全文获取类型
收费全文 | 25870篇 |
免费 | 3948篇 |
国内免费 | 2411篇 |
专业分类
化学 | 17974篇 |
晶体学 | 309篇 |
力学 | 1538篇 |
综合类 | 112篇 |
数学 | 2946篇 |
物理学 | 9350篇 |
出版年
2024年 | 70篇 |
2023年 | 526篇 |
2022年 | 949篇 |
2021年 | 963篇 |
2020年 | 1008篇 |
2019年 | 996篇 |
2018年 | 828篇 |
2017年 | 728篇 |
2016年 | 1204篇 |
2015年 | 1152篇 |
2014年 | 1346篇 |
2013年 | 1791篇 |
2012年 | 2402篇 |
2011年 | 2413篇 |
2010年 | 1578篇 |
2009年 | 1502篇 |
2008年 | 1646篇 |
2007年 | 1512篇 |
2006年 | 1362篇 |
2005年 | 1159篇 |
2004年 | 843篇 |
2003年 | 652篇 |
2002年 | 610篇 |
2001年 | 445篇 |
2000年 | 438篇 |
1999年 | 523篇 |
1998年 | 429篇 |
1997年 | 440篇 |
1996年 | 455篇 |
1995年 | 370篇 |
1994年 | 307篇 |
1993年 | 238篇 |
1992年 | 235篇 |
1991年 | 199篇 |
1990年 | 172篇 |
1989年 | 145篇 |
1988年 | 97篇 |
1987年 | 109篇 |
1986年 | 87篇 |
1985年 | 86篇 |
1984年 | 48篇 |
1983年 | 43篇 |
1982年 | 35篇 |
1981年 | 18篇 |
1980年 | 11篇 |
1979年 | 10篇 |
1978年 | 6篇 |
1976年 | 9篇 |
1975年 | 11篇 |
1957年 | 4篇 |
排序方式: 共有10000条查询结果,搜索用时 9 毫秒
951.
952.
Several hyperbranched polyimides (HBPIs) were applied in liquid crystal (LC) alignment layers and exhibited outstanding performance for LC alignment. The maximum pretilt angle was above 8°, and the minimum pretilt angle was 4.2°. The results of atomic force microscope measurement disclosed that a lot of grooves were aligned parallel to the rubbing direction and found that the grooves were not main factor for LC alignment. The LC alignment and pretilt angles are unambiguously associated with the intrinsic HBPI chemical structures. The results of thermal gravimetric analysis and ultraviolet–visible spectra showed that the HBPIs had good thermal stability and excellent transmittance. T5 and T10 were higher than 360°C and 400°C, respectively. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
953.
Eun‐Ju Ha Bong‐Soo Kim Eun‐Kyoung Park Ki‐Won Song Sun‐Gu Lee Seong Soo A. An Hyun‐jong Paik 《先进技术聚合物》2013,24(1):75-80
Ni2+‐complexed poly(2‐acetamidoacrylic acid) (PAAA) hydrogel beads were developed for the site‐specific reversible immobilization and purification of the histidine‐tagged green fluorescent protein (His‐tagged GFP). PAAA hydrogel beads were prepared by photopolymerization, and significantly improved mechanical properties of PAAA hydrogel beads were observed in comparison with PAAA hydrogel from our previous study. Confocal laser scanning microscopy was used to determine the binding of His‐tagged GFP to the hydrogel beads in three‐dimensional space. Photoluminescence spectroscopy revealed 89% of binding efficiency of His‐tagged GFP to the Ni2+‐PAAA hydrogel beads, 51% of yielding recovery. The maximum binding capacity of His‐tagged GFP was estimated to be 0.45 µg/mg of Ni2+‐PAAA hydrogel beads. The recombinant His‐tagged GFP from the soluble fraction of E. coli BL21(DE3) cell lysates was purified with Ni2+‐PAAA hydrogel beads. The major advantage of the Ni2+‐PAAA hydrogel beads system was simple preparation procedures of producing the matrix, because PAAA hydrogel beads had relatively enhanced mechanical strength than soft hydrogels. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
954.
The reaction of halogenated 9H-carbazoles or carbazole with bromoesters in DMF under microwave irradiation readily affords a series of 9H-carbazoles-9-hydroxylic acids. 相似文献
955.
