NH4F对化学镀镍液的作用机理及镀层性能的影响

氟元素是周期表中最活泼的非金属元素,有着最强的电负性,氟化物有着特殊的化学性能。关于氟化物在化学镀镍磷工艺中的应用已有报道,在镁基体上化学镀的前处理过程中,常用氢氟酸或氟化氢铵来进行活化处理;硅片表面上的化学镀也通常用HF与HNO3或HCl的混酸来活化,使硅片表面产生Si-H键。另外,如果在化学镀液中添加少量的氟化钠,则起到加速的作用[1]。对于氟化物在化学镀镍磷工艺中的报道仅限于此,未见有关氟化物在化学镀中其它作用的研究。鉴于此,本工作以氟化铵为研究对象,对其在弱碱性的条件下对化学镀液的缓冲能力、沉积速度以及所得镀层性能的影响进行了研究。     

化学镀镍法制备碳纳米管

以PdCl2为活化液,用化学镀镍法制备了具有活性中心的镀镍硅模板,通过催化裂解在镀镍硅模板上制备了碳纳米管。讨论了化学镀工艺参数对镀镍硅模板表面活性中心的尺寸和分布的影响。最佳的工艺条件为:在0.17mol·L-1的SnCl2中敏化10min,0.4g·L-1PdCl2中活化2min,50℃施镀3min所得的镍粒子活性中心的粒径为200nm~300nm。用扫描电镜观察到碳纳米管为竹节形状,直径为100nm~110nm。     

碳纳米管表面的无钯活化化学镀镍研究

本文提出碳纳米管表面无钯活化的化学镀镍方法.碳纳米管经硝酸氧化和碱中和后表面生成羧基,利用羧基吸附镍离子,之后吸附的镍离子被化学还原为镍的纳米微粒并成为化学镀镍的催化活性中心.红外吸收光谱和电子显微镜观察等证实了上述活化过程的机理.实验表明,新的活化方法对碳纳米管表面化学镀是切实可行的,文中同时对化学沉积层的不同形貌进行讨论.     

自组装膜吸附钯的化学镀前活化研究

提出了一种无需氯化亚锡敏化、基于分子自组装膜（SAMs）吸附钯的活化方法,成功地引发了在氧化铝粉末表面的化学镀铜.用XPS、AES、FTIR研究了钯的吸附机理,认为是由于氯化钯与SAMs上向外突出的氨基形成了化学键,并提出了相应的活化机理.金属化产物经XRD、FTIR、剖面金相显微表征分析与压片电阻率测定,示为金属铜完全包覆氧化铝的复合材料.该活化工艺具有活性引发层厚度薄、寿命长和与基底结合力强等优点,也可应用于其它表面富羟基的基底材料.     

钯银膜无电解镀共沉积的探讨

无电解镀共沉积钯银合金膜是纯化氢同位素最有发展前途的方法之一 .膜的制备技术有物理气相沉积法 [1 ]、化学气相沉积法 [2 ]、电镀 [3]和无电解镀法 [4]等 .无电解镀法使用设备简单、易于操作 ,而且可以均匀地沉积在形状复杂、硬度不同的基体上 .国内对电镀钯及有关钯银合金膜的研究 [5]较多 ,但无电解镀的研究甚少 .本文用无电解镀法制备含银量在摩尔分数2 3%～ 2 5 %的有支撑钯银膜 (膜厚为 3～ 5μm) .采用含有钯银两种离子的镀液制得的膜层 ,优于机械混合的均匀程度 .结果表明膜层没有合金化 .无电解镀条件为 :镀温 (5 0± 1 )℃ ,镀…     

自组装技术在电磁屏蔽织物加工中的应用

尼龙织物经功能性高分子壳聚糖(CS)预处理后,应用分子自组装技术于其表面自组装钯膜(镀镍前活化).该膜钯微粒为纳米级,比表面较大,催化活性较高.将成膜后的织物化学镀镍磷合金,即可得到屏蔽性能优异的电磁屏蔽织物.正交试验及单因素试验得出CS预处理的最佳工艺条件.SPM、SEM表征活化前后及施镀前后织物表面的形态变化.根据Schelkunoff理论,计算织物的电磁辐射屏蔽效能,其值高于30 dB,相当于屏蔽掉了96.0%以上的电磁波.     

陶瓷基钯银合金膜制备技术及性能研究

报道采用浆料涂敷与化学镀相结合法在陶瓷支撑上沉积钯银合金膜,采用浆料涂敷法,将含钯银的浆料涂敷在支撑体上,干燥后热分解,使支撑体表面沉积部分钯银。然后,采用化学镀在50℃下沉积钯银膜,热处理后,得到表面较光洁、厚度约为3μm、银含量为23%(原子百分含量)、合金化较完全的钯银合金膜,该膜在压差为0.1MPa,温度为300℃时的渗氢通量达45cm^3(STP)/(cm^2·min),分离因子达500,研究了钯银合金膜中银含量随热处理温度的变化规律,由实验结果发现,银逐渐向表面扩散,并在一定的温度条件达到基本平衡。     

陶瓷基钯银合金膜制备技术及性能研究

报道采用浆料涂敷与化学镀相结合法在陶瓷支撑上沉积钯银合金膜,采用浆料涂敷法,将含钯银的浆料涂敷在支撑体上,干燥后热分解,使支撑体表面沉积部分钯银。然后,采用化学镀在50℃下沉积钯银膜,热处理后,得到表面较光洁、厚度约为3μm、银含量为23%(原子百分含量)、合金化较完全的钯银合金膜,该膜在压差为0.1MPa,温度为300℃时的渗氢通量达45cm^3(STP)/(cm^2·min),分离因子达500,研究了钯银合金膜中银含量随热处理温度的变化规律,由实验结果发现,银逐渐向表面扩散,并在一定的温度条件达到基本平衡。     

NiCF/ABS复合材料的制备及电磁屏蔽效能研究

探讨了碳纤维(CF)表面镍金属的化学镀工艺,制备了镀镍碳纤维(NiCF),采用密炼工艺制备了ABS基体复合材料,研究了CF和NiCF含量对复合材料的导电性能及电磁屏蔽效能的影响。结果表明:采用化学镀的方法在碳纤维表面镀覆了金属镍,所形成的镀层均匀致密;镀覆时间为5min时,镀镍后的碳纤维电阻率降低两个数量级;复合材料电阻率随CF、NiCF含量的增加而逐渐减小;复合材料电磁屏蔽效能随CF、NiCF含量的增加而逐渐增加,当NiCF含量为25%(wt)(约13.3vol%)时,电磁屏蔽效能最高可达51dB。     

空心微珠表面化学镀Ni-Co-P合金

以无机非金属粉煤灰空心微珠为芯材, 利用化学镀工艺对其表面进行金属化改性, 可以得到表面完整包覆的导电粉体, 该粉体具有中空, 质轻, 粒度细, 高强度, 耐高温, 导电性能好等多种优异性能, 可部分代替金属和铁氧体微粉作为电磁波吸收剂. 采用SnCl2和PdCl2进行敏化-活化处理后, 在空心微珠表面化学包覆Ni-Co-P合金层, 利用XRD、EDS、SEM和镶嵌金相等方法对样品进行形貌观察和分析表征, 结果表明, 使用PdCl2作活化剂可以得到优质均匀的Ni-Co-P合金镀层, 镀层光亮, 均匀, 包覆完整. 化学镀后镀层呈非晶态, 450 ℃氢气气氛下热处理后出现结晶相Ni3P和六方晶系的α-Co单质.     

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.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

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.     

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.     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.