Determining the Uncertainty of X-Ray Absorption Measurements

X-ray absorption (or more properly, x-ray attenuation) techniques have been applied to study the moisture movement in and moisture content of materials like cement paste, mortar, and wood. An increase in the number of x-ray counts with time at a location in a specimen may indicate a decrease in moisture content. The uncertainty of measurements from an x-ray absorption system, which must be known to properly interpret the data, is often assumed to be the square root of the number of counts, as in a Poisson process. No detailed studies have heretofore been conducted to determine the uncertainty of x-ray absorption measurements or the effect of averaging data on the uncertainty. In this study, the Poisson estimate was found to adequately approximate normalized root mean square errors (a measure of uncertainty) of counts for point measurements and profile measurements of water specimens. The Poisson estimate, however, was not reliable in approximating the magnitude of the uncertainty when averaging data from paste and mortar specimens. Changes in uncertainty from differing averaging procedures were well-approximated by a Poisson process. The normalized root mean square errors decreased when the x-ray source intensity, integration time, collimator size, and number of scanning repetitions increased. Uncertainties in mean paste and mortar count profiles were kept below 2 % by averaging vertical profiles at horizontal spacings of 1 mm or larger with counts per point above 4000. Maximum normalized root mean square errors did not exceed 10 % in any of the tests conducted.     

Structural studies of copper sulfide films: effect of ambient atmosphere

We examined the structural properties of copper sulfide films as a function of the sulfurization time of 70-nm-thick Cu films. Copper sulfide films with various phases such as mixed metallic Cu-chalcocite, chalcocite, roxbyite, and covellite phases were formed with increasing sulfurization time. To evaluate the structural stability of various films, all the films were exposed to the ambient atmosphere for the same amount of time. Although the phase structure and stoichiometry of the films were maintained at a greater depth, the near-surface region of the films was oxidized and covered with overlayers of oxide, hydroxide, and/or sulfate species due to the exposure and reaction with the ambient atmosphere. The oxygen uptake and its reactivity with the copper sulfide film surfaces were enhanced with increasing sulfur content of the films. In addition, the type of divalent state of copper formed on the film surfaces depended on the phase structure, composition, and stoichiometry of the films.     

Structural studies of copper sulfide films: effect of ambient atmosphere

Abstract

We examined the structural properties of copper sulfide films as a function of the sulfurization time of 70-nm-thick Cu films. Copper sulfide films with various phases such as mixed metallic Cu-chalcocite, chalcocite, roxbyite, and covellite phases were formed with increasing sulfurization time. To evaluate the structural stability of various films, all the films were exposed to the ambient atmosphere for the same amount of time. Although the phase structure and stoichiometry of the films were maintained at a greater depth, the near-surface region of the films was oxidized and covered with overlayers of oxide, hydroxide, and/or sulfate species due to the exposure and reaction with the ambient atmosphere. The oxygen uptake and its reactivity with the copper sulfide film surfaces were enhanced with increasing sulfur content of the films. In addition, the type of divalent state of copper formed on the film surfaces depended on the phase structure, composition, and stoichiometry of the films.     

Ag型IPMC柔性驱动器的制备及性能

为了降低成本并改善材料性能,采用银替代铂制备IPMC电极。基于渗透还原工艺采用化学沉积方法制备了Pt基、Pt-Ag基和Ag基三种IPMC柔性驱动器试件。对试件的SEM和XRD分析结果表明本文提供的方法可以有效地将电极金属沉积在基膜中,且呈梯度分布;对样件的致动效果以及表面电阻特性测试结果表明Ag基IPMC驱动器具有最好的致动变形能力和最低的表面电阻。在相同尺寸与约束条件下,Ag基IPMC在1.5V时产生90°变形,Pt型与Pt-Ag型IPMC分别在3V和4V驱动电压下产生60°变形。     

Emerging methods and opportunities in nanoscale materials characterization

The emergence of powerful nanomaterials characterization techniques promises to underpin a new range of advances in materials research. There have been significant developments in the characterization of the phase, structure, composition, and dynamics of materials at the nanoscale. Articles in this issue report recent advances in three areas: atom probe tomography, x-ray nanobeam scattering and diffraction, and x-ray photon correlation spectroscopy. Each of these provides three-dimensional insight into hard materials in ways that have been previously unavailable. Taken together, these emerging methods have the potential to provide new tests for materials theory and computation and to extend significantly the range of questions that can be answered in materials research.     

