Effect of Pressure on Synthesis of Pr-Doped Zirconia Powders Produced by Microwave-Driven Hydrothermal Reaction

A high-pressure microwave reactor was used to study the hydrothermal synthesis of zirconia powders doped with 1 mol % Pr. The synthesis was performed in the pressure range from 2 to 8 MPa corresponding to a temperature range from 215C∘ to 305C∘. This technology permits a synthesis of nanopowders in short time not limited by thermal inertia of the vessel. Microwave heating permits to avoid contact of the reactants with heating elements, and is thus particularly well suited for synthesis of doped nanopowders in high purity conditions. A mixture of ZrO2 particles with tetragonal and monoclinic crystalline phases, about 15 nm in size, was obtained. The p/T threshold of about 5-6 MPa/265–280C∘ was necessary to obtain good quality of zirconia powder. A new method for quantitative description of grain-size distribution was applied, which is based on analysis of the fine structure of the X-ray diffraction line profiles. It permitted to follow separately the effect of synthesis conditions on the grain-size distribution of the monoclinic and tetragonal phases

Effect of pressure on synthesis of Pr-doped zirconia powders produced by microwave-driven hydrothermal reaction

A high-pressure microwave reactor was used to study the hydrothermal synthesis of zirconia powders doped with 1 mol % Pr.The synthesis was performed in the pressure range from 2 to 8MPa corresponding to a temperature range from 215◦C to 305◦C.This technology permits a synthesis of nanopowders in short time not limited by thermal inertia of the vessel. Microwave heatingpermits to avoid contact of the reactants with heating elements, and is thus particularly well suited for synthesis of dopednanopowders in high purity conditions. A mixture of ZrO2 particles with tetragonal and monoclinic crystalline phases, about15nm in size, was obtained. The p/T threshold of about 5-6MPa/265–280◦C was necessary to obtain good quality of zirconiapowder. A new method for quantitative description of grain-size distribution was applied, which is based on analysis of the finestructure of the X-ray diffraction line profiles. It permitted to follow separately the effect of synthesis conditions on the grain-size distribution of the monoclinic and tetragonal phases

Fabrication of corrugated Ge-doped silica fibers

We present a method of fabricating Ge-doped SiO2 fibers with corrugations around their full circumference for a desired length in the longitudinal direction. The procedure comprises three steps: hydrogenation of Ge-doped SiO2 fibers to increase photosensitivity, recording of Bragg gratings with ultraviolet light to achieve modulation of refractive index, and chemical etching. Finite-length, radially corrugated fibers may be used as couplers. Corrugated tapered fibers are used as high energy throughput probes in scanning near-field optical microscopy

Incorporation of the Pore Size Variation to Modeling of the Elastic Behavior of Metallic Open-Cell Foams

In the present paper we present the approach for modeling of the elastic behavior of open-cell metallic foams concerning non-uniform pore size distribution. This approach combines design of foam structures and numerical simulations of compression tests using finite element method (FEM). In the design stage, Laguerre-Voronoi tessellations (LVT) were performed on several sets of packed spheres with defined variation of radii, bringing about a set of foam structures with porosity ranging from 74 to 98% and different pore size variation quantified by the coefficient of pore volume variation, CV(V), from 0.5 to 2.1. Each structure was numerically subjected to uni-axial compression test along three directions within the elastic region. Basing on the numerical response, the effective Young’s modulus, Eeff, was calculated for each structure. It is shown that the Eeff is not only dependent on the porosity but also on the pore size variation

The use of X-ray computed microtomography for graptolite detection in rock based on core internal structure visualization

This paper presents for the first time X-ray computed microtomography (μCT) analysis as a technique for Silurian graptolite detection in rocks. The samples come from the Jantar Bituminous Claystones Member of the Opalino core, Baltic Basin, northern Poland. Images were obtained with spatial resolution of 25 μm, which enabled the authors to create a 3-D visualization and to calculate the ratio of fissure and graptolite volume to the total sample volume. A set of μCT slices was used to create a 3-D reconstruction of graptolite geometry. These μCT slices were processed to obtain a clearly visible image and the volume ratio. A copper X-ray source filter was used during exposure to reduce radiograph artifacts. Visualization of graptolite tubaria (rhabdosomes) enabled Demirastrites simulans to be identified. Numerical models of graptolites reveal promising applications for paleontological research and thus for the recognition and characterization of reservoir rocks

