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Coronary heart disease is still one of the most common sources for death in western industrial countries. Since 1986, a metal vessel scaffold (stent) has been inserted to prevent the vessel wall from collapsing. Most of these coronary stents are made from CrNiMosteel (316L). Due to its austenitic structure, the material shows a good combination of strength, ductility, corrosion resistance, and biocompatibility. However, this material has some disadvantages like its non-MRI compatibility and its poor fluoroscopic visibility. Other typically used materials are the CoBase alloys L-605 and F-562 which are MRI compatible as well as radiopaque. Another interesting fact is their excellent radial strength and therefore the ability to produce extra thin struts with increased strength. However, because of a strut diameter much less than 100 μm, the cross section consists of about 5 to 10 crystal grains (oligocrystalline). Thus, very few or even just one grain can be responsible for the success or failure of the whole stent. To investigate the relation between microstructure, mechanical factors and stent design, commercially available Cobalt-Chromium stents were investigated with focus on distinct inhomogeneous plastic deformation due to crimping and dilation. A characteristic, material related deformation behavior with predominantly primary slip was identified to be responsible for the special properties of CoCr stents.
The complex structural-phase composition, morphology and elemental composition of surface and nonmetallics in porous TiNi compounds produced by self-propagating high-temperature synthesis (SHS) in a flow reactor in the layer-by-layer combustion mode were analyzed. The samples were investigated using light microscopy (LM), X-ray diffraction (XRD), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and energy dispersive X-ray spectroscopy (EDS). The findings indicate that in addition to the TiNi and Ti2Ni intermetallic constituents, the pore's surface contains numerous Ti4Ni2(O,N,C) nanocrystalline oxycarbonitrides, spinels, polysilicates, and residual amorphous phases. The elemental composition of the surface and crystalline inclusions is investigated by the EDS method. LM, SEM, TEM, and EDS instrumental examination revealed the entire surface comprising a continuous shell of intermetallic superficial bulb-shaped structures, as well as crystalline inclusions of polysilicates and spinels in the intergranular peritectic phase. Prominent morphology was confirmed to appear throughout the pore's surface owing to the interaction of the peritectic liquid (PL) with reaction gases. The epitaxial, nanocrystalline strata of intermetallic oxycarbonitrides were shown to have the intricate nature. Reaction gases chemisorbed by the PL are responsible for the continuous and dense substrate, which ultrafine structure modulates a high corrosion resistance. On the contrary, the sparse and foamy overlay resulted from a convective transfer of the PL by reaction gases facilitates in vivo bio-integration of the alloy. Overall, this sheds light on and may be more indicative of the complex role of superficial strata and nonmetallic crystals in enhanced biocompatibility of the unwrought porous TiNi alloy.
The recovery of surfactants from organic mediums is of great economic and environmental interests in the field of petrochemicals sector. The aim of this study was to recover poly-dispersed nonionic surfactant (TX-100) from organic medium by the use of dehydrated and rehydrated kaolin. It was found that the presence of water after kaolin rehydration decreases considerably the amount of TX-100 adsorption from 28.7 μmol.g−1 onto dehydrated kaolin to 23.4 μmol.g−1 onto rehydrated kaolin. The estimation of the number of statistical layers of water deposited on kaolin was observed to be about 7 to 9. The effect of type of solvents (heptane, cyclohexane and benzene) on the adsorption onto rehydrated kaolin revealed a reduction in the adsorbed quantity; the adsorbed amounts were found to be 28.7 μmol.g−1, 26.7 μmol.g−1 and 24.2 μmol.g−1 in heptane, cycloheptane and benzene phases, respectively. On the other hand, it was observed that a temperature increased from 20 °C to 35 °C and 45 °C negatively affects the adsorption of TX-100 onto dehydrated and/or hydrated kaolin in heptane medium.
The biotribocorrosion behavior of newly developed nanocristalline near β-types Ti-15Nb and Ti-15Mo alloys surfaces, sintered by powder metallurgy and sequentially milled, has been investigated in SBF simulated body fluid (PBS solution) at OCP, an applied potential in the passive region and EIS. Reciprocating sliding tests using a ball-on-plate tribometer under differentes applied loads 3, 7 and 10 N load and anodic potentials were applied to evaluate the effect of applied lad and the effect of Nb and Mo elements on tribocorrosion behaviors of samples. Results showed that, Ti-Nb exhibited better anticorrosive properties than Ti-Mo. Under tribological action the nanostructured both of alloys showed similar friction coefficient, while Ti-Nb present lower tendency to corrosion compared to Ti-Mo. Furthermore, Nb diffusion increased the repassivation rate with respect to Ti-Mo surfaces due to its stable passive film. Due to the high chemical reaction rate in β-type Ti-15Mo alloy as compared to Ti-15Nb. The β- Ti-15Nb showed lower volume loss, lower friction coefficient values and exhibited better corrosion resistance during tribocorrosion tests than Ti-15Mo. Prevailing electrochemical conditions between -1 and 2 V influences the wear accelerated corrosion by increasing it with the applied potential and slightly increases the mechanical wear. Also, wear accelerated corrosion can be predicted by existing models as a function of electrochemical and mechanical parameters of the titanium alloys. However, considering biomedical applications, the β- Ti15 Mo and Ti15Nb alloys may be good candidates with low elastic modulus and without toxic alloying elements.
