Possibilities and limitations of synchrotron X-ray powder diffraction with double crystal and double multilayer monochromators for microscopic speciation studies

The performance of a combined microbeam X-ray fluorescence/X-ray powder diffraction (XRF/XRPD) measurement station at Hamburger Synchrotronstrahlungslabor (HASYLAB) Beamline L is discussed in comparison to that at European Synchrotron Radiation Facility (ESRF) ID18F/ID22. The angular resolution in the X-ray diffractograms is documented when different combinations of X-ray source, optics and X-ray diffraction detectors are employed. Typical angular resolution values in the range 0.3–0.5° are obtained at the bending magnet source when a ‘pink’ beam form of excitation is employed. A similar setup at European Synchrotron Radiation Facility beamlines ID18F and ID22 allows to reach angular resolution values of 0.1–0.15°. In order to document the possibilities and limitations for speciation of metals in environmental materials by means of Hamburger Synchrotronstrahlungslabor Beamline L X-ray fluorescence/X-ray powder diffraction setup, two case studies are discussed, one involved in the identification of the crystal phases in which heavy metals such as chromium, iron, barium and lead are present in polluted soils of an industrial site (Val Basento, Italy) and another involved in the speciation of uranium in depleted uranium particles (Ceja Mountains, Kosovo). In the former case, the angular resolution is sufficient to allow identification of most crystalline phases present while in the latter case, it is necessary to dispose of an angular resolution of ca. 0.2° to distinguish between different forms of oxidized uranium.     

Fabrication of self-assembled ultrathin photochromic films containing mixed-addenda polyoxometalates H5[PMo10V2O40] and 1,10-decanediamine

A layered phosphovanadomolybdate/1,10-decanediamine (1,10-DAD) self-assembled ultrathin film was fabricated by means of alternating adsorption of mixed-addenda polyoxometalates (POMs) (phosphovanadomolybdate, H₅[PMo₁₀V₂O₄₀]) and 1,10-DAD, and its photochromic properties were investigated. It is found that the self-assembled multilayer (SAM) film shows high-photochromic response, excellent photochromic stability and reversibility. The photochromic behavior of the SAM is closely related to the reduction potentials of addenda atoms in mixed-addenda POMs. In the case of photo-reduced mixed-addenda POMs, the electron is localized on the more reducible atom, and the addenda atoms with higher reduction potentials show prior photochromism compared with those with lower reduction potentials. The coloration speed is improved after introduction of V into molybdenum POM. The well-ordered lamellar structure of the film was well maintained during the coloration.     

Synthesis of Nitrogen Incorporated Carbon Nanotubes with Different Diameters by Catalytic Pyrolysis of Butylamine

Bamboo-like nitrogen-doped carbon(CNx) nanotubes were synthesized by chemical vapor deposition (CVD) at a high reaction temperature of 600―900 °C. The butylamine and Fe/SBA-15 molecular sieve have been used as precursor and catalyst, respectively. Transmission electron microscopy(TEM) and high resolution transmission electron microscopy(HRTEM) observations show that the outer diameter and wall thickness as well as the inner diameter were increased with increasing reaction temperature in a temperature range of 600―800 °C. A synergism mechanism of the growth through bulk diffusion and the competitive growth through surface diffusion functions during the synthesis of CNx nanotubes was proposed.     

Fabrication of polymer compound microlens by lens-on-lens microstructures

We proposed a novel method for fabricating polymer compound microlenses (PCMLs) using micro-inkjet technique and subsequent curing process. Two different types of PCMLs with sandwich microstructure (PDMS-Glycerol-PDMS), concave and convex PCMLs, have been designed and fabricated in experiments. Convex PCML has two real images and two foci. The concave PCML has one real and one virtual focal planes, which can generate one real image and one virtual image respectively. Moreover, the diameter of concave PCML can be controlled by adjusting the curing time and temperature. The proposed method is simple, efficient and suitable for realizing large-scale high numerical aperture PCMLs array, which has potential applications in diverse optical systems such as optical storage and three-dimensional imaging.     

