Precipitation Hardening at Elevated Temperatures above 400 °C and Subsequent Natural Age Hardening of Commercial Al–Si–Cu Alloy

The precipitation of intermetallic phases and the associated hardening by artificial aging treatments at elevated temperatures above 400 °C were systematically investigated in the commercially available AC2B alloy with a nominal composition of Al–6Si–3Cu (mass%). The natural age hardening of the artificially aged samples at various temperatures was also examined. A slight increase in hardness (approximately 5 HV) of the AC2B alloy was observed at an elevated temperature of 480 °C. The hardness change is attributed to the precipitation of metastable phases associated with the α-Al₁₅(Fe, Mn)₃Si₂ phase containing a large amount of impurity elements (Fe and Mn). At a lower temperature of 400 °C, a slight artificial-age hardening appeared. Subsequently, the hardness decreased moderately. This phenomenon was attributed to the precipitation of stable θ-Al₂Cu and Q-Al₄Cu₂Mg₈Si₆ phases and their coarsening after a long duration. The precipitation sequence was rationalized by thermodynamic calculations for the Al–Si–Cu–Fe–Mn–Mg system. The natural age-hardening behavior significantly varied depending on the prior artificial aging temperatures ranging from 400 °C to 500 °C. The natural age-hardening was found to strongly depend on the solute contents of Cu and Si in the Al matrix. This study provides fundamental insights into controlling the strength level of commercial Al–Si–Cu cast alloys with impurity elements using the cooling process after solution treatment at elevated temperatures above 400 °C.     

Structure and Properties of Heat-Resistant Alloys NiAl–Cr–Co–X (X = La,Mo, Zr,Ta, Re) and Fabrication of Powders for Additive Manufacturing

The NiAl–Cr–Co–X alloys were produced by centrifugal self-propagating high-temperature synthesis (SHS) casting. The effects of dopants X = La, Mo, Zr, Ta, and Re on combustion, as well as the phase composition, structure, and properties of the resulting cast alloys, have been studied. The greatest improvement in overall properties was achieved when the alloys were co-doped with 15% Mo and 1.5% Re. By forming a ductile matrix, molybdenum enhanced strength characteristics up to the values σ_ucs = 1604 ± 80 MPa, σ_ys = 1520 ± 80 MPa, and ε_pd = 0.79%, while annealing at T = 1250 ℃ and t = 180 min improved strength characteristics to the following level: σ_ucs = 1800 ± 80 MPa, σ_ys = 1670 ± 80 MPa, and ε_pd = 1.58%. Rhenium modified the structure of the alloy and further improved its properties. The mechanical properties of the NiAl, ZrNi₅, Ni_0.92Ta_0.08, (Al,Ta)Ni₃, and Al(Re,Ni)₃ phases were determined by nanoindentation. The three-level hierarchical structure of the NiAl–Cr–Co+15%Mo alloy was identified. The optimal plasma treatment regime was identified, and narrow-fraction powders (fraction 8–27 µm) characterized by 95% degree of spheroidization and the content of nanosized fraction <5% were obtained.     

Effects of Sc and Zr Addition on Microstructure and Mechanical Properties of AA5182

The effects of 0.1 wt.% Sc and 0.1 wt.% Zr addition in AA5182 on microstructure and mechanical properties were investigated. Results show that Al₃(Sc_xZr_1−x) dispersoids formed in AA5182. Observation of ingots microstructures showed that the grain size of 5182-Sc-Zr alloy was 56% lower than that of based AA5182. Isothermal annealing between 230 °C and 500 °C for 2 h was performed to study the recrystallization, tensile properties and dispersoid coarsening. The recrystallization was inhibited by the dispersoids, and the alloy microstructure remained deformed after annealing. Al₃(Sc_xZr_1−x) in AA5182 was stable when annealing below 400 °C, while parts of dispersoids coarsened significantly when heating at 500 °C. The addition of Sc and Zr allowed YS of 5182 alloy to achieve 247.8 MPa, which is 100 MPa higher than the corresponding AA5182. The contributions of Orowan strengthening and grain boundary strengthening were obtained by calculation.     