Absorption of methanol and toluene by polyester-based bottles

Absorption aspects of flavours and chemicals are important quality criteria when plastic bottles are reused or recycled. In the present study absorption of methanol and toluene by polyester-based bottles (PET and PEN) was studied at different temperatures in the range 20–40°C for a period of 16 weeks with two different ways of exposure: one-sided and two-sided. Saturation levels were not reached in such a period of storage. However, absorption levels are affected by temperature. An increase in temperature causes an increase in absorption level. Also, the polarity and size of the chemicals, the composition of the plastic (PET and/or PEN) and the crystallinity of the specimens influences absorption. The results did not show whether two-sided exposure is representative of the one-sided situation. © 1997 John Wiley & Sons, Ltd.     

X-Ray Microanalysis in the Variable Pressure (Environmental) Scanning Electron Microscope

Electron-excited x-ray microanalysis performed in the variable pressure and environmental scanning electron microscopes is subject to additional artifacts beyond those encountered in the conventional scanning electron microscope. Gas scattering leads to direct contributions to the spectrum from the environmental gas, as well as remote generation of x rays by electrons scattered out of the focussed beam. The analyst can exert some degree of control over these artifacts, but depending on the exact situation, spurious elements can appear at the trace (< 0.01 mass fraction), minor (0.01 mass fraction to 0.1 mass fraction), or even major (> 0.1 mass fraction) levels. Dispersed particle samples give the least compromised results, while fine scale microstructures are the most severely compromised. Procedures to optimize the situation based upon specimen preparation as well as spectral processing are described.     

XPS Studies of Magnesium Surfaces after Exposure to Dulbecco's Modified Eagle Medium,Hank's Buffered Salt Solution,and Simulated Body Fluid

Magnesium‐based biomaterials are gaining increasing interest, while in vitro corrosion tests are not standardized yet. Moreover, the effects of different corrosion media on the corrosion products are still not fully understood. To compare and evaluate the three main corrosion media applied in most in vitro studies, an XPS investigation of magnesium surfaces was carried out after exposure of the specimens to Dulbecco's modified eagle medium (DMEM), Hank's buffered salt solution (HBSS), and simulated body fluid (SBF). The effects of rinsing the specimens after immersion were also determined. XPS investigations especially on the Mg 2p state showed that MgO, Mg(OH)2, and MgCO3 species were the dominant corrosion products presenting in all specimens despite of the different corrosion media. However, the ratio of corrosion products depends on the medium composition. It was also shown that rinsing specimens after immersion experiments is a necessary procedure when surface analysis is employed afterward.     

Measurement of optical properties of highly scattering ceramic materials

Radiation transfer in highly scattering ceramics is described by a diffusion approximation based on the asymptotic relation of the radiant flux and the radiant energy density in material depth. In this approximation, a calculation of the effective absorption coefficient k and the radiation diffusion coefficient D is based on the measurement of normal-hemispherical transmission of specimens shaped as various-thickness disks. Taken into account are radiation field, twodimensionality, and the radiation boundary reflection effect. The optical property measurements have been performed on the experimental apparatus based on an integrating sphere, a collimated radiation source, and a twochannel data acquisition and processing system. Results of the measurements of k and D for the silica ceramic are given at room temperature.     

Development of Near-Surface Composition Anomaly

Many multi-element alloy specimens have been shown to possess a wide variety of near-surface elemental composition profiles, which are significantly different from the bulk composition. Such composition nonuniformity adversely affects the measurement of basic thermophysical properties in alloys. In this paper is presented a new investigation into the mechanisms by which such depth-dependent near-surface elemental composition develops. Specifically, specimens of a low melting-point metallic alloy, Wood's alloy, as a model system are examined under varying thermal cycling conditions within a chamber of controlled gaseous atmosphere. The near-surface composition and thermal diffusivity are measured as a function of depth. The method of time-resolved spectroscopy of laser-produced plasma plumes emanating from the specimen surface is used. Different surface composition profiles emerge depending on the dynamic range of the thermal cycling forced on a specimen.     