Metallic foam supported electrodes for molten carbonate fuel cells

This paper demonstrates the benefits of using a metallic foam support within molten carbonate fuel cell (MCFC) cathodes. A state-of-the-art fabrication process based on tape casting has been developed to produce microporous electrodes with a nickel foam scaffold. Surfactant was added to control the depth to which the slurry infiltrated the foam. New cathodes were used as an alternative to the traditional cathode in the single cell assembly and were tested for power density. Mechanical properties were compared with the current state-of-the-art. The results show that the use of metallic foams for high temperature fuel cell electrodes is beneficial from the technological point of view, especially in larger scale production. It was also found that the resultant continuous metallic structure of the microporous electrodes delivered a slight enhancement to fuel cell power density.publishedVersio

Image based analysis of complex microstructures of engineering materials

The paper presents various methods for quantitative description of material structures. The main focus is on direct methods of description based on image analysis. In particular, techniques for the estimation of the size, shape and spatial distribution of structural elements observed by different microscopic techniques are described. The application of these methods for the characterization of the structures of engineering materials is demonstrated on a stainless steel used in petrochemical installations. It is shown that the methods applied are useful for the assessment of service degradation of materials

Numerical approach in recognition of selected features of rock structure from hybrid hydrocarbon reservoir samples based on microtomography

The study employs numerical calculations in the characterization of reservoir sandstone samples based on high-resolution X-ray computed microtomography. The major goals were to determine porosity through pore size distribution, permeability characterization through pressure field, and structure impact on rock strength by simulation of a uniaxial compression test. Two Miocene samples were taken from well S-3, located in the eastern part of the Carpathian Foredeep. Due to the relation between sample size and image resolution, two X-ray irradiation series with two different sample sizes were performed. In the first approach, the voxel side was 27 µm and in the second it was up to 2 µm. Two samples from different depths have been studied here. Sample 1 has petrophysical features of conventional reservoir deposits, in contrast to sample 2. The approximate grain size of sample 1 is in the range 0.1–1.0 mm, whereas for sample 2 it is 0.01–0.1 mm with clear sedimentation lamination and heterogenic structure. The porosity, as determined by µCT, of sample 1 is twice (10.3%) that of sample 2 (5.3%). The equivalent diameter of a majority of pores is less than 0.027 mm and their pore size distribution is unimodal right-hand asymmetrical in the case of both samples. In relations to numerical permeability tests, the flow paths are in the few privileged directions where the pressure is uniformly decreasing. Nevertheless, there are visible connections in sample 1, as is confirmed by the homogenous distribution of particles in the pore space of the sample and demonstrated in the particle flow simulations. The estimated permeability of the first sample is approximately four times higher than that of the second one. The uniaxial compression test demonstrated the huge impact of even minimal heterogeneity of samples in terms of micropores: 4–5 times loss of strength compared to the undisturbed sample. The procedure presented shows the promising combination of microstructural analysis and numerical simulations. More specific calculations of lab tests with analysis of variable boundary conditions should be performed in the future

Microstructure and electrochemical behavior of layered cathodes for molten carbonate fuel cell

In the present paper, we demonstrate how modifications of the microstructure and the chemical composition can influence the electrochemical behavior of cathodes for molten carbonate fuel cells (MCFCs). Based on our experience, we designed new MCFC cathode microstructures combining layers made of porous silver, nickel oxide or nickel foam to overcome common issues with the internal resistance of the cell. The microstructures of the standard NiO cathode and manufactured cathodes were extensively investigated using scanning electron microscopy (SEM) and porosity measurements. The electrochemical behavior and overall cell performance were examined by means of electrochemical impedance spectroscopy and single-cell tests in operation conditions. The results show that a porous silver layer tape cast onto standard NiO cathode and nickel foam used as a support layer for tape cast NiO porous layer substantially decrease resistance components representing charge transfer and mass transport phenomena, respectively. Therefore, it is beneficial to combine them into a three-layer cathode since it facilitates separation of predominant physio-chemical processes of gas and ions transport in respective layers ensuring high efficiency. The superiority of the three-layer cathode has been proven by low impedance and high power density as compared to standard NiO cathode.publishedVersio