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Institute
Microstructure of the Laser Beam Welded Iron-Based Superalloy A286 after High Temperature Creep
(2002)
Cyclic deformation behaviour of austenitic CrMnMoN steel in solution annealed and cold worked states
(2004)
Microstructural changes within similar coronary stents produced from two different austenitic steels
(2009)
(Cr1-x Al x)N as a candidate for corrosion protection in high temperature segments of CCS plants
(2013)
Three (Cr1−x Al x )N (x = 0.33, 0.5, 0.66) coatings were deposited on Ni-super alloy IN718 using reactive magnetron sputtering. The oxidation behavior of all coatings at 900 °C up to 500 h in air was studied. Furthermore, the corrosion behavior of the (Cr0.33,Al0.66)N coating at 900 °C (corrosion type I) by spraying a uniform salt scale of Na2SO4 on the sample surface (1 mg/cm2) was investigated. It was found that the coated samples indicate significantly higher oxidation and corrosion resistance compared to uncoated Ni super alloy. This is mainly due to the formation of protective Cr2O3 and Al2O3 layers on the coating surface. With the increase of Al content, the coatings exhibited improved oxidation resistance. The formation of thin and adherent Al2O3 scale on the surface of Al rich coating is the reason for its better oxidation behavior. The detailed structures of the oxide scales and the interdiffusion between coating and substrate were studied using energy dispersive X-ray spectroscopy-analysis.
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.
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 literature review reveals that the honeycomb-structured thin sheet metals are not adequately investigated with regard to their fatigue strength. A question that remains almost completely ignored in the process is the direct comparability of structured thin sheet metals with flat reference specimens. A thin sheet is not a classic specimen to determine the fatigue strength because of the known problem of the fracture mechanics. Structured thin sheet metals of deep-drawing steel DC04 with a thickness of 0.5 mm were examined. Flat specimens were used as reference material. The frequency analysis was used for comparison.
Fundamental differences in the mechanical behavior between flat and structured sheets under cyclic load were observed. Whereas an extremely flat S-N curve in the low-cycle region with a high slope coefficient was observed for the smooth thin sheets, the structured specimens show a curve typical for notched specimens. Moreover, the smooth sheets have a specific cyclic hardening and/or softening behavior. The state of plane stress of a fine sheet in contrast to a multi-axial one for the structured sheet complicates the direct comparison. For this reason, such a comparison with respect to their fatigue strength in the Wohler diagram should only be considered with caution.
Investigation of the wear resistance properties of Cr/CrN multilayer coatings against sand erosion
(2015)
The wear of metallic components used in gas and steam turbines due to erosive sand particles lead to a tremendous decrease in their lifetime. This wear can be reduced by the use of suitable erosion resistant coatings resulting in lower maintenance costs. In this context, multilayer Cr/CrN PVD coatings using an industrial coater was designed and applied on Inconel 718, a material which finds its application in gas turbines. A variation in the bimodal period has been induced in order to achieve an optimal coating architecture providing optimum properties needed for the erosion resistant coatings. The coating was deposited using a single Cr- target with an induction of N2 during the nitriding phase at a temperature of 480-500 °C and the coating thickness of 24-26 µm was kept constant throughout. The erosion tests were conducted at angles of 30°, 60° and 90°. The sand used for the test is an irregular shaped SiO2. The erosion tests were followed by a detailed microscopic examination of the eroded coating structure in combination with nanoindentation and scratch tests.
This research work provides information about the influence of Ti2AlC MAX phase coatings on the
erosion resistance of Ti624 2alloy.Flat specimens were coated witha20 µm Ti2AlC film using an industrial siz emagnetron sputtering coater and annealed at 800 °C for 1h in vacuum for the formation of the MAX phase.The erosion resistance of the specimens was tested using high velocity particles at room
temperature.The results indicate that the erosion resistance of Ti6242 has been significantly enhanced
by the employment of MAX-phase coatings. This demonstrates the capability of using MAX phase
coatings as erosion protective medium for engine components exposed to similar damage conditions.
Additionally,the results show that uncoated Ti6242 samples with duplex microstructure have a better
durability against erosion attack compared to uncoated samples with globular microstructure.
Carbon fibre reinforced thermoplastics (CFRP) are intensively used in lightweight
applications due to their high strength to weight ratio. In addition they offer good crash,
damping and recycling properties. On the basis of their morphology they are suitable for large
scale manufacturing processes. A major disadvantage consists of its poor hardness properties,
which is again an important requirement to realize a good erosion and wear behaviour.
Design/methodology/approach: In this work the application of orthotropic carbon
fibre reinforced polymers (PA6), with protective TiAlN coatings, produced by physical
vapor deposition (PVD), is investigated. The characterization of the coating is performed
by nanoindentation tests, roughness measurements and scanning electron microscopy.
Furthermore micro hardness tests on selected well prepared cross sections are conducted,
to compare the coating quality with established coating systems.
Findings: By applying TiAlN coating, the hardness of the CFRP samples can be increased
substantially up to 15 GPa, in comparison to the basic substrate. In addition the quality of
the coating surface can be improved significantly by plasma etching pre-treatment.
Research limitations/implications: The presented findings are preliminary results to
prove the application of a standard processed ceramic coating on new composite types
for mass production. The PVD coating process as well as the utilized testing methods are
suitable to realize hard coatings on thermoplastic CFRP. This effect can be exploited for
several lightweight applications to increase the erosion and wear resistance of composite
materials.
