氨荒酸基二丁基锡配合物的波谱分析

合成了12种新的氨荒酸基二丁基锡配合物（n-C4H9)2Sn(S2CNRR)2,利用UV,IR和1H NMR表征了它们的结构,结果表明,氨荒酸是以双齿形式与锡原子配位的。     

激光促进异丁烷选择氧化制甲基丙烯酸

用共沉淀法制备了Fe和Mo的复合氧化物。运用XRD,IR,TPD和LSSR技术研究了其晶体结构,表面构造,化学吸附特性和激光促进异丁烷选择氧化反应性能,结果表明,Fe-Mo-O的主体物相为Fe2(MoO4)3,并有少量的MoO3相;其表面上存在Lewis碱位（Mo=O和Mo0O-Fe键中的O）及Lewis酸位Fe^3+,异丁烷的两个甲基H分别吸附在两个相邻的Lewis碱位（Mo=O)上形成双位分子吸附态;在常压和200度条件下,用一定频率的激光激发Mo=O键1000次,异丁烷的转化率为5．8％,其反应产物是异丁烯,甲基丙烯醛和甲基丙烯酸,其中甲基丙烯酸的选择性为80％,根据实验结果,探讨了激光促进异丁烷选择氧化为甲基丙烯酸的表面反应机理。     

过氧化氢氧化硫化钠反应体系的复杂振荡

研究了过氧化氢和硫化钠反应体系在连续流动搅拌反应器中的复杂振荡行为. 观察到11型振荡、12型振荡、非周期振荡以及衰减振荡; 在振荡周期内, 拐点附近区域H+扰动产生的延迟与振荡相位pH有关. 在完全基于硫价态变化的经验速率方程模型的基础上进行数值模拟, 得到的各种复杂振荡行为与实验现象基本一致, 证明了硫价态变化可驱动复杂非线性动力学行为.     

聚丙烯酸/聚(苯乙烯-丙烯酸)二苯酰基甲烷铕(Ⅲ)配合物的合成及其荧光性能

铕(Ⅲ)和二苯甲酰甲烷(HDBM)形成的有机配合物与聚丙烯酸(PAA)(M_n=5000)、聚(苯乙烯-丙烯酸)(PSAA)(M_n=3000)发生配位反应,分别得到配位聚合物Eu(Ⅲ)-DBM-PAA和NaEu(Ⅲ)-DBM-PSAA,产率分别为89.7%和87.3%.红外光谱、紫外光谱、X光电子能谱测试表明,Eu³⁺分别与PAA,PSAA和DBM-发生配位,元素分析和电导率测定结果证明,1个Eu³⁺分别与PAA中2个链节或PSAA中3个链节的羧基和1个DBM-发生配位.Eu³⁺离子在配位聚合物Eu(Ⅲ)-DBM-PAA和Eu(Ⅲ)-DBM-PSAA中的含量分别为28.46%和12.23%.荧光光谱表明,常温下配位聚合物在紫外光下发出强的红光,主要是Eu³⁺离子的5D0→7F2的能级跃迁.     

双层夹心膜电极电位法测定溶剂聚合物膜中杯芳烃-金属离子配合物的生成常数

以双层夹心膜电极为指示电极,采用电位法测定了聚合物膜中活性离子载体杯[6]芳烃乙酯与金属离子形成的配合物的生成常数.提出了一种新的测定夹心膜膜电位的方法,由测得的膜电位可计算出配合物的生成常数.以杯[6]芳烃乙酯为离子载体,测得其与Li⁺,Na⁺,K⁺,Cs⁺和NH⁺₄等离子的配合物生成常数的对数值分别为6.14,6.48.6.74,7.43和6.21.制备了以Cs⁺为主离子的选择性电极,采用固定干扰法,测得对Li⁺,Na⁺,K⁺和NH⁺₄等离子的选择性系数的对数值分别为-3.33,-2.54,-1.6和-2.9.实验结果表明,配合物的生成常数与选择性系数之间有较好的相关性.生成常数越大,电极对相应离子的选择性越高.     

