电子扫描深能级瞬态谱(SDLTS)测量系统及其应用

本文报导了在ＪＸＡ－３Ａ电子探针上，研制了电子束感生电流装置、电子束消隐装置、可微功低温样品台以及超慢速电子束扫描装置，配置Ｂｏｘｃａｒ平均器。成功地开发了电子束扫描深能级瞬态谱测量系统，它的温度范围为８０－４５０Ｋ，空间分辨率约１０μｍ，测量稳定度为１．５％。对ＧａＡｓ和Ｓｉ中的深能级及其空间分布进行了测量，并与其结构缺陷进行了对比研究。     

电感耦合等离子体原子发射光谱专家系统中谱线激发模型

阐述了ＩＣＰ－ＡＥＳ专家系统中ＡＥＳ电离和激发模型的基本原理，研究了模拟中应用ｎｏｎ－ＬＴＥ理论的正确性以及所需的支持数据库。利用Ｂｏｌｔｚｍａｎｎ曲线，讨论了Ｂｏｌｔｚｍａｎｎ温度的测量值随能级激发能变化的现象，并与类似条件下的经验Ｂｏｌｔｚｍａｎｎ曲线进行对比，证明了专家系统中ＡＥＳ电脑和激发模型可靠性。     

噁二唑载流子传输材料的合成及性能研究

合成了噁二唑类衍生物，利用偏光显微镜、差热扫描和广角X射线衍射等手段对材料的相结构进行了表征，并利用紫外—可见吸收光谱和电化学方法表征了材料的能级结构。在此基础上，设计制备了以噁二唑类衍生物为载流子传输材料，以MEH—PPV为发光材料的单层电致发光器件。结果表明，噁二唑类衍生物具有液晶性和电子传输特性，是一类较有发展前景的载流子传输材料。     

电化学扫描隧道显微术:以Cu在Au(111)表面初始阶段电沉积为例

电化学扫描隧道显微术能在电解质溶液中获得随电位变化的电极表面高空间分辨率的结构信息及跟踪某些反应过程，为从高空间分辨率的角度理解界面结构和电极过程提供了一种强有力的手段。本文以电化学扫描隧道显微术研究Cu在Au(111)上电沉积初始阶段过程为例，与读者交流电化学扫描隧道显微术实验方面的经验，涉及实验装置、实验操作、实验步骤和注意事项等。     

DDA在碱酸介质中的存在状态与缓蚀行为的关系

利用电化学方法、物理检测技术及表面分析技术，针对十二烷基胺（ＤＤＡ）作用于ＦｅＮｉＳｉＢ非晶合金表面时，在不同浓度范围内，缓蚀效率与缓蚀剂２在不同的对应关系的现象、探讨了ＤＤＡ的存在状态与其缓蚀行为的关系，利用物理测量技术对临界浓度前后ＤＤＡ的存在状态进行了分析，利用扫描隧道显微镜捕获了高浓度时ＤＤＡ在非晶合金表面的典型结构，详细阐述了ＤＤＡ对非晶合金的微观缓蚀机制。     

微量Gd对Ag－Cu基合金再结晶的影响

用硬度测量、示差扫描量热（ＤＳＣ）、金相显微镜、透射电镜和Ｘ射线衍射分析等技术研究了富Ａｇ的Ａｇ～Ｃｕ合金和含微量Ｇｄ的Ａｇ－Ｃｕ－Ｇｄ合金的再结晶。并根据Ａｇ－Ｃｕ－Ｇｄ三元系相图及合金显微结构分析，讨论了微量Ｇｄ对Ａｇ－Ｃｕ合金再结晶的影响。结果表明，在Ａｇ－Ｃｕ合金中，微量Ｇｄ的添加，使其再结晶温度大幅度提高，再结晶激活能增加。     

微量Gd对Ag—Cu基合金再结晶的影响

用硬度测量，示差扫描量热、金相显微镜、透射电镜和Ｘ射线衍射分析等技术研究了富Ａｇ的Ａｇ－Ｃｕ合金和含微量Ｇｄ的Ａｇ－Ｃｕ－Ｇｄ合金的再结晶。并根据Ａｇ－Ｃｕ－Ｇｄ三元系相图及合金显微结构分析，讨论了微量Ｇｄ对Ａｇ－Ｃｕ合金再结晶的影响。结果表明，在ＡＧ－Ｃｕ合金中，微量Ｇｄ的添，使其再结晶温度大幅度提高，再结晶激活能增加。     

基于扫描电镜和能谱仪的薄膜表面形貌和厚度同时测量研究

扫描电子显微镜通过电子束轰击样品产生的二次电子、背散射电子等实现对样品表面形貌的观测，通过对样品横断面的观测来获得薄膜厚度信息，但难以实现对薄膜表面形貌和厚度的同时观测。通过能谱仪研究各种厚度的薄膜同其激发的特征X射线计数率之间的关系，实现了通过特征X射线计数率来测量薄膜厚度的方法。对于激光吹气系统所需的钨薄膜而言，结果表明，计数率随薄膜厚度的增加先线性增加后趋于稳定，利用该曲线的直线部分作为刻度曲线，可实现对5～19μm范围内钨薄膜表面形貌和厚度的同时测量，精度约为10%,通过增加电子能量可实现对更厚样品的测量。该方法可推广到其他种类的薄膜研究，有助于推动薄膜物理研究的开展。     

氯乙烯的真空紫外光电离

利用同步辐射(SR)作为真空紫外光源,结合超声分子束装置,可从分子反应动力学的角度对各种分子及小团簇在全波长范围内进行光电离和光离解研究.例如:通过光电离质谱对各种反应产物进行认定;结合光电离效率曲线(PIE)测定分子及团簇的电离能,确定能级结构.本文报导了对C_2H_3Cl 在50—140nm 波长范围内进行光电离研究的初步结果.我们用四极质谱测量了各种离子碎片的光电离谱,讨论了该分子的单光子电离的反应通道.1 实验     

专利介绍

专利名称：水质测量装置 专利申请号：CN200420110604．3 公开号：CN2755610 申请日：2004—12—02 公开日：2006—02—01 申请人：台湾省廖益嘉 一种水质测量装置．其在一平板状主体上设立一凹陷处，该凹陷处可以容纳待测量水质的样品水，通过设置在该凹陷处内的正负极探针，将样品水的电荷信号传递至设于主体上的取样单元，再由微处理器运算得知其水质状况后，     

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%.     

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.     

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

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.     

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.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

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.