Structural evolution during mechanical milling and subsequent annealing of Cu–Ni–Al–Co–Cr–Fe–Ti alloys

This study reports the structural evolution of high-entropy alloys from elemental materials to amorphous phases during mechanical alloying, and further, to equilibrium phases during subsequent thermal annealing. Four alloys from quaternary Cu_0.5NiAlCo to septenary Cu_0.5NiAlCoCrFeTi were analyzed. Microstructure examinations reveal that during mechanical alloying, Cu and Ni first formed a solid solution, and then other elements gradually dissolved into the solid solution which was finally transformed into amorphous structures after prolonged milling. During thermal annealing, recovery of the amorphous powders begins at 100 °C, crystallization occurs at 250–280 °C, and precipitation and grain growth of equilibrium phases occur at higher temperatures. The glass transition temperature usually observed in bulk amorphous alloys was not observed in the present amorphous phases. These structural evolution reveal three physical significances for high-entropy alloys: (1) the annealed state of amorphous powders produces simple equilibrium solid solution phases instead of complex phases, confirming the high-entropy effect; (2) amorphization caused by mechanical milling still meets the minimum criterion for amorphization based on topological instability proposed by Egami; and (3) the nonexistence of a glass transition temperature suggests that Inoue's rules for bulk amorphous alloys are still crucial for the existence of glass transition for a high-entropy amorphous alloy.     

Joining of zirconia to metal with Cu–Ga–Ti and Cu–Sn–Pb–Ti fillers

The method of brazing by capillary impregnation of Cu–Ga melt through a titanium powder layer situated between brazed details is elaborated. Samples of ZrO₂ ceramic/metal brazed joints using Cu–Ga–Ti filler and Cu–Sn–Pb–Ti filler were fabricated. The joints’ shear strength was 277±37 MPa for the Cu–Ga–Ti and 156±25 MPa for the Cu–Sn–Pb–Ti.     

Solidification microstructures and mechanical properties of high-vanadium Fe–C–V and Fe–C–V–Si alloys

Fe–C–V and Fe–C–V–Si alloys of various C, V and Si compositions were investigated in this work. It was found that the phases present in both of these alloy systems were alloyed ferrite, alloyed cementite, and VC_x carbides. Depending on the alloy composition the solidified microstructural constituents were granular pearlite-like, lamellar pearlite, or mixtures of alloyed ferrite + granular pearlite-like or granular pearlite-like + lamellar pearlite. In addition, it is shown that in Fe–C–V alloys the C/V ratio influences (a) the type of matrix, (b) the fraction of vanadium carbides, f_v and (c) the eutectic cell count, N_F. In Fe–C–V alloys, a relationship between the alloy content corresponding to the eutectic line was experimentally determined and can be described by where C_e and V_e are the carbon and vanadium composition of the eutectic. Moreover, in the Fe–C–V alloys (depending on the alloy chemistry), the primary VC_x carbides crystallize with non-faceted or non-faceted/faceted interfaces, while the eutectic morphology is non-faceted/non-faceted with regular fiber-like structures, or it possesses a dual morphology (non-faceted/non-faceted with regular fiber-like structures + non-faceted/faceted with complex regular structures). In the Fe–C–V–Si system, the primary VC_x carbides solidify with a non-faceted/faceted interface, while the eutectic is non-faceted/faceted with complex regular structures. In particular, spiral eutectic growth is observed when Si is present in the Fe–C–V alloys. In general, it is found that as the matrix constituent shifts from predominantly ferrite to lamellar pearlite, the hardness, yield and tensile strengths exhibit substantial increases at expenses of ductility. Moreover, Si additions lead to alloy strengthening by solid solution hardening of the ferrite phase and/or through a reduction in the eutectic fiber spacings with a decrease in the alloy ductility.     

Preparation and mechanical properties of a new Zr–Al–Ti–Cu–Ni–Be bulk metallic glass

In this paper, a new Zr₃₇Al₁₀Ti_12.5Cu_11.25Ni₉Be_20.25 bulk metallic glass is reported. The present alloy was prepared by water quenching in a silica tube of φ10×85 mm. The amorphicity of the quenched bulk samples was examined using X-ray diffraction analysis and optical microscopy. The thermal stability was evaluated by differential scanning calorimetry (DSC) at a heating rate of 10 K/min. The characteristic data of the bulk metallic glass are presented, including glass transition temperature (T_g) and crystallization temperature (T_x). Results show that the present alloy exhibits large glass forming ability. For comparison with the well-known Zr–Ti–Cu–Ni–Be metallic glass, it was found that aluminum has a little effect on the vitrification of the present alloy but influences physical properties. Specifically, Al enhances the Young's modulus by 21.4% and Vickers hardness by 20% and reduces density by 7.2%.     

