Perspective high-temperature ceramic composite materials

The high-temperature glass-matrix and ceramic-matrix composites developed by the RIAM are overviewed. The distinctive properties of the developed composites are their high stability at temperatures above 1200°C in an oxidizing medium, high endurance and corrosion resistance, and low density and thermal expansion. Therefore, these composites are unique for production of heat-loaded units and parts of advanced engines. A characteristic feature of the SiC/SiC ceramic-matrix composite is its high resistance (by contrast to traditional monolithic ceramics) to thermocyclic loadings in the medium of fuel combustion products, which is due to its regulated and manageable structure.     

Electrochemistry of proton-conducting ceramic materials and cells

Journal of Solid State Electrochemistry -     

Strategy for Applying Microanalytical Techniques

A combination of microanalysis techniques is used to reveal with great precision the composition and microstructure of typical features in engineering materials. In this paper small particles, very thin films, interfaces and their contiguous region are considered. Small silicon nitride particles in an iron matrix produced by nitriding are characterized quantitatively with High Resolution Electron Microscopy (HREM) and Electron Probe Micro Analysis (EPMA) using Wavelength Dispersive X-ray Spectrometry (WDS). Thin aluminium-oxide films grown on aluminium substrates by thermal oxidation at low pressure are investigated with HREM and X-ray Photoelectron Spectroscopy (XPS). Their thickness, composition and degree of crystallinity are established as a function of oxidation temperature and time. At and near the oxide-layer/MCrAlY-coating (M=Ni and/or Co) interface the aluminium and chromium depletion behaviour of the coating material due to high-temperature oxidation is studied with high-resolution Scanning Electron Microscopy (SEM), EPMA and Auger electron spectroscopy (AES). The composition-depth profiles obtained for the coating material are used to determine the composition dependent diffusion coefficients. These properties are crucial for the prediction through computational modelling of the coating material oxidation behaviour and enable the development of new coating materials.     

Promising ultra-high-temperature ceramic materials for aerospace applications

Some aspects of heat transfer upon the interaction between components with a sharp leading edge and high-enthalpy high-speed flow of dissociated air have been considered; some material characteristics, which should be primarily taken into account when prognosticating the behavior of materials that are promising for using as components of hypersonic flight vehicles, have been substantiated; specific features of the oxidation of materials based on zirconium and hafnium diborides have been touched briefly; the methods of increasing oxidation resistance of these materials that have been developed by various groups of researchers have been demonstrate; some works concerning the behavior of samples under the effect of high-enthalpy flows of dissociated air have been described, including those that simulate sharp leading domes and edges of wings of hypersonic flight vehicles.     

Functional ceramic materials database: an online resource for materials research

We present work on the creation of a ceramic materials database which contains data gleaned from literature data sets as well as new data obtained from combinatorial experiments on the London University Search Instrument. At the time of this writing, the database contains data related to two main groups of materials, mainly in the perovskite family. Permittivity measurements of electroceramic materials are the first area of interest, while ion diffusion measurements of oxygen ion conductors are the second. The nature of the database design does not restrict the type of measurements which can be stored; as the available data increase, the database may become a generic, publicly available ceramic materials resource.     

Copolymers dispersions designed to shaping of ceramic materials

Journal of Thermal Analysis and Calorimetry - To study the effect of ionic liquids (ILs) of the microstructure on the surface of the coal, four ILs ([Emim][BF4], [Bmim][BF4], [Bmim][NO3], and...     

Effect of stock dispersity on properties of ceramic materials

Powdered ceramic piezoelectric phases of fixed chemical composition and prescribed particle size in the range from 15 to 350 nm were obtained using a unified synthesis technique. The dependence of their electrical parameters on the granulometric composition of the stock was studied.     

Flow injection spectrophotometric determination of boron in ceramic materials

A flow injection spectrophotometric method for the determination of boron in ceramic materials is described. The method is based on spectrophotometric measurement of the decrease in the pH produced by the reaction between boric acid and mannitol in the presence of an acid-base indicator. A bichannel FI (flow injection) manifold in which the sample solutions were injected into deionized water (at pH 5.4) and the stream was later merged with the reagent stream (a mannitol solution containing 1x10(-4) mol l(-1) bromocresol green at pH 5.4), was used. Transient signals were monitored at 616 nm. A theoretical model which describes the dependence between the absorbance values and boric acid concentration is presented. The model predicts a non linear dependence between the absorbance or increment in absorbance and the boric acid concentration. In contrast, the model predicts a linear dependence between the inverse of the absorbance values and the boric acid concentration. The calibration graphs (1/A vs mug ml(-1) B(2)O(3)) were linear over the range 1-30 mug ml(-1) of B(2)O(3). The relative standard deviations were 0.7 and 0.4% for 4 and 8 mug ml(-1) of B(2)O(3), respectively. The limit of detection was 0.02 mug ml(-1) of B(2)O(3) (3sigma criterium). The method was used to determine boron in nine ceramic materials with very different nominal boron compositions. The results were compared with those obtained using a potentiometric titration method as reference method. No significant differences (at 95% probability level) were found between the proposed and reference methods. The method is rapid, reliable, precise and free of interferences.     