Microstructure,Micro-Mechanical and Tribocorrosion Behavior of Oxygen Hardened Ti–13Nb–13Zr Alloy

In the present work, an oxygen hardening of near-β phase Ti–13Nb–13Zr alloy in plasma glow discharge at 700–1000 °C was studied. The influence of the surface treatment on the alloy microstructure, tribological and micromechanical properties, and corrosion resistance is presented. A strong influence of the treatment on the hardened zone thickness, refinement of the α’ laths and grain size of the bulk alloy were found. The outer hardened zone contained mainly an oxygen-rich Ti α’ (O) solid solution. The microhardness and elastic modulus of the hardened zone decreased with increasing hardening temperature. The hardened zone thickness, size of the α’ laths, and grain size of the bulk alloy increased with increasing treatment temperature. The wear resistance of the alloy oxygen-hardened at 1000 °C was about two hundred times, and at 700 °C, even five hundred times greater than that of the base alloy. Oxygen hardening also slightly improved the corrosion resistance. Tribocorrosion tests revealed that the alloy hardened at 700 °C was wear-resistant in a corrosive environment, and when the friction process was completed, the passive film was quickly restored. The results show that glow discharge plasma oxidation is a simple and effective method to enhance the micromechanical and tribological performance of the Ti–13Nb–13Zr alloy.     

Heat Treatment of Cast and Cold Rolled Al–Yb and Al–Mn–Yb–Zr Alloys

The microstructure, electrical properties and microhardness of as-cast and cold rolled AlYb and AlMnYbZr alloys were investigated. The addition of Mn, Yb and Zr has a positive influence on grain size. A deformed structure of the grains with no changes of their size was observed after cold rolling. The Al₃Yb particles coherent with the matrix were observed in the AlYb alloys. The size of the particles was about 20 nm in the initial state; after isochronal treatment up to 540 °C the particles coarsen, and their number density was lower. The deformation has a massive effect on the microhardness behavior until treatment at 390 °C, after which the difference in microhardness changes between as-cast and cold rolled alloys disappeared. Relative resistivity changes show a large decrease in the temperature interval of 330–540 °C which is probably caused by a combination of recovery of dislocations and precipitation of the Al₃(Yb,Zr) particles. Precipitation hardening was observed between 100 and 450 °C in the AlYb alloy after ageing at 625 °C/24 h and between 330 and 570 °C in the AlMnYbZr alloy after ageing at 625 °C/24 h.     

Dissimilar Brazing of Ti–15Mo–5Zr–3Al and Commercially Pure Titanium Using Ti–Cu–Ni Foil

Dissimilar brazing of Ti–15Mo–5Zr–3Al (Ti-1553) to commercially pure titanium (CP-Ti) using Ti–15Cu–15Ni foil was performed in this work. The microstructures in different sites of the brazed joint showed distinct morphologies, which resulted from the distributions of Mo, Cu, and Ni. In the brazed zone adhered to the Ti-1553 substrate, the partitioning of Mo from the Ti-1553 into the molten braze caused the formation of stabilized β-Ti without Ti₂Cu/Ti₂Ni precipitates. In the CP-Ti side, the brazed joint displayed a predominantly lamellar structure, composed of the elongated primary α-Ti and β-transformed eutectoid. The decrease in the Mo concentration in the brazed zone caused the eutectoid transformation of β-Ti to Ti₂Cu + α-Ti in that zone. The diffusion of Cu and Ni from the molten braze into the CP-Ti accounted for the precipitation of Ti₂Cu/Ti₂Ni in the transformed zone therein. The variation in the shear strength of the joints was related to the amount and distribution of brittle Ti₂Ni compounds. Prolonging the brazing time, the wider transformed zone, consisting of coarse elongated CP-Ti interspersed with sparse Ti₂Ni precipitates, was responsible for the improved shear strength of the joint.     

