Blended Elemental Powder Research Articles

Investigation of the Effect of Milling Time on Elemental Powders of Oxi‐Reduction Nickel and Hydrogenation–Dehydrogenation Titanium

Mechanical alloying (MA) is widely applied in the synthesis of blended elemental or prealloyed powders. This work evaluates the effect of milling time on elemental nickel and titanium powders produced by oxi‐reduction and the hydrogenation–dehydrogenation process, respectively. The powders are characterized by scanning electron microscopy, X‐ray diffraction, particle size, powder yield, and differential scanning calorimetry. It is observed that increasing the milling time promotes the formation of a structure composed of thin lamellae of nickel and titanium, which results in the beneficial effect of lowering the temperature for the formation of the intermetallic of the Ni–Ti system and in the powder yield achieved. The reduction of milling time in the MA process of NiTi alloys enhances technological efficiency by decreasing their overall processing time.

Mechanical energy absorption capacity of the porous Ti-6Al-4V alloy under quasi-static and dynamic compression

Porous materials are very efficient in absorbing mechanical energy in different applications. In the present study, porous materials based on the Ti-6(wt.%)Al-4V alloy were manufactured with the use of two different powder metallurgy methods: i) blended elemental powder approach using titanium hydride (TiH2) as well as V-Al master alloy powders and ii) using hydrogenated Ti-6-4 pre-alloyed powder. The powder compacts were sintered with additions of ammonium bicarbonate as a pore-holding removable agent. The emission of hydrogen from hydrogenated powders on vacuum sintering and the resulting shrinkage of powder particles permitted the control of the sintering process and creation of anticipated porous structures. Mechanical characteristics were evaluated under quasi-static and dynamic compressive loading conditions. Dynamic compression tests were performed using the direct impact Hopkinson pressure bar technique. All investigations aimed at characterizing the mechanical energy-absorbing ability of the obtained porous structures. The anticipated strength, plasticity, and energy-absorbing characteristics of porous Ti-6-4 material were evaluated, and the possibilities of their application were also discussed. Based on the obtained results, it was found that porous Ti-6-4 material produced with a blended elemental powder approach showed more promising energy absorption properties in comparison with pre-alloyed powder.

Microstructure, hardness, and creep of Co-Fe-Ni-based high-entropy superalloy processed by laser powder-bed fusion

A Co-Fe-Ni-based high-entropy superalloy (29Co-29Fe-29Ni-4.3Al-4.3Ti-4.3 V, at.%) designed to form a γ/γ′ microstructure was fabricated via laser powder-bed fusion, utilizing a blend of elemental powders. The hardness and microstructure were compared in terms of laser processing parameters, heat treatment conditions, and fabrication methods. Lower volumetric energy density (45 J/mm³) for fusion favor the formation of swirl-shaped, partially-mixed regions. The extent of elemental enrichment and depletion varies from region to region, even within the same sample. Upon direct aging of these inhomogeneous as-built samples, γ′ precipitates form along cell boundaries, which is attributed to strong segregation of Ni and Ti elements at these boundaries. After homogenization of the as-built samples, a uniform distribution of fine γ′ precipitates is achieved through aging. The hardness of a homogenized traditionally-cast sample is lower than that of an as-built sample, owing to differences in grain size. Nevertheless, both samples aged under the same conditions exhibited a similar level of hardness, attributed to strengthening by the γ′ phase.