Originality/value: The presented results show, that ceramic coatings can be deposited
on standard thermoplastic CFRP with polyamide 6 matrix. Therewith it can be expected,
that the PVD coating process can make a essential contribution to increase the range of
applications.
The topic of fatigue strength of joints of flat and honeycomb-structured thin sheets has not yet been adequately studied. This concerns, for example,the development of an appropriate test method. In many cases, there is still a lack of information, how effective joints of flat and structured sheet metals are in omparison with reference joints of flat sheets. Combinations of resistance spot-welded specimens of flat and honeycomb-structured thin sheets of deep-drawing steel DC04 with a thickness of 0.5 mm were examined. Adopted clamping plates were applied for the testing. Joined smooth specimens were used as a reference material. The analysis of the frequency [1] was applied for comparison. The fatigue limit of a joint of a flat and a structured sheet metal is not significantly affected by spot welding. The fatigue limit of these spot-welded joints is comparable to that of an non joined honeycomb-structured sheet. By means of frequency or stiffness analysis, stability and damage mechanisms of differently shaped joints were explained. The joining of bridges of the structure shows a better stability than the combination of honeycombs. The stiffness analysis is a favored method for the clarification of the damage mechanisms in a spot-welded joint. The reasons for the low fatigue strength values of the joined flat-structured specimens compared to flat-flat joints are strong notch effects in the bridge area and momentum effects by the structure height of the studied honeycomb structure. The spot weld with a pronounced indentation also affected the fatigue strength of both flat and structured joined sheet metals.
Thin sheet metals from deep drawing steel DC04 are very often used in the production of car body and case parts. Quality improvement of sheet
metal components by new constructive solutions (structuring) as well as
adapted joining technology is going on. Structured sheet metals differ from each other by their high bending stiffness. At the same time, they show certain anisotropy due to the structure. Therefore a typical testing
method of structured semi-finished parts (single sheet metals, sandwiches)is the bending test. The literature review revealed that in many
studies no special demands on tests of structured materials were made. This concerns particularly the structure arrangement, structure direction and structure location of the specimen relative to the mandrel position during bending tests, i. e., the direction of the fixed load relative to the structure. The aim of this study was to determine the influence of the test
specification on flexural behavior. In the present paper, honeycomb-structured
sheet metals were examined using 3-point bending tests. Bending stiffness and lightweight potential were calculated with respect to the location of load application and compared for different structure arrangements,directions and locations. The influence of the anisotropy on flexural
behavior of the honeycomb-patterned sheet metals was moderate.
This paper serves as an overview of the ongoing research in the field of multiscale and multidisciplinary analysis of deformation and damage in the case of oligocrystalline structures. The research focuses on experimental measurement and numerical calculation of ductile failure in the X2CrNiMo18-15-3 (AISI 316L) stainless steel. An embedding numerical technique is employed where crystal plasticity theory is used to represent plastic deformation in the material and element removal technique based on Rice&Tracey damage model for ductile void growth to simulate damage initiation inside the material, which is observed in the experiments. Additionally, the crystal plasticity model is supported by a hierarchical multiscale approach connecting nano-, micro- and meso-scales.
Role of alloying elements during thermocyclic oxidation of β/γ-TiAl alloys at high temperatures
(2016)
Gamma titanium aluminides are promising alloys known for their good mechanical properties and low densities, but their low oxidation resistance at high temperatures limits their
application. This work discusses the thermocyclic oxidation behavior of newly developed β/γ-TiAl alloys at temperatures between 600 °C and 900 °C. An influence of β-stabilizing alloying elements like Nb and V on the oxidation of these alloys has been investigated here.
The selected alloys are tested in an in-house developed thermocyclic furnace. The oxidation
study is supported by gravimetric measurements along with Scanning Electron Microscopy (SEM) and Electron Diffraction Spectroscopy (EDS) mapping of the oxide layers. Additionally, phase formation after oxidation has been determined using X-Ray Diffraction (XRD). Results show that the Nb containing alloys are more oxidation resistant as compared
to V containing alloys. The formation of a mixture of Al2O3 and TiO2 layers was found for all the alloys. The oxide kinetics controlled oxide growth and formation of
various phases at different testing temperatures.
Coating growth and mechanical properties of nanolamellar Cr2AlC coatings at various sputtering power were investigated in the present study. Cr2AlC coating was deposited on the IN 718 superalloy and (100) Si wafers by DC magnetron sputtering at different sputtering powers.
The structure and properties were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nanoindentation. It was found that coatings had columnar structure with nanocrystalline substructure. Deposition rate increased with the sputtering power. XRD results showed the presence of the Cr2AlC MAX phase, intermetallic
AlCr2 and Cr7C3 carbide phases, along with the change in preferential coating growth orientation. TEM observations confirmed the occurrence of these phases, and the SAED patterns demonstrated significant texture of the coatings. Hardness values were measured in the range between 11–14 GPa, showing a slight increase with the sputtering power.
