Co-deformation processing and modeling of <Emphasis Type="Italic">In-Situ</Emphasis> multiphase composites

A series of in-situ, deformation-processed metal matrix composites were produced by direct powder extrusion of blended constituents. The resulting composites are comprised of a metallic Ti-6Al-4V matrix containing dispersed and co-deformed discontinuously reinforced-intermetallic matrix composite (DR-IMC) reinforcements. The DR-IMCs are comprised of discontinuous TiB₂ particulate within a titanium trialuminide or near-γ Ti-47Al matrix. Thus, an example of a resulting composite would be Ti-6Al-4V+40 vol pct (Al₃Ti+30 vol pct TiB₂) or Ti-6Al-4V+40 vol pct (Ti-47Al+40 vol pct TiB₂), with the DR-IMCs having an aligned, high aspect ratio morphology as a consequence of deformation processing. The degree to which both constituents deform during extrusion has been examined using systematic variations in the percentage of TiB₂ within the DR-IMC, and by varying the percentage of DR-IMC within the metal matrix. In the former instance, variation of the TiB₂ percentage effects variations in relative flow behavior; while in the latter, varying the percentage of DR-IMC within the metallic matrix effects changes in strain distribution among components. The results indicate that successful co-deformation processing can occur within certain ranges of relative flow stress; however, the extent of commensurate flow will be limited by the constituents’ inherent capacity to plastically deform.     

Fatigue crack growth through alloyed niobium, Nb-Cr2Nb, and Nb-Nb5Si3 in situ composites

Fatigue cracks were grown through several niobium-based materials. For Nb-Cr-Ti composition materials, the single-phase alloy represented the matrix of two in situ composites with about 22 and 38 vol pct Cr₂Nb. Grain boundaries were coated with intermetallic in the lower-volume fraction material, while the 38 vol pct Cr₂Nb composite consisted of mainly spherical, dispersed intermetallic. The Nb-10Si composite was composed of about 28 vol pct primary Nb₅Si₃, with most of the matrix alloy in “fiberlike” shapes due to extrusion. Crack growth rates through the composites were generally faster than for unalloyed Nb, roughly in proportion to the volume fraction of intermetallic, although differences in microstructure make this comparison difficult. The presence of intermetallic greatly alters deformation of material near the crack tip. Particles of Cr₂Nb were broken during the crack growth process, leading to increased crack growth rates. These results suggest microstructural modifications that could be expected to enhance fatigue crack growth resistance.     

Room-Temperature strength and deformation of Tib2-reinforced near-γ titanium aluminides

A series of TiB₂-reinforced near-γ titanium aluminide (Ti-Al) matrix composites have been produced in investment-cast form and characterized with respect to microstructure and tensile deformation. The Ti-Al matrices of the composites examined are based upon the binary composition Ti-47 Al (at. pct), with varying proportions (2 to 6 cumulative percent) of manganese, vanadium, chromium, and niobium. TiB₂ has been introduced into the microstructuresvia XD* processing at levels of 7 and 12 vol pct and compared to unreinforced (0 vol pct TiB₂), base variants. The influences of heat-treatment temperature and time have also been studied for each composition and reinforcement variant. The addition of dispersed TiB₂ leads to a fine, stable, and homogeneous as-cast matrix microstructure. The measured TiB₂ size within the composites examined ranged from 1.4 to 2.6 μm. Increasing the volume fraction of TiB₂ leads to increased elastic moduli, increased ambient temperature tensile strengths, and in general, increased strain-hardening response. In some instances, the overall ductility of the alloy increases with the addition of TiB₂ reinforcement. The flow stresses of both the monolithic and composite variants exhibit conventional power-law plasticity. The results indicate that the strengthening and the flow behavior in these composites are derived from both indirect and direct sources. Strengthening contributions are indirectly derived from the microstructural changes within the matrix of the composite that evolve due to the presence of the reinforcement during its evolution and development, for example, due to grain refinement and reinforcement-derived interstitial solid-solution strengthening. Direct contributions to strength are those that can be specifically attributed to the presence of the reinforcement during deformation,e.g., through the interaction of dislocations with the reinforcing particles. When the estimates of the indirect contributions are isolated and arithmetically removed from the magnitude of the total observed strength of the composite, the increase in flow stress correlates in all instances with the inverse square root of the planar interparticle spacing for all alloy compositions, heat treatments, and levels of strain examined.     