Microstructural Variations in Laser Powder Bed Fused Al–15%Fe Alloy at Intermediate Temperatures

The samples of the Al–15Fe (mass%) binary alloy that were additively manufactured by laser powder bed fusion (L-PBF) were exposed to intermediate temperatures (300 and 500 °C), and the thermally induced variations in their microstructural characteristics were investigated. The L-PBF-manufactured sample was found to have a microstructure comprising a stable θ-Al₁₃Fe₄ phase localized around melt-pool boundaries and several spherical metastable Al₆Fe-phase particles surrounded by a nanoscale α-Al/Al₆Fe cellular structure in the melt pools. The morphology of the θ phase remained almost unchanged even after 1000 h of exposure at 300 °C. Moreover, the nanoscale α-Al/Al₆Fe cellular structure dissolved in the α-Al matrix; this was followed by the growth (and nucleation) of the spherical Al₆Fe-phase particles and the precipitation of the θ phase. Numerous equiaxed grains were formed in the α-Al matrix during the thermal exposure, which led to the formation of a relatively homogenous microstructure. The variations in these microstructural characteristics were more pronounced at the higher investigated temperature of 500 °C.     

Effect of Annealing Temperature on the Interfacial Microstructure and Bonding Strength of Cu/Al Clad Sheets with a Stainless Steel Interlayer

To explore the influence of annealing temperatures on the interfacial structure and peeling strength of Cu/Al clad sheets with a 304 stainless steel foil interlayer, an intermediate annealing treatment was performed at temperatures of 450 °C, 550 °C, and 600 °C, separately. The experimental results indicate that the interfacial atomic diffusion is significantly enhanced by increasing the intermediate annealing temperature. The average peeling strength of the clad sheets annealed at 550 °C can reach 34.3 N/mm and the crack propagation is along the steel/Cu interface, Cu-Al intermetallic compounds layer, and Al matrix. However, after high-temperature annealing treatment (600 °C), the liquid phase is formed at the bonding interface and the clear Cu/steel/Al interface is replaced by the chaotic composite interfaces. The clad sheet broke completely in the unduly thick intermetallic compounds layer, resulting in a sharp decrease in the interfacial bonding strength.     

Effect of Post-Fabricated Aging on Microstructure and Mechanical Properties in Underwater Friction Stir Additive Manufacturing of Al–Zn–Mg–Cu Alloy

The fabricated Al–Zn–Mg–Cu alloy build has low mechanical properties due to the dissolution of strengthening precipitates back into the matrix during friction stir additive manufacturing (FSAM). Post-fabricated aging was considered an effective approach to improve the mechanical performance of the build. In this study, various post-fabricated aging treatments were applied in the underwater FSAM of Al–7.5 Zn–1.85 Mg–1.3 Cu–0.135 Zr alloy. The effect of the post-fabricated aging on the microstructure, microhardness, and local tensile properties of the build was investigated. The results indicated that over-aging occurred in the low hardness zone (LHZ) of the build after artificial aging at 120 °C for 24 h as the high density of grain boundaries, subgrain boundaries, dislocations, and Al₃Zr particles facilitated the precipitation. Low-temperature aging treatment can effectively avoid the over-aging problem. After aging at 100 °C for 48 h, the average microhardness value of the build reached 178 HV; the yield strength of the LHZ and high hardness zone (HHZ) was 453 MPa and 463 MPa, respectively; and the ultimate tensile strength of the LHZ and HHZ increased to 504 MPa and 523 MPa, respectively.     

Drop–Dry Deposition of Ni(OH)2 Precursors for Fabrication of NiO Thin Films

Drop–dry deposition (DDD) is a method of depositing thin films by heating and drying the deposition solution dropped on a substrate. We prepared Ni(OH)₂ precursor thin films by DDD and annealed them in air to prepare NiO thin films. The appropriate deposition conditions were found by changing the number of drop–dry cycles and the concentrations of chemicals in the solution, and the Ni(OH)₂ precursor film with a thickness of 0.3 μm and optical transmittance of more than 95% was successfully deposited. Raman and X-ray diffraction measurements were performed, and it was found that the NiO film was successfully fabricated after annealing at 400 °C. The p-type conductivity of the annealed film was confirmed by photoelectrochemical measurements. In addition, we prepared n-type ZnO by electrochemical deposition on NiO thin films. The current–voltage measurement results show that the ZnO/NiO heterojunction had rectification properties.     