Controlled ion bombardment is a popular method to fabricate desirable coating structures and modify their properties. Substrate biasing at high frequencies is a possible technique, which allows higher ion density at the substrate compared with DC current bias. Moreover, high ion energy along with controlled adatom mobility would lead to improved coating growth. This paper focuses on a similar type of study, where effects of coating growth and properties of DC magnetron-sputtered chromium nitride (CrxN) coatings at various substrate bias frequencies are discussed. CrxN coatings were deposited by pulsed DC magnetron sputtering on Inconel 718 and (100) silicon substrates at 110, 160 and 280 kHz frequency at low duty cycle. Coating microstructure and morphology were studied by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), scratch adhesion testing and nanoindentation. Results indicate a transformation of columnar into glassy structure of CrxN coatings with the substrate bias frequency increase. This transformation is attributed to preferential formation of the Cr2N phase at high frequencies compared with CrN at low frequencies. Increase in frequency leads to an increase in deposition rate, which is believed to be due to increase in plasma ion density and energy of the incident adatoms. An increase in coating hardness along with decrease in elastic modulus was observed at high frequencies. Scratch tests show a slight increase in coating adhesion, whereas no clear increase in coating roughness can be found with the substrate bias frequency.
Hydrogen degradation is a serious problem in industrial applications like power plants (boilers, turbines), marine structures, car and aircraft components, as it leads to failures as well as to deterioration of properties. Inconel 718 is one of the most commonly used materials for these applications. Different metal nitrides like TiN coatings have been deposited in past to prevent hydrogen degradation, which are also known for their high hardness and good wear resistance [1, 2]. However, reports on hydrogen degradation of CrN coatings, which shows better oxidation and corrosion resistance, higher temperature stability and lower friction coefficient than TiN [3, 4] has not been reported till now. Despite a lot of publications about CrN films, up to now the effect of hydrogenation on mechanical and tribological properties of CrN coatings is still not completely understood. In the current work CrxN coatings were deposited by Direct Current Magnetron Sputtering (dcMS) on Inconel 718 substrate at different chamber pressures and substrate voltages. Substrate voltage is one of the most important process parameters which determines the structure of the coating and the adhesion between substrate and coating. Simultaneously a study of the chamber pressure is also needed to understand the deposited structure and growth rate because at higher pressures the high number of argon atoms reduce the number of ionized ions available for the deposition leading to low deposition rates [5]. Gas-phase hydrogenation of the samples was performed at a temperature of 600° C and hydrogen pressure of 2 atm. It was found that CrxN coatings are resistant against hydrogen exposure as compared to uncoated surfaces. The results of changes in the mechanical, tribological properties and phase composition of the coatings after hydrogenation are discussed. Coating microstructure was studied by scanning electron microscopy (SEM). The mechanical properties of the coatings were characterized by means of nanoindentation and scratch test.
Investigation of TiAlN HiPIMS coating deposited on the newly developed Ni-based superalloy AD730
(2016)
The development of new alloys for gas turbine engines has been focused on withstanding against increasing service temperatures. AD730™ is a recently developed nickel-based superalloy for turbine disk applications with superior
properties at 700°C, which is higher than the common service temperature for IN718. Use of coatings to enhance the properties of materials, such as wear resistance is widely known in various applications. This research presents an experimental study of TiAlN coatings, deposited onto AD730 superalloy using High Power Impulse Magnetron Sputtering (HiPIMS). Phase structure and chemical composition of the TiAlN films were characterized by X-ray diffractometry. Transmission electron microscopy as well as scanning electron microscopy were used to analyze the
microstructure of the coating. Mechanical properties, including hardness, Young's modulus, and adhesion strength were measured using nanoindentation und scratch test.
Effect of pulse time on structure and mechanical properties of HPPMS deposited AlTiN coatings
(2016)
The use of PVD AlTiN as a protective coating on cutting tools is well known. With the introduction of pulsed deposition techniques like High Power Pulsed Sputtering
(HPPMS), a possibility is provided to the coating developers to design their coatings by the variation in pulse parameters. To analyze the effect of pulse time HPPMS
AlTiN coatings were deposited on Si (100) as well as 100Cr6 steel plates at a temperature of 500°C in a reactive gas environment. Oscilloscope measurements depicted a change in current-voltage characteristics with variation in pulse time. This influence the coating structure, deposition rates and phase formations as well. Nanoindentation results show a variation in the mechanical properties of the coatings with the change in pulse time. This study focuses on the potential of HPPMS technology for enhancement of mechanical and structural properties of AlTiN coating.
Multi-layer constructions become more and more relevant in lightweight applications due to their high strength to
weight ratio. They offer excellent crash, damping and recycling properties. Also, the morphology of thermoplastic
carbon fibre reinforced plastics (CFRP) render them interesting for large scale manufacturing processes.
Nevertheless, a major disadvantage results in a poor resistance against wear and tear, e.g. erosion, which is
attributed to weak hardness properties. Hence, this work deals with tribological investigations on orthotropic
carbon fibre reinforced polymers (PA 6) either with protective ceramic coating or without. The chosen coating
system is a well-known protective covering of metal components, e.g. metal cutting tools, produced by physical
vapor deposition (PVD). To characterize the coating system on thermoplastic CFRP, standard analyzing methods are utilized, like optical and scanning electron microscopy (SEM). The tribological investigations are conducted by the tribological ball on disk method to generate wear tracks on the sample surfaces and hence to calculate the
wear rates. These results are compared to literature findings with respect to a certain protective coating system (TiN) and a second nano-structured gel coating system, where both systems are deposited on a thermosetting
material, i.e. carbon fibre reinforced epoxy resin, respectively. For this purpose the feasibility of depositing a protective ceramic layer on thermoplastic CFRP is demonstrated. First results on suitable surface pre-treatments have shown a significant influence on the coating quality. The improved performance regarding the wear behavior with respect to tribology compared to the poor substrate and existing technologies is shown additionally.
