Włodzimierz Bogdanowicz

Correlation between SEM and X-Ray Diffraction Imaging of Defect Structure in Single-Crystal Ni-Based Superalloy

In the work the single-crystalline alloy CMSX-4 was studied. The main aim of the study was an attempt to find correlations between images of X-Ray topography, X-ray diffraction maps of lattice parameter and misorientation angle and Scanning Electron Microscopy (SEM) images obtained by back-scattered electron (BSE) technique. Topography images were obtained by Auleytner method with wide beam. Diffractometer provided by EFG company was used for obtaining orientation and lattice parameter maps. Material for research was produced in Research and Development Laboratory for Aerospace Materials of Rzeszów University of Technology. Casts were obtained in ALD furnace by the Bridgman technique. It was found that X-ray topograms were correlated with SEM images of microstructures as well as with orientation and lattice parameter maps. X-Ray topograms showed high contrast bands which corresponded to dendrite arms. There was a correlation between low angle boundary and lattice parameter map.

Two-subgrain single quasicrystals Al–Cu–Co alloy growth and characterisation

Two-subgrain single quasicrystals with subgrain boundaries parallel to the direction of solidification were obtained by the modification of Bridgman method, with asymmetric heat abstraction. One of the subgrains of single quasicrystals was formed through the peritectic reaction of the Al(Cu,Co) phase. The other subgrain solidified directly from the melted phase. Two different types of band structures of single quasicrystals were determined by X-ray topography and metallography methods. The orientation of these structures in relation to the ten-fold symmetry axis of single quasicrystal and the solidification front was investigated. The formation mechanism of both kinds of structure were suggested.

Growth morphology of single-crystal grains obtained by directional crystallisation of an Al–Cu–Fe alloy

Quasicrystalline as well as crystalline faceted single grains of four phases were obtained during directional crystallisation of an Al–Cu–Fe alloy by the Bridgman technique. The monoclinic λ phase, Al13(Cu, Fe)4, dominating at high temperatures formed single-crystal lamellae 0.5 mm to 1 mm thick. A second type of attractive morphological form exhibiting flux dissolution terraces was observed on spherical single crystals of β phase Al(Fe, Cu). Rectangular, hexagonal and octagonal shaped dissolution terraces were revealed at the positions of two-, three- and four-fold symmetry axes, respectively. A single quasicrystalline ψ phase, Al6Cu2Fe, exhibited icosahedral symmetry with growth forms of a dodecahedron with pentagonal facets. The flux dissolution of the β phase apparently plays an essential role in a peritectic reaction leading to quasicrystalline ψ phase formation. Polygonal single grains of ω phase Al7Cu2Fe exhibiting tetragonal symmetry formed the fourth type of thermodynamically stable growth forms. Single grains of the ω phase crystallised in the form of pellets with an octagonal cross-section. The growth morphology of the stable phases was investigated by scanning electron microscopy. The chemical composition of the growth forms described was confirmed by X-ray microanalysis using a scanning electron microscope, whereas the phase composition was determined using electron selected area diffraction and X-ray powder diffraction.

X-Ray Topography Study of the Nickel Superalloy CMSX-4 Single Crystals

The paper attempts to determine structural perfection of monocrystalline nickel superalloys using X-ray topography. Monocrystalline bars and turbine blades were manufactured in an ALD Vacuum Technologies furnace using the Bridgman method. Pulling out rates typical for CMSX-4 nickel superalloys were used. It has been found that in the case of monocrystalline bars the structural perfection determined based on X-ray topograms does not depend on the distance from the selector. Instead, for blades the structural perfection significantly decreases with increasing distance from the selector.

