液相二氧化钛纳米微粒的荧光和共振散射光谱特性

以钛酸四丁酯(TBTi)为前驱体,利用微波高压反应法合成了纳米二氧化钛溶胶,并与Ti(SO4)2水解法制备出的二氧化钛纳米微粒对比.考察了两种前驱体制备的二氧化钛纳米微粒荧光光谱及共振散射光谱特性,用TBTi制备的二氧化钛纳米微粒在320 nm有一个共振散射峰,在470 nm有一个同步散射峰,在360,400和470 nm处有三个荧光发射峰;用Ti(SO4)2制备的二氧化钛纳米微粒在340 nm有个共振散射峰,在470 nm有一个同步散射峰,400和470 nm处有两个荧光发射峰.反应条件对共振散射强度的影响与其对荧光的影响变化趋势一致,但共振散射光强度较荧光强度强得多.     

Preparation of visible light responsive N doped TiO2 via a reduction-nitridation procedure by nonthermal plasma treatment

A visible light responsive N-doped TiO₂ was prepared via a reduction-nitridation procedure by nonthermal plasma treatment. X-ray diffraction, N₂ adsorption, UV-vis spectroscopy, photoluminescence, and X-ray photoelectron spectroscopy were used to characterize the prepared TiO₂ samples. The plasma treatment did not change the phase composition and particle sizes of TiO₂ samples, but extended its absorption edges to the visible light region. The photocatalytic activities were tested in the degradation of an aqueous solution of a reactive dyestuff, methylene blue, under visible light. The photocatalytic activities of TiO₂ prepared by reduction-nitridation procedure were much higher than that of samples prepared by simple nitridation treatment. The enhanced activity was ascribed to the substitutional N-doping and appropriate concentration of oxygen vacancies. TOHN10 prepared by reduction-nitridation procedure exhibited excellent photocatalytic stability. A possible mechanism for the photocatalysis was proposed.     

The dispersion of platinum on silica-correlation of esca and gas adsorption data

For five catalyst samples (Pt supported on silica) prepared by an ion exchange method, a correlation plot of chemisorption data against ESCA Pt/Si signal area ratio was a smooth curve essentially linear at low surface Pt levels but curving at high Pt values. Two samples prepared by an impregnation method were also studied. A line connecting points on the correlation plot for these samples was approximately parallel to but not coincident with the correlation curve obtained for samples prepared by ion exchange. The data strongly support the use of ESCA for measurements of metal particle size (dispersion) in catalyst systems such as these.     

Morphology,Crystallization and Formation Mechanism of Poly(Vinylidene Fluoride) Membranes Prepared with Immersion Precipitation: Effect of Maturation Time

Poly(vinylidene fluoride) (PVDF) membranes were prepared by the immersion precipitation method. Effects of the maturation time of dopes on the morphology and crystallization of the prepared membranes were investigated. The analysis showed that the maturation time played an important role in determining the morphology of the prepared membranes. For the dope prepared in the initial day, liquid–liquid demixing preceded solid–liquid demixing in the process of the membrane formation. The morphology of the cross section of the prepared membrane (M1) was finger-like structures with a sponge substrate beneath the porous skin. During the maturation, the dopes underwent a microscopic phase separation and the PVDF crystallized, which resulted in the existence of micro-liquid phases and micro-solid phase crystalline areas in the dopes. In the process of the membrane formation, liquid–liquid demixing took place by nucleation and growth of droplets of the polymer rich phase in the micro-liquid phase. The micro-solid phase crystallites were connected together by the polymer chains, and formed a three-dimensional network gelation morphology. The crystal structure of M1 was mainly β crystals. With increasing maturation time of the dopes, the proportion of β decreased crystals, but that of α crystals increased for the prepared membranes.     

Studies of porosity and diffusion coefficient in porous matrices by computer simulations

We present a series of molecular dynamics simulations to study the porosity on different matrix configurations. The matrices were prepared using two different processes. In the fist method we used direct simulations of a fluid at a fixed density and the matrix was taken from the last configuration of its particles. In the second method we simulated a binary mixture where one of the components served as a template material and the final porous matrix configuration was obtained by removing template particles from the mixture. Matrices were prepared at different densities and at different matrix particle interactions. The results showed that the matrix structure and the matrix porosity were affected by the way the porous matrices were prepared. Finally, we also investigated the diffusion of a fluid inside the matrices. The diffusion coefficient was measured by mean square displacements of the particles in the fluid. It was observed that this quantity was also affected by the kind of porous matrix employed. The calculations were performed for several fluids at different densities in the different porous matrices. From these studies we observed that the highest porosity and diffusion coefficient were found in matrices prepared with attractive particle interactions and without any template.     