In the current study, the properties of the CrₓN coatings deposited on the Inconel 718 superalloy using direct current reactive magnetron sputtering are investigated. The influence of working pressure on the microstructure, mechanical, and tribological properties of the CrₓN coatings before and after high-temperature hydrogen exposure is studied. The cross-sectional scanning electron micrographs indicate the columnar structure of the coatings, which changes from dense and compact columns to large columns with increasing working pressure. The Cr/N ratio increases from 1.4 to 1.9 with increasing working pressure from 300 to 900 mPa, respectively. X-ray diffraction analysis reveals a change from mixed hcp-Cr₂N and fcc-CrN structure to approximately stoichiometric Cr₂N phase. After gas-phase hydrogenation, the coating deposited at 300 mPa exhibits the lowest hydrogen absorption at 600 °C of all investigated coatings. The results indicate that the dense mixed cubic and hexagonal structure is preferential for hydrogen permeation resistance due to the presence of cubic phase with higher packing density in comparison to the hexagonal structure. After hydrogenation, no changes in phase composition were observed; however, a small amount of hydrogen is accumulated in the coatings. An increase of coating hardness and elastic modulus was observed after hydrogen exposure. Tribological tests reveal that hydrogenation leads to a decrease of the friction coefficient up to 20%–30%. The best value of 0.25 was reached for hydrogen exposed CrₓN coating deposited at 300 mPa.
Ti-Al-N coatings were deposited by direct current magnetron sputtering (DCMS) onto IN 718 at different nitrogen flow rates and deposition temperatures. The coatings’ properties were characterized using atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) as well as nanoindentation. It was found that higher deposition temperature leads to higher surface roughness and nitrogen flux influences the shape of grains. According to XPS, the bonding structure of all coatings exhibited the (Ti,Al)N phase. Mechanical properties depend on the Al content within the films. The coating with the best mechanical properties (deposited at 500 °C and 20 standard cubic centimeters per minute (sccm)) was further deposited onto tungsten carbide (WC) cutting tools for cylindrical turning experiments. A quasi-constant flank wear was observed until a machining volume of 23,500 mm³.
MAX phases (M = transition metal, A = A-group element, and X = C/N) are of special interest because they possess a unique combination of the advantages of both metals and ceramics. Most attention is attracted to the ternary carbide Cr2AlC because of its excellent high-temperature oxidation, as well as hot corrosion resistance. Despite lots of publications, up to now the influence of bias voltage on the chemical bonding structure, surface morphology, and mechanical properties of the film is still not well understood. In the current study, Cr-Al-C films were deposited on silicon wafers (100) and Inconel 718 super alloy by dc magnetron sputtering with different substrate bias voltages and investigated using Scanning Electron Microscopy (SEM), X-ray Photoelectron Spectroscopy (XPS), X-ray Diffraction (XRD), Atomic Force Microscopy (AFM), and nanoindentation. Transmission Electron Microscopy (TEM) was used to analyze the correlation between the growth of the films and the coating microstructure. The XPS results confirm the presence of Cr2AlC MAX phase due to a negative shift of 0.6–0.9 eV of the Al2p to pure aluminum carbide peak. The XRD results reveal the presence of Cr2AlC MAX Phase and carbide phases, as well as intermetallic AlCr2. The film thickness decreases from 8.95 to 6.98 µm with increasing bias voltage. The coatings deposited at 90 V exhibit the lowest roughness (33 nm) and granular size (76 nm) combined with the highest hardness (15.9 GPa). The ratio of Al carbide to carbide-like carbon state changes from 0.12 to 0.22 and correlates with the mechanical properties of the coatings. TEM confirms the columnar structure, with a nanocrystalline substructure, of the films.
Ti-Al-N coatings were deposited on high-speed steel substrates by filtered vacuum arc deposition (FVAD) during evaporation of aluminum and titanium cathodes. Distribution of elements, phase composition, and mechanical properties of Ti-Al-N coatings were investigated using Auger electron spectroscopy (AES), X-ray diffraction (XRD), transmission electron microscopy (TEM) and nanoindentation, respectively. Additionally, tribological tests and scratch tests of the coatings were performed. The stoichiometry of the coating changes from Ti0.6Al0.4N to Ti0.48Al0.52N with increasing aluminum arc current from 70 A to 90 A, respectively. XRD and TEM showed only face-centered cubic Ti-Al-N phase with preferred orientation of the crystallites in (220) direction with respect to the sample normal and without precipitates of AlN or intermetallics inside the coatings. Incorporation of Al into the TiN lattice caused shifting of the (220) reflex to a higher 2θ angle with increasing Al content. Low content and size of microdroplets were obtained using coaxial plasma filters, which provides good mechanical and tribological properties of the coatings. The highest value of microhardness (36 GPa) and the best wear-resistance were achieved for the coating with higher Al content, thus for Ti0.48Al0.52N. These coatings exhibit good adhesive properties up to 30 N load in the scratch tests.