High-temperature slow-strain-rate compression studies on CoAI-TiB2 composites

CoAl-base composites containing various volume fractions of TiB₂ particulates in the 1 to 3-μm size range were tested in compression over a range of strain rates at 1100 to 1300 K. Hotpressed and postcompression microstructures were characterized using optical and transmission electron microscopy. For a strain rate of 2 × 10^-6 s^-1, the flow stress at 1300 K of CoAl-20 vol pct TiB₂ was twice that of monolithic CoAl. Correspondingly, the stress exponent of CoAl-20 vol pct TiB₂ at 1300 K was ∼4.5 compared to ∼3.0 for stoichiometric monolithic CoAl. This increased resistance of the composite to deformation at elevated temperatures is attributed to TiB₂ particulate-dislocation interactions. The high-temperature compressive deformation behaviors of NiAl-TiB₂ and CoAl-TiB₂ composites are compared.     

Tribological properties of aluminum alloy matrix TiB2 composite prepared by in situ processing

An investigation of the wear behavior, in lubricated sliding and rolling of in situ prepared TiB₂ particle-reinforced 2024 T4 Al alloy matrix composites against 52100 steel and hardened pearlitic nodular cast iron, respectively, was undertaken. In sliding contact, the 10 vol pct 0.3-μm TiB₂-metal matrix composite (MMC) showed slightly less wear than the 10 vol pct 1.3-μm TiB₂-MMC. Transmission electron microscopy of cross sections, taken normal to the wear track and parallel to the sliding direction, revealed that the TiB₂ particles on the wear track were polished and particle pullout was largely absent. This was attributed to the strong interfacial bonding between the Al-alloy matrix and the TiB₂ reinforcing phase. The TiB₂ particles on the wear track inhibited spalling. Subsurface damage of the MMC did not occur. The wear of the steel mating surfaces worn against the TiB₂-MMCs was minor and caused by the cutting action of the TiB₂ particles that resided on the MMC wear track. In rolling contact, the 0.3-μm-size TiB₂-MMC showed 5 times higher weight loss than the 1.3-μm TiB₂-MMC for the same content of reinforcement, but the weight loss of the cast iron mating surface was less for the former. For the smaller particle size, the wear of 5 and 10 vol pct TiB₂-MMCs was the same. A high density of surface cracks was present on the wear track of the 0.3-μm TiB₂-MMC but not on the 1.3-μm MMC. The significance of strong particle/matrix interfacial bonding and particle size effect on the wear behavior of ceramic particulate-reinforced MMCs in lubricated sliding and rolling wear is discussed.     

Combustion synthesis of LiGa and LiAl intermetallic alloys

LiAl and LiGa intermetallic alloys have been synthesized using the simultaneous combustion mode of combustion synthesis. LiAl intermetallic is potentially suitable as a temper alloy for producing aluminum-lithium alloys and as an anodic material for high-energy batteries. LiGa can be used as a reduction alloy to recover valuable reactive metals from molten salt effluent in actinide recovery technology. The effects of particle size, preignition heating rate, and theoretical green density on the ignition and combustion temperatures have been studied in an effort to more precisely control the synthesis reaction of these intermetallics. A lithium particle size of -20/xm was found to be suitable when the combustion synthesis reaction was conducted at a high heating rate (>1.0 cC/s) and a moderate green density (55 to 65 pct theoretical). Preignition diffusion is suggested as the cause for low exothermic heat release at high green densities. A combustion temperature above the melting point of the LiGa intermetallic compound can be achieved under optimized conditions. However, the exothermicity and, therefore, the adiabatic temperature is too low for either LiAl or LiGa to be produced by the propagating mode of combustion synthesis. Formerly graduate student with the Kroll Institute for Extractive Metallurgy     

Microstructure, mechanical properties, and fracture mechanism of As-cast (Ti0.5Cu0.25Ni0.15Sn0.05Zr0.05)100−x Mo x composites