6H-SiC单晶中的微管和小角度晶界

利用透射偏光显微术、同步辐射X射线形貌术、高分辨X射线衍射方法对6H-SiC(0001)晶片中的微管和小角度晶界等缺陷进行了研究.实验发现,在透射偏光显微镜下,微管通常呈现为蝴蝶形,这是由于微管周围存在着应力场,且应力分布不均匀,当线偏振光在通过微管周围区域时传播速度不同造成的.从X射线背反射同步辐射形貌像得到晶片中微管的Burgers矢量大小在2c到10c之间.从晶片00012衍射的双晶衍射摇摆曲线可以看出,晶片的中间大部分区域质量很好,双晶衍射峰为单峰且半峰宽很窄,一般为35"左右.在外围区域双晶衍射峰的半峰宽变宽,有些区域还会出现衍射峰的分裂,这说明外围区域有嵌镶块结构存在.     

Na5[B2P3O13]晶体双晶结构的研究

采用泡生法和b向籽晶生长出尺寸为22mm×24mm×20mm的透明Na5[B2P3O13]晶体.晶体定向中发现(100)和(001)晶面的一级衍射出现双峰;正交偏光显微镜下观察晶体的(010)切片,看到清晰的明暗条纹;当一束激光正入射(010)切片时,产生衍射现象;用同步辐射白光X射线形貌术拍摄了(100)、(010)和(001)切片的Laue像,观察到了晶体的孪晶结构,再借助(010)切片的化学腐蚀研究,推出该晶体为规则的聚片双晶,其结合面为(001).     

三核铜(Ⅰ)配合物的合成与荧光光谱

室温下,通过双核配合物[Cu(dppm)(NO₃)]₂ (dppm=双二苯基膦甲烷)与四苯基硼钠在甲醇和二氯甲烷混合溶剂中反应制备了三核铜(Ⅰ)配合物[Cu₃(dppm)₃(NO₃)(OH)](NO₃),经过红外光谱、热重分析、核磁和ES-MS等现代分析手段表征了配合物的物理化学性质,并进一步研究了配合物在室温下的荧光光谱特征。     

Energy Band Structure of Alq3/TCAQ Heterostructure Complex Film Determinedby Surface Photovoltage Spectroscopy (SPS)

IntroductionOrganic light--emitting diodes (OLEDs) have been extensively investigated since Tanget al. [l] reported a low-voltage high-efficient device in 198712'3]. It has been found that multilayer heterostructures have fascinating advantages in the whole selection of emission color, intensive brightness, high efficiency and relatively low operating voltage['--'J. It is important todetermine the energy band structure of the multilayered film, which will be helpful to interpret the electrol…     

The ZnO non-polar (10 0) surface: an X-ray structural investigation

We performed a structural analysis of the non-polar ZnO (10 0) surface by means of grazing incidence X-ray diffraction. The analysis was conducted on ten rods, smooth surface domains, though of small coherent width, having been obtained after several Ar⁺ sputtering–annealing cycles. The surface derived from the bulk structure exposes one ZnO dimer per unit cell, parallel to the [001] axis. All the existing models, derived from ab initio calculations or low-energy electron diffraction (LEED) analyses, consist in a surface dimer whose O and Zn atoms are shifted inwards, with the O pointing outwards with respect to Zn. Whereas the LEED studies conclude on a dimer distance greater than in the bulk, the theoretical studies agree on a dimer contracted by amounts ranging from 5.5 to 7.5%. This contraction is interpreted as a result of the strong ionicity of ZnO, and is associated with a moderate dimer rotation. The latter, however, is found between 2.3 and 11.4°. Despite the discrepancies between the models, the Zn atom is always found shifted downwards by more than 0.25 Å. This is unambiguously rejected by our data, which show that the Zn atom keeps very close to its bulk position. It is displaced downwards by ΔZ_Zn=−0.06±0.02 Å, and it moves along [001] towards O by ΔX_Zn=0.05±0.02 Å. We denote a trend for the O atom to be displaced downwards too, with a concomitant displacement towards Zn. The faint X-ray scattering of O prevents us from assessing its position with accuracy. Depending on the choice of position for Zn in the error bar range, the buckling is evaluated as between −6.5 and 3°, or between −4 and 0.5°. The dimer distance is evaluated equal to 1.90 Å, with a deviation equal either to 0.06 or 0.11 Å.