Ni3(Tix,V1-x)合金系中的长周期结构

本文利用电子衍射及高分辨点阵象实验方法证实了Ni₃(Ti_x,V_1-x)合金系在铸态下存在有9R,10H,16H,20H,21H,44H等长周期结构以及2H结构。它们与体心四方基体相(结构与Ni₃V相同)及六角基体相(结构与Ni₃Ti相同)有固定取向关系:{001}_长周期∥{001}_(Ni3Ti)∥{112}_{Ni3V);〈100〉长周期∥〈100〉(Ni3Ti)∥〈110〉(Ni3V)。样品经长期高温退火处理后其它长周期结构均向9R结构转变。 关键词：}     

含烯烃配体的过渡金属卡宾络合物的研究——Ⅺ.新型环己二烯(二羰基)[乙氧基(芳基)卡宾]铁络合物的异构化产物的合成、波谱和晶体结构

1,3-环己二烯(三羰基)铁(Ⅰ)与芳基锂,ArLi(Ar=C_6H_5,m-,p-CH_(?)C_6H_4,p-CH_3OC_6H_4,p-CF_3C_6H_4),在乙醚中低温下反应,所生成的酰羰基锂盐随后用Et_3OBF_4在水溶液中0℃烷基化,生成5个组成为C_6H_8(CO)_2Fec(OC_2H_5)Ar的橙红色结晶化合物(Ⅱ—Ⅵ)。根据元素分析,光谱研究和X射线品体结构测定,Ⅱ—Ⅵ为环己二烯(二羰基)[乙氧基(芳基)卡宾]铁络合物的异构化产物。本文报道和讨论了它们的合成、光谱和X射线衍射的研究结果,并探讨了可能的反应机制。#原图像不清楚     

THE CRYSTAL STRUCTURE OF THE ADDITION COMPOUND OF DECAVANADIC ACID AND 5,7-DIMETHYL-2, 3-DIHYDRO-1, 4-DIAZEPINIUM

The title compound crystallizes in the space group C_(2h)~5-P2_1/n with unit cell constantsa=10.938 A, b=19.189 A, c=13.384 A and β=105.09°. Intensities of 4022 independent reflec-tions were collected with four-circle diffractometer using MoKa radiation. After reduction fordiffractometer data, we derived first the position parameters of all the V atoms by directmethod using SHELXTL program. The coordinates of all the non-hydrogen and hydrogenatoms were obtained from successive Fourier and difference sytheses. The block-diagonalleast-squares refinement for all atoms gave a final discrepancy weighted factor R_w=0.050. The result of structure analysis shows that four protons of each decavanadic acid arecaptured by the nitrogen atoms involved in the azepine molecules which are condensation pro-ducts of ethylenediamine with acetylaceton. In crystal, the isopoly-decavanadate anion, 7-member heterocyclic azepium and the crystal water are linked together by ionic forces andhydrogen bonding and the chemical content within a unit cell has been identified as 2[H_2V_(10)O_(28)]~(-4)·8[C_7N_2H_(13)]~( 1)·12H_2O.     

CRYSTAL STRUCTURE INVESTIGATION OF VANADYL COMPLEXES OF TRIDENTATE LIGAND (Ⅰ)——THE CRYSTAL STRUCTURES OF BIS[(1-(2,4-PENTANE- DIONATO(NITROBENZOYL) HYDRAZONE)-2- ETHOXY)OXOVANADIUM] AND BIS-[(1-(2, 4-PENTANEDIONATO-(3-NITROBENZOYL) HYDRAZONE)-2- METHO

The title complexes were obtained by the reactions of bis(2,4-pentanedionato)oxovanadium VO(Acac)_2 and m-nitrophenylhydrazide m-NO_2PhCONHNH_2 in the media EtOH and MeOH respectively. The compound (Ⅰ) crystallizes in the space group PT with unit cell dimensions a=8.123(2), b=10.409(5), c=10.822(4), α=65.78(3)°, β=85.50(3)°,γ=89.04(3)°. The compound (Ⅱ) crystallizes in the space group P2_1/a with unit cell dimensions a=7.745(2), b=19.164(5), c=10.787(4), β=107.87(2)°. The resuhs of structural analyses show that the two compounds have the same characteristics: the tridentate ligand formed by condensation occupies three of the four equatorial positions of vanadium and the rest equatorial position is occupied by alkoxy group RO~-. As RO~-group also bridges the sixth coordinated position of each vanadium atom, it brings about the formation of the new type binuclear complexes of vanadium.     

