Effect of preparation and metal content on the introduction of Fe in BEA zeolite, studied by DR UV-vis, EPR and Mössbauer spectroscopy

Fe-containing SiBEA zeolites were prepared by a two-step postsynthesis method: creation of vacant T-sites by dealumination of tetraethylammonium BEA zeolite with nitric acid and then impregnation of the resulting SiBEA zeolite with an aqueous solution of Fe(NO₃)₃. X-ray diffraction shows that iron is incorporated in SiBEA at lattice sites. The presence of Fe in its oxidation state +3 and at isolated tetrahedral sites for low metal content, was demonstrated by diffuse reflectance UV-vis, EPR and Mössbauer spectroscopy. For high iron content, diffuse reflectance UV-vis and Mössbauer spectra revealed the additional presence of extra-lattice FeO_x oligomers and superparamagnetic Fe-oxyhydroxide. Mössbauer spectroscopy identified superparamagnetic Fe-oxyhydroxide as the main phase when basic conditions are used for the preparation.     

In vitro reactivity of Na2O-MgO-SiO2 glasses

A variety of bioactive glasses have been investigated over the last two decades as substitute material for diseased or damaged tissues in a human body. In this investigation, three different melt derived bioactive glasses, each having 55% by mole SiO₂ and ratio of MgO to Na₂O varying from 1:8 to 8:1, were prepared by melting various oxides at temperature >1250 °C. After microstructure evolution, vitro reactivity of these glasses was examined by keeping them in simulated body fluid (trans buffered pH 7.25 at 25 cc). The surface reactivity of these glasses gradually increased with increasing Na₂O/MgO ratio.     

Optical and photocatalytic properties of nanocrystalline TiO2 synthesised by solid-state chemical reaction

Nanoparticulate TiO₂ is of interest for a variety of technological applications, including optically transparent UV-filters and photocatalysts for the destruction of chemical waste. The successful use of nanoparticulate TiO₂ in such applications requires an understanding of how the synthesis conditions effect the optical and photocatalytic properties. In this study, we have investigated the effect of heat treatment temperature on the properties of nanoparticulate TiO₂ powders that were synthesised by solid-state chemical reaction of anhydrous TiOSO₄ with Na₂CO₃. It was found that the photocatalytic activity increased with the heat treatment temperature up to a maximum at 600 °C and thereafter declined. In contrast, the optical transparency decreased monotonically with the heat treatment temperature. These results indicate that solid-state chemical reaction can be used to prepare powders of nanoparticulate TiO₂ with properties that are optimised for use as either optically transparent UV-filters or photocatalysts.     

The role of precursor gases on the surface restructuring of catalyst films during carbon nanotube growth

Catalyst films undergo considerable surface morphology restructuring prior to carbon nanotube nucleation, deeply influencing the nanostructures obtained. Here we study the influence of different gaseous atmospheres on the structure of thin Fe films. The morphology is influenced by process temperature and substrate interactions and varying the gas type and pressure can control the average catalyst island height.     

Synthesis of carbon nanotubes on Ni-alloy and Si-substrates using counterflow methane–air diffusion flames

We have conducted an experimental study to investigate the synthesis of multi-walled carbon nanotubes (CNTs) in counterflow methane–air diffusion flames, with emphasis on effects of catalyst, temperature, and the air-side strain rate of the flow on CNTs growth. The counterflow flame was formed by fuel (CH₄ or CH₄ + N₂) and air streams impinging on each other. Two types of substrates were used to deposit CNTs. Ni-alloy (60% Ni + 26% Cr + 14% Fe) wire substrates synthesized curved and entangled CNTs, which have both straight and bamboo-like structures; Si-substrates with porous anodic aluminum oxide (AAO) nanotemplates synthesized well-aligned, self-assembled CNTs. These CNTs grown inside nanopores had a uniform geometry with controllable length and diameter. The axial temperature profiles of the flow were measured by a 125 μm diameter Pt/10% Rh–Pt thermocouple with a 0.3 mm bead junction. It was found that temperature could affect not only the success of CNTs synthesis, but also the morphology of synthesized CNTs. It was also found, against previous general belief, that there was a common temperature region (1023–1073 K) in chemical vapor deposition (CVD) and counterflow diffusion flames where CNTs could be produced. CNTs synthesized in counterflow flames were significantly affected by air-side strain rate not through the residence time, but through carbon sources available for CNTs growth. Off-symmetric counterflow flames could synthesize high-quality CNTs because with this configuration carbon sources at the fuel side could easily diffuse across the stagnation surface to support CNTs growth. These results show the feasibility of using counterflow flames to synthesize CNTs for particular applications such as fabricating nanoscale electronic devices.     

