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Depth profile analysis of a hydrogenated Ti–6Al–4V alloy by glow discharge optical emission spectroscopy (GDOES) is described. Besides the earlier reported 'hydrogen effects', causing changes in emission intensities of other elements if hydrogen is present, the analysis of hydrogen itself was found to be affected by the redistribution of hydrogen in the region adjacent to the analyzed spot, due to sample heating and the thereby increased hydrogen diffusivity. A simple model of heat transfer within the sample during the GDOES analysis is proposed and the surface temperature of the analyzed spot is estimated to be ≈365 °C, in the given experimental setup. [ABSTRACT FROM AUTHOR]

This paper is devoted to an experimental and 3D atomistic study of the influence of loading rate on fracture toughness in dilute Fe–Si alloys and in bcc iron. We analyze new and previous experimental results from fracture tests performed at room temperature on bcc iron–silicon single crystals with edge cracks (1 ¯ 10) [110] (crack plane/crack front). The specimens of single edge notch-type were loaded in tension mode I under different loading rates. The ductile–brittle behavior at the crack front was monitored online via optical microscopy together with external force and prolongation of the specimens. About 30% decrease in fracture toughness was monitored in the new experiment under the highest loading rate. The nanoscopic processes produced by the crack itself were studied at room temperature via 3D molecular dynamics (MD) simulations in bcc iron under equivalent boundary conditions as in experiments to reveal (explain) the sensitivity of the crack to loading rate. For this purpose, this MD study utilizes the self-similar character of linear fracture mechanics. The results show that the emission of blunting dislocations from the crack is the most difficult under the highest loading rate, which leads to the reduced fracture toughness of the atomistic sample. This is in a qualitative agreement with the experimental (macro) results. Moreover, MD indicates that there may be some synergetic (resonant) effect between the loading rate and thermal activation that promotes dislocation emission. [ABSTRACT FROM AUTHOR]

In this study, the Zn-0.8Mg-0.28CaO wt.% composite was successfully prepared using different conditions of ball milling (rotations and time) followed by a direct extrusion process. These materials were characterized from the point of view of microstructure and compressive properties, and the correlation between those characteristics was found. Microstructures of individual materials possessed differences in grain size, where the grain size decreased with the intensified conditions (milling speed and time). However, the mutual relation between grain size and compressive strength was not linear. This was caused by the effect of other factors, such as texture, intermetallic phases, and pores. Material texture affects the mechanical properties by a different activity ratio between basal and pyramidal slips. The properties of intermetallic particles and pores were determined in material volume using micro-computed tomography (µCT), enhancing the precision of our assumptions compared with commonly applied methods. Based on that, and the analysis after the compressive tests, we were able to determine the influence of aspect ratio, feret diameters, and volume content of intermetallic phases and pores on mechanical behavior. The influence of the aspects on mechanical behavior is described and discussed. [ABSTRACT FROM AUTHOR]

Recently, the complex shearing of extruded tube (CSET) technique was proposed representing a new way of processing tubes from a bulk billet as a combination of extrusion with two passes of equal channel angular processing and possible mandrel rotation. In the present paper, the influence of mandrel rotation on the final microstructure and mechanical properties of the tube fabricated of a 3003 aluminium alloy was investigated. Electron back scatter diffraction (EBSD) revealed differences in grain size and misorientation angles between tubes processed with stationary and rotating mandrel. Kernel average misorientation maps obtained from EBSD experiments and ASTAR analysis performed in transmission electron microscopy proved differences in the dislocation density and arrangement. The tube processed using a stationary mandrel showed a recovered microstructure with elongated grains separated by low-angle grain boundaries into subgrains. The microstructure of the tube processed with a rotating mandrel was dynamically recrystallized with the grain size in submicrometer range. Vickers microhardness measurements revealed only a 40% HV increase in the sample prepared using stationary mandrel as compared with the initial billet. The mandrel rotation resulted in a much higher HV increase up to 200% as a result of substantial grain refinement. [ABSTRACT FROM AUTHOR]