Phase Composition of AlTiNbMoV, AlTiNbTaZr and AlTiNbMoCr Refractory Complex Concentrated Alloys: A Correlation of Predictions and Experiment

Designing complex concentrated alloys (CCA), also known as high entropy alloys (HEA), requires reliable and accessible thermodynamic predictions due to vast space of possible compositions. Numerous semiempirical parameters have been developed for phase predictions over the years. However, in this paper we show that none of these parameters is a robust indicator of phase content in various refractory CCA. CALPHAD proved to be a more powerful tool for phase predictions, however, the predictions face several limitations. AlTiNbMoV, AlTiNbTaZr and AlTiNbMoCr alloys were prepared using blended elemental powder metallurgy. Their phase and chemical composition were investigated by the means of scanning electron microscopy, energy-dispersive X-ray spectroscopy and X-ray diffraction. Apart from the minor contamination phases (Al2O3 and Ti(C,N,O)), AlTiNbMoV and AlTiNbMoCr exhibited single-phase solid solution microstructure at the homogenization temperature of 1400 °C, while Al3Zr5 based intermetallics were present in the AlTiNbTaZr alloy. None of the simple semiempirical parameter was able to predict phase content correctly in all three alloys. Predictions by CALPHAD (TCHEA4 database) were able to predict the phases with limited accuracy only. Critical limitation of the TCHEA4 database is that only binary and ternary phase diagrams are assessed and some more complex phases cannot be predicted.

Highly correlated deposition characteristics between individual elemental powders and elemental powder blends of MoNbTaTi in laser melt deposition

The laser melt deposition process often involves fabricating custom alloys from cost-effective elemental powder blends. However, discrepancies between the nominal ratio of the pre-mixed powders and the final composition of the deposited part are commonly observed due to variations in the material properties of the elemental powders. In this study, separate experiments were employed to investigate the relationship of deposition characteristics between individual elemental powders and elemental powder blends in the laser melt deposition process. To investigate the spatial distribution between elemental powder particles, powder flow characteristics in four different delivery systems were measured. Single-track deposition experiments were deployed to study the real powder catchment efficiency of elemental powder and the final composition of the deposited layer. In addition, a finite element model was established and validated with experimental data to predict the dilution rate and final chemical composition of the deposited layer. The experimental results indicate a strong correlation between the powder catchment efficiency of individual elemental powder and the final composition of the deposited layer. The simulation results agreed well with the actual composition of the deposited track. This study’s findings have the potential to predict and optimize the composition of the desired materials fabricated by elemental powder blends in the laser melt deposition process.

Laser directed energy deposition of Alnico-8H from blended elemental powders: Effect of nickel increase on magnetic properties

Alnico-8H (14 wt% Ni) and Alnico-8H (19 wt% Ni) were additively fabricated from a blend of elemental powders with compositions (in wt.%) of 38Co-29Fe-14Ni-8Al-8Ti-3Cu and 33Co-29Fe-19Ni-8Al-8Ti-3Cu, respectively, using laser-directed energy deposition technique. Post additive fabrication both compositions were subjected to homogenization heat treatment at 1250 °C for 30 min and magnetic annealed at 650 °C under 2.5 T magnetic field for 60 mins (1 hr). X-ray diffraction was employed for studying the phase evolution. Scanning and transmission electron microscopes were utilized for characterization of Alnico alloys. The targeted compositions for Alnico-8H (14 wt% Ni) and Alnico-8H (19 wt% Ni) were nearly achieved in the L-DED processed samples. homogenization at 1250 °C, followed by magnetic annealing at 650 °C, resulted in an increase in grain size. The transmission electron microscopy revealed the presence of ferromagnetic α1 and paramagnetic α2 phases in the magnetic annealed microstructure. The increase in Nickel content from 14 to 19 wt% resulted in increase in coercivity (242 to 255 Oe), remanence (4437 to 8659 G), and maximum energy product (BHmax) (0.27 to 0.53 MGOe).