Uptake studies of some fission products using ceramic materials

The uptake of Eu(III) and Zr(IV) was studied on ceramic materials of TiO₂, SiO₂ and Al₂O₃, prepared by the hydrolysis process. The uptake behavior of Eu(III) and Zr(IV) was investigated under different experimental conditions such as contact time, pH-value in the presence and in absence of complexing agent. X-ray fluorescence, powder morphology, specific surface area, X-ray diffraction analysis in addition to the DTA and TG were applied on the tested ceramic samples. The present study showed that the ceramic materials, prepared by an advanced technique are not only efficient for uptake of Eu(III) and Zr(IV), but also permitted the separation of these radioisotopes.     

Production of porous ceramic materials using nanodisperse SiC powder

Porous ceramic materials were produced by hot pressing of a nanocrystalline (19 nm) silicon carbide powder synthesized by a hybrid method that combined the sol–gel processing of a finely divided and chemically reactive SiO₂–C system and the carbothermic synthesis at moderate (1400°C) temperature in a vacuum. It was studied how such characteristics as density, porosity, sizes of crystallites and aggregates of SiC particles, specific surface area, and compressive strength depend on pressing temperature (1400, 1500, 1600, and 1700°C).     

Depollution of some radioactive residual waters on ceramic materials

The present paper deals with the study of retaining of⁵⁵⁺⁵⁹Fe³⁺ and¹¹⁵Cd²⁺ ions from residual waters, on ceramic materials. At the same time, the leaching of⁵⁵⁺⁵⁹Fe³⁺ ions previously retained on these ceramic materials in contact with a hydrochloric acid solution as corrosive agent, has been studied.     

Adsorption of plasmid DNA on ceramic hydroxyapatite chromatographic materials

The adsorption of plasmid DNA onto two different types of ceramic hydroxyapatite beads with a particle diameter of 20 μm, namely Ceramic Hydroxyapatite Type II and the Type III, which is not commercially available, were investigated. Type II and the Type III have a pore diameter of 80 and 240 nm, respectively. Equilibrium and dynamic binding capacity for a 4.9 kbp model plasmid on Ceramic Hydroxyapatite Type II and Type III were enhanced by addition of NaCl to the adsorption buffer. This result indicates that the adsorption mechanism cannot be solely explained by electrostatic interaction. The affinities of plasmid DNA for Ceramic Hydroxyapatite Type II (with a K(D) of ≈0.005 mg/mL) and to Hydroxyapatite Type III (with a K(D) of ≈0.045 mg/mL) were not affected by NaCl, whereas the binding capacity was. This observation corroborates the assumption that a change of the shape of the plasmid molecule is affected and could be the reason for increased binding capacity with salt. The maximal binding capacity shows that at least a part of the CHT II bead must be accessible for the plasmid, whereas CHT III can be saturated with the plasmid. In both cases, an extremely hindered transport takes place.     

Microanalytical determination of tin in organotin compounds

Existing procedures for the determination of tin in organotin compounds are reviewed, and a new procedure is described which can be used for the rapid microanalysis of most organotin compounds. Wet oxidation with sulphuric acid and 30% hydrogen peroxide is followed by spectrophotometric determination of the extracted ternary tin(IV)-chloride-oxine complex in chloroform. Time for a single determination is 20 min, and the relative standard deviation is 0.7% for 1-5 mg of tin. On account of their volatility, methyltin compounds must be subjected to a sealed-tube wet oxidation in sulphuric-nitric acid mixture. Addition of sulphamic acid after boiling to remove most of the nitric acid makes this compatible with the solvent extraction step. Tin present as organotin stabilizer in PVC samples can also be determined by this method, after destruction of the organic matter with sulphuric acid and 50% hydrogen peroxide.     

Application of analytical transmission electron microscopy to the characterization of interlayers in fibre-reinforced composites with ceramic and glass matrices

The microchemistry of interfaces and corresponding interlayers in different fibre-reinforced ceramic and glass composite systems has been investigated by using a dedicated scanning transmission electron microscope demonstrating the potential applicabilities of such an instrument to this large field of materials science. Energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy were used to determine the materials composition on a nanometre scale. Besides analyses performed in the spot mode of the electron probe the distributions of the elements present in the interface region were measured as line profiles across the relevant interface structure by X-ray spectroscopy with a lateral resolution of about 5 nm, even for the detection of a light element as carbon. Moreover, in the composite systems under investigation the two-dimensional element distribution was also attained by energy-filtered imaging. In addition, first results of energy loss near edge structure analyses are presented indicating variations of the chemical bonding of silicon at the interface in a Nicalon fibre/Duran glass composite.     