Porous TiNi alloys fabricated by self-propagating high-temperature synthesis (SHS) are biomaterials designed for medical application in substituting tissue lesions and they were clinically deployed more than 30 years ago. The SHS process, as a very fast and economically justified route of powder metallurgy, has distinctive features which impart special attributes to the resultant implant, facilitating its integration in terms of bio-mechanical/chemical compatibility. On the phenomenological level, the fact of high biocompatibility of porous SHS TiNi (PTN) material in vivo has been recognized and is not in dispute presently, but the rationale is somewhat disputable. The features of the SHS TiNi process led to a multifarious intermetallic Ti4Ni2(O,N,C)-based constituents in the amorphous-nanocrystalline superficial layer which entirely conceals the matrix and enhances the corrosion resistance of the unwrought alloy. In the current article, we briefly explore issues of the high biocompatibility level on which additional studies could be carried out, as well as recent progress and key fields of clinical application, yet allowing innovative solutions.
Aiming to develop alloys with better properties for orthopedic applications, the focus of the present research was to evaluate the effect of Mo at.% content on structural, mechanical, and tribological properties of hot isostatically pressed Ti-xMo (x = 4, 8, 12, 15, and 20 at.%) alloys. The structural evolution, mechanical properties, and tribological behavior of the nanostructured Ti-xMo alloys were evaluated using x-ray diffraction, scanning electron microscope, and ball-on-disk tribometer. Wear tests were conducted under different applied loads of 2, 8, and 16 N. Experimental results indicated that the structural evolution and morphological changes of the milled alloys were sensitive to their molybdenum (Mo) content. The morphological characterization showed that the crystallite size and the particle size decreased with increasing Mo content (at.%) reaching the lowest values of 27 and 26 nm in the case of Ti-15Mo and Ti-20Mo, respectively. On the other hand, the coefficient of friction and wear rates were found to be decreasing with increasing Mo content.
The bio-tribocorrosion behavior of newly developed near β-types Ti-15Nb and Ti-15Mo alloys was investigated in Phosphate-Buffered Saline (PBS) under different loads. Open-Circuit Potential (OCP), friction coefficient, wear volume and wear rate were evaluated. The results revealed that Ti-15Nb alloy exhibited lower wear rate, lower friction coefficient and better corrosion resistance during tribocorrosion than the Ti-15Mo alloy. This can be attributed to the diffusion of Nb which increases the repassivation rate (formation of a protective layer) in the Ti-15Nb alloy. In contrast Ti-15Mo shows a significantly higher rate of chemical reaction.
Low modulus β-type Ti-15Nb alloys were prepared by subjecting them to different sintering temperatures (800, 900, 1000 and 1100 °C) and their morphological and structural properties were evaluated. X-ray diffraction analysis was used for the morphological characterization which indicated that the mean pore and crystallite size continuously decreased with increasing sintering temperature to reach the lowest values of 41 nm and 27.5 nm at 1100 °C, respectively. Moreover, the higher sintering temperature resulted in higher relative density, greater hardness and young’s modulus of the Ti-15Nb alloys. Wear tests were conducted using a ball-on-plate type Oscillating tribometer, under different applied loads (2, 8 and 16 N) to evaluate their tribological characterization. The wear rate and friction coefficient were lower at higher sintering temperature. This enhancement in tribological properties was attributed to a grain refinement. The Ti-15Nb alloys sintered at 1100 °C showed the best tribological performance.
Ti–Ni powder compacts were prepared by mechanical alloying (MA), followed by hot isostatic pressing (HIP). Afterwards, the samples were sintered at different temperatures (950, 1050, 1150 and 1250 °C). Microhardness, density, crystallite size as well as microstrain of the sintered samples were measured and analyzed. Wear characteristics in phosphate-buffered saline (PBS) solution was tested under different applied loads of 2 N, 10 N, and 20 N, respectively. The results indicated that the crystallite size continuously decreases with increasing sintering temperature and reaches the lowest value of 31.3 nm at 1250 °C. The relative density of the sample sintered at 1250 °C is 98.0%. Moreover, the higher sintering temperatures lead to the higher relative density and the increase in hardness and young’s modulus of the sample. At the same time the friction coefficient and wear rate were lower for the samples sintered at 1250 °C. This improvement in friction and wear resistance is attributed to the grain size refinement. Ti–Ni sintered at 1250 °C showed good tribological performance under all test conditions.
The microstructural and functional behavior of TiNi-based wires with a silver content of 0–1.5 at.% was evaluated. The concentration range for Ag doping determined for the TiNi wires with potential for the medical industry was 0–0.2 at.%. Microstructure analysis of TiNi wires with different silver contents at room temperature indicated a multiphase structural state. Various internal structures with tangled grain boundaries were formed by intense plastic deformation. The nanocrystalline structure and phase state of wire with the minimum silver content (0.1 at.% Ag) provide full shape recovery, the greatest reversible strain, and optimal strength and ductility. TiNi ingots with a high Ag content (0.5–1.5 at.%) cracked under minimum load due to excess silver that crystallized along the grain boundaries and broke cohesion bonds between the TiNi grains.