Co–Ni–Al–W γ/γ′ superalloy with Cr and Ti additions fabricated via laser fusion of elemental powders

A Co-based superalloy (Co-0.20Ni-0.11Al-0.07W-0.04Cr-0.03Ti, mole fraction) was synthesized by laser powder-bed fusion of a blend of elemental powders. The as-built alloy shows a γ-FCC matrix where the high-melting Ti and Cr powders are fully dissolved, but the refractory W particles are only partially melted. Full dissolution of the W particles is achieved after homogenization at 1150 °C, resulting in a homogeneous, single-phase γ microstructure. Upon aging at 900 °C, a two-phase γ/γ′ microstructure forms, with a high-volume fraction of sub-micron γ′ precipitates with cuboidal shape. Compared to a control quaternary alloy without Cr and Ti fabricated by the same method, the present alloy has increased γ′ fraction and microhardness after aging for 300 h, maintaining a strong γ′ strengthening effect without forming γ′-depleted zone at grain boundaries. Micrometer-size γ′-precipitates at grain boundaries also shift the transition between diffusional and dislocation creep to lower stress levels, by inhibiting diffusional creep and grain-boundary sliding. However, overall creep resistance is lowered, consistent with a reduction of lattice mismatch due to Cr additions and rafting of γ′ precipitates. Furthermore, Cr and Ti additions improve oxidation resistance at 900 °C, due to the formation of a continuous Cr-, Ti- and Al-rich oxide layer.

Thermokinetics driven microstructure and phase evolution in laser-based additive manufacturing of Ti-25wt.%Nb and its performance in physiological solution

A bio-compatible Ti-25 wt% Nb alloy fabricated from a blend of pure elemental powders using laser powder bed fusion additive manufacturing technique. The present work investigated the effects of processing conditions on the evolution of microstructures and its consequential material attributes, such as mechanical properties and corrosion performance. Thermal management strategies comprising laser powers of 200 W and 300 W in complement with a shorter scan length (1 mm) and substrate preheating above β-transus temperature (1123 K) were considered to achieve complete dissolution of niobium particles. The microstructure in the 200 W sample showed thin α′′ martensite needles in β matrix while martensite laths in the 300 W condition appear coarse and were twice the area fraction compared to that in 200 W build. On the other hand, microstructures in the heated substrate sample exhibited the evolution of α and β phases. A multi-scale finite element method based thermo-kinetic model spanning from melt pool scale to the component scale was incorporated to understand the mechanism of the evolution of microstructures during liquid–solid and solid–solid state transformation. Electrochemical performance in the simulated body fluid of the printed alloys was found to be significantly affected by the presence of martensite fractions. Both mechanical and corrosion behaviors were favorably influenced by adoption of the substrate preheating during additive manufacturing due to promotion of diffusional transformation of β to α at the expense of martensitic transformation.

High-Pressure Torsion: A Path to Refractory High-Entropy Alloys from Elemental Powders

For the first time, the refractory high-entropy alloys with equiatomic compositions, HfNbTaTiZr and HfNbTiZr, were synthesized directly from a blend of elemental powders through ten revolutions of high-pressure torsion (HPT) at room temperature. This method has demonstrated its effectiveness and simplicity not only in producing solid bulk materials but also in manufacturing refractory high-entropy alloys (RHEAs). Unlike the melting route, which typically results in predominantly single BCC phase alloys, both systems formed new three-phase alloys. These phases were defined as the Zr-based hcp1 phase, the α-Ti-based hcp2 phase, and the Nb-based bcc phase. The volume fraction of the phases was dependent on the accumulated plastic strain. The thermal stability of the phases was studied by annealing samples at 500 °C for one hour, which resulted in the formation of a mixed structure consisting of the new two hexagonal and cubic phases.