Effect of Two-Stage Cooling on the Microstructure and Tribological Properties of Steel–Copper Bimetals

In this paper, the solid–liquid composite method is used to prepare the steel–copper bimetal sample through two-stage cooling process (forced air cooling and oil cooling). The relationship between the different microstructures and friction properties of the bimetal copper layer is clarified. The results show that: the friction and wear parameters are 250 N, the speed is 1500 r/min (3.86 m/s), the friction coefficient fluctuates in the range of 0.06–0.1, and the lowest point is 0.06 at 700 °C. The microstructure of the copper layer was α-Cu, δ, Cu₃P, and Pb phases, and Pb was free between α-Cu dendrites. When the solidification temperature is 900 °C, the secondary dendrite of α-Cu develops. With the decrease temperature, the growth of primary and secondary dendrites gradually tends to balance at 700 °C. During the wear process, Pb forms a self-lubricating film uniformly distributed on the surface of α-Cu, and the Cu₃P and δ phases are distributed in the wear mark to increase α-Cu wear resistance.     

Nickel Oxide Films Deposited by Sol-Gel Method: Effect of Annealing Temperature on Structural,Optical, and Electrical Properties

In our study, transparent and conductive films of NiO_x were successfully deposited by sol-gel technology. NiO_x films were obtained by spin coating on glass and Si substrates. The vibrational, optical, and electrical properties were studied as a function of the annealing temperatures from 200 to 500 °C. X-ray Photoelectron (XPS) spectroscopy revealed that NiO was formed at the annealing temperature of 400 °C and showed the presence of Ni⁺ states. The optical transparency of the films reached 90% in the visible range for 200 °C treated samples, and it was reduced to 76–78% after high-temperature annealing at 500 °C. The optical band gap of NiOx films was decreased with thermal treatments and the values were in the range of 3.92–3.68 eV. NiO_x thin films have good p-type electrical conductivity with a specific resistivity of about 4.8 × 10⁻³ Ω·cm. This makes these layers suitable for use as wideband semiconductors and as a hole transport layer (HTL) in transparent solar cells.     

Solution Synthesis of Cubic Spinel Mn–Ni–Cu–O Thermistor Powder

Toward the development of NTCR thermistors, nanocrystalline Mn–Ni–Cu–O powder was synthesized from a mixed chloride aqueous solution by a simple co-precipitation method.The introduction of an oxidizing agent (H₂O₂) into the solution led to the partial oxidation of Mn²⁺ ions into Mn³⁺ ions, which enabled the collected powder to be well crystallized at 650 °C. Such a low calcining temperature resulted in fine particles with a mean size of 60 nm, which significantly promoted densification of the resulting ceramics. As a result, a dense and homogenous microstructure with a relative density up to 97.2% was achieved for pellets sintered at 1100 °C. Furthermore, these sintered ceramics exhibited a room temperature resistivity (ρ₂₅) of 67 Ω·cmand a thermistor constant (B_25/85) of 2843 K, which make them suitable for use in industrial thermistors. In addition, electrical stability was greatly improved when the ceramics were prepared by a new two-step sintering method. The results suggest that the co-precipitation route with the introduction of H₂O₂ is suitable for the fabrication of cubic spinel thermistor nanopowders.     

Effect of Ti Content on the Microstructure and High-Temperature Creep Property of Cast Fe-Ni-Based Alloys with High-Al Content

The cast Fe-Ni-based austenitic heat-resistant alloys with 4.5 wt% Al and varying Ti content were developed for high-temperature application. With increase in Ti content, strength of model alloys increased gradually at 700 °C and 750 °C. At 750 °C, alloys with 35Ni–(2~4)Ti composition showed a significant increase in creep rupture life compared to 30Ni–1Ti alloy, attributed to the increase in γ’-Ni₃(Al,Ti) precipitates due to higher Ni and Ti content. Among the 35Ni–(2~4)Ti alloys, increasing Ti content from 2 to 4 wt% gradually increased the creep rupture life in the as-cast condition. The creep rupture life was improved after solution annealing treatment, however, the beneficial effect of higher Ti content was not evident for 35Ni–(2~4)Ti alloys. After solution annealing, interdendritic phases were partially dissolved, but coarse B2-NiAl phases were formed. The size and amount of coarse B2-NiAl phases increased with Ti content. In the creep-tested specimens, creep void nucleation and crack propagation were observed along the coarse B2-NiAl phases, especially for high-Ti alloys. Therefore, the beneficial effect of the increase in γ’-Ni₃(Al,Ti) precipitates for high-Ti alloys on creep property was limited due to the detrimental effect of the presence of coarse B2-NiAl phases.     

