An analysis of defects creation in the vicinity of the selector-root connection plane in single-crystalline turbine blades made of CMSX-4 Ni-base superalloy was performed using several experimental methods. A coupling of scanning electron microscopy and X-ray diffraction topography allowed the visualization of dendritic arrays and surface defects in the root part of the blades. As a result, contrast inversions and areas where internal stresses occur were observed. The defects on a microscopic scale were characterized using positron annihilation lifetime spectroscopy and transmission electron microscopy. The registered positron lifetimes, above 0.5 ns, beyond the range characteristic for defects generally reported in metals and their alloys suggest the presence extremely large void type defects. Herein, we have identified large defects, ca. 2–5 nm in diameter, formed due to the contraction of fluid metal, captured in inter-dendritic regions during the liquid-to-solid transition. This work is a precursor to the almost untouched area of the discussion of lifetimes characteristic for positron bound states, called positronium (>0.5 ns) in relation to the morphology of void-type defects in single-crystalline superalloys.
This paper presents the results of tribological tests on WE43 and WE54 magnesium alloys with rare earth metals performed in linear reciprocating motion for four different material couples (AISI 316-L steel, silicon nitride—Si3N4, WC tungsten carbide, and zirconium dioxide—ZrO2). Additionally, magnesium alloys were subjected to a complex heat treatment consisting of precipitation hardening combined with a deep cryogenic treatment. The study presents the effect of deep cryogenic treatment combined with precipitation hardening on the tribological properties of WE43 and WE54 alloys. Tribological tests revealed the most advantageous results for the magnesium alloy—AISI 316-L steel friction node. For both alloys tested after heat treatment, a nearly 2-fold reduction in specific wear rate has been achieved. Furthermore, microscopic examinations of the wear track areas and wear products were performed, and the wear mechanisms and types of wear products occurring in linear reciprocating friction were determined. Wear measurements were taken using the 3D profilometric method and compared with the results obtained from calculations performed in accordance with ASTM G133 and ASTM D7755, which were modified to improve the accuracy of the calculation results (the number of measured profiles was increased from four to eight). Appropriately selected calculation methods allow for obtaining reliable tribological test results and enabling the verification of both the most advantageous heat treatment variant and material couple, which results in an increase in the durability of the tested alloys.
The relationship between the angles of misorientation of macroscopic low-angle boundaries (LABs) and changes in the lattice parameter of the γ′-phase around the LABs in the root of single-crystalline (SX) turbine blades made of CMSX-4 superalloy were studied. The blades with an axial orientation of the [001] type were solidified using an industrial Bridgman furnace with a 3 mm/min withdrawal rate. X-ray diffraction topography, the EFG Ω-scan X-ray diffraction method, scanning electron microscopy, and Laue diffraction were used to study the thin lamellar samples with a thickness of 0.5 mm and orientation of the surface perpendicular to the [001] direction. It is found that in the areas with a width of a few millimetres around LABs, decreases in the lattice parameter of the γ′-phase occur. These lattice parameter changes are related to the internal stresses of the γ′-phase caused by local changes in the concentration of alloying elements and/or to the dendrite bending near the LABs. X-ray topography used on two surfaces of thin lamellar samples coupled with the lattice parameter measurements of the γ′-phase near the LAB allows separating the misorientation component of LAB diffraction contrast from the component and visualising the internal stresses of the γ′-phase.
The roots of cored single-crystalline turbine blades made of a nickel-based CMSX-4 superalloy were studied. The casts were solidified by the vertical Bridgman method in an industrial ALD furnace using the spiral selector and selector continuer situated asymmetrically in the blade root transverse section. Scanning electron microscopy, the Laue diffraction and X-ray diffraction topography were used to visualize the dendrite array and the local crystal misorientation of the roots. It has been stated that heterogeneity of the dendrite array and creation of low-angle boundaries (LABs) are mostly related to the lateral dendrite branching and rapid growth of the secondary and tertiary dendrites near the surface of the continuer–root connection. These processes have an unsteady character. Additionally, the influence of the mould walls on the dendrite array heterogeneity was studied. The processes of the lateral growth of the secondary dendrites and competitive longitudinal growth of the tertiary dendrites are discussed and a method of reducing the heterogeneity of the root dendrite array is proposed.