Unveiling the impact of heat treatment on powder-metallurgy α+β titanium alloy for achieving a superior strength-ductility combination

The present study investigated the effects of heat treatment (solid solution and aging treatments) on the microstructure and mechanical properties of a hot-rolled α+β Ti–3Al–5Mo–4.5V (TC16) produced through blended elemental powder metallurgy (BEPM) process using master alloy hydrogenation (MAH) approach. After solid solution treatment, metastable martensite α'' phase and athermal ω phase were formed. Aging treatment facilitated decomposition of metastable phases and precipitation of αs particles. Dispersion strengthening, resulting from the formation of a significant amount of α/β interfaces between fine secondary αs particles and β matrix, played a decisive role in enhancing the strength of the TC16 alloy. However, elevated aging temperatures promoted the coarsening of αs particles, leading to a reduction in the strengthening effect. A systematic investigation of the effects of the solid solution and aging treatments enabled the evolution of a bimodal microstructure with the precipitation of fine αs particles, contributing to an outstanding combination of strength and ductility. The ultimate tensile strength reached 1424.6 MPa with an elongation at break of 7.7%, while the hardness reached 380.2HV.

Ballistic performance of titanium-based layered composites made using blended elemental powder metallurgy and hot isostatic pressing

Metal matrix composites tiles based on Ti–6Al–4V (Ti64) alloy, reinforced with 10, 20, and 40 (vol%) of either TiC or TiB particles were made using press-and-sinter blended elemental powder metallurgy (BEPM) and then bonded together into 3-layer laminated plates using hot isostatic pressing (HIP). The laminates were ballistically tested and demonstrated superior performance. The microstructure and properties of the laminates were analyzed to determine the effect of the BEPM and HIP processing on the ballistic properties of the layered plates. The effect of porosity in sintered composites on further diffusion bonding of the plates during HIP is analyzed to understand the bonding features at the interfaces between different adjacent layers in the laminate. Exceptional ballistic performance of fabricated structures was explained by a significant reduction in the residual porosity of the BEPM products by their additional processing using HIP, which provides an unprecedented increase in the hardness of the layered composites. It is argued that the combination of the used two technologies, BEPM and HIP is principally complimentary for the materials in question with the abilities to solve the essential problems of each used individually.

Refractory High‐Entropy Alloys Produced from Elemental Powders by Severe Plastic Deformation

A comparative investigation of two fundamentally different approaches for the synthesis, microstructure evolution, and mechanical properties of the refractory high‐entropy alloys (RHEA) HfNbTaTiZr and HfNbTiZr is performed. The two methods comprises conventional arc (button) melting and a powder route based on mechanical alloying and consolidation via severe plastic deformation. In particular, blended elemental powder is pre‐compacted and subjected to one or four passes of equal channel angular pressing (ECAP) at 500 °C and then 10 revolutions of high pressure torsion (HPT) at room temperature to an effective strain between 4 and 40. Some samples are then annealed at 500 °C for 1 h to investigate the thermal stability of the phases. The four ECAP passes at 500 °C do not result in the formation of the body‐centered cubic (BCC) phase typical for the program RHEAs despite the presence of interfacial zones between particles and defect‐driven diffusion. Nevertheless, a single ECAP pass is sufficient to create a solid bulk sample for subsequent HPT. After 10 HPT revolutions, in contrast to melting route resulting in a single BCC phase alloy, both alloys form new phases comprising a Nb‐rich BCC phase and a ZrHf‐rich HCP phase in both alloys.

Analysis of initial stage of liquid-phase sintering by combined multi-phase-field/discrete-element method

A combined multi-phase-field/discrete-element method in two dimensions is applied to the liquid phase sintering process of blended elemental powders. The boundary migration, diffusion of elements, and phase transformation between two dissimilar particles are calculated using a multi-phase-field method for sintering based on Gibbs energy functions. The sintering shrinkage is computed with the discrete-element method taking account of the neck size and sintering force, which are obtained from a multi-phase-field simulation. In this study, a pair or small cluster consisting of two elemental powders in a binary eutectic alloy is used as a model system. First, the formation of a liquid phase around the contact area between two dissimilar particles above the eutectic temperature of the system, and the motions of the particles due to grain boundary sliding along the liquid films are confirmed. Second, an Sn–Bi system is selected as the real eutectic system, and the sintering behavior of powder compacts with various mixing ratios of Sn and Bi particles is demonstrated. Finally, transient liquid-phase sintering of Sn–Bi system is simulated, that is, the generation and extinction of the liquid phase due to interdiffusion between Sn and Bi particles are calculated.