The central commitment of the 2015 World Climate Conference is to limit geothermal heating by massively reducing greenhouse gas emissions by decreasing the use of fossil fuels and promoting environmentally friendly energy. However, since renewable energies have so far not been available as required and are difficult to store, there is a short-term solution in the conversion, storage and reuse of climate-damaging combustion gases. An efficient solution for using CO2 is to convert it into a gas that can be stored and used to generate energy. With the so-called “power-to-gas technology”, a significant reduction in greenhouse gas emissions can be achieved by methanation of CO2 if methane slip is avoided. Methanation is a chemical reaction in which carbon dioxide reacts with hydrogen to methane. This transformation, which normally takes place at 350 ° C to 600 ° C, is also known as the Sabatier reaction. In addition to methane and water, the remaining reactants such as carbon dioxide, hydrogen, oxygen and nitrogen as well as small amounts of impurities from the combustion process, occur as reaction products. Reaction containers and lines are usually made of stainless steel. Due to high ambient temperature and aggressive ambient media, corrosion can also occur with the generally temperature and corrosion-resistant 316L material, influence material properties and lead to material failure. To assess the influence of the CO2 methanation process on 316L, a laboratory-scale methanation reactor was fractioned and examined after use. Corrosion deposits were found in various components of the reactor (gas supply line, gas outlet, reactor segment). Depending on their position within the component, these corrosion layers are structured very differently. Microstructure and element composition of the layers were analyzed using scanning electron microscopy combined with energy-dispersive X-ray spectroscopy. While the gas supply shows only moderate corrosion attack, crevice, contact- and pitting corrosion were detected in the corroded area of the gas outlet. Three zones (multilayer structure, particle accumulation and brittle passive film) were identified within the corrosion layers. The multi-layer zone is composed of columnar and granular structures, the particle accumulations consist of cylindrical and spherical particles. The element composition within the corrosion layers suggests contact corrosion caused by the material of the sealing rings.
Impulse Friction Stir Welding (IFSW) was utilized to join 6082–T6 alloy plates at various impulse frequencies. A distinctive feature of IFSW is the generation of mechanical impulses that enhances the forging action of the tool, and thereby, alters the weld microstructure. The microstructural evolution in the Stir Zone (SZ) with special focus on the strengthening precipitation behavior, and overall mechanical properties of the IFSW joints have been investigated. It was demonstrated that the strengthening β″ precipitates reprecipitated in the SZ of the IFSW joints during natural aging. In contrast, no precipitates were found in the SZ of the Friction Stir Welding (FSW) weld. Partial reversion of β″ after IFSW is supposed to occur due to more developed subgrain network and higher dislocation density introduced by impulses that accelerated precipitation kinetics. Dynamic recrystallisation was facilitated by impulses resulting in a fine, homogeneous structure. There was no significant difference between the microhardness in the SZ, tensile and yield strength of the FSW and IFSW joints. However, the application of impulses demonstrated the smoothing of the hardness reduction in the transition region at the advancing side. The shift of the fracture location from the Heat-Affected Zone (HAZ) by FSW to the SZ as well as higher elongation of the joints by IFSW of lower frequencies could be related to the grain refinement and the change of the grain orientation.
The effect of milling time on the microstructure and mechanical properties of Ti-6Al-4Fe alloys
(2021)
Replacement of toxic and expensive vanadium (V) in medical grade titanium alloys with cheaper and non-toxic elements such as iron (Fe) or niobium (Nb), is an important step forward in developing safer and less expensive biomaterials. Evaluating the effect of different process parameters such as the milling time on the properties of these newly developed alloys helps in understanding and controlling their behavior. Hence, in this study, the influence of ball-milling duration (2, 6, 8, 12 and 18 h) on crystalline structure, phase evolution, densification, and mechanical characteristics of biomedical nanocrystalline Ti-6Al-4Fe (wt. %) alloys is investigated. X-ray diffraction (XRD) confirmed that after 6 h of milling, aluminum (Al) and Fe completely dissolved into Ti matrix to form a solid solution of Ti (Al, Fe). XRD further revealed that the crystallite size decreased from 56 to 30 nm and the micro-strain increased with an increase in milling time. A decrease in porosity along with an increase in density is also observed for the alloys with increasing milling time. Moreover, the values of porosity obtained for the developed Ti-6Al-4Fe alloys ranged from 1 to 12 %, which is comparable to the porosity of one of the cortical bones making it a potential candidate for bone replacements. Microhardness measurements showed that the hardness of the Ti-6Al-4Fe alloys was greater than the hardness of the conventional Ti-6Al-4V alloys. It was observed that the Ti-6Al-4Fe alloy fabricated with the powders milled for 2 h showed the lowest value of Young’s Modulus. Milling time also had a significant effect on the surface roughness of the alloy samples, which showed a decreasing trend with increasing milling times.
This article describes hot Cr target magnetron sputtering enhanced by a radio-frequency inductively coupled plasma (RF-ICP) source in an Ar + N2 atmosphere. Optical emission spectroscopy revealed an opportunity to perform magnetron sputtering in an inert (Ar) atmosphere, while the CrNx coating can be deposited on a substrate in a chemically reactive atmosphere formed by the RF-ICP source. High stability and repeatability of deposition process were observed, and the deposition rate of the CrNx coatings increased from 106 to 127 nm/min as N2 flow rate rose. The power of the RF-ICP source and the N2 flow rate can be used to tailor and control deposition conditions. The XRD and WDS measurements showed the effect of deposition conditions on the crystal structure and elemental composition of CrNx coatings. It was found that the change of substrate bias, RF-ICP source power and N2 flow rate result in variation of coating stoichiometry from pure Cr to CrN.
