Multifractal analysis of elemental distributions in SEM/EDX images of palladium conditioned ET-AAS platforms

A tool of non-linear physics, the multifractal analysis of density distributions, is applied to the analysis of elemental dot maps imaged by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM/EDX). This example concerns distribution patterns of palladium modifier deposits on the graphite platform of an electrothermal atomic absorption spectrometer (ET-AAS). The geometries of palladium distributions were quantitatively determined by multifractal analysis for two types of modifiers: (i) 0.1% (w/v) tetraamminepalladium (II) chloride and (ii) 0.1% (w/v) tetraamminepalladium (II) chloride with 1% (w/v) ammonium oxalate. The multifractal spectra of the generalized fractal dimensions (D _b (q)) do not differ forq = 0 (D _b (0) 1.80±0.08), which reflects the surface topography of the graphite platform. For higher moments ofq significant differences occur (e.g.,D _b (10) 1.35±0.13 without ammonium oxalate andD _b (10) 1.55±0.10 in the presence of ammonium oxalate). These multifractal characteristics, which are due to different probabilities of deposition processes, were observed over a spatial range around 0.01–1 mm. The quantitative assessment of the geometrical distributions substantiate that ammonium oxalate promotes processes which lead to a more homogeneous distribution of palladium, thus enhancing the stabilizing effect.     

Microanalytical characterization of inclusions in Cr-doped LEC GaAs

Inclusions of different morphologies were observed by Infrared (IR) microscopy and Scanning Electron Microscopy (SEM) in the last-to-freeze region of a Cr-doped GaAs single crystal grown by the Liquid Encapsulated Czochralski (LEC) technique.Energy dispersive X-ray analysis (EDX) revealed that these inclusions consist of different chromium compounds. Compositions correspond to the following binary phases and compounds: CrGa₄, Cr₃As₂, Cr₂As₃. Additionally, the quasi-ternary system of Cr₃Ga₄ + CrAs has been found. Sometimes, additional carbon particles have been detected within the heterogeneous inclusions. The possible generation mechanism of inclusions under supercritical growth conditions is discussed.Dedicated to Professor Dr. rer. nat. Dr. h. c. Hubertus Nickel on the occasion of his 65th birthday     

Chemical modifications of Pb(Zr<Subscript>0.3</Subscript>,Ti<Subscript>0.7</Subscript>)O<Subscript>3</Subscript> precursor solutions and their influence on the morphological and electrical properties of the resulting thin films

Tetragonal lead zirconate titanate thin films on platinized silicon wafers have been prepared from chemically different precursor solutions by chemical solution deposition. Literature known routes have been evaluated and an optimized standard process has been developed leading to Pb(Zr_0.3,Ti_0.7)O₃ films with a high degree of (111) orientation which consequently shows square hysteris loops with Pr values of 34 μC/cm². Other solvents, different alkoxides of the transition metals, and different carboxylates of lead have been systematically introduced in this standard process and their influence on the final morphological and electrical properties has been studied. It has been found that the use of lead (II) propionate and titanium tetra n-butoxide for solution synthesis leads to a decrease of the remanent polarization of ∼50%. Furthermore the reaction atmosphere after spinning and during the pyrolysis has been investigated. Increased ambient humidity after the spin coating process also caused a significant deterioration of the final film properties. The findings have been explained in terms of a hindered formation of the (111) texture promoting intermediate Pt _x Pb phase.     

Nickel- and cobalt-based heterogeneous catalytic systems for selective primary amination of alcohol with ammonia

It is one of the critical fields of green chemistry to catalyze the selective conversion of biomass-derived alcohol and ammonia to primary amines with extensive application. Recently, catalytic systems consisting of non-noble metal nickel- and cobalt-based catalysts have been developed for catalytic alcohol amination. This paper reviewed these two types of catalytic systems, which are classified as skeleton Co and Ni catalytic systems, supported and modified Co and Ni catalytic systems, emphasized on catalysts and catalysis, and clearly explained where zero-valent cobalt or nickel is active species for catalytic reaction. In supported catalysts, the catalytic active sites constituted by the catalytic active species and its micro-environment can regulate the efficiency of catalytic the reaction. While in modified catalysts, modifiers such as metal Fe, Re and Bi may modulate the catalytic active sites and change the catalytic selectivity. There are differences in structure and size between catalysts prepared by different methods, resulting in distinct interface and electronic properties for alcohol amination, which determines the structure–activity relationships of the catalytic system.     

Process optimization and characterization of thin films of SrFeO3-x by the pechini method

Nanostructured coatings have recently attracted increasing interest because of the possibilities of synthesizing materials with unique physical-chemical properties. Highly sophisticated surface related properties, such as optical, magnetic, electronic, catalytic, mechanical, chemical and tribological properties can be obtained by advanced nanostructured coatings, making them attractive for various industrial applications. In this report we describe our efforts at developing methodology for the fabrication of SrFeO_3-x based thin films using a modified Pechini method. Thin films of SrFeO_3-x were fabricated using spin coating and a drop coating method developed in-house on Al₂O₃ and Si- substrates. The films annealed at 600°C for one hour show a perovskite phase. The grain size increases with increase in annealing temperature. The influence of various variables such as metal to chelant ratio, drying control reagents, calcination conditions, substrate type and mode of film formation were studied using XRD, optical microscopy, SEM and AFM.     