The Formation of 14H-LPSO in Mg–9Gd–2Y–2Zn–0.5Zr Alloy during Heat Treatment

There is a new long-period stacking ordered structure in Mg–RE–Zn magnesium alloys, namely the LPSO phase, which can effectively improve the yield strength, elongation, and corrosion resistance of Mg alloys. According to different types of Mg–RE–Zn alloy systems, two transformation modes are involved in the heat treatment transformation process. The first is the alloy without LPSO phase in the as-cast alloy, and the Mg_xRE phase changes to 14H-LPSO phase. The second is the alloy containing LPSO phase in the as-cast state, and the 14H-LPSO phase is obtained by the transformations of 6H, 18R, and 24R. The effects of different solution parameters on the second phase of Mg–9Gd–2Y–2Zn–0.5Zr alloy were studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The precipitation mechanism of 14H-LPSO phase during solution treatment was further clarified. At a solution time of 13 h, the grain size increased rapidly initially and then decreased slightly with increasing solution temperature. The analysis of the volume fraction of the second phase and lattice constant showed that Gd and Y elements in the alloy precipitated from the matrix and formed 14H-LPSO phase after solution treatment at 490 °C for 13 h. At this time, the hardness of the alloy reached the maximum of 74.6 HV. After solution treatment at 500 °C for 13 h, the solid solution degree of the alloy increases, and the grain size and hardness of the alloy remain basically unchanged.     

In Situ Observation of the Tensile Deformation and Fracture Behavior of Ti–5Al–5Mo–5V–1Cr–1Fe Alloy with Different Microstructures

The plastic deformation processes and fracture behavior of a Ti–5Al–5Mo–5V–1Cr–1Fe alloy with bimodal and lamellar microstructures were studied by room-temperature tensile tests with in situ scanning electron microscopy (SEM) observations. The results indicate that a bimodal microstructure has a lower strength but higher ductility than a lamellar microstructure. For the bimodal microstructure, parallel, deep slip bands (SBs) are first noticed in the primary α (α_p) phase lying at an angle of about 45° to the direction of the applied tension, while they are first observed in the coarse lath α (α_L) phase or its interface at grain boundaries (GBs) for the lamellar microstructure. The β matrix undergoes larger plastic deformation than the α_L phase in the bimodal microstructure before fracture. Microcracks are prone to nucleate at the α_p/β interface and interconnect, finally causing the fracture of the bimodal microstructure. The plastic deformation is mainly restricted to within the coarse α_L phase at GBs, which promotes the formation of microcracks and the intergranular fracture of the lamellar microstructure.     

Effect of Fabrication Technique on the Microgap of CAD/CAM Cobalt–Chrome and Zirconia Abutments on a Conical Connection Implant: An In Vitro Study

The aim of this in vitro study was to investigate the microgaps at the implant–abutment interface when zirconia (Zr) and CAD/CAM or cast Co–Cr abutments were used. Methods: Sixty-four conical connection implants and their abutments were divided into four groups (Co–Cr (milled, laser-sintered and castable) and Zirconia (milled)). After chewing simulation (300,000 cycles, under 200 N loads at 2 Hz at a 30° angle) and thermocycling (10,000 cycles, 5 to 50 °C, dwelling time 55 s), the implant–abutment microgap was measured 14 times at each of the four anatomical aspects on each specimen by using a scanning electron microscope (SEM). Kruskal–Wallis and pair-wise comparison were used to analyze the data (α = 0.05). Results: The SEM analysis revealed smaller microgaps with Co–Cr milled abutments (0.69–8.39 μm) followed by Zr abutments (0.12–6.57 μm), Co–Cr sintered (7.31–25.7 μm) and cast Co–Cr (1.68–85.97 μm). Statistically significant differences were found between milled and cast Co–Cr, milled and laser-sintered Co–Cr, and between Zr and cast and laser-sintered Co–Cr (p < 0.05). Conclusions: The material and the abutment fabrication technique affected the implant–abutment microgap magnitude. The Zr and the milled Co–Cr presented smaller microgaps. Although the CAD/CAM abutments presented the most favorable values, all tested groups had microgaps within a range of 10 to 150 μm.     