Meng Sun Xiaoxing Ma Juntao Wang Weina Wang Qiuhua Wu Chun Wang Zhi Wang 《Journal of separation science》2013,36(8):1478-1485
In this paper, a novel graphene (G) grafted silica‐coated Fe3O4 nanocomposite was fabricated by the chemical bonding of G onto the surface of silica‐coated Fe3O4 nanoparticles. Some carbamates (metolcarb, carbaryl, pirimicarb, and diethofencarb) in cucumber and pear samples were enriched by this nanocomposite prior to their determination by HPLC with UV detection. Experimental parameters that may affect the extraction efficiency were investigated. Under the optimum conditions, a linear response was achieved in the concentration range of 0.5–100.0 ng/g for metolcarb, carbaryl, and diethofencarb, and 1.0–100 ng/g for pirimicarb with the correlation coefficients (r) ranging from 0.9956 to 0.9984. The LOD (S/N = 3) of the method were found to be in the range from 0.08 to 0.2 ng/g. The RSDs were in the range from 2.4 to 5.8%. The results indicated that the G grafted silica‐coated Fe3O4 nanocomposite was stable and efficient for magnetic SPE and has a great application potential for the preconcentration of other organic pollutants from real samples. 相似文献
956.
Yang Sun Xiaoqing Wang Yilei Huang Zaifa Pan Lili Wang 《Journal of separation science》2013,36(14):2268-2276
Derivatization at the injection port following hollow‐fiber‐based liquid–liquid–liquid microextraction with tetramethylammonium acetate as a dual‐function reagent, i.e. an acceptor and derivatization reagent, for the determination of benzoic acid (BA) and sorbic acid (SA) in real samples by GC was developed. BA and SA were extracted from aqueous samples to an organic phase impregnated into the pores of the hollow fiber wall, and then back‐extracted to the acceptor solution located inside the lumen of the hollow fiber. Upon injection, the extracted analytes were quantitatively derivatized to their methyl esters with tetramethylammonium acetate in the GC injection port. Several parameters related to the derivatization and extraction efficiency were optimized. The linearity was satisfactory over a concentration range of 0.1–50 mg/L with r > 0.993 for both analytes. The LODs were 2.0 μg/L for SA and 20 μg/L for BA. The recoveries (83–116%) and precisions (RSDs of 1.2–11.4% (n = 3)) were examined by analyzing real spiked samples. The enrichment factors of BA and SA were 300 and 425. The results demonstrated that this is a simple, rapid, accurate, and sensitive method for the determination of BA and SA in various samples. 相似文献
957.
Zhixiong Shi Yifei Wang Piye Niu Jiandi Wang Zhiwei Sun Shuhua Zhang Yongning Wu 《Journal of separation science》2013,36(20):3402-3410
A method has been developed and validated for the concurrent extraction, clean‐up, and analysis of polybrominated diphenyl ethers (PBDEs), α‐, β‐, and γ‐hexabromocyclododecane (HBCD), and tetrabromobisphenol A (TBBPA) in human milk and serum. Milk and serum samples were extracted using accelerated solvent extraction with acetone/hexane 1:1, v/v and liquid–liquid extraction with methyl‐tert‐butyl ether/hexane 1:1, v/v, respectively. The removal of co‐extracted biogenic materials was achieved by gel permeation chromatography followed by sulfuric acid treatment. The fractionation of the PBDEs and HBCD/TBBPA was performed using a Supelco LC‐Si SPE cartridge. The detection of the PBDEs was then performed by GC–MS and that of the HBCDs and the TBBPA was performed using UPLC–MS/MS. The pretreatment procedure was optimized, and the characteristic ions and fragmentation of the analytes were studied by MS or MS/MS. A recovery test was performed using a matrix spiking test at concentrations of 0.05–10 ng/g. The recoveries ranged from 78.6–108.8% with RSDs equal to or lower than 14.04%. The LODs were 1.8–60 pg/g. The usefulness of the developed method was tested by the analysis of real human samples, and several brominated flame retardants in different samples were detected and analyzed. 相似文献
958.
Ping Wang Hai tao Lv Ai hua Zhang Hui Sun Guang li Yan Ying Han Xiu hong Wu Xi jun Wang 《Journal of separation science》2013,36(21-22):3511-3516
959.
A facile and efficient synthetic method of esters from their corresponding carboxylic acids and amino acids is described. The esterification reaction of carboxylic acids and amino acids could be greatly accelerated under microwave irradiation because the reactions described in this article took place in only 5 min with almost quantitative yields, and distinct acidity of catalytic acids was well tolerated. Unlike the racemation problem in microwave-assisted N-acylation reactions, the esters of chiral amino acids could be achieved with retention of configuration under this condition. 相似文献
960.
A green and efficient method for the synthesis of 2,4,5-triarylimidazoles by one-step condensation reaction of benzil, aromatic aldehyde, and ammonium acetate under catalyst-free, solvent-free, and microwave-irradiation conditions is reported. This method had many dramatic advantages, such as the short reaction time (3–5 min), good yields (80–99%), environmental friendliness, and convenient operation. 相似文献