Effect of thickness and chemical composition on thermal resistance of steel dilatometric specimens under heating-cooling cycles by Joule heating

The effect of thickness and chemical composition on the electrical power and thermal resistance of dilatometric specimens heated by Joule heating are analyzed in different steels, using stepped tests of constant temperature and electrical current. In the stepped constant temperature tests, the electric current necessary to maintain the target temperature in a specific time is measured, while in the electric current tests the electrical current is maintained until the maximum temperature stabilizes. The results show that the electrical power behaves linearly with the thickness associated with the transfer area, while the thermal resistance behaves potentially; both values depend on the chemical composition due to electrical resistivity. The steels with a higher concentration of alloying elements have a better response to Joule heating. However, thickness is the parameter that most influences electrical power due to changes in transfer area and electrical current density, as well as in the mass of the specimen to be heated. Finally, based on the results obtained, predictions are realized for the design of thicker specimens, maintaining the observed behavior; i. e., as the thickness of the specimen increases, the increase in electrical power and thermal resistance is maintained.     

Preparation and characterization of Pb1−x Sn x Te pseudobinary alloy semiconductors

Ap-type pseudo-binary alloy semiconductor, Pb_0·3Sn_0·7Te, has been prepared fromp-type specimens of PbTe and SnTe and lattice constants determined with an accuracy of 0.0001 nm. Vacuum annealing of Pb_0·3Sn_0·7 Te reveals two new x-ray powder diffraction lines bearing indices (444) and (800), while others become more sharp, CuK_a-doublets get clearly resolved and the lattice constant is increased by ∼ 0·0002 nm. Slight deviation from Vegard’s law linearity is observed showing that the sample must be considered as ternary in nature. Thin films deposited on mica and glass substrates kept at room temperature are found to have a little higher SnTe content. The effective carrier concentration calculated from Hall measurements at room temperature is ∼ 3·4×10²⁶ m⁻³.     

Characterisation of oxide scales formed on nickel superalloy using impedance spectroscopy

Abstract

Impedance spectroscopy has been used to measure the electrical properties of oxide scales formed from oxidation of IN738LC superalloy at high temperature. Electrical resistance and capacitance of the oxide scales were obtained from the simulation of the measured impedance diagrams based on the equivalent circuit model, which represents the features of the oxide scales. For oxidation of IN738LC superalloy, the electrical resistance of oxide scales increased with increasing oxidation time for the specimens exposed to air at 900°C. However, for the specimens oxidised at 1,200°C, the oxide scales showed very low electrical resistance, which indicated that cracking and spallation in oxide scales occurred continuously. By using scanning electron microscopy and X-ray diffraction techniques, the composition and microstructure of the oxide scales were examined. It was found that electrical properties were determined, not only by the microstructure of oxide scales, but also by the composition of the oxide scales. By determining the relationship between electrical properties, microstructure and composition of oxide scales, impedance spectroscopy could be used as a non-destructive technique for monitoring the oxidation of metallic alloys at high temperature.     

聚全氟乙丙膜电子束引发预辐射接枝AA和SSS制备阳离子交换膜的性能

利用电子束引发预辐射接枝技术,在聚全氟乙丙烯(FEP)膜上接枝丙烯酸(AA)和对苯乙烯磺酸钠(SSS)两单体,制备出一种含羧酸基团和磺酸基团的阳离子交换膜,接枝率越高,接枝膜的吸碱性能越好。差示量热扫描及X射线衍射测试表明,接枝膜结晶度随接枝率的升高而降低。这是接枝膜中FEP组份的“结晶变形”及接枝链对晶区的“稀释作用”综合影响的结果。     

Gradient interpenetrating polymer networks

The methods of synthesis and properties of gradient interpenetrating polymer networks (IPN) are discussed based on literature and authors' own experimental data. Gradient IPN can be treated as a sequence of an infinite number of layers of IPNs, whose composition and properties vary gradually from the surface to the core of specimens. These are analysed the most important properties of gradient IPNs: temperature transitions, thermodynamic and physico-mechanical characteristics and the main direction of practical application of gradient IPN-based materials.     

