon nanotubes by capillary electrophoresis (CE) is demonstrated. Real-time Raman spectroscopy of the separation process and single-wavelength UV/vis detection show the ability of CE to provide high-resolution separations of nanotube fractions with baseline separation. AFM images of collected fractions demonstrate that separations are based on tube length. The separation method is suggested to be based on alignment of the nanotubes along the separation field. 相似文献
958.
An amperometric sensor for the determination of indole-3-acetic acid (IAA) based on the CeCl3-DHP film modified gold electrode was developed. CeCl3 was dissolved into water in the presence of dihexadecyl hydrogen phosphate (DHP). The IAA sensor was prepared via evaporating
solvent of the CeCl3-DHP dispersion on the gold electrode surface. The amperometric response of IAA on the CeCl3-DHP film modified gold electrode was investigated. The experimental results indicate that the passivation of the electrode
due to the adsorption of the oxidation product of IAA decreases significantly at the CeCl3-DHP film modified gold electrode, in contrast to that at the bare and the DHP modified gold electrode. The experimental parameters
were optimized and an electrochemical method for the determination of IAA was established. The oxidation peak current is linearly
with the concentration of IAA from 1 × 10−7 to 2 × 10−5 mol l−1 and the detection limit is 3 × 10−8 mol l−1. The relative standard deviation of eight measurements is 3.2% for 5 × 10−7 mol l−1 IAA. The IAA in plant leaves were extracted and determined by the IAA sensor. 相似文献
959.
Comparison and characterization of polysaccharides from natural and cultured Cordyceps on the basis of their chemical characteristics such as glycosidic linkages were performed for the first time using saccharide
mapping. The results showed that polysaccharides from most of the natural and cultured Cordyceps had similar responses to enzymatic digestion. These polysaccharides mainly contained (1→4)-β-D-glucosidic linkages, and (1→4)-α-glucosidic, (1→6)-α-glucosidic, 1,4-β-D-mannosidic, as well as (1→4)-α-D-galactosiduronic linkages also existed in some polysaccharides. Especially, natural and cultured Cordyceps polysaccharides could be discriminated on the basis of high performance liquid chromatography profiles of pectinase hydrolysates,
which is helpful to control the quality of polysaccharides from Cordyceps. 相似文献
960.