Features of Microstructural Evolution and Corrosion Behavior of Ti6Al4V Titanium Alloy Fabricated from Elemental Powder Blends

Sintered Ti6Al4V titanium alloys prepared from TiH2/60Al40V powder blends under various technological conditions were studied. The microstructural evolution was investigated by X-ray diffraction, scanning electron microscopy, optical microscopy, and energy dispersive X-ray analysis. The corrosion resistance of sintered titanium alloy was evaluated by the static immersion test in 40 wt.% H2SO4 acid, according to ASTM standard G31-72(2004). Depending on powder metallurgy processing parameters (compaction pressure or sintering temperature), the Ti6Al4V alloy was obtained with various structural features (porosity and structural heterogeneity). It was shown that those structural features of sintered Ti6Al4V titanium alloy are a key microstructural factor that determines their corrosion resistance. For instance, an increase in porosity leads to enhanced corrosion resistance. Based on the current research, the optimal manufacturing regimes of powder metallurgy of Ti6Al4V titanium alloy ensure the achievement of characteristics sufficient for practical use in aggressive conditions of the chemical industry were obtained.

A Comprehensive Study on Hot Deformation Behavior of the Metastable β Titanium Alloy Prepared by Blended Elemental Powder Metallurgy Approach

A Comprehensive Study on Hot Deformation Behavior of the Metastable β Titanium Alloy Prepared by Blended Elemental Powder Metallurgy Approach

Significant hardening effect of high-temperature aging of alloy Ti-6Al-4V composite reinforced with TiC

Titanium alloy composites, reinforced with a light second phase and made using inexpensive powder metallurgy, attract considerable attention due to the directness of their intentional hardness increase without compromising low weight of materials. In this study the metal-matrix composites (MMC) of Ti-6Al-4V alloy reinforced with light and hard particles of TiC (up to 80%, vol.) were made using blended elemental powder metallurgy of hydrogenated titanium. Post-sintering solution treatment for 45 min. at 880 °C and 1000 °C and water quenching followed by the 5 hrs. aging at 550 °C was used to additionally refine the microstructure and properties of MMC. For the duration of thermal exposure throughout solution treatment and additional aging the matrix and reinforcement phase underwent distinct structural changes that modified the mechanical properties of materials. It has been shown that the used reinforcement presents an exceptional opportunity for hardening of Ti-based composites without compromising their low specific weigh. It can increase the hardness of material by more than 40% due to the ability of TiC to chemically react with the matrix to form a strong interfacial bond and its ability to form hard compounds of Ti2C and Ti3AlC in the expense of the relatively soft matrix alloy.

Powder metallurgy processing of Nb-modified near β titanium alloys prepared with elemental powders

ABSTRACT Near β Ti alloys typically show high specific strength and provide a wide spectrum of mechanical properties with different heat treatments. In this work, a commercial near β Ti alloy Ti-5553 (Ti-5Al-5V-5Mo-3Cr-0.5Fe) was prepared through powder metallurgy using the blended elemental powder approach. Additionally, alloy modifications with 6 wt.% Nb (Ti-6Nb-5Al-2.5V-5Mo-3Cr-0.5Fe) and 12 wt.% Nb (Ti-12Nb-5Al-5Mo-3Cr-0.5Fe) were investigated. Specimens were prepared by uniaxial cold compaction of blended powders at room temperature with sintering conducted at 1300°C for 2 h under Ar atmosphere. Microstructure investigation revealed reasonable homogenisation of alloying elements and colony sizes in the order of 80-100 μm with porosity below 10%. Moreover, the bending strength of as-sintered Ti-12Nb-5Al-5Mo-3Cr-0.5Fe was about 850 MPa and the micro-Vickers hardness was approximately 370 HV. The alloy modifications with Nb increased strength without loss in flexural strain.