Improving the Mechanical Response of Al–Mg–Si 6082 Structural Alloys during High-Temperature Exposure through Dispersoid Strengthening

The feasibility and efficacy of improving the mechanical response of Al–Mg–Si 6082 structural alloys during high temperature exposure through the incorporation of a high number of α-dispersoids in the aluminum matrix were investigated. The mechanical response of the alloys was characterized based on the instantaneous high-temperature and residual room-temperature strengths during and after isothermal exposure at various temperatures and durations. When exposed to 200 °C, the yield strength (YS) of the alloys was largely governed by β” precipitates. At 300 °C, β” transformed into coarse β’, thereby leading to the degradation of the instantaneous and residual YSs of the alloys. The strength improvement by the fine and dense dispersoids became evident owing to their complementary strengthening effect. At higher exposure temperatures (350–450 °C), the further improvement of the mechanical response became much more pronounced for the alloy containing fine and dense dispersoids. Its instantaneous YS was improved by 150–180% relative to the base alloy free of dispersoids, and the residual YS was raised by 140% after being exposed to 400–450 °C for 2 h. The results demonstrate that introducing thermally stable dispersoids is a cost-effective and promising approach for improving the mechanical response of aluminum structures during high temperature exposure.     

Microstructural and Mechanical Properties of Novel Co-Free Maraging Steel M789 Prepared by Additive Manufacturing

This research aims to characterize and examine the microstructure and mechanical properties of the newly developed M789 steel, applied in additive manufacturing. The data presented herein will bring about a broader understanding of the processing–microstructure–property–performance relationships in this material based on its chemical composition and heat treatment. Samples were printed using the laser powder bed fusion (LPBF) process and then the solution was annealed at 1000 °C for 1 h, followed by aging at 500 °C for soaking times of 3, 6 and 9 h. The AM components showed a relative density of 99.1%, which arose from processing with the following parameters: laser power of 200 W, laser speed of 340 mm/s, and hatch distance of 120 µm. Optical and electron microscopy observations revealed microstructural defects, typical for LPBF processes, like voids appearing between the melted pools of different sizes with round or creviced geometries, nonmelted powder particle formation inside such cavities, and small spherical porosity that was preferentially located between the molten pools. In addition, in heat-treated conditions, AM maraging steel has combined oxide inclusions of Ti and Al (TiO₂:Al₂O₃) that reside along the grain boundaries and secondary porosities; these may act as preferential zones for crack initiation and may increase the brittleness of the AM steel under aged conditions. Consequently, the elongation of the AM alloy was low (<3%) for both annealed and aged solution conditions. The tensile strength of AM M789 increased from 968 MPa (solution annealed) to 1500–1600 MPa after the aging process due to precipitation within the intermetallic η-phase. A tensile strength and yield point of 1607 ± 26 and 1617 ± 45 MPa were obtained, respectively, after a full heat treatment at 500 °C/6 h. The results show that 3 h aging of solution annealed AM M789 steel achieves satisfactory material properties in industrial practice. Extending the aging time of printed parts to 6 h yields slightly improved properties but may not be worth the effort, while long-term aging (9 h) was shown to even reduce quality.     

Effects of Zn Contents on Microstructure and Mechanical Properties of Semisolid Rheo-Diecasting Al-xZn-2Mg-1.5Cu Alloys

The microstructure and mechanical properties of semisolid rheo-diecasting Al-xZn-2Mg-1.5Cu alloys with different Zn contents were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), hardness testing (HV) and room temperature tensile testing. Results show that the as-cast microstructure mainly consists of spherical α-Al and Mg(Al, Cu, Zn)₂ phases. Furthermore, a small amounts of Al₇Cu₂Fe phases were also detected along the grain boundary. Increasing the Zn contents from 8–12%, the volume fraction of the Mg(Al, Cu, Zn)₂ phases increases from 4.9–7.4%. After solution heat treatment at 470 °C for 8 h, most of the Mg(Al, Cu, Zn)₂ dissolves into the α-Al matrix, while the Al₇Cu₂Fe phase keeps with remains. The yield strength linearly increases from 482 ± 5 MPa of 8% Zn to 529 ± 5 MPa of 12% Zn. While, the ultimate strength of 10% Zn is 584 ± 2 MPa, which is higher than that of the other two alloys. Moreover, the average elongation dramatically decreases from 13% for the 8% Zn alloy to 2% for the 12% Zn alloy.