Coatings like TiAlN (titanium content more than 50 %) or AlTiN (aluminium content more than 50 %) are well established as hard and wear resistant tool coatings, often prepared by physical vapour deposition (PVD) like arc evaporation or direct current magnetron sputtering (dcMS). With increasing challenges of operating conditions, a constant need in improvement of mechanical properties is required to withstand extreme loading conditions. This can be obtained by a higher amount of ionized sputtered metal atoms during the deposition process. To increase the metal-ion flux a high-power pulse magnetron sputtering (HPPMS) was developed. In order to understand the relation between HPPMS process parameters and mechanical properties of the AlTiN coatings, the present study discusses how different pulse frequencies (for a constant pulse length) influence AlTiN coating structure growth and their mechanical properties. In addition, film deposition rate and phase formation are influenced by altering process parameters like pulse length and frequency. Hence, different pulse-frequencies produce specific coatings with corresponding properties for functional requirements. Based on the established findings, answers to new scientific queries along with the demand to further optimize these coatings for tool applications are required.
New process chains involving additive manufacturing and metal forming - a chance for saving energy?
(2017)
The effect of low energy plasma immersion ion implantation and deposition of titanium on microstructure, defect structure and hydrogen trapping in zirconium alloy Zr-1Nb was studied. Defect structure and distribution were analyzed by Doppler broadening using slow positron beam. The surface microstructure after modification is represented by nanostructured Ti grains with random orientation. The gradient distribution of titanium as well as vacancy type defects were analyzed. The concentration of vacancy type defects is rising with increasing bias voltage. Gas-phase hydrogenation of the Ti-modified Zr-1Nb alloy was performed at 400 °C for 60 min. The strong interaction of hydrogen with vacancy type defects was demonstrated. Two different changes in the defect structure after hydrogenation were observed: when a titanium film is formed on the surface (after deposition at 500 V) hydrogen trapping occurs with the formation of titanium hydride phases, while in the implanted layer (deposition at 1000 and 1500 V) hydrogen is trapped due to interaction with vacancy type defects. The physical basis of Ti diffusion and its influence on the evolution of defect structure after surface modification and hydrogenation were discussed.
In the current work, the microstructure, hydrogen permeability, and properties of chromium nitride (CrNₓ) thin films deposited on the Inconel 718 superalloy using direct current reactive sputtering are investigated. The influence of the substrate bias voltage on the crystal structure, mechanical, and tribological properties before and after hydrogen exposure was studied. It was found that increasing the substrate bias voltage leads to densification of the coating. X-ray diffraction (XRD) results reveal a change from mixed fcc-CrN + hcp-Cr₂N to the approximately stoichiometric hcp-Cr₂N phase with increasing substrate bias confirmed by wavelength-dispersive X-ray spectroscopy (WDS). The texture coefficients of (113), (110), and (111) planes vary significantly with increasing substrate bias voltage. The hydrogen permeability was measured by gas-phase hydrogenation. The CrN coating deposited at 60 V with mixed c-CrN and (113) textured hcp-Cr₂N phases exhibits the lowest hydrogen absorption at 873 K. It is suggested that the crystal orientation is only one parameter influencing the permeation resistance of the CrNx coating together with the film structure, the presence of mixing phases, and the packing density of the structure. After hydrogenation, the hardness increased for all coatings, which could be related to the formation of a Cr₂O₃ oxide film on the surface, as well as the defect formation after hydrogen loading. Tribological tests reveal that hydrogenation leads to a decrease of the friction coefficient by up to 40%. The lowest value of 0.25 ± 0.02 was reached for the CrNₓ coating deposited at 60 V after hydrogenation.
Oxidation Behavior of Zr–1Nb Corroded in Air at 400 °C after Plasma Immersion Titanium Implantation
(2018)
In this paper, the influence of plasma immersion titanium implantation into the zirconium alloy Zr-1Nb on the oxidation behavior at 400 °C for 5, 24, 72, and 240 h in air under normal atmospheric pressure (101.3 kPa) was shown. The influence of implantation on the protective properties of the modified layer was shown. The valence of the oxides before and after implantation was analyzed by means of X-ray photoelectron spectroscopy (XPS). Grazing incidence X-ray diffraction (GIXRD) was carried out to examine the phase composition after titanium ion implantation and oxidation. Differential scanning calorimetry (DSC) revealed that titanium implantation exhibited effects of stabilizing the β phase. The formation of the t-ZrO2 and m-ZrO2 was observed during the oxidation of the as-received and modified Zr-1Nb. The measurement of weight gain showed an improvement in oxidation resistance of Ti implanted Zr-1Nb at the oxidation up to 24 h when compared with that of the as-received Zr-1Nb. However, at longer oxidation cycle the oxidation rate of Ti-implanted zirconium alloy is the same with the as-received alloy, which attributed to the layer thickness. Nevertheless, the corrosion of the Ti-implanted alloy is more uniform, while a local corrosion and cracks was detected on the surface of the as-received alloy.
