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101.
自然界中砷和砷的化合物一般可通过水、大气和食物等途径进入人体,危害人体健康,原子荧光光谱法测定砷含量被广泛应用。为准确测定样品中砷的含量,以原子荧光光谱法(AFS)测定土壤中总砷含量为例,重点研究高价态砷(Ⅴ)还原为低价态砷(Ⅲ)的实验条件,采用正交实验进行条件优化,建立适合的实验方法。通过设计L9(34)正交实验,高价态砷的还原反应与四个因素有关,即与反应温度、反应时间、盐酸加入量和硫脲的用量呈一定的正相关,结果表明,四个因素中硫脲用量的影响最为显著,其次是盐酸加入量、反应时间和反应温度。通过对四个因素的多水平检验,优化后的实验条件为:硫脲用量2.0 mL、盐酸加入量10%、反应时间20 min、温度20~35 ℃(即普通室温)。采用土壤标准物质验证优化后条件的可行性,得出砷的测定值在标准值范围内,RSD在2.2%~4.2%,精密度和准确性均满足质控要求。优化后的实验条件使得操作简便易行,提高了工作效率。 相似文献
102.
103.
Mezna Saleh Altowyan Saied M. Soliman Matti Haukka Nora Hamad Al-Shaalan Aminah A. Alkharboush Assem Barakat 《Molecules (Basel, Switzerland)》2022,27(13)
In the present work, a novel heterocyclic hybrid of a spirooxindole system was synthesized via the attachment of ferrocene and triazole motifs into an azomethine ylide by [3 + 2] cycloaddition reaction protocol. The X-ray structure of the heterocyclic hybrid (1″R,2″S,3R)-2″-(1-(3-chloro-4-fluorophenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl)-5-methyl-1″-(ferrocin-2-yl)-1″,2″,5″,6″,7″,7a″-hexahydrospiro[indoline-3,3″-pyrrolizin]-2-one revealed very well the expected structure, by using different analytical tools (FTIR and NMR spectroscopy). It crystallized in the triclinic-crystal system and the P-1-space group. The unit cell parameters are a = 9.1442(2) Å, b = 12.0872(3) Å, c = 14.1223(4) Å, α = 102.1700(10)°, β = 97.4190(10)°, γ = 99.1600(10)°, and V = 1484.81(7) Å3. There are two molecules per unit cell and one formula unit per asymmetric unit. Hirshfeld analysis was used to study the molecular packing of the heterocyclic hybrid. H···H (50.8%), H···C (14.2%), Cl···H (8.9%), O···H (7.3%), and N···H (5.1%) are the most dominant intermolecular contacts in the crystal structure. O···H, N···H, H···C, F···H, F···C, and O···O are the only contacts that have the characteristic features of short and significant interactions. AIM study indicated predominant covalent characters for the Fe–C interactions. Also, the electron density (ρ(r)) at the bond critical point correlated inversely with the Fe–C distances. 相似文献
104.
一步法直接合成碳酸二甲酯催化剂 总被引:5,自引:0,他引:5
采用浸渍法以MgO、海泡石(Sep)。γ-Al2O3为载体,制备了一系列金属盐Lewis酸-无机碱双组分负载型催化剂,以环氧丙烷(PO)一步合成碳酸二甲酯(DMC)反应为探针。考察了催化剂的不同载体活性组分和反应条件对合成DMC的产率及选择性的影响。结果表明,催化剂的活性次序为:NaOH—LiCl/MgO)NaOH—LiCl/Sep)NaOH—LiCl/γ-Al2O3;选择性的次序为:NaOH—LiCl/Sep)NaOH—LiCl/MgO)NaOH—LiCl/γ-Al2O3。NaOH—LiCl/SeP催化剂具有较高的活性和选择性;其最佳反应条件为:反应温度160℃。反应时间5h,甲醇与PO的量之比为1:1。在最佳条件下。PO转化率为82.6%,DMC的产率达到7.68%。 相似文献
105.
AbdElAziz A. Nayl Ashraf A. Aly Wael A. A. Arafa Ismail M. Ahmed Ahmed I. Abd-Elhamid Esmail M. El-Fakharany Mohamed A. Abdelgawad Hendawy N. Tawfeek Stefan Brse 《Molecules (Basel, Switzerland)》2022,27(12)
In this review, we focus on some interesting and recent examples of various applications of organic azides such as their intermolecular or intramolecular, under thermal, catalyzed, or noncatalyzed reaction conditions. The aforementioned reactions in the aim to prepare basic five-, six-, organometallic heterocyclic-membered systems and/or their fused analogs. This review article also provides a report on the developed methods describing the synthesis of various heterocycles from organic azides, especially those reported in recent papers (till 2020). At the outset, this review groups the synthetic methods of organic azides into different categories. Secondly, the review deals with the functionality of the azido group in chemical reactions. This is followed by a major section on the following: (1) the synthetic tools of various heterocycles from the corresponding organic azides by one-pot domino reaction; (2) the utility of the chosen catalysts in the chemoselectivity favoring C−H and C-N bonds; (3) one-pot procedures (i.e., Ugi four-component reaction); (4) nucleophilic addition, such as Aza-Michael addition; (5) cycloaddition reactions, such as [3+2] cycloaddition; (6) mixed addition/cyclization/oxygen; and (7) insertion reaction of C-H amination. The review also includes the synthetic procedures of fused heterocycles, such as quinazoline derivatives and organometal heterocycles (i.e., phosphorus-, boron- and aluminum-containing heterocycles). Due to many references that have dealt with the reactions of azides in heterocyclic synthesis (currently more than 32,000), we selected according to generality and timeliness. This is considered a recent review that focuses on selected interesting examples of various heterocycles from the mechanistic aspects of organic azides. 相似文献
106.
