We overview recent findings achieved in the field of model-driven development of additively manufactured porous materials for the development of a new generation of bioactive implants for orthopedic applications. Porous structures produced from biocompatible titanium alloys using selective laser melting can present a promising material to design scaffolds with regulated mechanical properties and with the capacity to be loaded with pharmaceutical products. Adjusting pore geometry, one could control elastic modulus and strength/fatigue properties of the engineered structures to be compatible with bone tissues, thus preventing the stress shield effect when replacing a diseased bone fragment. Adsorption of medicals by internal spaces would make it possible to emit the antibiotic and anti-tumor agents into surrounding tissues. The developed internal porosity and surface roughness can provide the desired vascularization and osteointegration. We critically analyze the recent advances in the field featuring model design approaches, virtual testing of the designed structures, capabilities of additive printing of porous structures, biomedical issues of the engineered scaffolds, and so on. Special attention is paid to highlighting the actual problems in the field and the ways of their solutions.
Ti15Mo metastable beta Ti alloy was solution treated and subsequently deformed by high-pressure torsion (HPT). HPT-deformed and benchmark non-deformed solution-treated materials were annealed at 400 °C and 500 °C in order to investigate the effect of UFG microstructure on the α-phase precipitation. Phase evolution was examined using laboratory X-ray diffraction (XRD) and by high-energy synchrotron X-ray diffraction (HEXRD), which provided more accurate measurements. Microstructure was observed by scanning electron microscopy (SEM) and microhardness was measured for all conditions. HPT deformation was found to significantly enhance the α phase precipitation due the introduction of lattice defects such as dislocations or grain boundaries, which act as preferential nucleation sites. Moreover, in HPT-deformed material, α precipitates are small and equiaxed, contrary to the α lamellae in the non-deformed material. ω phase formation is suppressed due to massive α precipitation and consequent element partitioning. Despite that, HPT-deformed material after ageing exhibits the high microhardness exceeding 450 HV.
The influence of the ultrafine-grained structure formed by equal-channel angular pressing via the “Conform” scheme on the fatigue behavior of metastable β-alloy Ti-15Mo has been studied. It is shown that the alloy with a two-phase ultrafine-grained structure achieved the best mechanical properties and enhanced fatigue endurance limit (up to 710 MPa on the basis of 107 cycles) due to the total contribution of grain boundary, dislocation, and phase strengthening mechanisms. A fractographic analysis of the fracture surface of samples after fatigue tests showed the features of fatigue crack propagation depending on the type of alloy microstructure. The general and distinctive features of fatigue failure of alloy samples in the initial coarse-grained (α + β)-, single-phase coarse-grained β-, and ultrafine-grained (α + β)-states are revealed. In all of the samples, a fatigue crack nucleated on the surface and propagated downward, i.e., perpendicular to the direction of the applied pressures. It is shown that fracture surfaces of the ultrafine-grained samples had a high roughness and were characterized by the presence of a large number of secondary cracks, as compared to the coarse-grained analogues.
Ti15Mo alloy was subjected to two techniques of intensive plastic deformation, namely high pressure torsion and rotary swaging at room temperature. The imposed strain resulted in the formation of an ultrafine-grained structure in both deformed conditions. Detailed inspection of the microstructure revealed the presence of grains with a size of around 100 nm in both conditions. The microstructure after rotary swaging also contained elongated grains with a length up to 1 µm. Isothermal ageing at 400 °C and 500 °C up to 16 h was applied to both conditions to investigate the kinetics of precipitation of the α phase and the recovery of lattice defects. Positron annihilation spectroscopy indicated that the recovery of lattice defects in the β matrix had already occurred at 400 °C and, in terms of positron trapping, was partly compensated by the precipitation of incoherent α particles. At 500 °C the recovery was fully offset by the formation of incoherent α/β interfaces. Contrary to common coarse-grained material, in which the α phase precipitates in the form of lamellae, precipitation of small and equiaxed α particles occurred in the deformed condition. A refined two-phase equiaxed microstructure with α particles and β grain sizes below 1 μm is achievable by simple rotary swaging followed by ageing.
The problem of the optimization of properties for biocompatible coatings as functional materials requires in-depth understanding of the coating formation processes; this allows for precise manufacturing of new generation implantable devices. Plasma electrolytic oxidation (PEO) opens the possibility for the design of biomimetic surfaces for better biocompatibility of titanium materials. The pulsed bipolar PEO process of cp-Ti under voltage control was investigated using joint analysis of the surface characterization and by in situ methods of impedance spectroscopy and optical emission spectroscopy. Scanning electron microscopy, X-ray diffractometry, coating thickness, and roughness measurements were used to characterize the surface morphology evolution during the treatment for 5 min. In situ impedance spectroscopy facilitated the evaluation of the PEO process frequency response and proposed the underlying equivalent circuit where parameters were correlated with the coating layer properties. In situ optical emission spectroscopy helped to analyze the spectral line evolutions for the substrate material and electrolyte species and to justify a method to estimate the coating thickness via the relation of the spectral line intensities. As a result, the optimal treatment time was established as 2 min; this provides a 9–11 µm thick PEO coating with Ra 1 µm, 3–5% porosity, and containing 75% of anatase. The methods for in-situ spectral diagnostics of the coating thickness and roughness were justified so that the treatment time can be corrected online when the coating achieves the required properties.
At present, researchers pay great attention to the development of metastable β-titanium alloys. A task of current importance is the enhancement of their strength and fatigue properties. An efficient method for increasing the strength of such alloys could be severe plastic deformation. The object of this study was a medical metastable β-titanium alloy Ti-15Mo (ASTM F2066). The alloy in the (α + β) state was for the first time deformed by combined processing, including equal channel angular pressing-conform and drawing. Such processing enabled the production of long-length rods with a length of 1500 mm. The aim of the work was to study the effect of the combined processing on the alloy’s microstructure and mechanical properties. An ultrafine-grained structure with an average size of structural elements less than 100 nm was obtained. At the same time, high strength and ductility (σuts = 1590 MPa, δ = 10%) were achieved, which led to a record increase in the endurance limit (σ−1 = 710 MPa) under tension-compression terms.