EDITORIAL COLUMN
SUBSTANCES ANALYSIS
An approach to analysis of advanced sensor materials based on cobalt oxide modified with zinc or nickel oxides is developed using X- ray fluorescence analysis (XRF) and inductively coupled plasma mass spectrometry (ICP-MS). It is shown that determination of Ni, Zn and Co in novel materials based on cobalt oxide using ICP-MS in solutions is possible, standard deviation being 0.06, 0.06, and 0.05, respectively. The results of the ICP-MS determination of the elements in solutions are used to certify the results obtained by XRF method without sample preparation. It is shown that NixCo3–xO4–д samples can be correctly analyzed without decomposition using X- ray fluorescence analysis. The results of the determination match theoretically calculated values both for the samples obtained from nitrates and from nickel and cobalt oxalates as well. However, calibration based on the ICP-MS results is necessary for X-ray fluorescence analysis of ZnxCo3–xO4 samples. It is shown that zinc content in the samples exceeds the theoretical determined value by 10 – 30% due to incomplete precipitation of cobalt from the solution upon synthesis.
At present, high-temperature composites of the Nb-Si-system are the most promising for use as High-temperature composites of Nb – Si-system are among the most promising materials to be used as heat-resistant structural materials and as an alternative to high- temperature nickel-based alloys that have largely exhausted their ability to increase the operating temperature. The next generation of high-temperature materials for casting blades of gas turbine engines should provide a temperature of about 1350°C or higher which can significantly improve the efficiency of engines and contribute to their environmental performance. Nb – Si composites are obtained by traditional methods of ingot production and powder metallurgy. Statutory regulations impose heavy demands on the chemical composition of aviation materials used for manufacturing heavy-duty parts of gas turbine engines. We present a technique for determination of the alloying elements Si, Ti, W, Mo, Hf, Cr, and Al in advanced high-temperature Nb – Si based composite materials (CM) using inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and microwave sample preparation. Conditions of sample dissolution, method of calibration line construction, and analytical lines free of significant spectral overlapping are specified to determine all the alloying elements of Nb – Si-based composites. To assess the metrological characteristics of the developed technique we used model solutions of Nb – Si composites prepared from state standard reference sample of solutions of ions of the elements. The repeatability of the technique does not exceed 1% rel., the intermediate precision does not exceed 3% rel.
Microwave and traditional methods of dissolving charge and single crystals of complex borates Ca3Y2(BO3)4,Ca3Nd2(BO3)4,Ca3Gd2(BO3)4 are proposed. The advantages and prospects of using microwave heating for solubilization of complex borates are shown. Procedures for determination of the macrocomponents Ca, Y, Nd, Gd, B in complex borates are developed. Correctness of determination of the main components in complex borates is confirmed on model solutions in spiking tests method and on the real samples using the method of sample weight variation
PHYSICAL METHODS OF RESEARCH AND MONITORING
Advantages of direct laser cladding of metal consisting in the possibility of directional crystallization of 316L stainless steel samples are shown. Direct laser cladding of metal offers exciting possibilities for production of single crystal structures by directional crystallization of the deposited metal. The growth direction of dendritic crystals is driven by the thermal center determined by the position of the laser spot. We present a technique of manufacturing stainless steel products by direct laser deposition using the developed algorithm which allowed us to connect the movement of the robotic cell and turntable with a sample, laser switching and feeding of the gas powder mixture. The possibility of x-ray tomographic quality control of the obtained products, determination of the parameters of the laser spot on the substrate surface using high-speed photography, estimation of the phase composition of the deposited metal using x-ray diffraction analysis is demonstrated. The structure of obtained metal samples is represented by dendritic crystals oriented in the direction of the thermal center. The sample structure in the sample cross section is represented in the form of a honeycomb formed by the first order axes of dendritic crystals. It is shown that 200-мm thickness of the deposited layer in the central part of the sample does not interfere with the development of the dendritic structure and promotes the possibility of obtaining single- crystal structures free of pores and cracks. The possibility of estimating the inclination angle of dendritic crystals in the metal relative to the symmetry axis of the sample using a metallographic software package for analysis of digital images of the microstructures is shown. It is demonstrated that the roughness of the obtained samples is determined by the size of the powder particles and can be eliminated by the mechanical treatment.
