温度对AACVD法制备AZO透明导电薄膜的影响

低成本、大面积、沉积速率高、均匀性好、光电性能优良的Al掺杂ZnO薄膜(AZO)制备技术依然是透明导电薄膜领域研究的重点之一。本文采用冷壁式气溶胶辅助化学气相沉积(AACVD)技术在玻璃衬底上制备了AZO透明导电薄膜,研究了衬底温度对薄膜结构和光、电性能的影响。利用X射线衍射、原子力显微镜、紫外-可见光谱和光致发光光谱等对样品进行了表征。结果表明:在AACVD法生长AZO薄膜的过程中,衬底温度对AZO薄膜晶面的择优取向生长影响呈起伏式变化。明显的电学性能的转变温度发生在约400℃,光学性能和晶面的择优取向生长变化出现在约450℃。讨论了温度对AACVD法制备AZO透明导电薄膜结构和光、电性能影响的微观机制。400℃时沉积的AZO薄膜方阻190Ω/□,平均透过率为80%。     

微纳加工技术在超微电极制备中的应用

从电极材料、绝缘材料、薄膜的图形化等方面,评述了微纳加工技术在单超微电极和超微电极阵列制备中的应用。在单超微电极的制备中,随着微纳加工技术的引入,可以实现具有规则几何形状和微小电极尖端的单超微电极的重复性制备。     

制备条件对铝掺杂氧化锌(AZO)薄膜结构和电学性质的影响

本文利用溶胶-凝胶法在玻璃基底上制备得到了AZO透明导电薄膜,就两种不同的热处理-退火方式对薄膜的结构与性质的影响做了比较,研究了掺杂浓度、退火温度对薄膜结构及性质的影响规律.结果表明,高温、分层退火、铝掺杂均有利于生成结晶度高、具有C轴优先取向的AZO薄膜;高温和分层退火有利于晶粒长大,相反铝掺杂却有碍晶粒长大;薄膜的电学性质随退火温度和铝掺杂量的变化呈现规律的变化.通过分析AZO薄膜内的晶体生长过程,本文认为主要是制备条件和AZO晶体的晶面习性导致了薄膜的结晶度、晶体生长取向性和晶粒尺寸等方面的差异.     

浸蚀多孔金属铝模板制备超亲水/超疏水镍阵列材料

本文论述了用一种新型的金属铝隧道孔模板制备较大面积的纳/微分级结构阵列材料。结合化学镀法在该高纯铝隧道孔模板中制备了具有微纳米阵列结构的金属镍薄膜。研究发现,制备的镍阵列薄膜材料表面呈现超亲水性,以低表面能氟硅烷修饰后,该表面变为超疏水性。     

微纳多孔聚合物薄膜的制备与应用

膜技术在化学技术中占有重要地位,并被广泛应用于生产生活中。随着薄膜技术的不断发展,如何制备获得孔径和分布可控、机械性能优异、功能多样性的多孔聚合物薄膜成为了一个亟待解决的问题。相对于无孔致密聚合物薄膜而言,微纳多孔聚合物薄膜一般密度较低、质轻、比表面积高,并且具有隔音隔热、渗透性好、可塑性强的特点。本综述首先对微纳多孔聚合物薄膜的制备方法进行了总结,包括模板法(硬模板和软模板)、相分离法、静电纺丝、刻蚀法以及其他一些方法。然后阐述了对多孔聚合物薄膜中渗透膜的结构及其相关性能表征测试方法。接着对多孔渗透膜在气体分离、能源、环境和生物工程等方面应用进行了归纳。最后,对当前微纳多孔聚合物薄膜制备方法中存在的缺点与挑战进行了总结,并对其未来的创新应用提出了展望。     