氧化石墨烯/聚电解质层层自组装制备单价离子选择性膜

采用层层自组装法在改性聚丙烯腈(PAN)膜表面交替沉积聚乙烯亚胺(PEI)和聚丙烯酸-氧化石墨烯(PAA-GO)混合液,制得了单价离子选择性复合膜。X射线衍射(XRD)测试结果表明成功合成了氧化石墨烯(GO)并在复合膜中均匀分散。扫描电镜(SEM)观察结果证实了多层聚电解质PEI/PAA-GO成功地组装在基膜上,并用紫外-可见(UV-Vis)光谱进一步证实了组装过程的均匀性和连续性。接触角和性能测试表明加入GO后,复合膜的亲水性和单价阳离子的选择性明显增大。这种高通量、高选择性的防污复合膜在分离和水的软化方面有很好的应用前景。     

Fabrication of Covalently Linked PAH/PVS Layer-by-layer Assembled Multilayers via a Post-photochemical Cross-linking Strategy

A post-photochemical cross-linking strategy was successfully demonstrated to enhance the stability of polyelectrolyte poly(allylamine hydrochloride)(PAH)/poly(vinylsulfonic acid sodium salt)(PVS) multilayers. Conventional polyelectrolyte multilayers of PAH/PVS are usually fabricated through electrostatic layer-by-layer(LbL) assembly, resulting in poor stability, especially in basic solutions, which leads to the urgent demand for converting weak electrostatic interactions into covalent bonds to enhance the stability of the multilayers. This stability problem has been ultimately addressed by post-infiltrating a photosensitive cross-linking agent, 4,4'-diazostilbene-2,2'- disulfonic acid disodium salt(DAS), into the LbL assembled films to initiate the photochemical reaction to cross-link the multilayers. The obviously improved stability of the photo-cross-linked multilayers was demonstrated through experiments with basic solution treatments. Compared to the complete decomposition of uncross-linked multilayers in basic solution, over 74.4% of the covalently cross-linked multilayers were retained under the same conditions, even after a longer duration of basic solution treatment.     

多层光变防伪膜的非均匀垂直偏振光反射特性

基于非均匀光波在导电介质中传播时其相移传播方向和振幅衰减方向的不一致性,利用光波动方程的解由电磁场边界条件导出非均匀垂直偏振光在多层超薄金属膜与透明介质膜组合膜系中光波的传输递推公式.为验证方法的可靠性,给出了不同厚度金属膜防伪光变膜系的能量反射率算例,并与现有算法进行对比,结果表明:两种算法得到的能量反射曲线的分布特征具有很好的相似性,但本文算法表现出金属膜具有强的吸收特性和窄带反射效应.     

Geometry-induced electron doping in periodic semiconductor nanostructures

Recently, new quantum features have been observed and studied in the area of nanostructured layers. Nanograting on the surface of the thin layer imposes additional boundary conditions on the electron wave function and induces G-doping or geometry doping. G-doping is equivalent to donor doping from the point of view of the increase in electron concentration n. However, there are no ionized impurities. This preserves charge carrier scattering to the intrinsic semiconductor level and increases carrier mobility with respect to the donor-doped layer. G-doping involves electron confinement to the nanograting layer. Here, we investigate the system of multiple nanograting layers forming a series of hetero- or homojunctions. The system includes main and barrier layers. In the case of heterojunctions, both types of layers were G-doped. In the case of homojunctions, main layers were G-doped and barrier layers were donor-doped. In such systems, the dependence of n on layer geometry and material parameters was analysed. Si and GaAs homojunctions and GaAs/AlGaAs, Si/SiGe, GaInP/AlGAs, and InP/InAlAs heterojunctions were studied. G-doping levels of 10¹⁸–10¹⁹ cm⁻³ were obtained in homojunctions and type II heterojunctions. High G-doping levels were attained only when the difference between band gap values was low.     

Investigation in the interface roughness of DC-sputtered Mo/B4C multilayer mirrors with variable layer pairs for 7-nm soft X-ray polarizers

The surface and interface roughness of Mo/B₄C multilayer mirrors for 7-nm soft X-ray polarizer with variable layer pairs (N = 50, 70, 90 and 110), fabricated by DC sputtering technique is investigated by atomic force microscopy and X-ray scattering and reflecting. The experimental results present that the surface and interface roughness of Mo/B₄C multilayer mirrors increase layer by layer from its substrate as its Mo layer thickness greater than 2 nm, and the roughness grown tendency could be characterized by a quadratic function.     

Temporal diffraction characteristics of transmitted multilayer volume holographic grating illuminated by an ultrashort pulse

Based on the coupled wave theory of Kogelnik and Fourier optics, the time-domain diffraction characteristics of tramsmitted multilayer volume holographic grating (MVHG) under an ultrashort pulse readout are investigated. It is shown that the temporal diffraction characteristics depend not only on the numbers of the grating layers, but also on the thicknesses of the grating layers and buffer layers, grating period and the refractive index modulation. Furthermore, using group velocity dispersion we give explanation on the time-delay of diffraction pulse with respect to the center of the readout pulse. Results of our discussion may find applications in optical communications, pulse shaping and processing.