Zinc-based materials are intensively studied in relation to the possible application like bioabsorbable medical devices including stents or various fixation devices like screws, and plates. Zinc is favourable due to its excellent biocompatibility and rather low corrosion rate with the absence of concomitant hydrogen release making him an interesting alternative to Mg-based bioabsorbable implants. To comply with the high requirements on mechanical and degradation properties, zinc has to be appropriately alloyed and thermomechanically processed enabling significant improvement in strength and also elongation. One of the remnant shortcomings is related to the pour mechanical strength at increased temperate (even body temperature at 37 °C) and low creep resistance, both these factors are related to the low recrystallization temperature of pure zinc. In the last years, powder metallurgy techniques have been suggested to overcome the issues of low strength and poor creep behaviour, further with the tendency to support a more homogeneous corrosion process preceding the onset of localized corrosion. In this work we try to insight into the behaviour of several materials consisting of key suggested alloying elements for zinc (Mg, Ag, Sr) and processed by various techniques including conventional casting and extrusion but also powder metallurgy methods including mechanical alloying (MA) and spark plasma sintering (SPS). Our results indicated a strong positive effect of thermomechanical processing (hot extrusion) on materials microstructure with a reduced grain size of up to 2 μm and increased mechanical properties (strength, elongation). However, these results were even overcome by the application of powder metallurgy methods resulting in grain and intermetallic particle size below 1 μm and slightly improved strength over conventionally processed materials attacking 400 MPa. Furthermore, a higher tendency for uniform corrosion has been observed. In sum, powder metallurgy products are suggested as highly competitive to conventionally processed alloys. The study has been funded by the Czech Science Foundation, project 21-11439K. [ABSTRACT FROM AUTHOR]

secondary twinning inside a primary twin has been observed on the (0001) fracture surface of zinc after quenching of a single crystal grown by the Bridgman method. This type of double twinning was previously observed in magnesium with a quite different c/a axial ratio. A geometrical analysis is presented that can explain why the observed secondary twins are activated. [ABSTRACT FROM AUTHOR]

An interest in biodegradable metallic materials has been increasing in the last two decades. Besides magnesium based materials, iron-manganese alloys have been considered as possible candidates for fabrication of biodegradable stents and orthopedic implants. In this study, we prepared a hot forged FeMn30 (wt.%) alloy and investigated its microstructural, mechanical and corrosion characteristics as well as cytotoxicity towards mouse L 929 fibroblasts. The obtained results were compared with those of iron. The FeMn30 alloy was composed of antiferromagnetic γ-austenite and ε-martensite phases and possessed better mechanical properties than iron and even that of 316L steel. The potentiodynamic measurements in simulated body fluids showed that alloying with manganese lowered the free corrosion potential and enhanced the corrosion rate, compared to iron. On the other hand, the corrosion rate of FeMn30 obtained by a semi-static immersion test was significantly lower than that of iron, most likely due to a higher degree of alkalization in sample surrounding. The presence of manganese in the alloy slightly enhanced toxicity towards the L 929 cells; however, the toxicity did not exceed the allowed limit and FeMn30 alloy fulfilled the requirements of the ISO 10993-5 standard. [ABSTRACT FROM AUTHOR]

Research into biodegradable porous materials has been increasingly focused on iron-based materials because such materials possess suitable properties for orthopedic applications. In this study, we prepared porous iron with porosities of 32-82 vol.% by powder metallurgy using ammonium bicarbonate as a space-holder material. We studied the influence of initial powder size and compacting pressure on sample microstructure, contamination and mechanical characteristics. The experimental results were analyzed as well, using Gibson-Ashby model and this analysis showed a good agreement in theoretical and experimental data. Whereas increasing compression pressure decreased porosity, the use of finer iron powder led to an increase in porosity. Increasing the amount of space-holder material in the initial mixture increased the total porosity, improved compressibility and consequently decreased the number of pores originating from imperfect compaction. A higher compacting pressure and the use of finer powder enhanced both the flexural and compressive properties. Even the most porous samples prepared from the fine iron powder possessed mechanical properties comparable to human cancellous bone. Based on these results, we can claim that the use of fine initial iron powder is necessary to obtain highly porous iron, which appears to be suitable for orthopedic applications. [ABSTRACT FROM AUTHOR]

The demand for porous biodegradable load-bearing implants has been increasing recently. Based on investigations of biodegradable stents, porous iron may be a suitable material for such applications. In this study, we prepared porous iron samples with porosities of 34–51 vol.% by powder metallurgy using ammonium bicarbonate as a space-holder material. We studied sample microstructure (SEM-EDX and XRD), flexural and compressive behaviors (universal loading machine) and hardness HV5 (hardness tester) of the prepared samples. Sample porosity increased with the amount of spacer in the initial mixtures. Only the pore surfaces had insignificant oxidation and no other contamination was observed. Increasing porosity decreased the mechanical properties of the samples; although, the properties were still comparable with human bone and higher than those of porous non-metallic biomaterials and porous magnesium prepared in a similar way. Based on these results, powder metallurgy appears to be a suitable method for the preparation of porous iron for orthopedic applications. [ABSTRACT FROM AUTHOR]