The variation of the crystal orientation and the dendrite array generated in the root of the single-crystalline (SX) turbine blades made of CMSX-4 superalloy were studied. The blades with an axial orientation of the [001] type were solidified by the industrial Bridgman technique using a spiral selector at a withdrawal rate of 3 mm/min. The analysis of the crystal orientation and dendrite arrangement was carried out using scanning electron microscopy, X-ray diffraction topography, and Laue diffraction. It was found that the lateral growth of such secondary dendrite arms, which are defined as “leading” and grow in the root at first, is related to the rotation of their crystal lattice, which is the reason for creation of the low-angle boundary (LAB) type defects. The primary crystal orientation of the selector extension (SE) area determines the areas and directions of the lateral growth of the leading arms. Additionally, it was found that in the SE areas of the root, near the connection with the selector, the spatial distribution of the [001]γ′ crystallographic direction has a complex wave-like character and may be related to the shape of the crystallization front.
The thin-walled airfoil areas of as-cast single-crystalline turbine blades made of CMSX-4 superalloy were studied. The blades were produced by the industrial Bridgman technique at withdrawal rates of 2, 3 and 4 mm/min. The angle between the [001] crystallographic direction and blade axis, related to the primary orientation, was defined by the Ω-scan X-ray diffraction method at points on the camber line located near the tip of an airfoil and at points of a line located in parallel and near the trailing edge. Additionally, primary crystal orientation was determined by Laue diffraction at the selected points of an airfoil. The influence of mould wall inclination on the primary crystal orientation of the thin-walled areas is discussed. The effect of change in the [001] crystallographic direction, named as "force directing", was considered with regard to the arrangement of primary dendrite arms in relation to the trailing edge and the camber line. It was stated that when the distance between the mould walls is less than the critical value of about 1.5 mm the "force directing" increases as the distance between the walls of the mould decreases. The effect may be controlled by selecting an appropriate secondary orientation using a seed crystal in the blade production process. The model of dendrite interaction with the mould walls, including bending and "deflection", was proposed.
An analysis of the defects in the vicinity of the selector–root connection plane occurring during the creation of single-crystalline turbine blades made of CMSX-6 Ni-based superalloy was performed. X-ray diffraction topography, scanning electron microscopy, and positron annihilation lifetime spectroscopy were used. Comparing the area of undisturbed axial growth of dendrites to the area of lateral growth concluded that the low-angle boundaries-like (LAB-like) defects were created in the root as a result of unsteady-state lateral growth of some secondary dendrite arms in layers of the root located directly at the selector–root connection plane. Additional macroscopic low-angle boundaries (LABs) with higher misorientation angles were created as a result of concave curvatures of liquidus isotherm in platform-like regions near selector–root connections. Two kinds of vacancy-type defects, mono-vacancies and vacancy clusters, were determined in relation to the LABs and LAB-like defects. Only mono-vacancies appeared in the areas of undisturbed axial growth. Reasons for the creation of macroscopic LABs and LAB-like defects, and their relationships with vacancy-type defects were discussed.
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.
Static and dynamic heterogeneity of disordered system is one of the current topics in materials science. In disordered ferroelectric materials with random fields, dynamic polar nanoregions (PNRs) appear at Burns temperature and freeze into nanodomain state below Curie temperature ( T C ). This state is very sensitive to external electric field and aging by which it gradually switches into macrodomain state. However, the role of PNRs in such states below T C is still a puzzling issue of materials science. Electric field and aging effects of uniaxial ferroelectric Sr x Ba 1− x Nb 2 O 6 ( x = 0.40, SBN40) single crystals were studied using Brillouin scattering to clarify the critical nature of PNRs in domain states below T C . On field heating, a broad anomaly in longitudinal acoustic (LA) velocity at low temperature region was due to an incomplete alignment of nanodomains caused by the interaction between PNRs. A sharp anomaly near T C was attributed to the complete switching of nanodomain to macrodomain state owing to the lack of interaction among PNRs. After isothermal aging below T C , the noticeable increase of LA velocity was observed. It was unaffected by cyclic temperature measurements up to T C , and recovered to initial state outside of a narrow temperature range above and below aging temperature.
