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261.
本文合成了3种套索冠醚4、5和6,分别测定了它们与Hg^2^ 、Pb^2^ 、Zn^2^ 、cd^2^ 、Ni^2^ 、Co^2^ 、Cu^2^ 、Ag^ 、Tb^3^ 和Eu^3^ 所形成的络合物的紫外吸收光谱,用电喷雾液相色谱-质谱联用仪分别表征了它们与TB^3^ 形成的络合物,结果显示它们对上述金属离子有很好的络合性。 相似文献
262.
以α ,β ,γ ,δ 四 (5 磺基噻吩 )卟啉为柱前衍生试剂 ,用含 pH 9.0的 10mmol·L- 1的硼酸 氢氧化钠缓冲溶液和 2 .0× 10 - 3mol·L- 1四丁基溴化胺 (TBA .Br)的甲醇 水 (40∶6 0 )溶液作流动相 ,检测波长为 4 2 3nm ,在C18柱上同时分离和测定了铜、锌两种金属络合物 ,检出限 (S/N =3)分别为 0 .2 3和 0 .30ng·ml- 1,方法用于天然水样分析获得满意结果。 相似文献
263.
银杏叶黄酮糖苷精制工艺的研究 总被引:2,自引:0,他引:2
银杏叶用5倍重的70%乙醇水溶液回流提取4次,每次30min,银杏叶黄酮糖苷的平均浸出率为93.8%,不同型号大孔吸附树脂的精制效果研究表明,在确定的精制条件下制备的银杏叶提取物,其得率为2.50%~2.92%,黄酮糖苷含量25.7%~34.6%. 相似文献
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265.
用于浆态床FT合成的Fe-Cu-K-Si催化剂的初步考察 总被引:1,自引:2,他引:1
使用连续共沉淀反应器制备了浆态床FT合成用的Fe-Cu-K-Si催化剂。考察了钾含量、粘合剂的添加以及催化剂还原方法等对催化剂性能的影响。1L高压搅拌釜的试验结果表明粘合剂添加方法B和低压CO还原条件下的No.9催化剂性能较好。在质量空速为无载体Fe-Cu-K催化剂1.5倍的条件下,No.9催化剂的合成气转化率,C1^ 和C5^ 产物的产率均高于无载体Fe-Cu-K催化剂,甲烷选择性为3.2%。特别在富CO合成气条件下C5^ 的单程产率达到130g/m^3(CO H2)以上。假设对氢为一级反应动力学的条件下,使用表观速率常数对o.9催化剂的反应活性的经时变化作了考察,结果表明表观速率常数较合成气转化率能相对地反映不同反应条件下的催化剂活性。 相似文献
266.
Online restricted‐access material combined with high‐performance liquid chromatography and tandem mass spectrometry for the simultaneous determination of vanillin and its vanillic acid metabolite in human plasma 下载免费PDF全文
De‐qiang Li Zhi‐qing Zhang Xiu‐ling Yang Chun‐hua Zhou Jin‐long Qi 《Journal of separation science》2016,39(17):3318-3326
An automated online solid‐phase extraction with restricted‐access material combined with high‐performance liquid chromatography and tandem mass spectrometry was developed and validated for the simultaneous quantification of vanillin and its vanillic acid metabolite in human plasma. After protein precipitation by methanol, which contained the internal standards, the supernatant of plasma samples was injected to the system, the endogenous large molecules were flushed out, and target analytes were trapped and enriched on the adsorbent, resulting in a minimization of sample complexity and ion suppression effects. Calibration curves were linear over the concentrations of 5–1000 ng/mL for vanillin and 10–5000 ng/mL for vanillic acid with a coefficient of determination >0.999 for the determined compounds. The lower limits of quantification of vanillin and vanillic acid were 5.0 and 10.0 ng/mL, respectively. The intra‐ and inter‐run precisions expressed as the relative standard deviation were 2.6–8.6 and 3.2–10.2%, respectively, and the accuracies expressed as the relative error were in the range of –6.1 to 7.3%. Extraction recoveries of analytes were between 89.5 and 97.4%. There was no notable matrix effect for any analyte concentration. The developed method was proved to be sensitive, repeatable, and accurate for the quantification of vanillin and its vanillic acid metabolite in human plasma. 相似文献
267.
Lü‐qiang Yu Shi‐Xi Zhao Qi‐long Wu Jian‐Wei Zhao Guo‐dan Wei 《Advanced functional materials》2020,30(16)
Carbon materials are frequently used to improve the cycle and rate performance of VS4 as anode material for lithium ion batteries. However, the interfacial interaction between VS4 and carbon has not been elucidated clearly. Various VS4@C composites are prepared and the interface between VS4 and porous carbon is investigated by X‐ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy, and first‐principles calculations. The interfacial structure between VS4 and carbon and the mechanism of flower‐like VS4 growth on carbon substrate are revealed clearly. The results indicate that C?V bonds and C?O?V bonds are formed when oxygen functional groups are introduced into the porous carbon, and the C?V bonds and C?O?V bonds accelerate the electron transport and enhance structural stability of the VS4@C composite. Deriving from the unique structure and robust interfacial interaction, the electrochemical performances of VS4@C composite are much better than that of pure VS4. Moreover, through the study of lithium storage mechanism of VS4 anode, it is found that there is an irreversible amorphization change of the original VS4 in the first cycle, and that during the following electrochemical process, the main storage behavior of lithium ions derives from the insertion?extraction reactions in the amorphous VS4 with the reaction between V4+ and V3+. 相似文献
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270.
以Li2CO3为Mn源,采用醇水混合溶剂分散与中温固相反应法考察了Mn(NO3)2@6H2O,Mn(MeCO2)2@4H2O,MnCO3,化学MnO2(CMD)和电解MnO2(EMD)等不同Mn前驱物对制备Li1+xMn2-xO4尖晶石正极材料的电化学性能的影响,并采用XRD,BET,TEM等手段对材料进行了表征.结果表明,由不同Mn前驱物制备的正极材料均呈尖晶石结构,其容量大小和循环性能(依Mn源为顺序)为EMD>Mn(NO3)2@6H2O>MnCO3>Mn(MeCO)2@4H2O>CMD.材料呈立方晶体,比表面积(依Mn源为顺序)为CMD>MnCO3>Mn(NO3)2@6H2OMn(MeCO2)2@4H2O>EMD,正好与容量及稳定性顺序相反.采用本文的制备方法时,EMD和Mn(NO3)2@6H2O都是较好的Mn前驱物,Mn(MeCO2)2@4H2O和MnCO3也可以做Mn源,但焙烧时需要富氧气氛,CMD不适宜作Mn前驱物. 相似文献