Synthesis of multi-walled carbon nanotubes for NH3 gas detection

It has been recently demonstrated that carbon nanotubes (CNTs) represent a new type of chemical sensor capable of detecting a small concentration of molecules such as CO, NO₂, NH₃.In this work, CNTs were synthesized by chemical vapor deposition (CVD) on the SiO₂/Si substrate by decomposition of acetylene (C₂H₂) on sputtered Ni catalyst nanoparticles. Their structural properties are studied by atomic force microscopy, high-resolution scanning electron microscopy (HRSEM) and Raman spectroscopy. The CNTs grown at 700 °C exhibit a low dispersion in size, are about 1 μm long and their average diameter varies in the range 25–60 nm as a function of the deposition time. We have shown that their diameter can be reduced either by annealing in oxygen environment or by growing at lower temperature (less than 600 °C).We developed a test device with interdigital Pt electrodes on an Al₂O₃ substrate in order to evaluate the CNTs-based gas sensor capabilities. We performed room temperature current–voltage measurements for various gas concentrations. The CNT films are found to exhibit a fast response and a high sensitivity to NH₃ gas.     

A second-order accurate numerical method for the two-dimensional fractional diffusion equation

Spatially fractional order diffusion equations are generalizations of classical diffusion equations which are used in modeling practical superdiffusive problems in fluid flow, finance and others. In this paper, we present an accurate and efficient numerical method to solve a fractional superdiffusive differential equation. This numerical method combines the alternating directions implicit (ADI) approach with a Crank–Nicolson discretization and a Richardson extrapolation to obtain an unconditionally stable second-order accurate finite difference method. The stability and the consistency of the method are established. Numerical solutions for an example super-diffusion equation with a known analytic solution are obtained and the behavior of the errors are analyzed to demonstrate the order of convergence of the method.     

Structure refinements of cadmium substituted lead fluoroapatites by powder X-ray pattern fitting

Solid solutions of cadmium and lead fluoroapatite [Pb_(10−x)Cd_x(PO₄)₆F₂ (0?x?5)] were synthesized by a wet process in a basic medium. Replacement of lead by cadmium induces a linear variation of the crystallographic parameters “a” and “c” according to Végard's law. The cadmium content, as obtained from the refinement, is in agreement with the chemical analysis. The distribution of the lead and cadmium ions between two non-equivalent crystallographic sites, M(1) and M(2), was determined by the Rietveld method. The site-occupancy factors of atoms clearly indicate a preference of cadmium for site M(1) in the apatite structure in agreement with its smaller ionic radii. A progressive shift of the F⁻ ion toward the center of the triangles formed by the site M(2) metals has been observed with increasing cadmium content.     

二元编码光栅的误差扩散算法研究

为了研究二元误差扩散算法,采用计算机仿真的方法产生光栅模板用于位相测量轮廓术,分析误差扩散点数和误差分配系数对编码方法和测量精度的影响.结果表明,应用3种常见的误差分配系数用于产生正弦光场都具有较高的测量精度,三者间没有显著性差异.误差扩散点数对编码方法和相位测量精度的影响较小.实验证明,采用误差扩散编码后,系统综合误差可以控制在1%的等效波长以内,验证了二元误差扩散方法的可行性与精确性.     

Fabrication of Silicon Inverse Woodpile Photonic Crystals

Silicon inverse woodpile photonic crystals are fabricated for the first time. Our approach, which is based on direct laser writing of polymeric templates and a novel silicon single‐inversion procedure, leads to high‐quality structures with gap/midgap ratios of 14.2 %, centered at a wavelength of 2.5 μm. It is shown that gap/midgap ratios as large as 20.5 %, centered at 1.55 μm, may become possible in the future.