Nowadays, the recycled fine aggregate sourced from construction and demolition waste is not frequently used in manufacturing of epoxy resin coatings. Therefore, the main novelty of the article is to prepare green epoxy resin coatings modified with recycled fine aggregate in a replacement ratio of natural fine aggregate ranged from 20 to 100%. The microstructural properties of the aggregates and epoxy resin were analyzed using micro-computed tomography, scanning electron microscopy and nanoindentation. The macroscopic mechanical properties were examined using pull-off strength tests. The highest improvement of the mechanical properties was observed for epoxy resin coatings modified with 20% of natural fine aggregate and 80% of recycled fine aggregate. It has been found that even 100% of natural fine aggregate can be successfully replaced using the recycled fine aggregate with consequent improvement of the pull-off strength of analyzed epoxy resin coatings. In order to confirm the assumptions resulting from the conducted research, an original analytical and numerical failure model proved the superior behavior of modified coating was developed.
Während in einem konventionellen Ultraschallprüfkopf ein Kunststoffdämpfungskörper mit Kleber oder Öl an einen Piezoschwinger angekoppelt ist, werden als Hochtemperaturlösung feinporöse sintermetallische Dämpfungsmaterialien mit einer Flüssigglasankopplung eingesetzt. Um dabei das Sintermetall vor dem korrosiven Angriff der Glasschmelze zu schützten, wird am Dämpfungskörper gegenwärtig Gold- oder Platinfolie zeit- und kostenaufwendig appliziert.
In der aktuellen Arbeit wurde eine Methode zum Korrosionsschutz der sintermetallischen Oberfläche aus rostfreiem Stahl mittels Laser-Pulverauftragschweißen entwickelt. Im Laufe einer Schweißparameterstudie auf dem Substratmaterial aus massivem rostfreiem Stahl wurde die Eignung unterschiedlicher Auftragsmaterialien auf Nickel- und Kobaltbasis untersucht. Dabei wurde zunächst der Einfluss verschiedener Schweißparameter wie Laserleistung, Vorschubgeschwindigkeit und Pulvermenge auf die Auftragsqualität (Nahtform, Vermischungsgrad, Porosität) metallografisch bewertet. Anschließend wurden die aufgetragenen Schichten hinsichtlich ihrer Korrosionsbeständigkeit getestet. Der Kontakt mit einer flüssigen Glasmischung bei 500 °C hat bei keiner der beschichteten Proben sichtbare Korrosionswirkung gezeigt. Als Resultat der Schweißparameterstudie haben sich besonders die nickelbasierten
Pulver als gut geeignete Materialien für den Prozess gezeigt. Die identifizierten Schweißparameter wurden im nächsten Schritt erfolgreich an das sintermetallische Substrat angepasst.
Magnetron sputtering is one of the most commonly used deposition techniques, which has received considerable attention in industrial applications. In particular, owing to its compatibility with conventional fabrication processes, it can produce and fabricate high-quality dense thin films of a wide range of materials. In the present study, nitrogen (N) was combined with pure vanadium in order to form binary nitride to improve its mechanical and tribological performance. To evaluate the influence of nitrogen on the structure of the as-deposited vanadium nitride (VN) coatings, the following techniques were used: XPS, XRD, SEM, AFM and optical profilometry. The residual stresses were determined by the curvature method using Stoney’s formula. The hardness and Young’s modulus were obtained by nanoindentation measurements. The friction behavior and wear characteristics of the films were evaluated by using a ball-on-disk tribometer. The obtained results showed that the N/V ratio increased with increasing the N2 flow rate while the deposition rate decreased. The preferred orientation was changed from (200) to (111) as the N2 flow rate increased with the presence of V–N and V–O binding energies as confirmed by XPS analysis. The nitrogen addition resulted in a columnar morphology and a fine structure with fine surface roughness. The VN thin film containing 49.5 at.% of nitrogen showed the best performance: highest mechanical properties (hardness = 25 GPa), lowest friction coefficient (μ = 0.37) and lowest wear rate (Ws = 2.72 × 10−5 mm3N−1 m−1). A good correlation between the film microstructure, crystallite size, residual stress and mechanical and tribological properties was observed.
Structured materials can be progressive alternatives to commonly used
flat sheets because of their higher bending stiffness and stability compared to flat sheet metals, made of the same alloy. The application of sheet metals requires accurate information regarding their strength and deformation behavior. Such data are not commonly available and have to be measured by specific test setups and implementation
of tests. The aim of this work is to obtain new knowledge about deformation mechanisms of structured sheet metals. Structured sheet metals (SSM) made of conventional deep-drawing steel DC04 were investigated by means of tensile tests. The influence of the structure type arrangement on the deformation behavior was analyzed. The evolution of local strains was analyzed by means of strain gauge
measurements as well as 3D-displacement measurements with an ARAMIS highresolution camera system. Local orientation changes in different structural elements were measured using the electron backscatter diffraction technique.
Ultrasonic probes for high-temperature applications are provided with metallic wedges, which can withstand the contact with the high temperature of the inspected structure. The ultrasonic signal travels within the wedge and gets reflected from its boundaries, causing interference signals called “ghost echoes”. The current work presents an investigation of the additional damping effect provided by porous sintered metal plates applied onto the surface of the wedge. In particular, the study evaluates the effect of damping plate thickness on the interference signal level at different transmission frequencies. Damping plates made of sintered metal SIKA-R 15 AX were attached to a wedge prototype made of steel 1.4301. The study revealed, that the most effective thickness of damping plates in the selected frequency interval of 1 to 4 MHz is equal to 4 mm. The evaluation of the interference signal has shown that the application of such damping plates to the wedge surface contributes to an additional attenuation of an interference signal of 10 to 30 dB after 500 µs of signal propagation.