锑基红色发光薄膜材料的制备与表征——一个复合材料创新型实验

将复合发光薄膜材料研究成果转化为化学和材料类专业的本科实验教学内容，设计了一个复合材料创新型实验——锑基红色发光薄膜材料的制备与表征。以苄基溴、吡啶和氧化锑等为原料，制备了一种五溴合锑酸苄基吡啶季铵盐（[BzPy]₂[SbBr₅]）,再以聚环氧乙烯（PEO）为载体通过静电纺丝技术制成发光薄膜材料PEO@[BzPy]₂[SbBr₅]。运用单晶X-射线衍射仪、红外光谱、激光拉曼光谱、固体紫外-可见漫反射光谱、粉末X-射线衍射仪和荧光光谱等手段对薄膜材料的结构和性能进行了表征。学生通过实验可以了解水热法和复合薄膜材料的制备方法，掌握多种分析测试手段表征薄膜材料的结构与性质的技能，激发学习兴趣，锻炼学生科研思维，树立绿色制造理念，提高解决实际问题的能力。     

基于胶体晶体刻蚀构筑含金纳米碗的柱状结构阵列

以二氧化硅微球为掩板,利用各向异性等离子体刻蚀技术对光固化树脂薄膜进行选择性刻蚀,制备出微纳级的顶端带凹陷的柱状结构.在材料表面蒸镀一层金后,得到微纳米级柱顶端带有金纳米碗的特殊结构.通过调整刻蚀时间可以改变光固化树脂薄膜表面的柱状结构的高度.随着柱状结构高度的增加,材料的特征峰从500 nm红移至760 nm.运用时域有限差分(FDTD)方法对这种含贵金属结构的电场分布进行模拟,发现在金纳米碗状结构的边缘处存在高强度的电场,这是材料特征峰产生的原因.这种由材料表面结构变化导致材料在光谱中特征峰迁移的现象在传感、光通讯及小型化光学器件和药物筛选等领域具有潜在应用的价值.     

自卷曲技术在微型储能器件上的应用

微型能源存储器件在可穿戴电子产品、微型自驱动探测器等领域有重要的应用前景,同时为研究储能器件电极结构、电子/离子传导率以及电化学动力学之间的内在联系提供了理想的平台。自卷曲技术是利用材料内部存在的残余应力而实现二维薄膜材料自行弯曲的一种方法。相比于传统微纳制备工艺,这种方法可以在微米尺度下将二维薄膜电极材料有序卷曲排列,为微型储能器件的制备提供了有效、便捷的途径。本文介绍了近些年自卷曲技术在微型能源存储器件上的重要进展,其中包括材料自卷曲的原理、自卷曲电极及其储能性质,并以此为基础,着重阐述了自卷曲技术制备单根管微型锂离子电池和电容阵列的应用实例。总结并展望了自卷曲技术在微型储能器件应用上的未来挑战和重要机遇。     

溶剂热法制备铝掺杂的氧化锌透明导电薄膜

采用溶剂热法在玻璃基片上沉积铝掺杂的氧化锌透明导电膜(AZO)。研究了前驱溶液中Al3+与Zn2+的物质的量的比nAl3+/nZn2+、溶剂热反应温度和反应时间对薄膜物相、形貌、可见光透过率和电阻率的影响。结果表明,溶剂热法所制备的AZO薄膜具有六方纤锌矿结构,Al3+不仅改善薄膜的导电性而且起矿化剂的作用促进薄膜生长,溶剂热反应时间的增加没有使薄膜显著增厚。采用溶剂热法可制备出可见光平均透过率大于80%、方块电阻小于500Ω的AZO薄膜。     

无机微/纳空心球*

无机微/纳空心球材料以其独特的结构、优异的物理化学性能和广阔的应用前景,成为微/纳米材料研究和开发的一个热点领域之一。到目前为止,已研究开发出若干微/纳空心球材料的制备方法,并已制备出具有特殊物理和化学性能的空心球材料。其中,近年来的相关报道尤其多。本文主要回顾了近年来微/纳空心球材料研究和开发的最新进展,其中包括各种制备方法的原理、优缺点和适用范围,并展望了微/纳空心球材料的应用前景。     

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%.     

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.     

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.     

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.     

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.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

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.