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991.
992.
对高效镇痛药盐酸二氢埃托啡的衍生化条件、色谱及质谱行为进行了研究。通过对不同衍生化试剂、衍生化反应温度、反应时间等条件的优化,选择七氟丁酰咪唑与二氢埃托啡在室温反应5min,即可生成较完全的单取代七氟丁酰衍生物。该衍生物具有较好的气相色谱和电子轰击质谱行为。其单取代分子离子的质量数为m/z609,基峰离子为m/z522,主要碎片离子分别为m/z508、534和576,并对这些离子的产生进行了解析。这些离子均有较强的相对丰度,可作为微量二氢埃托啡的多离子选择定性。而基峰离子m/z522作为其特征离子,可用于微量二氢埃托啡的单离子选择定量。最低检测限为1pg。 相似文献
993.
采用体积排斥色谱法/ 示差折光指数/ 直角激光光散射/ 示差粘度三检测联用技术表征了氘化聚苯乙烯、聚苯乙烯和氘化聚苯乙烯- 聚异戊二烯。结果表明,在θ条件下,虽然氘化聚苯乙烯的化学依赖性常数υT,DPS比聚苯乙烯的化学依赖性常数υT,PS大,但25 ℃时在四氢呋喃中,氘化聚苯乙烯的分子尺寸仍小于聚苯乙烯的分子尺寸。由于嵌段共聚物的淋洗体积随组成变化,所以用传统的SEC/RI得不到准确的分子量。经比较膜渗透、小角激光光散射和基质辅助激光脱吸与离子化时间飞行质谱等的实验结果,证明体积排斥色谱法/ 示差折光指数/ 直角激光光散射/ 示差粘度三检测技术能准确地得到氘化二嵌段共聚物的分子量以及其它重要信息。 相似文献
994.
不含金属的碳材料通过廉价且易获得的柚子皮经KOH活化和高温热解获得,该碳材料具有高比表面积(1 055 m~2·g~(-1))和高石墨化程度的类蜂窝状结构。将多孔碳(PAC)材料修饰后的电极作为工作电极,采用阳极溶出伏安法(SWASV)同步检测Cd~(2+)、Pb~(2+)和Cu~(2+)离子,表现出较高的灵敏度、可重复性、稳定性和较低的检测限。研究认为PAC的微孔和中孔可以充当有效的离子传递通道,从而加速离子的扩散并显著提高交换效率,而高的石墨化程度提高了材料的导电性,加速了电子传输。 相似文献
995.
The molecular species of phosphatidylcholine from freshwater sources (Macrobranchium nipponense and Macrobranchium rosenbergii) and marine sources (Euphausia superba and Penaeus chinesis) were characterized by high-resolution mass spectrometry. The tandem secondary mass spectrometry (MS/MS) fragmentation allowed for the identification of fatty acyl residues of phosphatidylcholine molecular species. (16:0–18:1)Phosphatidylcholine was the main phosphatidylcholine molecular species determined in all shrimp samples, especially in E. superba. Macrobranchium rosenbergii phosphatidylcholine was particularly rich in (16:0–20:5)phosphatidylcholine and (16:0–22:6)phosphatidylcholine. The proportion of the two molecular species was next to the phosphatidylcholine of E. superba. Therefore, M. rosenbergii appears to be a potential freshwater source for the supplementation of polyunsaturated fatty acids, particularly eicosapentaenoic acid (20:5) and docosahexaenoic acid (22:6). This approach may be used as an efficient method for the identification of natural phosphatidylcholine sources from the broad range of plant, animal, and marine origins. 相似文献
996.
以5-氨基-1H-1,2,4-三唑-3-羧酸(HAtca)为配体,通过水热法和溶液扩散法分别合成了2个新的配合物[Zn(Athy) Br]n(1,HAthy=5-氨基-1H-1,2,4-三唑-3-醇)和[Mn(Atca)2(H2O)2](2)。单晶结构分析表明配合物1和2分别属于正交和单斜晶系,结晶于Pbca和P21/c空间群。配合物1为2D层状结构,2是单核配合物。在配合物1中不存在氢键,而配合物2中含有丰富的氢键作用,并且通过氢键的作用形成了一个三维的网格结构。同时在固态下,配合物1和2分别在360、462 nm和382、402 nm处有较强的荧光发射峰。 相似文献
997.