The issues regarding the reliability of assessing health of the oiled joints of aircraft gas turbine engines (GTE) proceeding from the results of spectral and ferrographic measurement of the parameters of wear particles are considered. It is shown that, due to design features of the oil system analysis of the oil sample does not provide enough information about the wear processes in the GTE joints. Growth of the number of diagnostic parameters (particle concentration, form and size) does not significantly in- crease the reliability of health assessment, whereas analysis of the oil filter wipe sampling provides full information about engine wear processes. The main measurement instrumentation requirements are considered. High reliability of diagnostic results can be attained when the parameters of wear particles are measured over the full range of their variation. Issues regarding the recurrence of engine health assessment in case of using fine-meshed oil filter with 600-h lifetime are discussed. The use of expendable oil filters with a diagnostic layer can solve the problem. Diagnostic potentials of some promising methods of assessment and prognosis of the oiingl system health in aircraft GTE are evaluated.
Substantiation of using fractal analysis in studying the images of Palmquist microcracks is presented. The numerical values of the fractal dimension of the Palmquist microcracks (PMC) at various sites of crack propagation (the Vickers indenter) are determined. A sintered carbide alloy (cermet) based of titanium carbonitride with nickel-molybdenum binder (KNT12) was taken as a test object. A method of quantitative analysis in the study of the PMC images obtained using scanning electron microscope is considered. An example of the length measurements in which the measured value depends on the scale of measurements (Richardson coastline paradox) is taken as a basis. We used a simple method of covering the curve image on the plane by the squares of different sizes to determine the fractal dimension of the curve. Fractal dimension (parameter) of the image of the PMC contour was determined in two ways: i) at a constant magnification and ii) using series of images with a monotonically varying magnification.
MATERIALS MECHANICS: STRENGTH, DURABILITY, SAFETY
A computational and experimental modeling of the scatter in technologies is presented for steel 15Kh2NMFA at room temperature to reveal possible variations in the ultimate strength at a limited number of melts. The developed method of step-by-step “mixing” of technological samples (up to seven samples) is used to determine and assess the values of the parameters of the distribution functions and probability density functions. An increase in the total number of samples and melts makes it possible to improve the accuracy of the determination of the material characteristics in the region of large and small probabilities (1 – 5%) and estimate the features of intra-melt scattering. The results showed that with the extension of the range of distribution functions to probabilities of 1 – 99% with increasing number of samples and the number of melts, the normal distribution functions of the mechanical properties usually remain similar and close to the two- threshold distribution both for single melt and for the sum of several melts (a trend to 3 – 3.5 -fold increase of intra-melt scattering is observed). “Heavy tails” can appear on the distribution curves at low probabilities (below the defective level). Presence of “heavy tails” interferes with direct use of the minimum guaranteed roperties without relevant tests and leads to violation in strength and resource calculations. The considered problems also touch on the analysis of safety and risks.
Conditions of brittle fracture arrest occurring in rolled sheet of low-alloyed steels at a specific temperature are considered. The problem of revealing correlation between this temperature, thickness of testing specimen and material properties is analyzed using finite element method for computer simulation of unstable crack propagation in 3D setting with specified local criteria of brittle and ductile fracture.
The issues of deformation processing of low-carbon steel billets using combined impact of extrusion and screw pressing (ESP) are considered. The results of low-temperature tensile tests of steel samples are presented. It is shown that the characteristics of strength and plasticity (ductility) of steel subjected to ESP at lower test temperatures (213 K) are higher than that at room temperature. A fractographic study of the destruction mechanisms of the steel in as-received condition and after ESP processing at room temperature and at a test temperature of 213 K revealed a ductile (viscous) character of the destruction mechanism with micro pits and pits present in all areas of the fracture surface.
MATHEMATICAL METHODS OF INVESTIGATION
The problems of correct and effective choice of the methods and means used for leakage monitoring by penetrating substances (gases) on the basis of certain criteria are considered. Methods of mathematical statistics are used for classification analysis of the main characteristics of the leakage test methods and approaches in the framework of general theoretical research to prioritize them in compliance with current GOST 51780–2001. In other words, an attempt has been made to search for and identify the effective ways of ordering the classification structure from the main characteristics of the methods and means of leak testing necessary for the researcher at the preparatory stage of testing. This is partly due to the lack of clear recommendations in this standard regarding the significance of these characteristics for leakage control in real conditions and possibility of its implementation. The procedure rests on the proposed nonparametric algorithm which includes classification of the characteristics based on pairwise clustering. The expert evaluation method is used for effective addressing the problem of nonparametric analysis. Solutions of multivariate analysis are given for the problem of inverse reduction of characteristics to a small number of groups formed on the basis of generalizing features using discriminative analysis on the basis of nonparametric criteria to check statistically significant difference. Comparatively high posterior probability of attributing the classification features to the groups distributed among six clusters is determined as a result of studying characteristics pertaining mainly to the leakage test facilities (as the most numerous ones compared to test methods). We also consider and assess the possibility of introducing some clarifications to refine the current standard.
ISSN 2588-0187 (Online)