活化液中稀土离子Ce3+对铜粉化学法镀银的促进作用

通过化学镀活化液中添加微量稀土元素Ce3+,采用电化学在Cu粉表面化学镀银,用电化学法和扫描电子显微镜测试技术分别研究了含稀土活化液的极化曲线、镀银层的表面形貌、银包覆率。结果表明,稀土以适宜比例添加到Pd2+活化液中,能使静止电极电位正移,极化度减小,过电位绝对值增大,活化液中的反应易于进行。适量稀土介入活化液中有助于提高镀银铜粉表面银在铜粉表面的沉积速度和包覆率,逐渐增加稀土含量,使镀层晶粒和组织逐渐细化且致密。 最佳加入值为0.32 g/L     

Fe-Ni-S软磁薄膜的电沉积

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。     

5,5′-二甲基乙内酰脲体系电沉积金(英文)

开发了以5,5′-二甲基乙内酰脲(DMH)为配位剂的无氰电镀金工艺。利用扫描电镜(SEM)和线性扫描伏安曲线对电镀时间和添加剂(由丁炔二醇、糖精和十二烷基硫酸钠组成)对镀金层表面、断面形貌和镀液性能的影响进行了测试,结果表明随着电镀时间的延长镀金层表面形貌几乎没有发生变化,光亮剂的加入增大了阴极极化同时使镀金层结晶变得细致均匀,在由HAuCl4,DMH,K3PO4和KH2PO4组成的基础镀液中金的沉积速度可达0.3μm.min-1,镀液中添加剂的加入没有影响金的沉积速度。利用X射线衍射技术(XRD)和X射线光电子能谱技术(XPS)对镀金层性能进行了测试,结果表明镀金层沿着(111)晶面择优生长并且由纯金组成。利用循化伏安曲线和旋转圆盘电极对Au(Ⅲ)在镀液中的电化学还原机制进行了研究,结果表明当研究电极为玻碳电极(GCE),镀液温度为45℃时,镀液中金的电沉积过程是受扩散控制的不可逆的过程。同时利用循环伏安曲线对镀金液的稳定性进行了分析。     

稀土铈在锌-铁合金电沉积中的作用

研究了铈盐对电沉积锌-铁合金镀液及镀层性能的影响, 通过盐水浸泡实验, 抗高温氧化性实验及分散能力、阴极极化曲线测定, 得出在镀液中添加一定量的铈盐能改善镀液性能, 同时还可提高镀层的耐蚀性及抗高温氧化性.     

镀液中金属杂质离子对电镀镍层性能的影响

向镍电镀原液中引入2 g/L的Co~(2+),Cr3+,Mn~(2+),Fe~(2+),Cd~(2+),Zn~(2+)等离子,通过电镀得到不同的镀层.X射线衍射(XRD)、X射线光电子能谱(XPS)及扫描电子显微镜(SEM)的结果表明,不同金属离子对镍沉积影响不同,金属杂质离子的存在会使镀层中晶粒尺寸变小,影响镍镀层的均匀性和致密度.通过阴极极化曲线、计时电位和交流阻抗等方法探讨了含有不同金属杂质的镀液在电镀过程中电化学行为的规律性.通过镀液的浓度梯度、耐腐蚀、耐热循环及耐高温等实验获得了不同条件下金属杂质在镀液中所允许的浓度范围.     

络离子在电镀液中起些什么作用

我们在电镀时,常会遇到下列种种问题:例如镀银时溶解硝酸银作为镀银液,则阴极所得镀层是灰黑色且疏松的粒状或针状或叶片状的银晶粒,在硝酸银液中加入过量的氰化钾,使硝酸银溶解后的溶液作为镀银液,则阴极所得的镀层即为色泽洁白结构密致的银晶粒。镀锌时用硫酸锌作为镀液,则阴极所得镀层一     