Properties of Calcium Phosphate Cements With Different Tetracalcium Phosphate and Dicalcium Phosphate Anhydrous Molar Ratios

Calcium phosphate cements (CPCs) were prepared using mixtures of tetracalcium phosphate (TTCP) and dicalcium phosphate anhydrous (DCPA), with TTCP/DCPA molar ratios of 1/1, 1/2, or 1/3, with the powder and water as the liquid. Diametral tensile strength (DTS), porosity, and phase composition (powder x-ray diffraction) were determined after the set specimens have been immersed in a physiological-like solution (PLS) for 1 d, 5 d, and 10 d. Cement dissolution rates in an acidified PLS were measured using a dual constant composition method. Setting times ((30 ± 1) min) were the same for all cements. DTS decreased with decreasing TTCP/DCPA ratio and, in some cases, also decreased with PLS immersion time. Porosity and hydroxyapatite (HA) formation increased with PLS immersion time. Cements with TTCP/DCPA ratios of 1/2 and 1/3, which formed calcium-deficient HA, dissolved more rapidly than the cement with a ratio of 1/1. In conclusion, cements may be prepared with a range of TTCP/DCPA ratios, and those with lower ratio had lower strengths but dissolved more rapidly in acidified PLS.     

Significance of crystallographic grain orientation for oxide scale formation on FeCrAl ODS alloys studied by AFM and MCs+-SIMS

Abstract

Single crystalline specimens were prepared by spark erosion of large grains in an extremely coarse textured bar of an FeCrAl based ODS alloy. These flat single crystalline specimens were studied in respect to oxidation behaviour at 800°C and 1,000°C in air. Initially the oxide scales appeared to grow by outward diffusion of aluminium but subsequently scale growth proceeded by grain boundary oxygen diffusion. The composition, grain size and growth rate of the transient oxide appeared to be dependent on the crystallographic orientation of the alloy. After the inward diffusion of oxygen had become dominant, the oxides on specimens with different crystallographic orientations showed clear differences in their growth rates. Correlation of SIMS results with quantitative grain size analysis performed by AFM showed that the different oxide growth rates, which pertained during longer exposure times, were related to differences in the oxide grain size and therefore the density of oxygen diffusion paths with different crystallographic orientations.     

Gradient interpenetrating polymer networks

The methods of synthesis and properties of gradient interpenetrating polymer networks (IPN) are discussed based on literature and authors' own experimental data. Gradient IPN can be treated as a sequence of an infinite number of layers of IPNs, whose composition and properties vary gradually from the surface to the core of specimens. These are analysed the most important properties of gradient IPNs: temperature transitions, thermodynamic and physico-mechanical characteristics and the main direction of practical application of gradient IPN-based materials.     

Barriers to Quantitative Electron Probe X-Ray Microanalysis for Low Voltage Scanning Electron Microscopy

Low voltage x-ray microanalysis, defined as being performed with an incident beam energy ≤5 keV, can achieve spatial resolution, laterally and in depth, of 100 nm or less, depending on the exact selection of beam energy and the composition of the target. The shallow depth of beam penetration, with the consequent short path length for x-ray absorption, and the low overvoltage, the ratio of beam energy to the critical ionization energy, both contribute to minimizing the matrix effects in quantitative x-ray microanalysis when the unknown is compared to pure element standards. The low beam energy restricts the energy of the atomic shells that can be excited, forcing the analyst to choose unfamiliar shells/characteristic peaks. The low photon energy shells are subject to low fluorescence yield, so that the peak-to-continuum background is reduced, severely limiting detectability. The limited resolution of semiconductor energy dispersive spectrometry results in frequent peak interference situations and further exacerbates detection limits. Future improvements to the x-ray spectrometry limitations are possible with x-ray optics-augmented wavelength dispersive spectrometry and microcalorimeter energy dispersive spectrometry.     

Study on microwave absorption properties of metal-containing foam glass

Materials with the properties of electromagnetic (EM) wave absorption are attractive topics. In this work, we report that EM wave absorption composites, consisting of foam glass, zinc and zinc oxide, were prepared by sintering mixture of foam glass raw material and zinc powder. Microwave reflection loss of composite was calculated based on the permittivity in the range of 8.2-12.4 GHz. The results show that zinc-containing foam glass absorbs efficiently microwaves. The sample with zinc filler to foam glass mass ratio of 3/18 had a reflection loss below −10 dB in the range of 11.3-12.4 GHz, and the minimum reflectivity was −15.6 dB at both 12.0 and 12.4 GHz. Microwave absorption performances of specimens can be controlled by changing the ratio between zinc powder and foam glass mass. The detailed mechanism of the control was investigated through X-ray diffraction (XRD) analysis and scanning electrical microscopy (SEM) observations.