Abstract: There has recently been an increased demand for porous magnesium materials in many applications, especially in the medical field. Powder metallurgy appears to be a promising approach for the preparation of such materials. Many works have dealt with the preparation of porous magnesium; however, the effect of sintering conditions on material properties has rarely been investigated. In this work, we investigated porous magnesium samples that were prepared by powder metallurgy using ammonium bicarbonate spacer particles. The effects of the purity of the argon atmosphere and sintering time on the microstructure (SEM, EDX and XRD) and mechanical behaviour (universal loading machine and Vickers hardness tester) of porous magnesium were studied. The porosities of the prepared samples ranged from 24 to 29 vol.% depending on the sintering conditions. The purity of atmosphere played a significant role when the sintering time exceeded 6h. Under a gettered argon atmosphere, a prolonged sintering time enhanced diffusion connections between magnesium particles and improved the mechanical properties of the samples, whereas under a technical argon atmosphere, oxidation at the particle surfaces caused deterioration in the mechanical properties of the samples. These results suggest that a refined atmosphere is required to improve the mechanical properties of porous magnesium. [Copyright &y& Elsevier]

The equiatomic alloy of nickel and titanium, known as nitinol, possesses unique properties such as superelasticity, pseudoplasticity, shape memory, while maintaining good corrosion resistance and sufficient biocompatibility. Therefore it is used for production of various devices including surgery implants. Heat treatment of nickel-rich NiTi alloys can result in precipitation of nickel-rich phases, which strongly influence tensile and fatigue behaviour of the material. In this work we studied influence of short-period heat treatment on tensile behaviour and fatigue life of the NiTi (50.9 at. % Ni) wire intended for fabrication of surgery stents. [ABSTRACT FROM AUTHOR]

The increasing incidence of trauma in medicine brings with it new demands on the materials used for the surgical treatment of bone fractures. Titanium, its alloys, and steel are used worldwide in the treatment of skeletal injuries. These metallic materials, although inert, are often removed after the injured bone has healed. The second-stage procedure—the removal of the plates and screws—can overwhelm patients and overload healthcare systems. The development of suitable absorbable metallic materials would help us to overcome these issues. In this experimental study, we analyzed an extruded Zn-0.8Mg-0.2Sr (wt.%) alloy on a rabbit model. From this alloy we developed screws which were implanted into the rabbit tibia. After 120, 240, and 360 days, we tested the toxicity at the site of implantation and also within the vital organs: the liver, kidneys, and brain. The results were compared with a control group, implanted with a Ti-based screw and sacrificed after 360 days. The samples were analyzed using X-ray, micro-CT, and a scanning electron microscope. Chemical analysis revealed only small concentrations of zinc, strontium, and magnesium in the liver, kidneys, and brain. Histologically, the alloy was verified to possess very good biocompatibility after 360 days, without any signs of toxicity at the site of implantation. We did not observe raised levels of Sr, Zn, or Mg in any of the vital organs when compared with the Ti group at 360 days. The material was found to slowly degrade in vivo, forming solid corrosion products on its surface. [ABSTRACT FROM AUTHOR]

There is currently an increasing demand for metals with a hexagonal close-packed structure (HCP). Particularly, titanium and its alloys are widely used in aerospace, aircraft and the medical industry [[1]]; zirconium is used in the nuclear industry [[1]] and Mg-based alloys in the automotive and aircraft industry [[1]]. Fojt et al. [[12]] dealt with the corrosion behavior of a SLM-processed Ti alloy. From the aforementioned, it is clear that the mechanical behavior of metals and alloys with a HCP structure is very sensitive to the microstructure and texture of the material. [Extracted from the article]

Abstract: Porous magnesium-based materials are biodegradable and promising for use in orthopaedic applications, but their applications are hampered by their difficult fabrication. This work reports the preparation of porous magnesium materials by a powder metallurgy technique using ammonium bicarbonate as spacer particles. The porosity of the materials depended on the amount of ammonium bicarbonate and was found to have strong negative effects on flexural strength and corrosion behaviour. However, the flexural strength of materials with porosities of up to 28vol.% was higher than the flexural strength of non-metallic biomaterials and comparable with that of natural bone. [Copyright &y& Elsevier]

