应用等离子体溅射方法制备钯-银合金复合膜及其膜表征

研究应用等离子体溅射方法制备钯 银合金复合膜 ,并用电子显微镜和高温气体渗透测定来表征膜的质量 .用sol gel方法在工业微滤氧化铝陶瓷膜上沉积纳米孔γ Al2 O3 膜 ,以改善衬底表面的粗糙度 ,降低气相沉积过程中的阴影效应 .以改进钯 银合金膜的气密性为目标来优化等离子体溅射方法的沉积条件 (衬底温度及沉积压力等 ) .典型的钯 银合金复合膜具有氢渗透速率 :0 .0 36× 10 -5 ～ 1.17× 10 -5cm3 /cm2 ·s·Pa ,氢对氮的分离选择性 :5 1.5～ 10 0 0 ,测试条件 :温度为 35 0～ 45 0℃ ,膜两侧压力降为 10 4～ 10 5 Pa     

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。     

Pd-Y合金膜的MOCVD研制

采用金属有机化合物的化学气相淀积法,以β-二酮螯合物为源物质,在多孔Al₂O₃衬底上成功制备了超薄钯钇合金膜.用Pd(AcAc)₂+Y(AcAc)₃混合源制备的钯钇合金膜的晶粒尺寸(21nm×10nm)比单独用Pd(AcAc)₂制备的钯膜的尺寸(30nm×10nm)小.XPS研究发现,制备的Pd-Y合金膜中Y/Pd比小于源物质的.氢的透气性实验表明,合金膜的氢渗透率高于Pd膜,且在200～350℃范围内渗透率稳定.     

表面改性SUS316L不锈钢的电化学行为研究

分别以表面镀Rh,表面离子束增强沉积Ta2O5膜及溶胶凝胶法沉积TiO2膜对冠状动脉支架用材料SUS316L不锈钢进行表面改性.采用电化学方法研究了该表面改性试样在Tyrode's模拟人工体液中的电化学行为.结果表明,上述3种表面改性方法均可提高SUS316L不锈钢在模拟人工体液中的阳极极化性能.其中对于采用离子束增强法沉积的Ta2O5膜和溶胶凝胶法沉积的TiO2膜,因Ta和Ti上的d轨道空位已被氧的电子占据,不利于氢吸附,从而抑制了阴极的析氢过程.X射线衍射分析发现,3种改性方法在SUS316L不锈钢表面依次形成均匀而致密的Rh金属层,Ta2O5的无序膜层和TiO2晶态膜层,阻止了合金元素的溶解,改善不锈钢的电化学性能.     

液相放电法合成氮化碳晶体

自从 Cohen等 [1,2 ] 预言了一种碳氮化合物 ( β- C3N4 )可能具有比金刚石还高的硬度和其它优异的力学、电学和光学性能以来 ,人们竟相采用各种技术手段 (如化学气相沉积、磁控溅射、离子束沉积和激光刻蚀等 )尝试合成这种新材料 [3,4 ] .但是 ,大多数合成的氮化碳材料为非晶或者是少量的晶体包埋在非晶的碳和 CNx 材料中 ,尚未制得可以精确地研究其晶体结构的足够大的单晶 .1 999年 ,Fu等 [5] 将液相电沉积技术应用于氮化碳材料的合成 ,从乙腈中沉积了氮含量为 2 5 %的氮化碳薄膜 .目前电化学沉积法制备的氮化碳薄膜多为非晶膜 [6～ 9]…     

Er-Bi合金膜在有机溶剂中的电沉积研究

利用循环伏安法和恒电位电解法探讨了室温条件下在二甲基亚砜(DMSO)中Er-Bi合金膜的电化学制备.研究了沉积电位、电流密度以及主盐浓度比对沉积膜质量的影响.实验结果表明,在ErCl3-Bi(NO3)3-LiCl-DMSO体系中,当控制恰当的体系组成和沉积条件,均可得到表面均匀、附着力强、有金属光泽的灰黑色非晶态Er-Bi合金膜,其中稀土Er的质量分数可达24.09％～46.56％.通过SEM、EDS分析得到沉积膜表面形貌和组成,通过XRD和DSC确定了合金膜的物相组成.结果表明,当所制备的合金膜在723 K进行热处理1 h后,可形成稳定的Er-Bi合金相.     

在有机溶剂中Eu-Co-Ni合金薄膜的电化学制备

利用恒电位沉积、循环电位沉积和脉冲电沉积法在DMSO体系中在铜基体上探讨了Eu-Co-Ni合金薄膜的制备.实验结果表明,在0.10mol/LEuCl3-0.10mol/L CoCl2-0.10mol/L NiCl2-0.1 0mol/l LiClO4-DMSO体系中,恒电位沉积技术制备出的Eu-Co-Ni合金膜表面较为粗糙,其中Eu含量为5.46～6.01 wt%,脉冲电沉积技术制备的Eu-Co-Ni合金膜表面平整,致密,附着力好,且有金属光泽,其中Eu含量为6.76%,循环电位扫描技术制备的Eu-Co-Ni合金膜表面平整,致密,附着力好,其中Eu含量为12.43%.通过XRD证明所得的合金薄膜为非晶态.     

脉冲激光沉积纳米NiO薄膜

Na Cl型 Ni O是一种 p型半导体 ,广泛用于传感器、催化剂、涂料、磁性材料及电极材料等领域[1～ 5] .最近 ,Poizot等 [6] 又报道了 Ni O可作为锂离子电池的阳极材料 ,使 Ni O成为又一新的研究热点 .纳米 Ni O粉末的制备方法有多种 ,主要包括化学沉淀法和沉淀转换法 ,Ni O薄膜的制备主要采用磁控溅射、化学气相沉积和电沉积等方法 [7～ 12 ] .脉冲激光沉积法具有操作简单和成膜纯净等优点 ,因此是制备薄膜的重要方法之一 .本文采用脉冲激光沉积 (PLD)法在氧气氛中使用金属镍作为靶材料 ,不锈钢作为基片 ,对 Ni O薄膜的制备进行了研究…     

热处理对SILAR法制备CuInSe_2薄膜性能的影响

0引言铜铟硒(CIS)具有合适的带隙、高光吸收系数、适当的电荷密度和迁移率,是一种用于薄膜太阳能电池的备受关注的吸收材料[1]。目前CuInSe2薄膜已采用多种方法进行制备,如金属前驱体硒化法[2]、共沉积法[3]、溅射法[4]、电沉积法[5]和化学气相沉积法[6]等。这些方法都有各自的     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

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.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

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.     

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.     

Microwave-assisted copper-catalyzed stereoselective ring expansion of three-membered heterocycles with α-diazo-β-dicarbonyl compounds

Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular S_N2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

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.