Krzysztof Bryła

Ultra-fine grained and even nanostructured magnesium alloys obtained by processing with methods of severe plastic deformation (SPD) are promising biomaterials for absorbable orthopaedic implants due to their enhanced mechanical properties, adequate corrosion resistance and biocompatibility. This paper presents an overview of the impact of the most important SPD methods – equal-channel angular pressing (ECAP) and high-pressure torsion (HPT) – on microstructure refinement and improvement of the mechanical properties of magnesium alloys intended for medical implants. Several selected groups of magnesium alloys which have the potential for use as bioabsorbable implants are discussed. The presented results of many years of research indicate the beneficial effect of SPD methods on obtaining ultra-fine and even nanostructures of magnesium alloys with improved mechanical and better functional properties, which are necessary for bioabsorbable implants.

Titanium diboride (TiB₂) is a hard, refractory material, attractive for a number of applications, including wear-resistant machine parts and tools, but it is difficult to densify. The spark plasma sintering (SPS) method allows producing TiB₂-based composites of high density with different sintering aids, among them titanium silicides. In this paper, Ti₅Si₃ is used as a sintering aid for the sintering of TiB₂/10 wt % Ti₅Si₃ and TiB₂/20 wt % Ti₅Si₃ composites at 1600 °C and 1700 °C for 10 min. The phase composition of the initial powders and produced composites was analyzed by the X-ray diffraction method using CuK_α radiation. The microstructure was examined using scanning electron microscopy, accompanied by energy-dispersive spectroscopy (EDS). The hardness was determined using a diamond indenter of Vickers geometry loaded at 9.81 N. Friction–wear properties were tested in the dry sliding test in a ball-on-disc configuration, using WC as a counterpart material. The major phases present in the TiB₂/Ti₅Si₃ composites were TiB₂ and Ti₅Si_3. Traces of TiC were also identified. The hardness of the TiB₂/Ti₅Si₃ composites was in the range of 1860–2056 HV1 and decreased with Ti₅Si₃ content, as well as the specific wear rate W_v. The coefficient of friction for the composites was in the range of 0.5–0.54, almost the same as for TiB₂ sinters. The main mechanism of wear was abrasive.

As part of the tests, a two-phase NiAl/Ni₃Al alloy and a composite based on this alloy with 4 vol% addition of TiB₂ were produced by the reactive FAST/SPS (Field Assisted Sintering Technology/Spark Plasma Sintering) sintering method. The sintering process was carried out at 1273 K for 30 s under an argon atmosphere. The effect of reactive SPS on the density, microstructure, and mechanical and tribological properties of a dual-phase Ni-Al intermetallic compound and Ni-Al-TiB₂ composite was investigated. Products obtained were characterized by a high degree of sintering (over 99% of the theoretical density). The microstructure of sinters was characterized by a large diversity, mainly in regard to the structure of the dual-phase alloy (matrix). Compression tests showed satisfactory plastic properties of the manufactured materials, especially at high temperature (1073 K). For both materials at room temperature, the compressive strength was over 3 GPa. The stress–strain curves were observed to assume a different course for the matrix material and composite material, including differences in the maximum plastic flow stress depending on the test temperature. The brittle-to-ductile transition temperature was determined to be above 873 K. The research has revealed differences in the physical, mechanical and tribological properties of the produced sinters. However, the differences favourable for the composite were mostly the result of the addition of TiB₂ ceramic particles uniformly distributed on grain boundaries.

Low-temperature phase transitions in the EZ33A Mg-cast alloy have been investigated. Based on the structure assessment of the alloy after annealing at 150 °C (1826 h) and at 200 °C (2371 h) a grain boundary wetting transition by a second solid phase was documented. Within a 50 °C temperature range, substantial differences in the α(Mg) grain boundary fraction wetted by the (Mg,Zn)₁₂RE intermetallic were observed. In contrast to what was reported in the literature, two different types of precipitates were found within α(Mg) grains. With increasing annealing temperatures, both types of precipitates dissolved.

Producing ultrafine-grained (UFG) materials by means of severe plastic deformation (SPD) methods has made a significant progress within the past few decades. The topic has been of interest since the beginning of the last century at least, yet the historical studies on this subject are less-known in the SPD society. In this manuscript, the studies of the Polish scientist Stanisław Erbel including his book entitled “Mechanism of Change of Properties of Metals Subjected to Large Deformations” written in 1976 are reviewed. Although American physicist Percy W. Bridgman published a book earlier on the principles of SPD in 1952, Erbel’s book is probably the first book dedicated to the formation of UFG materials by SPD processing. In this book, Erbel presented details of a high-pressure torsion (HPT) device for obtaining large strains, mechanism of microstructural fragmentation during large straining, evolution of mechanical properties (hardness, tensile properties and torque), and characterization of the microstructure by means of transmission electron microscopy (TEM). The TEM studies included not only ex-situ observations but also in-situ observations to examine the dislocation motion and thermal stability.

Cylindrical tubes made of commercially-pure titanium (CP-Ti) filled with various mandrels (metallic as well as non-metallic materials) were processed by Equal Channel Angular Pressing (ECAP). Different temperatures (500°C down to room temperature), routes (Bc, B 120 , C), tools and number of passes (1-6) were applied depending on the mandrel material. For reasons of comparison, solid bolts made of metallic mandrel materials were processed at the same ECAP conditions. The mechanical properties of as-received as well as ECAP tubes and core materials were characterised by hardness mappings (in order to reveal the homogeneity) and tensile tests. The results can be summarised as follows: i) It is feasible to process tubes by ECAP; ii) Using appropriate mandrels, tubes made of CP-Ti can be processed by ECAP at significantly lower temperatures, even at room temperature, as compared to solid bolts; iii) Mechanical properties of tubes and mandrel materials after ECAP are similar to or even better than those of their solid counterparts; iv) Tubes after ECAP at low temperatures show higher strength than what can be achieved in bulk material; v) Excellent homogeneity of microhardness is achieved at least when metallic mandrels and a sufficient number of ECAP passes are used.