Synthesis and characterization of new magnetically recoverable molybdenum nanocatalyst for epoxidation of olefins

New heterogeneous molybdenum catalyst was prepared through covalent attachment of a Schiff base ligand on the surface of silica coated magnetite nanoparticles via aminopropyl spacer and subsequent complexation with MoO₂(acac)₂. The prepared nanocatalyst was characterized with Fourier transform infrared spectroscopy, X-ray diffraction, scanning and transmission electron microscopies and vibrating sample magnetometry. Catalytic epoxidation of some olefins and allylic alcohols by prepared nanocatalyst using tert-butyl hydroperoxide and cumene hydroperoxide as oxidants was achieved with good activities and selectivities.     

微柱电泳与紫外-可见分光光度法的在线联用

自制了紫外-可见分光光度计的微柱电泳高效分离附件, 介绍了X射线衍射法在电泳微柱制备中的应用以及微柱电泳与紫外-可见分光光度法的在线联用。使用水热法合成均匀石英微米晶粒,采用X射线衍射法表征和控制产物的晶相,并用扫描电子显微镜观察产物形貌。将合成的石英微米晶粒均匀填充在2 mm i.d.石英管中,制成电泳微柱。通过微柱电泳与紫外-可见分光光度法在线联用,对非衍生的色氨酸、苯丙氨酸和酪氨酸进行了分离检测。检出限分别为0.037, 0.20和0.20 μmol·L-1,色氨酸的分离效率为每米4.5×104,电泳微柱的样品容量达到35 μL。实验结果表明,填充石英微米晶粒的微柱电泳可抑制大柱径电泳热效应,增大样品容量,提高检测灵敏度。微柱电泳与常规紫外-可见分光光度法联用可简便地对混合物进行在线分离和测定,进一步拓宽了紫外-可见分光光度计在光谱重叠组分痕量分析中的应用。     

透射光谱法测试双面薄膜的光学参数

由于普通的化学气相沉积法制作高掺Sn的二氧化硅薄膜比较容易产生结晶,而溶胶-凝胶法制备薄膜化学组成比较容易控制,可以制作出掺Sn浓度较大的材料。文章采用了溶胶-凝胶的方法制备出了66 mol%和75 mol%两种不同浓度的掺Sn的SiO₂薄膜,用浸渍法多次提拉薄膜以增加薄膜的厚度,之后用紫外-可见分光光度计测量了薄膜的透射光谱。之前基于透射光谱的方法计算玻璃基底上薄膜的光学参数都是针对单面薄膜,该文针对浸渍法产生的双面薄膜,建立了相对应的薄膜模型,并分别用包络线法计算出了两种不同薄膜样品的光学参数。计算结果表明两种不同薄膜样品的折射率随着波长的增加而增加,薄膜的厚度都为900 nm左右。     

自支撑聚酰亚胺/锆膜的制备及性能改善

 采用直流磁控溅射法制备自支撑锆(Zr)膜,采用二步法制备聚酰亚胺(PI)膜,在Zr膜表面沉积PI膜得到自支撑PI/Zr复合膜。均苯四甲酸酐(PMDA)和二甲基二苯醚(ODA)在二甲基乙酰胺(DMAC)中反应得到聚酰胺酸(PAA),然后PAA高温亚胺化得到PI;PI成膜时采用提拉法成膜。经国家同步辐射实验室计量线站测定,实际测量结果与理论分析一致,PI膜的引入虽然会导致自支撑薄膜透过率有所下降,但在类镍-银软X射线13.9 nm波段PI(200 nm)/Zr(300 nm)和PI(200 nm)/Zr(400 nm)自支撑薄膜的透过率仍然分别达到14.9%和7.5%。     

制备工艺对掺杂NaYF4:Er3+,Yb3+发光纳米晶的聚合物光波导放大器性能的影响

制备了NaYF₄：Er³⁺,Yb³⁺纳米晶,表征了纳米晶的形貌,通过物理掺杂的方式将纳米粒子掺杂到SU-8中作为光波导放大器的芯层材料,优化了波导放大器的尺寸,利用旋涂、刻蚀等工艺,在二氧化硅衬底上制备了光波导放大器。实验中用光漂白法和湿法刻蚀两种方法制备光波导放大器,分别给出了两种方法制备的器件的结构、工艺流程、光场模拟结果,并对两种方法制备的器件的放大特性进行了测试。测试结果表明,当980 nm波长的泵浦光功率为241 mW且1 550 nm波长的信号光功率为0.1 mW时,使用湿法刻蚀法制备的放大器得到2.7 dB的相对增益。当980 nm波长的泵浦光功率为235 mW且1 550 nm波长的信号光功率为0.1 mW时,使用光漂白法制备的放大器得到4.5 dB的相对增益。根据以上测试结果,分析了两种工艺对器件性能的影响。