Thermomechanical processing of Ti–5Al–5Mo–5V–3Cr

The constitutive behaviour and microstructural evolution of the near-β alloy Ti–5Al–5Mo–5V–3Cr in the α + β condition has been characterised during isothermal subtransus forging at a range of temperatures and strain rates. The results indicate that Ti–5Al–5Mo–5V–3Cr has a shallower approach curve, and therefore, offers a more controllable microstructure than the near-β alloy Ti–10V–2Fe–3Al. Flow softening is small in magnitude in both alloys in the α + β condition. The steady state flow stresses obey a Norton–Hoff constitutive law with an activation energy of Q = 183 kJ mol⁻¹, which is similar to the activation energy for self-diffusion in the β phase, suggesting deformation is dominated by dynamic recovery in the β matrix. Good evidence is found for the existence of ω phase after both air cooling and water quenching from above the β transus. In addition, dissolution of the α phase is found to be slow at near-transus temperatures.     

SiNx-Submikrometerschichten – Parameteroptimierung –

SiN_x-submicrometer coatings – Optimization of the film properties – The influence of the deposition conditions on the properties of SiN_x-coatings was investigated. The characterized SiN_x-coatings were deposited by the help of reactive magnetron sputtering. Gas pressure and film thickness were varied. Scanning electron microscopic views of the cross sections show a columnar structure varying with the deposition parameters. The different structures are comparable to the known structure zone models. There is a transition from dense structures to open columnar structures with increasing gas pressure. The Microstructure of coatings also changes with increasing film thickness. Especially deposition conditions promoting shadowing effects lead to a large growth of the column diameter with increasing thickness. The intrinsic stresses and the ultramicrohardness of the coatings change with changing gas pressure, too. Dense structures have high intrinsic stresses and a high hardness while coarse columnar structures have low intrinsic stresses and a low hardness. The influence of the deposition parameters on wear behaviour and adhesion of the SiN_x-coatings was investigated by cavitation tests. Dense coatings with high intrinsic stresses show adhesion failures, and coatings with lower stresses and coarse columnar structures fail because of their lower intrinsic stability. Thus, there is an optimum gas pressure, at which the best properties are reached. It can be shown that with decreasing film thickness adhesion increases.     

Phase diagram calculation and experimental research on Fe–12Cr–B–Al–alloys

The vertical sections of Fe–12%Cr–B–xAl–C system with different aluminum contents have been calculated by use of Thermo‐Calc software and the influence of aluminum content on the phase regions and the parameters of eutectic point have been analyzed. Fe–12.0%Cr–1.0%B–2.0%Al–0.3%C and Fe–12.0%Cr–1.0%B–4.0%Al–0.3%C alloy were chosen to be studied by experiment. The phase transition temperatures were measured by differential scanning calorimetry and the microstructure and the phase type was detected by scanning electrone microscope‐energy dispersive X‐ray spectroscopy and X‐ray diffraction. The results indicate that calculated phase diagrams agree well with the experimental results and further prove the thermodynamics database of Thermo‐Calc software is reliable and it can be used to help design the alloy composition and heat treatment process.     

Aging behaviour of Al–Cu–Mg alloy–SiC composites

The age-hardening kinetics of powder metallurgy processed Al–Cu–Mg alloy and composites with 5, 15 or 25 vol.% SiC reinforcements, subjected to solution treatment at 495 °C for 0.5 h or at 504 °C for 4 h followed by aging at 191 °C, have been studied. The Al–SiC interfaces in composites show undissolved, coarse intermetallic precipitates rich in Cu, Fe, and Mg, with its extent varying with processing conditions. Examination of aging kinetics indicates that the peak-age hardness values are higher, and the time taken for peak aging is an hour longer on solutionizing at 504 °C for 4 h, due to greater solute dissolution. Contrary to the accepted view, the composites have taken longer time to peak-age than the alloy, probably due to lower vacancy concentration, large-scale interfacial segregation of alloying elements, and inadequate density of dislocations in matrix. The composite with 5 vol.% SiC with the lowest inter-particle spacing has shown the highest hardness.     

Design and deformation behavior of high strength Fe–Mn–Al–Cr–C duplex steel

The influence of cold rolling reduction on microstructures and mechanical properties at room temperature of the duplex Fe–28Mn–7Al–5Cr–0.3C steel was investigated. In the Fe–28Mn–7Al alloy system, the duplex microstructure was obtained by lowering the carbon content to about 0.3 wt.%. The steel was austenito-ferritic with a low to moderate stacking fault energy. Two thermomechanical cycles were performed, which included cold rolling/annealing at 1100 °C, and cold rolling/annealing at 1100 °C/cold rolling/annealing at 1000 °C.The effects produced by cold rolling on the duplex steel were grain refinement and different strain-induced marks within the ferrite and austenite phases. They were easily observed within the austenite phase at a relatively smaller reduction than within the ferrite phase. Mechanical twinning plays a dominant role within the austenite phase during deformation at room temperature, resulting in extreme mechanical properties. No edge or longitudinal cracks were observed during cold rolling of the duplex steel.     