This paper describes the hydrogenation behavior of Zr-1Nb alloy Ti-implanted by plasma immersion ion implantation (PIII). Hydrogen sorption kinetics of the Ti-modified alloy was investigated under gas-phase hydrogenation at 400 °C for 1 h. The influence of implantation time on the protective properties of the modified layer was shown. The lowest hydrogen absorption as well as the highest hydrogen trapping efficiency was achieved after PIII for 30 min. The main contribution to the reduction of hydrogen permeation is the formation of an oxide layer consisting of mixed TiO2 and ZrO2 on the modified surface of the alloy. X-ray photoelectron spectroscopy (XPS) revealed that PIII titanium oxide exists on the surface in the form of TiO2, which transforms to mixed Ti2O3 and TiO2 after hydrogenation. The thickness of the modified layer increases with implantation time that improves the efficiency of hydrogen trapping. All the absorbed hydrogen is gradually distributed in the modified layer and no hydrides are formed after hydrogenation in Ti-modified Zr-1Nb for 15 and 30 min.
Knowledge of the properties of dissimilar welds is of great significance for the development of multi-material lightweight structures. In this study, stainless steel (1.4301) and aluminum alloy (6082-T6) sheets were welded in overlap configuration in keyhole mode. The resulting weld metals were investigated with respect to their mechanical properties. Several samples were cut out of different locations along the welds and their cross-sections were subjected to indentation testing and energy dispersive X-ray (EDS) analysis. Young's modulus E, yield stress σy, and strain hardening exponent n, were determined by means of reverse analysis of the indentation load (P) – depth (h) curves, allowing construction of true stress – true strain relations. An essential increase in yield stress in comparison to the one of the base alloys was observed inside the weld metal. In contrary, Young's modulus and strain hardening exponent of the welds were almost identical to corresponding values of the base steel metal. Due to the sensitivity of yield stress to the aluminum content, slight variations of the welding parameters lead to significant changes in elastic-plastic behavior of the weld metal.
Oxidation behavior of Zr–1Nb in air at 400°C after Titanium Plasma Immersion Ion Implantation
(2018)
Zirconium alloys have been widely used in nuclear reactors due to low thermal neutron capture cross-section, excellent corrosion resistance and acceptable mechanical properties [1, 2]. Nowadays several methods apply for improving hydrogen and corrosion resistance such as addition of stabilizing additives (yttrium) [3, 4], deposition of thin solid films [5, 6], micro-arc oxidation [7] and modification of the surface by electron beam [8, 9]. Despite the multiplicity of the methods hydrogen embrittlement is still a pressing issue. Previous results [10, 11] have shown the positive influence of plasma immersion titanium implantation on the hydrogenation behavior of Zr–1Nb and Zr–2.5 Nb. After Ti implantation hydrogen preferably accumulates in the modified surface layer comprising the implanted Ti. Furthermore, the hydrogen concentration is considerably less inside the zirconium modified sample than in the as-received samples.
The integration of elements into the zirconium lattice can influence the valence of the surface and change corrosion and oxidation rates of the alloys. So it is very important not to decrease the zirconium oxidation resistance due to Ti implantation. Therefore, the purpose of this research is to study of the influence of Ti implantation on surface morphology, oxidation rate and phase structure of the Zr–1Nb alloy after oxidation on air at 400 0C for 5, 24, 72 and 240 h. The surface structure of the samples and their elemental composition were investigated with the scanning electron microscope Mira II XMH (Tescan) with energy dispersive x-ray spectroscopy system (EDS). X-ray photoelectron spectroscopy (XPS), differential scanning calorimetry (DSC) as well as X-ray diffraction (XRD) was used to characterise the influence of titanium implantation on the oxidation behaviour. The results show that the oxidation kinetics after Ti modification of the zirconium alloy changed. Although the weight gain of the implanted sample remains approximately the same, it can be considered that Ti implantation stabilizes the oxide layer and has beneficial influence on the oxidation protection of Zr-1Nb.
As power generation from variable renewable energy sources such as wind and solar power continues to increase in the future, fewer baseload power plants will be needed. As a result, high operational flexibility is becoming a vital requirement for conventional power plants to allow for the smooth integration of the variable renewable energy sources (v-RES) into the grid. To understand the impact of high operational flexibility (increased cycling) for coal-fired power plant materials, five commercial coal boiler superheater and reheater materials were investigated under isothermal and cyclic conditions for 1000 h each. The candidate alloys investigated were: T91, VM12-SHC, TP347-HFG, DMV304 HCu and DMV310 N. The results (weight change kinetics and metallographic analysis) after exposure at a metal surface temperature of 650 °C clearly showed the impact of increased flexibility on the corrosion and oxidation of the materials. Oxide growth (weight gain), metal loss, oxide spallation, and grain boundary attack were found to be more severe under cyclic conditions than under isothermal conditions.
Hydrogen Interaction with Deep Surface Modified Zr-1Nb Alloy by High Intensity Ti Ion Implantation
(2018)
A deep surface modified TiZr layer was fabricated by high-intensity low-energy titanium ion implantation into zirconium alloy Zr-1Nb. Gas-phase hydrogenation was performed to evaluate protective properties of the modified layer against hydrogen permeation into Zr-1Nb alloy. The effects of ion implantation and hydrogen on microstructure, phase composition and elemental distribution of TiZr layer were analyzed by scanning electron microscopy, X-ray diffraction, and glow-discharge optical emission spectroscopy, respectively. It was revealed that TiZr layer (~10 μm thickness) is represented by α′ + α(TiZr) lamellar microstructure with gradient distribution of Ti through the layer depth. It was shown that the formation of TiZr layer provides significant reduction of hydrogen uptake by zirconium alloy at 400 and 500 °C. Hydrogenation of the modified layer leads to refinement of lamellar plates and formation of more homogenous microstructure. Hydrogen desorption from Ti-implanted Zr-1Nb alloy was analyzed by thermal desorption spectroscopy. Hydrogen interaction with the surface modified TiZr layer, as well as its resistance properties, are discussed.