An Investigation into the Microstructural Response to Flexural Stresses of a Metastable β‐Phase Ti Alloy produced by Blended Elemental Powder Metallurgy

A Ti‐10V‐3Al‐3Fe metastable β Ti alloy is strained under three‐point bending conditions according to the ASTM E290‐14 standard. A combination of electron backscatter diffraction (EBSD) mapping and high‐resolution scanning transmission electron microscopy (STEM) is used to investigate the microstructural response to flexural stress. Results reveal a delayed formation of the deformation products, due to the load‐bearing capacity of the constituent voids. The deformation products are confined in narrow bands on either side of the fracture surface. {332}⟨113⟩ twinning system is identified as the primary deformation mode followed by the formation of α″ martensite both in β matrix and β twins. Accommodation of the microscopic strain arising from the development of α″ structure and β‐twinning triggers the formation of fine deformation‐induced ω plates, which are observed predominantly at the interfacial plane of β/β twin and β/α″, and also in the interior of the β twins.

Mechanical Properties of Ti–5Al–5V–5Mo–3Cr Alloy Sintered From Blended Elemental Powders

The field-assisted sintering technique (FAST) was successfully used to sinter, homogenize, and age the Ti–5Al–5V–5Mo–3Cr (Ti-5553) aerospace alloy from blended elemental powders in a single processing run. Sintering at a comparatively high temperature of 1500 °C assured chemical homogeneity of the material. Subsequently, without cooling to the room temperature, the temperature was lowered to 600 °C for 30 min to provide annealing treatment and to produce a desired lamellar α + β microstructure. Using an in-house designed assembly, a fully dense rod of 15 mm in diameter and 70 mm in length was successfully sintered. Microstructural and mechanical properties of the alloy were investigated and compared with the conventionally processed Ti-5553 alloy. A good combination of strength (1183 MPa) and ductility (6 pct) was achieved; these values are fully comparable to the conventional cast, forged, and aged Ti-5553 alloy. It was shown that homogeneous Ti-5553 alloy can be produced by FAST, FAST can instantly provide necessary annealing steps, and the FAST process can be upscaled to produce homogeneous rods.

In-situ synthesized TiC/Ti-6Al-4V composites by elemental powder mixing and spark plasma sintering: Microstructural evolution and mechanical properties

Titanium matrix composites synthesized using powder metallurgy methods have attracted significant attention due to their extraordinary mechanical properties. In this study, cost-effective and high-performance TiC/Ti-6Al-4 V matrix composites were synthesized and characterized using a combined elemental powder mixing and spark plasma sintering method. Studies on the effect of graphene nanoplate (GNP) content on microstructures of Ti-6Al-4 V matrix composites showed typical Widmanstatten structures without apparent pores and microcracks. The grain size of composites was decreased significantly with the increase of GNP content, mainly due to the pinning effect of in-situ generated TiC particles at grain boundaries, which limited the rapid grain growth of the matrix. Mechanical test results showed that their yield strength and ultimate tensile strength were 889.0 MPa and 988.3 MPa, respectively, and their total fracture elongation was maintained at ∼14.2 %. GNPs/Ti-6Al-4 V exhibited superior strength (e.g., yield and ultimate tensile strength of 1028.4 and 1121.6 MPa, which are 14.4 % and 13.5 % higher than those of the matrix) and maintained a good ductility of ∼ 9.8 % with only 0.1 wt% GNP addition. Carbon nanomaterial (such as graphene nanoplates) induced the precipitation of needle-like nano-secondary phases in trigeminal grain boundary β phases, which strengthened the β-Ti soft phase. The reinforced strength of the composite is mainly attributed to the grain refinement, secondary α phases precipitation strength and dislocations strengthening. This work provides a new methodology for fabrication of high-performance titanium matrix composites (TMCs) combination blended elemental powder metallurgy (BEPM) and sintering technology.