(±)-5,3’-二羟基-7,8-(2,2-二甲基吡喃)-4’-甲氧基黄烷酮的首次全合成

以廉价的异香草醛和2,4,6-三羟基苯乙酮为起始原料,经过C-异戊烯基化、环化、选择性的保护酚羟基、羟醛缩合、催化环化等步骤,脱保护基,以6.7%的总收率首次完成了天然吡喃型黄烷酮(±)-5,3’-二羟基-7,8-(2,2-二甲基吡喃)-4’-甲氧基黄烷酮的全合成.所有新化合物的结构都经过IR,1H NMR,MS,HRMS确认.     

负载型钙钛矿La0.8Sr0.2MnO3/SBA-15催化燃烧甲苯的研究

采用逐层负载-孔道内氨/水蒸气原位羟化法制备了一系列负载型钙钛矿La_0.8Sr_0.2MnO₃/SBA-15催化剂,用XRD、BET、TG-DTG、XPS、H₂-TPR等手段对催化剂的物性结构等进行了表征,并在常压连续流动固定床反应器上评价了该催化剂对甲苯催化燃烧的催化性能。结果表明,逐层负载-孔道内氨/水蒸气原位羟化法的使用有助于活性组分La_0.8Sr_0.2MnO₃进入SBA-15的孔道,并在SBA-15上形成钙钛矿结构。La_0.8Sr_0.2MnO₃/SBA-15上钙钛矿结构的形成和晶格氧的出现,可为催化剂提供较多的活性中心,有利于其催化燃烧甲苯的活性。     

糖芯片制备和应用的最新研究进展

糖芯片是一种研究微量糖与生物大分子之间相互作用的生物检测技术,因其具有用量少、快速、高效和高通量等特点,现已被广泛应用到药物开发、免疫学,临床诊断和细菌检测等诸多领域中。近年来,尽管对糖芯片的制备方法和应用进行了较为深入的研究,但对糖芯片的制备方法和应用的综述还较少报道。本文主要介绍糖芯片的制备原理、非化学修饰和化学修饰制备糖芯片的最新方法,然后对糖芯片在自组装等方面应用的最新进展进行综述,并对糖芯片所遇到的挑战和发展趋势也作了展望。     

2,5-二(4’-羧基苯基)-1-苯基吡咯对胺的“点亮”荧光检测

基于水溶性2,5-二(4’-羧基苯基)-1-苯基吡咯的羧酸钠盐(TPP-2COONa)具有质子化荧光淬灭、去质子化荧光增强的特征.在研究了TPP-2COONa的紫外吸收光谱和荧光发射光谱对pH的响应规律的同时,以此为荧光探针,证实了TPP-2COOH对于多种胺类(氨水、二异丙胺、异丙胺和三乙胺)荧光增强响应明显,而对芳香胺(吡咯、苯胺、吡啶)没有任何荧光响应,其中对于氨水最为敏感,在很窄的pH区间和低浓度范围内荧光强度大幅度增长,体现了该探针对于氨水具有良好的选择性和灵敏度,并可简易实现"在线裸眼检测".     

S波段相对论速调管放大器锁相特性

对相对论速调管放大器（RKA）锁相特性进行了粒子模拟与实验研究。在2.5维粒子模拟中,研究了电子束电压波形特征对RKA锁相特性的影响,结果表明:电子束电压波形上冲对RKA锁相特性有正面影响,即能够减小相位差达到锁定状态的时间,幅度为20%的上冲导致大约23的相位差变化;波形顶降则对RKA锁相特性有负面影响,可使相位差过早地偏离稳定值,幅度为5%的顶降大约能引起50的相位差偏离;电压波形的上升时间对RKA相位锁定特性也有影响,但规律不明显。在三维粒子模拟和实验中,研究了导引磁场大小对RKA锁相特性的影响,结果表明,在1.6 T以下,RKA输出微波与种子源微波之间的相位差锁定值总体上随导引磁场的增大而减小,在细节上,呈现阶跃形式,即一定范围内导引磁场大小变化不会导致相位差的改变。实验研究表明,在导引磁场范围为0.6~1.2 T时,RKA锁定相位差随导引磁场的增大而减小,阶跃现象不明显。