The paper presents the characteristics of Ti-Mo-xTiC composites manufactured under experimentally selected conditions using the upgraded field-assisted sintering technique (U-FAST). Mixtures of microstructural titanium powders and nc-Ti0.9Mo0.1C/C carbide powders protected from oxidation by a carbon shell were subjected to sintering. The powders with nc-Ti0.9Mo0.1C/C contents of 10 and 20 wt% were used. The content of carbon forming the carbon shell was approximately 3 or 40 wt%. Composites with near full density were reinforced with titanium carbides in a Ti-Mo matrix. The composites with the highest content of reinforcing phase are characterized by the highest values of hardness, Young's modulus and wear resistance. Although the hardness of these composites is similar to that of ceramics, their nature is not brittle. Despite the high value of the Young's modulus, the addition of hard particles of the reinforcing phase to the titanium matrix significantly increases the values of the H/E ratio of the composites compared to the reference samples of cp-Ti and Ti6Al4V. A comparison of the research results for the composites with the highest share of titanium carbides showed that lowering the sintering temperature from 1300 to 1150 °C resulted in the inhibition of grain growth, a reduction in composite heterogeneity, composite roughness and hardness as well as a rise in the Young's modulus. An increase in the sintering temperature from 1150 to 1300 °C contributed to the higher high angle grain boundaries (HAGB) content.
The effect of heat treatment at various temperatures (650, 850, 1050, and 1100°C) and dwell times (10 min and 1 h) on the metallurgical and microstructural evolution as well as on the related tensile properties of stainless steel 316L processed by selective laser melting (SLM) has been systematically evaluated. The metallurgical and microstructural features such as defects, stability of the columnar–cellular structure and substructure, second phase particles, and phase transformation imparted by SLM and heat treatment have been discussed. It has been shown that the processing conditions specific to SLM significantly alter the kinetics of phase evolution compared to standard welding techniques which affects the accuracy of the prediction. The influence of these characteristics on tensile properties and hardness was elucidated. It was disclosed that with increasing heat treatment temperature there was a gradual increase in elongation but a decrease in strength related to the dislocation density and the development of the microstructure.
Microhardness variations across the friction stir welded (FSW) and impulse friction stir welded (IFSW) AA2024–T351 joints have been elucidated by the transformations of the S–Al2CuMg phase with a special focus on a distinguished hardness peak within the heat-affected zone (HAZ) of the impulse welds. The increase in hardness within the stir zone (SZ) originated from the partial re-precipitation of the initial Guinier-Preston-Bagaryatsky zones (GPB) and metastable S needles, previously dissolved.) Formation and growth of stable S precipitates via coalescence accounted for the softening through the thermo-mechanically affected zone (TMAZ). The peak strengthening within the HAZ of the IFSW joints was mainly caused by the dense needle-shaped S particles, which can be explained by a mutual influence of the process specific temperature and strain cycles. Dislocations and subgrain boundaries introduced to the material due to plastic deformation facilitated the nucleation of strengthening S precipitates in the HAZ. It demonstrates that the impact of deformation should be considered by the characterization of the precipitation development in the HAZ.
CrNx coatings were deposited at high rates (100–130 nm/min) using hot Cr target magnetron sputtering enhanced by a radio-frequency inductively coupled plasma (RF-ICP) source in an Ar + N2 atmosphere. Besides separation of inert and reactive atmosphere, the RF-ICP source can be an effective tool for ion assistance in case of coating growth and to tailor film parameters. The effects of nitrogen flow rate and substrate bias potential on microstructure and functional properties of the CrNx coatings were investigated. An increase in nitrogen flow rate favored the formation of a looser microstructure of the coatings, while substrate biasing had the opposite effect. The functional properties were strongly dependent on the phase composition of the CrNx coatings. The change in coating microstructure significantly affected hardness, elastic modulus, adhesion, friction coefficients and corrosion resistance. The results indicated that ion assistance can be a key feature for regulating functional properties in the considered type of coating deposition. Cr2N and CrN compound coatings with high hardness (∼20 GPa) and low corrosion current density (icorr ∼ 3–5·10−9 A/cm2) in a 3.5 wt% NaCl solution were obtained by high-rate deposition.
Chromium carbonitride coatings were deposited by cathodic arc physical vapor deposition technology at a temperature of 300 °C, as were used the reactive gasses CH4 and N2. The structural analysis of the CrN coating showed a polycrystalline structure with mixed CrN and Cr2N phases. All studied coatings, including the CrC exhibits fcc structure. The phases were confirmed by X-ray photoelectron spectroscopy measurements where a surface oxidation was also detected. The increase of the CH4 gas flow during the deposition process leads to a parabolic trend with the highest hardness of 33.5 GPa for the coating deposited at CH4 / N2 = 0.53. At the same time the lowest coefficient of friction for both counterparts Al2O3 and ZrO2 (0.28 and 0.26, respectively) were measured at CH4 / N2 = 1.86. The tribological tests reveal that the wear of the coatings increases with an increasing CH4 flow rate, whereas the coefficient of friction decreases. This observed contradiction is explained by a phenomenon described as the effect of Rebinder.
