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1.
利用恒电流沉积法,在p-Si上制备出不同W含量和不同结构的Ni-W薄膜,研究了镀液温度,pH值,电流密度对镀层组成的影响,结果表明,提高温度有利于获得高W含量的合金。 相似文献
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Fe-Ni-S软磁薄膜的电沉积 总被引:1,自引:0,他引:1
酸性镀液中以硼酸为缓冲剂、柠檬酸三钠为配合剂,在紫铜箔上电沉积得到非晶Fe-Ni-S合金薄膜。 采用扫描电子显微镜和能谱分析技术(EDS)研究了镀液组成和沉积条件对镀层表面形貌和组成的影响。 结果表明,在镀液中加入2 g/L C7H5O3NS(糖精)和0.4 g/L 1,4-丁炔二醇可获得表面平整无裂缝和较小内应力的合金镀层;电流密度和镀液pH值对镀层组成影响较小,但施镀温度对镀层组成影响较大。 获得了理想的镀液组成和沉积条件,所得Fe73Ni9.5S17.5薄膜的X射线衍射表明其为非晶结构,在室温下具有较高的饱和磁化强度(Ms约为876.25 kA/m)和较低的矫顽力(Hc约为4.96 kA/m),具有良好的软磁性能。 循环伏安曲线和阴极极化曲线均表明,镀液中CS(NH2)2会促进Fe-Ni-S共沉积。 相似文献
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以蚀刻金属铝箔为模板,用化学镀制备了具有微米阵列结构的Ni-P合金材料,使用扫描电镜、能量散射谱及X-射线衍射等表征手段对所得材料的微观形貌与物质组成进行了分析,并通过电化学方法研究了化学镀温度、施镀时间对材料析氢催化活性的影响。结果表明,70℃制得的Ni-P微阵列材料作电极其析氢过电位最小,电流密度为15m A/cm2时比光面Ni-P镀层下降了约100m V;同时表现出最高的交换电流密度13.53×10-6A/cm2,高出光面Ni-P镀层近1个数量级;70℃施镀4h能够得到析氢过电位较低且结构完整的镀层,延长镀时没有继续提升其性能。为直观衡量材料的催化活性,在双室槽中进行了光解水析氢测试。Ni-P微阵列材料表现出良好的催化活性,析氢速率较光面电极上升约200%。 相似文献
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Ni-P化学镀反应速率及机理研究 总被引:7,自引:0,他引:7
通过镀层分析和析氢量测量得到Ni-P镀层的沉积速度和H2PO2的分解速度·以混合电位理论为基础,对Ni-P电极在不同组成饮液中的极化曲线进行分解得到以化学镀电流形式所表示的反应速率·将两种方法所得结果进行对照,确定H2PO2氧化时电子迁移数为1,并用原子红-电化学联合理论解释溶液PH对反应速率及化学镀效率的景响. 相似文献
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化学沉积镍-铁-磷合金和它的伏安行为 总被引:4,自引:1,他引:3
在以次亚磷酸钠为还原剂,硼酸为缓冲剂和柠檬酸钠为络合剂的碱性介质中,研究了镍-铁-磷合金化学沉积条件(pH值,温度及[Fe^2 ]/([Ni^2 ] [Fe^2 ])物质的量比)对沉积速率和镀层组成的影响;并由此建立镀液稳定的最佳沉积工艺.实验表明,镀液中硫酸亚铁对沉积镍-铁-磷合金有阻碍作用(降低了化学沉积速率)。造成镀层中铁含量不高(小于20%),使用循环伏安技术研究了镍-铁-磷合金的电沉积机理.结果发现铁对次亚磷酸钠的氧化不起催化作用,提高镀液温度和pH值有增加沉积速率之效. 相似文献
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镍硫析氢活性阴极的电化学制备及其电催化机理 总被引:2,自引:0,他引:2
以硫代硫酸钠作为硫源, 在基本的瓦特浴镀液体系中通过恒电流电沉积方法获得了不同晶体结构的镍硫合金活性阴极. 通过能量散射谱(EDS)、X射线衍射(XRD)以及扫描电子显微镜(SEM)对镀层的化学成分、晶体结构以及表面形貌进行了分析, 并对活性阴极的电催化活性以及析氢过程机理进行了研究. XRD测试结果表明, 随着镀层中硫含量的变化, 镀层的晶体结构呈现出非晶态/Ni3S2混晶和金属间化合物(Ni3S2)两种晶体结构, 其中, 硫含量为33.9%(原子分数)的非晶态/Ni3S2混晶结构的活性阴极在碱性溶液中具有很好的析氢活性, 其优良的析氢活性主要来自于Ni3S2很强的吸附氢能力. 交流阻抗的测试结果表明, Ni3S2金属间化合物的析氢过程只存在一个电化学反应步骤, 而非晶态/Ni3S2混晶镍硫合金活性阴极的析氢过程存在三个电化学反应步骤. 相似文献
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直接以氯金酸作为主盐、 羟基乙叉二膦酸(HEDP)作为镀液稳定剂和镀层细化剂、 结合添加剂, 组成亚硫酸盐无氰镀金新工艺; 研究镀液稳定性、 镀层形态及金电沉积机制。结果表明, HEDP可明显提升镀液稳定性;不含HEDP的亚硫酸盐镀金液中, 镀层呈棒状晶粒并随沉积时间延长而逐渐生长,导致镀层外观随镀层厚度增加由金黄色转变为红棕色。镀液含有HEDP时, 金晶粒形态由棒状转变为棱锥状, 且棱锥状晶粒随沉积时间延长生长速率较小, 镀层厚度为1 μm时仍呈现金外观。电化学实验表明金电沉积不经历成核过程。 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献