Microanalytical systems for separations of stratum corneum ceramides

The small amount of lipids from human skin obtained with noninvasive sampling method led us to investigate microanalytical separation techniques. The lipid class analysis was performed with a micro polyvinyl alcohol-silica (PVA-Sil) column. The gradient elution was from heptane to acetone/butanol 90:10 v/v in 4%/min at 78 microL/min. In addition an evaporative light scattering detector (ELSD) was modified for micro-LC. All solvents contained 0.1% of triethylamine and formic acid in stoichiometric amount, which increased the ELSD response. In these conditions, the cholesterol eluted before free fatty acid, and squalene and triglycerides close to the dead volume. The various ceramide classes eluted following the order of the increased number of hydroxyl groups. The LOD for ceramides was 2.2 ng. The advantages of this method are the use of a normal stationary phase more reliable due to its chemical stability, its surface homogeneity and its development in microchromatography without chlorinated solvents which offers small LOD and the whole profile of lipids present in stratum corneum (SC). A method using a narrow-bore PVA-Sil column was used to collect ceramide fraction. Then the molecular species were analysed with a porous graphitic carbon column in capillary LC using a gradient from CH3OH/CHCl3 70:30 v/v to CHCl3 at 2%/min with a flow rate at 5 microL/min. The LOD obtained for ceramide was 1 ng. Both methods were assessed with SC samples obtained by rinsing a 5.7 cm2 area of the forearm with 25 mL of ethanol.     

Microanalytical determination of metallic constituents of river sediments

Summary The distribution of metallic constituents in torrential rivers as a function of the size particle cannot be frequently achieved by conventional analytical procedures, because of the lack of sufficient amounts of the fine fractions. For the study of river sediments in the Basque Country, microanalytical methods have been developed both for major (Na, K, Ca, Mg, Fe, Al, Si) and trace (Cu, Zn, Mn, Cr, Pb, Ni, Cd) components. Wet digestion in PTFE vessels at 140°C was done with 0.05 g sample using HNO₃-HClO₄-HF-H₃BO₃ or HNO₃-HClO₄, respectively. Further determinations were made by i) emission spectrometry (Na, K), ii) visible spectrophotometry (Al), iii) FIA (Fe, Si) and iv) AAS with flow spoiler (Ca, Mg, Cu, Zn, Mn) or graphite furnace (Cr, Pb, Ni, Cd). The proposed method has been checked with a standard sample obtaining mean values almost coincident with the certified ones and variation coefficients lower than 2% for major and 8% for trace components. Then it was applied to total samples and the fine fractions (<63 m) of 26 samples of sediments from three torrential rivers. Replicated values with analogous variation coefficients were obtained. Some considerations on distribution of major and trace constituents as a function of particle size are also included.     

Cathodic electrodeposition of ceramic and organoceramic materials. Fundamental aspects

Electrodeposition of ceramic materials can be performed by electrophoretic (EPD) or electrolytic (ELD) deposition. Electrophoretic deposition is achieved via motion of charged particles towards an electrode under an applied electric field. Electrolytic deposition produces colloidal particles in cathodic reactions for subsequent deposition. Various electrochemical strategies and deposition mechanisms have been developed for electrodeposition of ceramic and organoceramic films, and are discussed in the present article. Electrode-position of ceramic and organoceramic materials includes mass transport, accumulation of particles near the electrode and their coagulation to form a cathodic deposit. Various types of interparticle forces that govern colloidal stability in the absence and presence of processing additives are discussed. Novel theoretical contributions towards an interpretation of particle coagulation near the electrode surface are reviewed. Background information is given on the methods of particle charging, stabilization of colloids in aqueous and non-aqueous media, electrophoretic mobility of ceramic particles and polyelectrolytes, and electrode reactions. This review also covers recent developments in the electrodeposition of ceramic and organoceramic materials.     

Characterization of metallic and ceramic high-temperature materials for energy systems

For the development of metallic and ceramic high temperature materials used, for example, in heat exchanger components, in turbine blades for stationary gas turbines, in ceramic industrial products and fusion reactor components, modern physico-chemical characterization methods are required. The formation stability of naturally formed protective scales is of prime importance in the successful application of metallic materials at high temperatures in aggressive atmospheres. For the characterization and investigation of the growth mechanisms of such surface scales, the main emphasis is placed on such modern spectroscopical methods as SIMS, SNMS, GDOS, EPMA and RBS. The morphology and composition of oxide scales have been investigated by imaging and diffraction techniques. The thermal and mechanical damage behaviour of high-temperature materials for application in fusion reactor components is of importance. Damage behaviour has been simulated by electron beam and laser irradiation experiments, especially by means of in situ techniques in a scanning electron microscope. By such techniques the material erosion, crack formation and crack propagation were studied for ceramic high temperature materials as a function of load parameters. The erosion and the crack formation processes are superim-posed by a redeposition of vaporized material and by thermally activated creep of the binder phases. The application potential for all methods discussed is outlined and available results are presented.