High quality of solid solution single crystals SrxBa1‐xNb2O6 (0.35
Pure and undoped strontium-barium niobate Sr0.40Ba0.60Nb2O6 (SBN40) single crystals grown by the Czochralski method were investigated by single crystal X-ray diffraction methods. The study below TC (429 K for SBN40) confirmed the structure with P4bm space group. Above this temperature the structure transforms into the paraelectric, centrosymmetric one with P4/mbm space group. Analysis of the recorded diffraction patterns allowed to observe several signs of crystal structure modulation. On the registered diffraction images satellite reflections were found. A modulation vector q = (δ,±δ, ), where δ = 0.3075(6) (at room temperature) was found and it was similar to that occurring in the SBN61. In addition, above the phase transition temperature on the (hk) planes with l integer a weak diffuse scattering was observed.
Pure and undoped strontium-barium niobate Sr0.72Ba0.25Nb2O5.97 single crystals grown by the Czochralski method were investigated. Using X-ray Bond's method lattice parameters of this crystals are determined with high accuracy in the order of Δd/d=10−5. Based on the lattice parameter data measured at 298 K it was ascertained that the Sr0.72Ba0.25Nb2O5.97 single crystals belong to the tetragonal system. The additional analysis of the diffraction patterns performed by the Laue method confirmed the occurrence of a four-fold axis of symmetry.
Changes of lattice parameters of Sr x Ba 1‒ x Nb 2 O 6 (0.35 < x < 0.72) solid solution single crystals were measured as a function of temperature. The X‐ray Bond’ method was used to carry out very precise measurements of the lattice parameters. Fine correlations between values of the lattice parameter and the Sr concentration in the solid solution of Sr x Ba 1‒ x Nb 2 O 6 single crystals are found. A conventional analysis of lattice parameter data in terms of spontaneous strain and strain/order parameter coupling shows that a normal structural phase transition does occur. While the ferroelectric system (SBN26) displays a nearly tricritical behavior, β ≈ 0.20, the relaxor one (SBN61) complies with the two‐dimensional Ising‐model‐like criticality, β ≈ 0.17.
Single crystals of SrxBa1-x\Nb2O6 (0.26 < x < 0.75) solid solutions obtained by the Czochralski method were investigated. The lattice parameter measurements with high precision and accuracy were carried out in the temperature range of 290-520 K. These measurements showed the different character of lattice parameter changes. It was found that the a parameter monotonically increases with increasing of temperature, while the c parameter decreases up to the phase transition temperature T-C, and the next it begins increasing slowly. It was ascertained that with the increase of the Sr concentration in the studied crystals the changes of the lattice parameters were observed. They can be described according to the following relations: a = - 2.418 . 10(-5) x(2) + 1.050 . 10(-3) x + 12.479 angstrom and c = - 0.0015 x + 4.0216 angstrom. Basing on the obtained results the character of the phase transition was able to do.
Single crystals of SrxBa1-xNb2O6(0.26 a parameter monotonically increases with increasing of temperature, while the c parameter decreases up to the phase transition temperature TC, and the next it begins increasing slowly. It was ascertained that with the increase of the Sr concentration in the studied crystals the changes of the lattice parameters were observed. They can be described according to the following relations: a = - 2.418 • 10-5 x2+ 1.050 • 10-3 x + 12.479 Å and c = - 0.0015 x + 4.0216 Å. Basing on the obtained results the character of the phase transition was able to do.