A new severe plastic deformation technique, known as the complex shearing of extruded tube (CSET), was applied to a 3003 based model aluminium alloy. This technique, consisting of a combination of extrusion and two consecutive Equal Chanel Angular Pressing (ECAP) passes accompanied with concurrent torsional straining, is capable to produce a fine-grained tubular sample directly from a bulk metallic cylinder in one forming operation. In the present paper, the microstructural development of the alloy during partial processes of CSET was studied in detail using light microscopy, electron backscatter diffraction, and transmission electron microscopy. It was found that CSET technique refines the grain size down to 0.4 µm and, consequently, increases the microhardness from the initial value of 40 HV to the final value of 120 HV. The contributions of partial processes of CSET to the total strain were estimated. [ABSTRACT FROM AUTHOR]

In this pilot study, we investigated the biocompatibility and degradation rate of an extruded Zn–0.8Mg–0.2Sr (wt.%) alloy on a rabbit model. An alloy screw was implanted into one of the tibiae of New Zealand White rabbits. After 120 days, the animals were euthanized. Evaluation included clinical assessment, microCT, histological examination of implants, analyses of the adjacent bone, and assessment of zinc, magnesium, and strontium in vital organs (liver, kidneys, brain). The bone sections with the implanted screw were examined via scanning electron microscopy and energy dispersive spectroscopy (SEM-EDS). This method showed that the implant was covered by a thin layer of phosphate-based solid corrosion products with a thickness ranging between 4 and 5 µm. Only negligible changes of the implant volume and area were observed. The degradation was not connected with gas evolution. The screws were fibrointegrated, partially osseointegrated histologically. We observed no inflammatory reaction or bone resorption. Periosteal apposition and formation of new bone with a regular structure were frequently observed near the implant surface. The histological evaluation of the liver, kidneys, and brain showed no toxic changes. The levels of Zn, Mg, and Sr after 120 days in the liver, kidneys, and brain did not exceed the reference values for these elements. The alloy was safe, biocompatible, and well-tolerated. [ABSTRACT FROM AUTHOR]

In this study, we prepared zinc wires with a diameter of 250 µm by direct extrusion using an extrusion ratio of 576. We studied the influence of the extrusion temperature and microstructure of the initial Zn billets on the microstructural and mechanical characteristics of the extruded wires. The extrusion temperature played a significant role in the final grain size. The wires extruded at 300 °C possessed a coarse-grained microstructure and the shape of their tensile stress–strain curves suggested that twinning played an important role during their deformation. A significant influence of the initial grain size on the final microstructure was observed after the extrusion at 100 °C. The wires prepared from the billet with a very coarse-grained microstructure possessed a bimodal grain size. A significant coarsening of their microstructure was observed after the tensile test. The wires prepared from the medium-grained billets at 100 °C were relatively coarse-grained, but their grain size was stable during the straining, resulting in the highest ultimate tensile strength. This preliminary study shows that strong attention should be paid to the extrusion parameters and the microstructure of the initial billets, because they significantly influence the microstructure and mechanical behavior of the obtained wires. [ABSTRACT FROM AUTHOR]

Zinc and its alloys seem to be promising candidates for biodegradable applications. Those materials are often modified by other elements or compounds in order to enhance their properties. The combination of zinc and apatites is challenging for several reasons. However, the advantages connected with the biological aspects suggest the need for further research into such materials. In this study, three zinc-based composites with 4 and 8 wt. % of nanohydroxyapatite or nanomonetite (Zn-4MO, Zn-4HA, Zn-8HA) were prepared by sintering and subsequent extrusion. Materials prepared in this way were characterized from the microstructural, mechanical and corrosion point of view. The obtained results showed a significant influence of particle character (amount and morphology) on the strength and ductility of the prepared materials. In case of Zn-4MO, the presence of monetite significantly increased the ductility compared with the other materials. In addition, the increment of the degradation rate caused by the presence of monetite was observed as well. All obtained results pointed out to significant advantages of monetite for the preparation of Zn-apatite composites compared with hydroxyapatite. [ABSTRACT FROM AUTHOR]