Ni–Zr–Ti–Si–Sn/Cu metallic glass composites prepared by magnetic compaction

Ni–Zr–Ti–Si–Sn/Cu metallic glass (BMG) composites were fabricated by magnetic compaction of powder mixtures. A considerable plastic deformation took place without apparent failure during the dynamic compaction even at room temperature and at a high strain rate. The BMG particles retained their amorphous phase after the dynamic magnetic compaction at 450 °C. The resulting Ni_52.65Zr_28.71Ti_13.57Si_1.33Sn_3.74/60% Cu composite exhibited a remarkable tensile ductility at room temperature combined with high strength: tensile elongation of 28% and ultimate tensile stress up to 1.1 GPa.     

Macromechanics study of stable fatigue crack growth in Al–Cu–Li–Mg–Ag alloy

This study was made on a fresh variety of Al–Li base alloy to investigate the role of ageing precipitates and microstructure dimensions in the fatigue crack growth resistance. The fatigue crack growth rate was measured in three different states of the material (i.e. base metal in T8 condition, friction stir weld and laser beam weld in full‐aged condition). Metallurgical analysis showed that the base metal in T8 temper is precipitation hardened by an equivalent amount of δ′ (AL₃Li), T₁ (AI₂CuLi) and θ′ (AI₂Cu) precipitates. The friction stir weld retained the morphology of strengthening precipitate; however, coarsening of Cu containing precipitates has occurred. On the other hand, laser beam weld showed a different type of CuAl phase morphology, which is characteristic of cast metal. The results of fatigue tests confirmed that fatigue crack growth resistance largely depends on microstructural features, specifically the strengthening phases. The fatigue crack resistance was in the order of base metal > laser beam weldment > friction stir weldment. The CuAl phase played a vital role in the crack closure of the laser beam weldment, thus enhancing the fatigue life as compared with the friction stir weldment, which was evident from the plot between log of da/dN (crack growth in each cycle) and log of ΔK (stress intensity range).     

The microstructure and mechanical properties of prolonged and lower temperature aged Fe–Ni–Mn–Mo–Ti–Cr maraging steel

In this study, the microstructure and mechanical properties of Fe–Ni–Mn–Mo–Ti–Cr maraging steel at low temperature and prolonged aging condition were investigated. Optical and scanning electron microscopy examinations, tensile and hardness tests were conducted to study the microstructure, aging behavior and mechanical properties of the cold‐rolled steel. The results showed that aging of cold rolled Fe–Ni–Mn–Mo–Ti–Cr maraging steel resulted in the formation of Mo rich and Ti rich Lave phase precipitates. Existence of many dislocation cores due to cold rolling and subsequently, low temperature aging caused to formation of uniform distribution of very fine precipitates. The presence of these precipitates increased the yield and ultimate tensile strengths but couldn't improve the uniform tensile ductility. This alloy showed ultra‐high fracture stress of about 1950 MPa with a negligible tensile elongation (about 2 %) at the peak aged condition. The fractographic studies indicated this alloy shows semi‐brittle fracture in the subsequent aging treatment.     

Experimental studies on the dynamic tensile behavior of Ti–6Al–2Sn–2Zr–3Mo–1Cr–2Nb–Si alloy with Widmanstatten microstructure at elevated temperatures

The tensile behavior of a newly developed Ti–6Al–2Sn–2Zr–3Mo–1Cr–2Nb–Si alloy, referred as TC21, is investigated at temperatures ranging from 298 to 1023 K and under constant strain rate loadings ranging from 0.001 to 1270 s⁻¹. The results show that temperature and strain rate have significant effects on the tensile behavior of the material. At low strain rates of 0.001 and 0.05 s⁻¹, a discontinuity is found in the yield stress–temperature curve. And the discontinuity temperature increases with increasing strain rate. The analysis of temperature and strain rate dependence of unstable strain indicates a high-velocity-ductility phenomenon at elevated temperatures. Scanning electron microscope (SEM) analysis shows that the material is broken in a mixture manner of ductile fracture and intergranular fracture under low strain rates at room temperature, while the fracture manner changes to totally ductile fracture under other testing conditions. The width and depth of ductile dimples increase with increasing temperature. No adiabatic shear band is found in the tensile deformation of the material.