The current trend shows an increasing demand for composites due to their high stiffness to weight ratio and the recent progress in manufacturing and cost reduction of composites. To combine high strength and stiffness in a cost-effective way, composites are often joined with steel or aluminum. However, joining of thermoset composite materials is challenging because circular holes are often used to join them with their metal counterparts. These design based circular holes induce high stress concentration around the hole. The purpose of this paper is to focus on layup configuration and its impact on notch stress distribution. To ensure high quality and uniformity, the holes were machined by a 5 kW continuous wave (cw) CO2 laser. The stress distribution was evaluated and compared by using finite element analysis and Lekhnitskii’s equations. For further understanding, the notch strength of the laminates was compared and strain distributions were analyzed using the digital image correlation technique.
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.
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.
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.
The effect of sintering temperature (1073–1373 K) on the structural and tribological properties of nanostructured ball-milled β-type Ti–15Mo samples was investigated. The prepared samples were characterized using various apperatus such as X-ray diffractometer, scanning electron microscope (SEM) and ball-on-plate type oscillating tribometer. Wear tests were conducted under different applied loads (2, 8 and 16 N). Structural results showed that the mean pore and crystallite size continuously decreased with increasing sintering temperature to reach the lowest values of 4 nm and 29 nm at 1373 K, respectively. The relative density of the sintered sample at 1373 K was as high as 97.0%. Moreover, a higher sintering temperature resulted in higher relative density, greater hardness and elastic modulus of the sample. It was observed that both the friction coefficient and wear rate were lower in the sample sintered at 1373 K which was attributed to the closed porosity.
A deep surface modified TiZr layer was fabricated by high-intensity low-energy titanium ion implantation into zirconium alloy Zr-1Nb alloy with the various dose in the range of (5.4–9.56) × 1020 ion/cm2. The gradient distribution of titanium as well as vacancy type defects were analysed. The effects of ion implantation on microstructure, phase composition and elemental distribution of TiZr layer were analysed by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and glow-discharge optical emission spectroscopy, respectively. The results show the appearance of Zr-Ti intermetallic phases of different stoichiometry after Ti implantation. The intermetallic phases are transformed from both Zr0.7Ti0.3 and Zr0.5Ti0.5 to single Zr0.6Ti0.4 phase with the increase in the implantation dose.
The depth of Ti penetration into the bulk of Zr increases from 6 to 13 μm with the implantation dose. The higher current density (170 mA/cm2) leads to the increase in the grain size and surface roughness. It was revealed that TiZr layer (~10 μm thickness) is represented by α′ + α(TiZr) lamellar microstructure with gradient distribution of Ti through the layer depth. Transmission electron microscopy was used for investigation of the physical basis of Ti diffusion and its influence on the evolution of the defect structure after surface modification. Furthermore, it was found that on the surface between substrate and implanted layer was found an amorphous layer, which occur as a result of further stress accumulations from the higher implantation doses.
Data-driven or machine learning approaches are increasingly being used in material science and research. Specifically, machine learning has been implemented in the fields of materials discovery, prediction of phase diagrams and material modelling. In this work, the application of machine learning to the traditional phenomenological flow stress modelling of the titanium aluminide (TiAl) alloy TNM-B1 (Ti-43.5Al-4Nb-1Mo-0.1B) is investigated. Three model types were developed, analyzed and compared; a physics-based phenomenological model (PM) originally developed for steel by Cingara and McQueen, a purely data-driven machine learning model (MLM), and a hybrid model (HM), which uses characteristic points predicted by a learning algorithm as input for the phenomenological model. The same amount of data was used to both fit the PM and train the MLM and HM. The models were analyzed and compared based on the accuracy of their predictions, development and computing time, and their ability to predict on interpolated and extrapolated inputs. The results revealed that for the same amount of experimental data, the MLM was more accurate than the PM. In addition, the MLM was better able to capture the characteristic peak stress in the TNM-B1 the flow curves, and could be developed and computed faster. Furthermore, the MLM was able to make realistic predictions for inputs outside the experimental data used for training. The HM showed comparable accuracy to the PM for the experimental conditions. However, the HM was able to produce a better fit for input conditions outside the training data.
Structured materials can be a progressive alternative to commonly
used flat sheets. There is an enormous range of possibilities for
using structured sheet metals due to their better stability. However, the effective use of these materials as well as their implementation in production requires precise knowledge about specific properties of structured sheet metals. The aim of this work is to obtain new knowledge about stiffness and stability during the deformation of this material. The structured sheet metals were investigated by means of buckling tests. The steel type investigated is a commonly used deep-drawing steel DC04. Six types of structure
arrangements were compared to non-structured (flat) specimens
as a reference. The influence of the type of structure arrangement
as well as the deformation speed on the mechanical properties
was investigated.