三氯乙酸刻蚀法观测尼龙球晶形态

筛选出特效刻蚀剂——三氯乙酸溶液,建立了简便、可靠且十分有效的表征本体尼龙-6球晶形态的方法,借助SEM首次对MC尼龙及其改性样品的结晶形态进行了直接观测,三维结构的球晶清晰可见,球晶直径为几十微米.利用三氯乙酸及其溶剂与各种添加剂的物理或化学作用,可有效地研究改性尼龙的球晶缺陷.     

Poly(ethylene-2,6-naphthalate) microfiber prepared by carbon dioxide laser-thinning method

Poly(ethylene-2,6-naphthalate) (PEN) microfiber was continuously obtained by using a carbon dioxide (CO₂) laser-thinning method. As a winding speed increased, the fiber diameter decreased, and its birefringence increased. When the PEN microfiber, obtained by irradiating the laser operated at a power density of 9.15 W cm⁻² to the original fiber supplied at 0.33 m min⁻¹, was wound up at 1594 m min⁻¹, the obtained microfiber had a diameter of 2.8 μm, a birefringence of 0.174, tensile modulus of 5.4 GPa, and a tensile strength of 0.36 GPa.     

Effect of expired doxofylline drug on corrosion protection of soft steel in 1 M HCl: Electrochemical,quantum chemical and synergistic effect studies

The corrosion inhibition property of expired Doxofylline (DF) was tested for soft steel in 1 M hydrochloric acid solution by adopting mass change and electrochemical measurement techniques. At 200 ppm concentration of DF, maximum of 72.84% inhibition efficiency was noticed. However with addition of 50 ppm of KI, it enhances the percentage inhibition efficiency up to 88.48%. DF resists both anodic and cathodic reactions and functioned as mixed-inhibition mechanism. At higher temperatures, electrochemical impedance response noticed that, the diameter of the semicircle decreases as solution temperature increases As a result, in both absence and presence of the inhibitor the R_p values were decreased. Quantum chemical studies revealed about structural and electronic effects in relation to the inhibition efficiencies. Surface morphology of both inhibited and corroded soft steel was assessed by means of scanning electron microscopy (SEM)) and atomic force microscope (AFM). The SEM images of soft steel reflect the inhibitive property of the DF at optimized concentration and a significant decrease in the surface roughness was observed (surface roughness was reduced from 606 nm to 294 nm as measured by AFM)). UV-Visible absorption peaks signifies that CC and CO groups from the inhibitor were interacted with iron cations, which is the evidence for the formation protective film over the soft steel surface.     

Influence of particle size on the crystallization process and the bioactive behavior of a bioactive glass system

Bioactive glasses have attracted considerable interest in recent years, due to their technological application, especially in biomaterials research. Differential scanning calorimetry (DSC) has been used in the study of the crystallization mechanism in the SiO₂–Na₂O–CaO–P₂O₅ glass system, as a function of particle size. The curve of the bulk glass presents a slightly asymmetric crystallization peak that could be deconvoluted into two separate peaks, their separation being followed in the form of powder glasses. Also, a shift of the crystallization peaks to lower temperatures was observed with the decrease of the particle size. FTIR studies – that are confirmed by XRD measurements – proved that the different peaks could be attributed to different crystallization mechanisms. Moreover, it is presented the bioactive behavior of the specific glass as a function of particle size. The study of bioactivity is performed through the process of its immersion in simulated human blood plasma (simulated body fluid, SBF) and the subsequent examination of the development of carbonate-containing hydroxyapatite layer on the surface of the particles. The bioactive response is improved with the increase of the particle size of powders up to 80 μm and remains almost unchanged for further increase, following the specific surface to volume ratio decrease.     

Characterization and enzymatic degradation of microbial copolyester P(3HB-co-3HV)s produced by metabolic reaction model-based system

The two types of poly(3-hydroxybutyrate-co-3-hydroxyvalerate)s [P(3HB-co-3HV)s] were produced by Paracoccus denitrificans ATCC 17741 using two different feeding methods. The produced P(3HB-co-3HV)s were fractionated and the copolymer sequence distributions were analyzed by ¹H and ¹³C NMR spectroscopy. It was found that the P(3HB-co-3HV) samples produced by conventional feeding method were statistically random copolymers. The sequence distributions of P(3HB-co-3HV) samples produced by optimization method were different from random P(3HB-co-3HV)s. The thermal properties and melting behaviors were analyzed by differential scanning calorimetry (DSC). These results demonstrated that P(3HB-co-3HV) samples produced by optimization method are close in nature to P(3HB-co-3HV)s rich in long-sequence of block 3HB units, but less in 3HV random regions. The enzymatic degradation profile of P(3HB-co-3HV) films was investigated in the presence of 3-hydroxybutyrate depolymerase from Pseudomonase lemoignei. The degradation process was observed by monitoring the time-dependent change in the weight loss of copolymer films. The surface erosion of copolymer films was qualitatively monitored by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The highest degradation rate of 2.6% per day was observed for random P(3HB-co-38%3HV) produced by conventional method. In comparison, the hydrolysis degradation rates of random P(3HB-co-3HV)s were about one time faster than those of P(3HB-co-3HV)s produced by optimization method.