甲基磺酸亚锡溶液中不同稳定剂的作用机制及电化学性质

研究了对苯二酚、邻苯二酚、间苯二酚和抗坏血酸4种稳定剂对甲基磺酸亚锡电镀液稳定性、电极极化及镀层表面形貌的影响.采用循环伏安法探究了镀液稳定性与稳定剂电化学性质的关系,通过交流阻抗和计时电位考察了稳定剂对镀液阴极极化性能的影响,分析了对苯二酚在电镀过程中的循环使用原理及对苯二酚的最佳使用浓度.结果表明,镀液的稳定性与稳定剂自身的还原能力及电化学活性之间存在重要联系,4种稳定剂对镀液稳定作用的大小顺序为对苯二酚邻苯二酚抗坏血酸间苯二酚,稳定效果最好的对苯二酚可以将镀液的储存时间延长一倍;苯二酚类稳定剂可以提高锡沉积的阴极极化程度,使晶粒细化,而抗坏血酸对锡沉积起到去极化作用;对苯二酚在电镀锡过程中兼具抗氧化剂、光亮剂和整平剂的作用,镀层的耐蚀性能测试结果表明,对苯二酚的最佳浓度为1.0 g/L.     

不同分子量PEG的铜电镀液对电化学沉积铜行为的研究

研究了在酸性镀铜溶液中添加不同分子量的PEG对直径为50微米、深径比为1的镀层盲孔填充效果的影响.结果表明,随着PEG分子量的增加,电镀铜溶液的微孔填充力明显提高.电流密度为2 A/dm2,添加剂PEG分子量(u)超过6000时,镀液可以完全填充盲孔,镀层不出现任何空洞和缝隙.这是由于添加剂PEG能明显加强电镀铜镀液阴极极化,抑制了电镀铜的沉积.同时,PEG于镀液中的扩散系数还随其分子量的增加而降低,从而增加了SPS在微孔底部的吸附力,加速了电镀铜在微孔底部的沉积.进一步,增大PEG分子量,沉积铜膜的表面粗糙度、铜膜结晶度和电阻率均有所降低.     

酸性溶液化学镀Ni-P-B合金及结构性能表征(英文)

联用次亚磷酸钠和硼氢化钠两种还原剂 ,从酸性镀液中沉积出不同硼含量的Ni_P_B镀层 ,并用原子力显微镜、X_射线衍射、透射电镜、动电位扫描等实验技术对其镀态结构及性能进行了表征。实验表明 ,镀液中硼氢化钠含量对沉积速度影响不大 ,但能显著影响镀层的化学组成。硼的共沉积使镍晶格点阵产生扭变 ,导致镀层晶粒增大 ,表面粗糙 ,颗粒分布不均匀 ,并使镀层由非晶态向微晶结构转变 ,且微晶成分随镀层中硼含量的增加而增多。Ni_P_B镀层的硬度随镀层中硼含量的增加而增大 ,热处理能显著提高镀层的硬度 ,且服从沉淀硬化机理。在 3.5wt%NaCl和 40wt%NaOH两种介质中 ,Ni_P_B合金的耐腐蚀能力优于Ni_P合金。镀层中硼含量越高 ,其耐腐蚀能力越强。     

纳米CeO_2对Pb-WC-CeO_2复合镀层结构及耐腐蚀性的影响

通过对阴极极化曲线、交流阻抗测试技术和塔菲尔曲线的测量,以及镀层微观形貌和能谱图的分析,考察了在电解液中添加不同浓度的纳米CeO2对Pb-WC-CeO2复合镀层微观结构和耐腐蚀性能的影响。结果表明:CeO2的加入,可增大阴极极化,有效促进WC的共沉积,使镀层晶粒更细,表面更均匀平整,有良好的结合力;当其浓度为40 g·L-1时,镀层表面微观形貌最均匀致密,平整有序,有最好的耐蚀性能,镀层中Ce和W含量达到最大值8.75wt%和3.18%,但W和Ce元素的含量与溶液中CeO2的浓度并不完全呈线性变化。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

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.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

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.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

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%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.