The osteoarthritis and degenerative diseases osteoporosis as well as trauma lead to the bone mechanical properties degradation due to absence of normal biological self healing processes or excessive loading [1–5]. These problems solution are artificial biomaterials, as surgical implantation of appropriate shapes helps restore function for the otherwise functionally compromised structures [1–5]. Biocompatibility is considered to be optimal once tissue neoformation and later function occurs around implantable devices [6]. The efficacy of biomaterials implants is determined mostly by their surface characteristics such as microstructure, surface morphology, composition and biological properties [2]. Aiming to develop alloys with better properties for orthopedic applications, the focus of the present research was to evaluate the effect of Zr at. % content on structural, mechanical and tribological properties of hot isostatically pressed Ti-25Nb-xZr (x = 5, 10, 15, 20 and 25 at. %) alloys. The structural evolution, and mechanical properties of the nanostructured Ti-Nb-xZr alloys were evaluated using X-Ray diffraction, scanning electron microscope. The mechanical properties were performed using Vickers hardness and berkovich nanoindentation. Experimental results indicated that the structural evolution and morphological changes of the milled alloys were sensitive to their Zirconium (at. %) content. The morphological characterization showed that the crystallite size and the particle size decreased with increasing Zr content (at. %). As well, as the Zr was added to the Ti-25NbXZr system, there was a clear decrease in the Vickers hardness and young’s modulus. On the other hand, the coefficient of friction and wear rates were found to be decreasing with increasing Zr content.
In special cases of angle beam ultrasonic measurement – e.g. defect detection in hot solids as well as flow measurement of liquid gases or energy storage mediums [1] – the applied transducer has to withstand extreme temperatures. Since the irradiation angle into the specific material is determined not only by wedge design, but also by the speed of sound in both the wedge material and the tested object, the developer must take into account the speed of the wave propagation in a wedge material over the whole temperature range of transducers application.
In this study we investigate the temperature dependence of the speed of longitudinal wave propagation in 10 different materials in the range from -200 °C to 400 °C. The investigated materials belong to different material classes (ceramics, glass, as well as ferrous and non-ferrous metals) and are all temperature-resistant up to at least 600 °C, and therefore applicable as wedge materials in an ultrasonic transducer for use at extreme temperatures.
Study of the photocatalytic degradation of Orange methyl dye in the presence of titanium dioxide
(2019)
The use of photocatalytic techniques for water purification and
wastewater treatment is very widespread, in our work we used
TiO2 to photocatalyrate orange methyl (MO). In addition, the
effects of some parameters on photodegradation of MO have
been studied, such as the presence and / or absence of light
(UV). The use of TiO2 showed a high MO degradation
efficiency of up to 98%. The presence of H2O2 in the
photocatalytic reaction may favor the photocatalytic
degradation efficiencies. In addition, the experimental results
have demonstrated an excellent rate of the order of 99%.
In this paper the relationship between surface energy and flexural strength of metal laminate made by reinforcing glass fibre reinforced polymer on steel surfaces was investigated. Sand blasting was performed on 22MnB5 steel surface. This steel was stacked together with layers of unidirectional glass/polyamide-6 prepreg, followed by pressing in a hot press. Influenced parameters are pressure, temperature and time. 3D profilometer analysis was used to investigate the roughness profile on the surface of the steel generated by the sand blasting. The surface energy of the steel surface was calculated from a set of contact angles measured by three different liquids. To identify the optimal surface treatment, the variation of surface energy, flexural strength and roughness of the steel surface was determined as function of the surface treatment. Surface roughness (Ra of 1.08 μm), results indicate that increasing surface roughness leads to improvement in flexural modulus. The increase further leads to decrease in flexural modulus. In addition, the influence of surface energy and flexural strength on the impact damage behaviour was investigated too. The results showed that the sample with highest flexural modulus had the lowest impact-induced damage area.
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.
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.
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.
Hexavalent chromium pollution from industrial waste water is a serious problem as it can cause adverse effects on the environment. Several methods are used to reduce the harmful effects of this pollutant, especially physico-chemical methods, such as adsorption technology. The present study aims to remove Cr (VI) from industrial sources in a fixed-bed column of activated carbon. The experiments were carried out at natural pH and temperature with a flow rate (5, 10, and 20 mL/min) and bed height (3.5 cm). Breakthrough curves for feed concentrations (0.01, 0.03, and 0.05 mol/L) were investigated. The results indicated a marked decrease up to 99%. The value of the flow constant for the Thomas model decreased with the increase in the concentration of the incoming substance, but increased with the increase in the flow rate.
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.
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.
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.
Mixing of steel and aluminum within the weld pool during keyhole laser welding results in a complex dissimilar microstructure, which in turn, initiates a shift in weld metal mechanical properties. In this study, a numerical model for computation of distortions in laser-welded dissimilar overlap joints (austenitic stainless steel 304 – 6082-T6 aluminum alloy), which considers properties of the mixed steel-aluminum weld metal was developed. The required yield strength, Young's modulus, and strain hardening exponent of the weld metal were experimentally determined using the indentation technique coupled with energy-dispersive X-ray spectroscopy. The designed material model calculates the weld elastic-plastic properties as a function of the aluminum concentration. The softening of the alloys in the heat-affected zone was determined by physical simulations and considered as a function of maximum temperature. Computed and measured distortions showed good agreement for various welding regimes with an average deviation of 18.4%. The sensitivity analyses indicated that the application of the developed weld material model significantly improves the accuracy of the thermomechanical simulations.
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.
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.
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.