The objective of this work is to investigate the strain localization
and slip activation of the microstructure of oligo-crystalline 316LVM steel struts evolving during different cyclic bending deformation stages (number of cycles) and loading conditions (maximum stress and neutral). A micro-scale three-point bending fixture was designed and incorporated into a micro tensile/compression machine inside a scanning electron microscope (SEM) to perform in-situ electron backscatter diffraction (EBSD) measurements during different phases of cyclic fatigue testing. The following results were obtained:
1) The quantitative strain could be compared after each stage of
deformation.
2) The rotation of the grains orientations is observed during the cyclic deformation while the morphology did not change significantly. The results contribute to the understanding of the evolution of the microstructure at low strain variations under bending fatigue conditions, and can support the prediction of the fatigue life of 316LVM stainless steel oligocrystalline microdevices like coronary artery stents.
In this study, heat-treated and multisurface engineered DIN 1.2367 tool steel was subjected to room and elevated temperature wear tests, and the effect of nitriding on its tribological behavior was investigated. CrN, AlTiN, and CrN/AlTiN coatings with a total thickness of 2 µm were obtained by arc cathodic physical vapor deposition on conventional heat-treated and gas-nitrided steels. The white layer formed during nitriding was removed, and a diffusion layer (100 µm) was achieved in the cross section of the steel having a tempered martensitic matrix. The highest surface hardness was attained with an integral coating (CrN/AlTiN), and surface hardness increased even more after nitriding due to the formation of a multicomponent ceramic layer on top of the diffusion layer. The room temperature wear tests performed against an alumina counterpart revealed that (i) CrN/AlTiN-coated steel had the highest friction coefficient of 0.26, which further increased to 0.33 by nitriding due to the increase in shear strength, and that (ii) with increasing surface hardness, the specific wear rates (W) of the heat-treated and coated steels could be ranked as follows: WCrN/AlTiN < WAlTiN < WCrN. The wear rates decreased when nitriding was carried out prior to coating. In order to simulate the aluminum extrusion conditions, hot wear behavior of the surfaces against AA6080 alloy at 450 °C was investigated. The hot wear tests revealed that (i) high friction coefficients were reached due to the adhesive characteristic of aluminum to the surfaces, (ii) the nitrided and CrN/AlTiN-coated sample exhibited the lowest wear rate among all studied surfaces, and (iii) the film damage on the worn surfaces mostly occurred in the form of droplet delamination.
A necklace structure composed of fine grains formed by dynamic recrystallization was uncommonly observed at the pre-existing grain boundaries during the hot compression of a BCC Fe-25Al-1.5Ta alloy containing C14 - (Fe, Al)2Ta Laves phase precipitates. Two possible mechanisms for necklace formation were proposed; particle-stimulated nucleation and grain boundary bulging, depending on whether the original grain boundaries are occupied by C14 particles, or they are free of them. Recrystallization was initiated preferentially around the clusters of large particles at the boundaries containing particles. In contrast, the bulging of the original grain boundaries by strain-induced boundary migration was observed as a preliminary stage for necklace formation at the particle-free boundaries. The necklace structure expanded into the deformed volume in such a way that low-angle subgrain boundaries decorating the necklace layers transformed into grains with increasing deformation strain.
In the cast condition g titanium aluminide alloys that solidify completely through the b phase are
characterized by fine and homogeneous microstructures, weak textures and low segregation. For these reasons such alloys have a relatively good workability and can be closed-die forged without preceding ingot breakdown even if the alloys contain no large fractions of the b phase at the working temperature. The present work was devoted to a combined study of the constitution and microstructural morphologies that develop in various two-step heat treatments of a single-step forged b solidifying alloy. The
study included high-energy X-ray diffraction for in situ investigations of the constitution at the heat treatment temperature. It was observed that the phase ransformations are quite sluggish in the material which results in fine microstructures and some conditions that significantly deviate from thermodynamic equilibrium. Further, tensile and creep testing was carried out on the different material conditions in order to identify the range in which the properties can be varied. It is found that this easily forgeable material exhibits comparable strength, ductility and creep strength as more conventional peritectically solidifying alloys.
The influence of milling time on the tribological behavior of a Co–Cr–Mo alloy designed for biomedical applications, synthesized via mechanical alloying is investigated. Elemental Co, Cr and Mo powders are milled using different milling times (2, 6, 12 and 18 h) in a high-energy ball mill. The resulting powders were subjected to cold uniaxial and hot isostatic pressing respectively, followed by sintering to obtain cylindrical samples, which were evaluated for their structural, mechanical and the wear behavior. Results showed that the grain and crystallite sizes of the powders decreased with increasing milling time, reaching low values of <10 μm and 32 μm respectively, at higher milling times. Furthermore, the wear rates and the coefficients of friction were lower, at higher milling times due to high densities (96%), and higher elasto-plastic resistance, as presented by the H/E and H3/E2 values of 0.026 and 0.0021 GPa, respectively. Increased milling time enables the refinement of grains and reduction in porosity in the Co–Cr–Mo alloy, which in turn increases the alloy's elasto-plastic resistance and enhances its wear resistance.
The aim of this study was to investigate the influence of thermo-cyclic treatments on the mechanical characteristics (Hardness and Resilience) of low-alloy 42CD4 steel. Thermocyclic treatment on 42CD4 steel was operated for four cycles at 850 °C for 30 min. After each cycle, the steel sample was cooled in different medium (open air and water) in order to check the effect of the cooling rate on the microstructure characteristics. It was found that the cooling rate can affect the mechanical characteristics of the steel. The hardness values of steel cooled in water were higher than those of steel cooled in air. Additionally, there was an increase in the resilience of steel sample with the increase of thermocyclic number.