Zinc and its alloys belong to a group of biodegradable materials, which can be potentially used for the preparation of temporary orthopedic implants. The research of biodegradable zinc materials revealed a lot of limitations; however, the new processing approaches of those materials can enhance their properties, which are insufficient for now. In this study, the zinc composite with 8 wt.% of hydroxyapatite (Zn/HA8) prepared for the first time by extrusion process was characterized from the point of view of the structural, mechanical and corrosion properties. The extrusion process led to good integrity of the interfaces between the zinc and hydroxyapatite particles. Mechanical behavior confirmed the role of hydroxyapatite as a defect in the material structure, which led to a decrease of the Zn/HA8 mechanical properties by approximately 30% (compressive yield strength (CYS) = 154 MPa Zn, 113 MPa Zn/HA8). Despite that, the Zn/HA8 composite showed sufficient mechanical properties for cancellous bone replacement and reached the lower limit for cortical bone. Additionally, the presence of hydroxyapatite caused the preferential precipitation of hydroxyapatite (HA) from the solution and can lead to a significant enhancement of the tissue/implant interface interactions. [ABSTRACT FROM AUTHOR]

Zinc-based alloys containing the elements of the second group of the periodic table have been extensively studied as potential candidates for applications as a biodegradable material. In this study, the ZnMg0.8Ca0.2 (wt%) alloy was prepared and treated by annealing and extrusion at various conditions. The evolution of microstructure and mechanical properties during annealing and after extrusion was performed in detail. Both annealing and extrusion caused microstructural changes influencing mechanical properties. Annealing caused a homogenization of the microstructure and transformation of metastable phases. The extrusion caused a rearrangement of the intermetallic phases, a refinement and a texturing of the zinc matrix. Those lead to a significant strengthening and to an increase in the ductility, but also to mechanical anisotropy. In this paper, the influence of the processing on the microstructure and mechanical properties is discussed in detail based on the results obtained by various methods, such as scanning and transmission electron microscopy, electron backscattered diffraction, tensile and compressive mechanical testing and nanoindentation. • Solidification mechanism of a ZnMg0.8Ca0.2 (wt%) alloy was proposed. • Formation of Zn-MgZn 2 eutectics was observed. • Influence of annealing and extrusion was studied. • Anisotropy of the extruded alloy was explained. [ABSTRACT FROM AUTHOR]

Zinc and zinc alloys have been studied due to their corrosion properties as potentially biodegradable materials. In this study, a zinc/hydroxyapatite composite (Zn/HA) containing 16 wt % HA was prepared by spark plasma sintering and characterized in detail. The microstructure, mechanical and corrosion properties were studied and the mutual relations between properties and microstructure were found. The porosity was evaluated to be approximately 18%. The mechanical properties (ultimate compression strength = 65 MPa and ultimate flexural strength = 120 MPa) are sufficient for the potential scaffolding and augmentation of cancellous bone. The flexural properties of these materials were measured for the first time. Immersion tests and subsequent analyses confirmed no direct participation of hydroxyapatite in the corrosion process and an ideal corrosion rate of approximately 0.4 mm/year. The amount of released zinc was between 4–6 mg/day corresponding with the maximal usable surface area of 25 cm2. All the results suggest that the Zn/HA composite is suitable as a potential biodegradable material (from the point of view of mechanical and corrosion properties) for the replacement of cancellous bones. [ABSTRACT FROM AUTHOR]

The authors cited Project No. 16-06110S in the acknowledgements of the article. Please note the correct project is Project No. 18-06110S of The Czech Science Foundation. [ABSTRACT FROM AUTHOR]

Zinc-based alloys represent one of the most highly developed areas regarding biodegradable materials. Despite this, some general deficiencies such as cytotoxicity and poor mechanical properties (especially elongation), are not properly solved. In this work, a Zn-5Mg (5 wt.% Mg) composite material with tailored mechanical and superior corrosion properties is prepared by powder metallurgy techniques. Pure Zn and Mg are mixed and subsequently compacted by extrusion at 200 °C and an extrusion ratio of 10. The final product possesses appropriate mechanical properties (tensile yield strength = 148 MPa, ultimate tensile strength = 183 MPa, and elongation = 16%) and decreased by four times the release of Zn in the initial stage of degradation compared to pure Zn, which can highly decrease cytotoxicity effects and therefore positively affect the initial stage of the healing process. [ABSTRACT FROM AUTHOR]

This work aims to optimize the parameters of the SHS process for the preparation of NiTi shape memory alloy to obtain a high-purity, low-porosity material. For this purpose, high heating rate (over 300 °C min−1), temperature of 1100 °C and process duration of 20 min were determined as the optimal parameters. To prevent nickel depletion of the product and to minimize the porosity, the use of coarse titanium particles (200–600 μm) with fresh surface can be recommended. SHS products were composed of NiTi with the admixture of Ti2Ni phase. The formation of this phase cannot be fully avoided in SHS preparation route. [ABSTRACT FROM AUTHOR]