Olga Bakulina Anton Bannykh Ekaterina Levashova Mikhail Krasavin 《Molecules (Basel, Switzerland)》2022,27(12)
Screening of a library of novel N-hydroxylactams amenable by the Castagnoli-Cushman reaction identified four lead compounds that facilitated 55Fe transport into P. aeruginosa cells (one of these synthetic siderophores was found to be as efficient at promoting iron uptake as the natural siderophores pyoverdine, pyochelin or enterobactin). Conjugates of the four lead siderophores with ciprofloxacin were tested for antibacterial activity against P. aeruginosa POA1 (wild type) and the ∆pvdF∆pchA mutant strain. The antibacterial activity was found to be pronounced against the ∆pvdF∆pchA mutant strain grown in CAA medium but not for the POA1 strain. This may be indicative of these compounds being ‘Trojan horse’ antibiotics. Further scrutiny of the mechanism of the antibacterial action of the newly developed conjugates is warranted. 相似文献
107.
采用聚丙烯胺溶胶-凝胶法制备了类钙钛矿La1-xNDxSrCoO4(x=0.1~0.9)复合氧化物催化剂,考察了其对CO和C3H8的催化氧化活性,并运用XRD、IR和TPR等手段对催化剂进行了表征.结果表明,所制备的样品均具有K2NiF4型结构,适量Nd2O3的加入增加了LaSrCoO4的催化活性,使LaSrCoO4催化剂粒度变小、晶格畸变率变大及与氧的结合能力减弱,从而有利于CO和C3H8氧化活性的提高. 相似文献
108.
New derivatives obtained by the combination of unique 1,2,4,5-tetrazine and 4H-1,2,4-triazole rings have great application potential in many fields. Therefore, two synthetic few-step methodologies, which make use of commercially available 4-cyanobenzoic acid (method A) and ethyl diazoacetate (method B), were applied to produce two groups of the aforementioned heterocyclic conjugates. In both cases, the target compounds were obtained in various combinations, by introducing electron-donating or electron-withdrawing substituents into the terminal rings, together with aromatic or aliphatic substituents on the triazole nitrogen atom. Synthesis of such designed systems made it possible to analyze the influence of individual elements of the structure on the reaction course, as well as the absorption and emission properties. The structure of all products was confirmed by conventional spectroscopic methods, and their luminescent properties were also determined. 相似文献
109.
The thermal decomposition of Zn-MPA complex was investigated under microwave irradiation. ZnO and ZnS nanocrystals could be obtained by decomposing Zn-MPA(3-mercaptopropionic acid) complex under different reaction conditions. It was found that both the pH value of the solution and the molar ratio of Zn2+ and MPA can play an important role in the formation of ZnO and ZnS nanocrystals. MPA mainly acts as an S source or as a complexing agent. This study provides a new route for the controllable preparation of semiconductor nanocrystals. 相似文献
110.
Hiago N. Silva Srgio Hiroshi Toma Artur Luís Hennemann Josu M. Gonalves Marcelo Nakamura Koiti Araki Marcos Makoto Toyama Henrique Eisi Toma 《Molecules (Basel, Switzerland)》2022,27(14)
A new supramolecular electrocatalyst for Oxygen Evolution Reaction (OER) was synthesized from a central multibridging cobalt tetrapyridylporphyrazine (CoTPyPz) species by attaching four [Ru(bpy)2Cl]+ groups. Both CoTPyPz and the tetraruthenated cobalt porphyrazine species, TRuCoTPyPz, form very homogenous molecular films just by dropcasting their methanol solutions onto GCE electrodes. Such films exhibited low overpotentials for O2 evolution, e.g., 560 e 340 mV, respectively, displaying high stability, typically exceeding 15 h. The kinetic parameters obtained from the Tafel plots showed that the peripheral complexes are very important for the electrocatalytic activity. Hyperspectral Raman images taken along the electrochemical process demonstrated that the cobalt center is the primary active catalyst site, but its performance is enhanced by the ruthenium complexes, which act as electron-donating groups, in the supramolecular system. 相似文献