Die Weltklimakonferenz fordert eine massive Senkung der Treibhausgasemissionen mittels Abkehr von der Nutzung fossiler Brennstoffe hin zur Verwendung umweltverträglich hergestellter Energie. Da erneuerbare Energien aber bisher nicht durchweg bedarfsgerecht zur Verfügung stehen und schlecht speicherbar sind, besteht eine kurzfristige Lösungsmöglichkeit in Umwandlung, Speicherung und Wiederverwendung klimaschädlicher Verbrennungsgase. Eine effiziente Lösung zur Nutzung von CO2 ist dessen Umwandlung in ein speicherbares, zur Energieerzeugung nutzbares Gas. Mit der Methanisierung von CO2 kann eine erhebliche Reduzierung der Treibhausgasemissionen erreicht werden, wenn Methanschlupf vermieden wird. Bei dieser sogenannten Sabatier-Reaktion, die normalerweise bei 350°C bis 600°C stattfindet, reagiert Kohlendioxid mit Wasserstoff zu Methan. Als Reaktionsprodukte treten außer Methan und Wasser die Rest-Reaktanten sowie kleine Mengen an Verunreinigungen aus dem Verbrennungsprozess auf.
Reaktionsbehälter und Leitungen bestehen üblicherweise aus Edelstahl. Durch hohe Umgebungs-temperatur und aggressive Umgebungsmedien kann auch bei dem normalerweise temperatur- und korrosionsbeständigen Werkstoff 316L Korrosion auftreten, Materialeigenschaften beeinflussen und zu Materialversagen führen. Zur Bewertung des Einflusses des CO2 Methanisierungs-Prozesses auf 316L wurde ein Methanisierungs-Reaktor im Labormaßstab nach der Nutzung demontiert und untersucht. In verschiedenen Bauteilen des Reaktors (Gaszuleitung, Gasaustritt, Reaktorsegment) wurden Korrosionsbeläge gefunden. Abhängig von ihrer Lage im Bauteil sind diese Korrosionsschichten sehr unterschiedlich aufgebaut. Mikrostruktur und Elementzusammensetzung der Schichten wurden mittels Rasterelektronenmikroskopie kombiniert mit energiedispersiver Röntgenspektroskopie analysiert. Während die Gaszuleitung nur moderaten Korrosionsangriff zeigt konnten im Bereich des Gasaustritts Spalt-, Kontakt- und Lochkorrosion nachgewiesen werden. Innerhalb der Korrosions¬schichten wurden drei Zonen (Mehrschichtenstruktur, Partikelansammlung und brüchiger Passivfilm) identifiziert. Die Mehrschichtzone setzt sich aus kolumnaren und granularen Strukturen zusammen, die Partikelansammlungen bestehen aus zylinderförmigen und kugelförmigen Partikeln. Die Elementzusammensetzung innerhalb der Korrosionsschichten lässt auf Kontaktkorrosion verursacht durch das Material der Dichtringe schließen.
This paper describes the microstructure and properties of titanium-based composites obtained as a result of a reactive spark plasma sintering of a mixture of titanium and nanostructured (Ti,Mo)C-type carbide in a carbon shell. Composites with different ceramic addition mass percentage (10 and 20 wt %) were produced. Effect of content of elemental carbon covering nc-(Ti,Mo)C reinforcing phase particles on the microstructure, mechanical, tribological, and corrosion properties of the titanium-based composites was investigated. The microstructural evolution, mechanical properties, and tribological behavior of the Ti + (Ti,Mo)C/C composites were evaluated using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), electron backscatter diffraction analysis (EBSD), X-ray photoelectron spectroscopy (XPS), 3D confocal laser scanning microscopy, nanoindentation, and ball-on-disk wear test. Moreover, corrosion resistance in a 3.5 wt % NaCl solution at RT were also investigated. It was found that the carbon content affected the tested properties. With the increase of carbon content from ca. 3 to 40 wt % in the (Ti,Mo)C/C reinforcing phase, an increase in the Young’s modulus, hardness, and fracture toughness of spark plasma sintered composites was observed. The results of abrasive and corrosive resistance tests were presented and compared with experimental data obtained for cp-Ti and Ti-6Al-4V alloy without the reinforcing phase. Moreover, it was found that an increase in the percentage of carbon increased the resistance to abrasive wear and to electrochemical corrosion of composites, measured by the relatively lower values of the friction coefficient and volume of wear and higher values of resistance polarization. This resistance results from the fact that a stable of TiO2 layer doped with MoO3 is formed on the surface of the composites. The results of experimental studies on the composites were compared with those obtained for cp-Ti and Ti-6Al-4V alloy without the reinforcing phase.
β-type Ti–20Nb–13Zr alloys with low Young’s modulus were prepared at different sintering temperatures (950, 1050, 1150, and 1250 °C). The morphological and structural characteristics of as-prepared samples were investigated by several methods. Wear tests were conducted using a ball-on-plate type oscillating tribometer under different applied loads (2, 10, and 20 N). The morphological characterization indicated that the mean pore and crystallite size continuously decreased with increasing sintering temperature to reach lowest values of 40 nm and 38 nm at 1250 °C, respectively. The relative density of the 1250 °C sintered sample was as high as 98.7%. Moreover, the higher sintering temperature resulted in higher relative density and closed porosity of the sample. Both the friction coefficient and wear rate were lower in the sample sintered at 1250 °C as compared to other samples. This enhancement in tribological properties was attributed to a closed porosity.