Characterization of Single-Crystal Turbine Blades by X-Ray Diffraction Methods

Characterization of structure defects in turbine blades is the basis for determination of the overall crystalline perfections. This work presents the possibilities of identifying casting defects by combining different X-ray diffraction techniques. The investigation was conducted on samples prepared from as-cast turbine blades airfoil and tips. It was found that X-ray topograms revealed dendritic structure and macro strain areas. The defects areas which have appeared on topograms were also investigated by X-ray diffraction mapping technique by EFG diffractometer. Additionally, the X-ray investigation was complemented by macro SEM images obtained by stitching several images of microstructure. The X-ray maps of misorientation angle and X-ray topograms revealed deviation between the γ’ direction and the blade axis and rotation of the primary dendrite arm around this axis.

Structural Perfection of a Single Crystal Nickel-Based CMSX-4 Superalloy

The aircraft engines turbine blades are manufactured from nickel-base superalloys and they are often in a single crystal form. This ensures the best high-temperature creep resistance as compared with blades of equiaxial grains microstructure and of columnar grains microstructure. Turbine blades were manufactured in an ALD Vacuum Technologies furnace. The study has examined structural perfection of single crystal blades obtained by Bridgeman method from CMSX-4 nickel superalloy at various withdrawal rates: 1, 2, 3, 4 and 5mm/min.

Microstructure of a composite with a quasicrystalline phase fraction obtained by directional solidification of Al61Cu27Fe12 alloy

The microstructure of a composite containing a quasicrystal phase, i.e. so-called crystal–quasicrystal (CQ) composite, was studied. The CQ composite was obtained by the Bridgman method via solidification of Al61Cu27Fe12 alloy (numbers indicate at%). The process was conducted at a pull out rate of v = 0.07 mm/min. The average temperature gradient in the heating zone was 43 K/cm. The composite matrix consisted of cubic β phase Al(Fe, Cu), with reinforcement of λ-phase rod-shaped fibres surrounded by a quasicrystal icosahedral ψ phase, which also existed in the fibre core. The fibres were rhomboidal in cross-section. The composite was studied using X-ray and electron diffraction, light-optical and scanning electron microscopy (SEM), X-ray topography and Laue diffraction.

β′-SnSb single crystals obtained by the method of inclined front crystallization

Abstract β′ phase plates of single crystals of SnSb alloy were obtained by using a modification of the horizontal Bridgman method. It was ascertained that during crystallization the single crystals grow in the upper layer of the charge. It was found that the thickness of the single crystal (single crystal layer) and also its relative antimony content, depend on the growth rate and on the angle of inclination of the crystallization front relative to the growth direction. A model proposed for the crystallization process permits the description of these relations obtained. This method for obtaining single crystals, the inclined front crystallization (IFC) method, offers new possibilities for control of chemical composition of plate single crystals of intermetallic phases, by varying the angle of inclination of the crystallization front.

Structural Defects of Initial Crystallization Areas in Single-Crystalline Turbine Blades

The as-cast single-crystalline turbine blades made of CMSX-4 superalloy were studied. The blades were obtained by the Bridgman technique at a withdrawal rate of 5mm/min. The as-cast samples were prepared by cutting the blade root with a fragment of selector. The dendritic structure of obtained samples was studied by Scanning Electron Microscopy. The crystal orientation and lattice parameters were analyzed by Ω-scan mapping method. Additionally, the X-ray diffraction topography was applied. It was found that the most structural defects are created in the areas where a change in the shape and dimensions of the blades occur. Even minor changes in their geometry and the unevenness of mold walls may also affect the formation of defects.

Two Methods of Studying Structure Perfection of Single Crystal Nickel-Based Superalloys

The article presents the comparison of two methods: classical X-ray topography and the modern automatic X-ray OD-EFG diffractometer. Both methods were applied to study the crystal orientation of turbine blades of single crystal nickel-based superalloys. The solidification of a hollow assembly structure for 5 various blades was carried out by the Bridgman method at the Research and Development Laboratory for Aerospace Materials at Rzeszow University of Technology using an ALD Vacuum Technologies vacuum furnace. Ceramic moulds made of Al2O3 were used. The alloy temperature during casting into the mould amounted to 1550°C. The specimens for Laue method tests were cut out from the blades at withdrawal rates of 1, 2, 3, 4, and 5 mm/min.