无溶剂一锅法合成1,4-二氢吡啶

碳酸氢铵、醛和1, 3-二羰基化合物于70 ℃无溶剂条件下缩合以86～97%的产率得到1, 4-二氢吡啶.     

固定化辣根过氧化物酶在有机/水混合溶液中的电化学

用魔芋多糖(KGM)将辣根过氧化物酶(HRP)固定在玻碳电极(GCE)表面, 制备了HRP-KGM膜修饰电极. 在乙醇等亲水性有机溶剂与水的混合溶液中, 包埋在KGM中的HRP 可以与电极发生直接电子传递, 且能催化还原过氧化氢、氢过氧化异丙基苯、氢过氧化叔丁基、过氧化丁酮等过氧化物. HRP-KGM膜修饰电极具有较好的稳定性和重现性, 可用于这些物质的定量检测.     

窄分布聚丙烯酸-g-聚甲基丙烯酸酯接枝共聚物的合成

利用合成的一种新型原子转移自由基聚合大分子引发剂和从主干接枝的方法制备了窄分布的两亲性接枝共聚物聚丙烯酸-g-聚甲基丙烯酸酯, 并对其结构进行表征. 产物主链和侧链的分子量可分别通过调整单体与引发剂的投料比和反应时间进行控制, 结构规整, 侧链单体适用范围广. 该合成方法不仅推动了接枝共聚物合成研究的进展, 其产物更为两亲性接枝共聚物自组装行为的研究提供了很好的研究对象.     

Kinetics of the transformation process of PbSO4 to PbO2 in a lead anodic film

The kinetics of the nucleation and growth of PbO₂ during the potentiostatic oxidation of PbSO₄ in a lead anodic film was studied using linear sweep voltammetry, potential-step and ac impedance tracing methods. The film investigated is the partially reduced anodic PbO₂ film formed by polarizing a lead electrode in 4.5 M H₂SO₄ solution first at 1.3 V vs. Hg|HgSO₄ for 20 min and then at 0.9 V for 5 min. The nucleation and growth process begins some time after the potential step and is completed within 60 s. The pre- and post-nucleation and growth processes correspond to the growth of the anodic film formed by the oxidation of the lead substrate. The mathematical equations representing the current-time and capacitance-time transients are derived taking the background oxidation current into account. The experimental results are well fitted by these equations. The process obeys the laws of two-dimensional instantaneous nucleation and growth.     

Ru2(ap)4(sigma-oligo(phenyleneethynyl)) molecular wires: synthesis and electronic characterization

Reported in this contribution are the synthesis, characterization, and charge transport properties of wire-like Ru2(ap)4(OPEn), where ap is 2-anilinopyridinate and OPE is -(CCC6H4)nSCH2CH2SiMe3 with n = 1 (1) and 2 (2). Scanning tunneling microscopy (STM) measurements of compound 2 inserted into a SAM of C11 thiol reveal that molecule 2 exhibits (i) the stochastic switching characteristic of wire molecules embedded in insulating SAMs and (ii) higher conductivity than the C11 thiol SAM. More importantly, analysis of the molecular electronic decay constant (beta) exhibits a decrease of at least 15% as compared to purely organic molecular analogues. Hence, the transport characteristics of molecules can be significantly improved for nanoscale electronics through the incorporation of a Ru2 fragment into conjugated backbone.     

CPCWS中水质子的核磁共振自旋晶格弛豫时间和化学位移

运用核磁共振手段，揭示了浆体中水的形态及其动态行为，并研究浆体性质与之的关联.实验测得神府煤-石油焦-水浆（CPCWS）中水质子的化学位移与煤焦中煤的百分含量的线性关系.并从NMR测得束缚水的化学位移δb ，导出计算浆体中束缚水百分含量的公式.从CPCWS中水质子的化学位移与浆体表观粘度的相关曲线可确定最佳配比的浆体.测得全焦浆中水质子自旋-晶格驰豫时间T1比全煤浆大42倍，讨论了CPCWS的T1随煤含量的变化趋势.实验表明,T1可作为CPCWS中碳质点的疏水或亲水性以及水分子形态和动态行为的定量表征.     

两亲型聚L-亮氨酸-聚乙二醇单甲醚嵌段共聚物的合成与表征

开环聚合;生物降解共聚物;两亲型聚L-亮氨酸-聚乙二醇单甲醚嵌段共聚物的合成与表征     

Design and Performances of a Carbon Monoxide Sensor Using Mid-Infrared Absorption Spectroscopy Technique at 4.6 µm

Based on infrared absorption spectroscopy technique, a carbon monoxide sensor was developed using the fundamental absorption band of carbon monoxide molecule at the wavelength around 4.6 µm. The developed sensor consists of pulse-modulated wideband incandescence, open ellipsoid light-collector gas-cell, dual-channel detector, and control and signal-processing module. With the prepared standard carbon monoxide gas sample, sensing characteristics on carbon monoxide were investigated using the sensor. Experimental results reveal that the limit of detection is about 10 ppm, the relative error at the limit of detection point is less than 14%, and that is less than 7.8% within the low concentration range of 20～180 ppm. The maximum absolute errors of 50 min long-term measurement on the 0 and 14 ppm CO gas samples are about 3 and 3.17 ppm, respectively, and the standard deviations are as small as 0.18 and 1.25 ppm, respectively. Compared with the reported carbon monoxide detection systems utilizing quantum cascaded lasers and distributed feedback lasers, the proposed sensor shows potential applications in carbon monoxide detection under the circumstances of coal-mine and environmental protection, by virtue of high performance, low cost, simple optical structure, and so on.     

HgCdTe薄膜的输运特性及其应力调控

窄禁带直接带隙半导体材料碲镉汞(Hg1–xCdxTe)是一种在红外探测与自旋轨道耦合效应基础研究方面都具有重要应用意义的材料.本文对单晶生长的体材料Hg0.851Cd0.149Te进行阳极氧化以形成表面反型层,将样品粘贴在压电陶瓷上减薄后进行磁输运测试,在压电陶瓷未加电压时观察到了明显的SdH振荡效应.对填充因子与磁场倒数进行线性拟合,获得样品反型层二维电子气的载流子浓度为ns=1.25×10^16m^-2.在不同磁场下,利用压电陶瓷对样品进行应力调控,观测到具有不同特征的现象,分析应是样品中存在二维电子气与体材料两个导电通道.零磁场下体材料主导的电阻的变化应来源于应力导致的带隙的改变;而高场下产生类振荡现象的原因应为应力导致的二维电子气能级的分裂.     

红色磷光喹喔啉铂(II)配合物及其有机电致发光器件的制备

利用2,3-二苯基喹喔啉和氯亚铂酸钾(K2PtCl4)反应,合成了一种新型喹喔啉铂的配合物(DPQ)Pt(acac),通过元素分析,1HNMR测定对配合物结构进行了表征,结果显示得到的是目标化合物.利用紫外光谱和荧光光谱对配合物进行了研究.利用该材料作为磷光染料制备了结构为ITO/NPB(21nm)/NPB∶7%(DPQ)Pt(acac)(17.5nm)/BCP(7nm)/Alq3(21nm)/Mg∶Ag(10∶1)(120nm)/Ag(10nm)的有机电致发光器件(OLED).结果表明,该配合物在442和485nm处存在单重态1MLCT(金属到配体的电荷跃迁)和三重态3MLCT的吸收峰;在632nm处有较强的金属配合物三重态的磷光发射;该器件的启动电压是5.0V,器件的最大亮度为1516cd·m-2,外量子效率为0.66%,流明效率为0.26lm·W-1,是一种红色磷光材料.