In the present work, a combined process of laser powder bed fusion (LPBF) and hot working in terms of microstructure refinement was investigated for Fe-25Al-1.5Ta alloy samples. Uniaxial compression tests were carried out parallel and perpendicular to the building direction (BD) at 1000 °C, where BCC A2-phase was stable, at a strain rate of 0.0013 s−1. The true stress–true strain curves indicated a broad flow stress peak followed by a slight decrease, which is typical for dynamic recrystallization (DRX) of conventional BCC metals such as ferritic iron. A negligible dependence in the flow stress behavior on the compression direction was observed. DRX initiated at a stress of 18.7 MPa for the sample compressed parallel to the BD, corresponding to a true strain of 0.011, and at 18.1 MPa for the samples compressed normal to the BD, which corresponded to a true strain of 0.010. The microstructural investigations by electron backscatter diffraction (EBSD) showed that the relatively coarse and elongated grains of the as-LPBF builds were significantly refined after hot working. The microstructure of the compressed samples mainly consisted deformed grains. These were fragmented by sub-grains bounded by low-angle boundaries independent of the compression axis, indicating the occurrence of dynamic recovery (DRV) during hot working. In addition, a few equiaxed, small grains were observed in the pre-existing grain boundaries, which formed due to DRX. Most pores in the as-LPBF builds were closed after hot compression, particularly in the central region of the deformed specimens where the compressive stress state is dominant. In summary, hot compression reveals a practical thermomechanical post-processing treatment for Fe-Al-Ta iron aluminides built by LPBF. The hot working refines the epitaxially elongated microstructure of the as-LPBF builds by DRV/DRX and reduces the porosity.
The objective of this study was to examine the mechanism how the surface of porous TiNi compounds produced by SHS method evolves. The prepared samples were investigated using light-microscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive x-ray spectroscopy (EDS). The results indicated that the surface of all pores is represented by a granular stratum due to dendrite liquation by peritectic crystallization mechanism. The voids of 2–15 μm in size are formed owing to a capillary spreading of the liquid. Reaction gases with dissociated carbon, nitrogen, and oxygen are responsible for heat-and-mass transfer through the forming pores. High pressure-temperature effect of reaction gases on the melt causes the forming voids to coalesce, as well as transfers the peritectic liquid (PL) throughout the open pores catalyzing a distinctive spitted topography. It is through the chemisorption of gasiform nonmetallics by the pore surface melt, where these impurities are chemically bound, that it was formed a massive corrosion-resistant amorphous-nanocrystalline stratified shell deduced as an intermetallic oxycarbonitride layer.
The study aimed to characterize the structural-phase composition of the porous SHS TiNi surface explored by the GIXRD method. The surface layers at a depth of up to 100 nm mainly consist of amorphous nanocrystalline intermetallic oxycarbonitrides Ti₄Ni₂(O,N,C) with nonmetallic inclusions of different structural variants and routes of origin. Fine-porous alloys were synthesized at ignition temperatures of 450-480 °C. A distinct feature of the surface of crystalline phases therein was shown to be a low degree of crystallinity (up to 40%) and presence of multifarious glass and cermet phases evident as NiSi₂, NaAlSiO (SO₄), SiO₂, MgSi₂, and CaCO₃. Conversely, large-pore alloys ignited at temperatures of 280-330 °C have a higher degree of crystallinity (up to 70%). An individually selected GIXRD technique and precision structural phase analysis are capable to determine a set of other superficial nonmetallic and cermet phases reported as CaTiO₃, Si (P2O₇), CaSiO₃, MgAl₂O₄, TiNiAl, as well as the Ti₃SiC₂MAX phase.
Hot isostatically forged TiAl turbine blades made of TNM-B1 are commercially used in aircraft engines, as they offer significantly lower weight than the traditional nickel-based blades while exhibiting similar strength. Like other TiAl alloys, TNM-B1 displays high peak stress followed by a strong softening behavior (i.e. stress reduction) during hot deformation. This softening can be used to accelerate the deformation process by reducing the processing time and in turn the costs for TNM-B1 parts. In order to avoid increased damage during the accelerated process, a pre-heat treatment (HT) for the hot isostatically pressed material (HIP) is required. To simulate the accelerated forming process, hot compression tests were performed with a DIL805A/D/T dilatometer from TA Instruments (New Castle, Delaware, USA) with different strain rates (0.0013, 0.005, 0.01 and 0.05) and temperatures (T=1150, 1175 and 1200°C). Deformation of the heat-treated state revealed lower flow stress (in both, peak stresses and steady state stresses) and fewer voids compared to the HIP state (Fig. 1.a). The compression test data were used to develop material and temperature specific strain rate profiles based on a material model. Subsequently, hot compression tests were performed with different strain rate profiles (starting strain rates 0.0013 and 0.0052) for the HIP and the HT state. The results were evaluated with regard to their microstructure, deformation, and damage behavior. A reduction of the processing time for all tested strain rates profiles by factors 2-3 could be achieved compared to constant strain rates. Furthermore, the results indicated that the deformation with strain rate profiles (compared to constant strain rates) did not significantly change the resulting microstructure or damage tolerance of the HT state.