以K2PdCl4/K2Ni(CN)4为前驱体制备了具有凝胶特性的氰胶(Cyanogels), 利用硼氢化钠还原氰胶得到三维多孔珊瑚状PdNi合金前驱体, 在此基础上通过原位Galvanic置换反应, 制备得到内核为PdNi合金、 表面具有不同厚度Au层的三维多孔PdNi@Au催化剂. X射线衍射(XRD)分析和透射电子显微镜(TEM)观测结果显示, 该三维网状结构由粒径约7 nm的纳米颗粒相互连接形成; 能量分散光谱(EDX)线性扫描和元素分布(Mapping)分析显示该催化剂具有典型的核壳结构. 电化学测试结果表明, 表面Au层的厚度影响PdNi@Au催化剂的性能, 当Au的含量(摩尔分数)为5.6%时, 催化剂显示出对甲酸最佳的电催化活性, 对甲酸电催化氧化的峰电流密度达到商业化铂黑催化剂的7.2倍. 相似文献
998.
Intumescent flame retardant (IFR) has received the considerable attention ascribed to the inherent advantages including non‐halogen, low toxicity, low smoke release and environmentally friendly. In this work, a novel charring agent poly (piperazine phenylaminophosphamide) named as PPTA was successfully synthesized and characterized by Fourier transform infrared spectra (FTIR) and X‐ray photoelectron spectroscopy (XPS). Then, a series of flame‐retardant EP samples were prepared by blending with ammonium polyphosphate (APP) and PPTA. Combustion tests include oxygen Index (LOI), vertical Burning Test (UL‐94) and cone calorimeter testing,these test results showed that PPTA greatly enhances the flame retardancy of EP/APP. According to detailed results, EP containing 10 wt% APP had a LOI value of 30.2%,but had no enhancement on UL‐94 rating. However, after both 7.5 wt% APP and 2.5 wt% PPTA were added, EP‐7 passed UL‐94 V‐0 rating with a LOI value of 33.0%. Moreover, the peak heat release rate (PHRR) and peak of smoke product rate (PSPR) of EP‐7 were greatly decreased. Meanwhile, the flame‐retardant mechanism of EP‐7 was investigated by scanning electron microscopy (SEM), thermogravimetric analysis/infrared spectrometry (TG‐IR) and X‐ray photoelectron spectroscopy (XPS). The corresponding results presented PPTA significantly increased the density of char layer, resulting in the good flame retardancy. 相似文献
999.
Yongjie Zhang Xiaopei Li Wenqin Zhu Mingshuai Fan Shuwei Wang Minjie Qu Yi Zhang Shuai Wang 《先进技术聚合物》2020,31(7):1602-1611
Polysiloxane/polyolefin copolymers have drawn much attention recently and emerged as a new group of functional polyolefin since they possess distinctive properties and find great potential applications in many areas (eg, compatibilizer, processing aid and surface modifier). However, traditional routes to synthesize polysiloxane/polyolefin copolymers generally require multi‐step labor‐consuming procedures. Herein, we report a novel one‐step synthesis of polydimethylsiloxane graft polyethylene (PDMS‐g‐PE) mimics. It was found that PDMS‐g‐PE mimics, namely vinylmethylsiloxane‐dimethylsiloxane‐(C30‐45 alkyl)methylsiloxane copolymers (short for VD‐AMS), could be formed via a one‐step synthetic procedure based on the siloxane equilibrium process between silanol‐terminated vinylmethylsiloxane‐methylsiloxane copolymer and (C30‐45 alkyl)methylsilicone. The chemical structures of VD‐AMS were characterized unambiguously using Fourier transform infrared spectroscopy, nuclear magnetic resonance, gel permeation chromatography, differential scanning calorimetry. The correlation between reaction conditions and the structural parameters of VD‐AMS was established. Based on our experimental results, a plausible mechanism for the synthesis of VD‐AMS was proposed. Scanning electron microscopy micrographs showed that VD‐AMS could function as an efficient compatibilizer for immiscible PE/silicone blend. Given that the precursors of VD‐AMS are commercially available with low prices and that VD‐AMS can be easily synthesized under mild conditions, we believe VD‐AMS can represent as a competitive potential compatibilizer due to its relatively low cost. 相似文献
1000.
Heng Yi Pengfei Hu Scott A. Snyder 《Angewandte Chemie (International ed. in English)》2020,59(7):2674-2678
Pd‐catalyzed sequences involving oxidative addition, cyclization, and termination through intermolecular nucleophile capture have tremendous utility. Indeed, they can generate a plethora of different polycyclic structures possessing a diverse range of functionality. However, one area of deficiency for Pd0/PdII variants is the ability to conclude them with oxygen‐based species. Inspired by the recent discovery of one such reaction in the course of a total synthesis program, we delineate herein that it has significant strength, both in terms of substrate scope as well as the terminating oxygen nucleophile. As a result, the reaction proved critical in achieving total syntheses of two oxygenated natural products, one of which was prone to over‐oxidation. Finally, a mechanistic proposal that accounts for its success is provided. 相似文献