Copper mold cast cylinders of (Ti_0.5Cu_0.25Ni_0.15Sn_0.05Zr_0.05)_100−x Mo _x composites are prepared. Addition of Mo in the bulk glass-forming alloy induces the formation of a dendrite/matrix composite. For 3-mm-diameter cylinders, the matrix exhibits a homogenous ultrafine microstructure for Mo content of 2.5 at. pct, and a fine eutectic microstructure for 5 at. pct Mo. For 5-mm-diameter cylinders, the matrix exhibits a dendritic microstructure for 2.5 at. pct Mo, and exhibits a coarser eutectic microstructure for 5 at. pct Mo. Despite the formation of a dendrite/nanostructured matrix composite in the cylinders, the quenched surface layer with a nanoscale grain size dominates the deformation and fracture of the 3-mm-diameter cylinders. More than 56 vol pct quenched layer leads to a distensile fracture mode and the samples exhibit high fracture strength and high Young’s modulus but low ductility. For 5-mm-diameter cylinders, the composite microstructure becomes dominant due to its more than 64 vol pct volume fraction leading to a cone-shaped fracture surface. The samples exhibit lower yield strength and lower Young’s modulus but better ductility compared to the 3-mm-diameter cylinders. The mechanical behavior of the Mo-bearing composites strongly depends on the microstructural homogeneity and casting defects formed upon solidification.     

Microstructure and properties of In situ Al/TiB2 composite fabricated by in-melt reaction method

A novel in situ reaction process-in-melt reaction method was developed. TiB₂ particles form in situ through the reaction of TiO₂, H₃BO₃, and Na₃AlF₆ in an aluminum alloy melt. The results showed that the in situ TiB₂ particles formed were spherical in shape and had an average diameter of about 0.93 μm. Moreover, the distribution of TiB₂ particles in the matrix was uniform. The interface between the TiB₂ particles and the matrix showed good cohesion. The tensile strength and the yield strength of the composite increase with increasing TiB₂ content. When TiB₂ particle content in the matrix was 10 vol pct, the tensile strength, yield strength, and elongation of Al-4.5Cu/TiB₂ composite were 417 MPa, 317 MPa, and 3.3 pct, respectively.     

Effect of Sn on microstructure and mechanical properties of Ti-base dendrite/ultrafine-structured multicomponent alloys

Ti_57−x Cu₁₅Ni₁₄Sn_4+x Nb₁₀ (x = 0, 5, or 10) alloys were prepared by copper mold casting. At Sn = 4 at. pct, a dendrite/ultrafine-structured multicomponent alloy was obtained, which exhibits 1271 MPa yield strength, 77 GPa Young’s modulus, and 2 pct plasticity at room temperature for 3-mm-diameter samples. The cooling rate significantly affects the as-cast microstructure and the mechanical properties. For 5-mm-diameter samples, the alloy exhibits 1226 MPa yield strength, 63 GPa Young’s modulus, and 2.5 pct plasticity. At Sn = 9 at. pct, Ti-, Sn-, and Nb-rich particles precipitate primarily. This near-hypereutectic alloy composition leads to the precipitation of intermetallics, which deteriorate the mechanical properties and result in the coexistence of ductile and brittle fracture mechanisms. At Sn = 14 at. pct, the alloy composition is completely in the intermetallic region, thus inducing the formation of Ti₂Cu, Ti₂Ni, and Ti₃Sn intermetallics. The alloy becomes very brittle because the intermetallic compounds dominate the fracture process.     

Superplastic behavior and cavitation in high-strain-rate superplastic Si3N4p /Al-Mg-Si composites

High-strain-rate superplastic behavior has been investigated for Si₃N_4p /Al-Mg-Si (6061) composites with a V _f =20 and 30 pct, respectively, where V _f is the volume fraction of reinforcements. A maximum elongation was attained at a temperature close to the onset temperature for melting for both composites. The maximum elongation for the 30 vol pct composite was larger than that for the 20 vol pct composite. Development of cavities transverse to the tensile direction is responsible for the lower maximum elongation of the 20 vol pct composite. However, development of the transverse cavities was limited to the optimum superplastic temperature for the 30 vol pct composite. The differential scanning calorimetry (DSC) investigation showed that a sharp endothermic peak appeared for the 30 vol pct composite, indicating that sufficient partial melting occurs. It is, therefore, likely that the stress concentrations are sufficiently relaxed by a liquid phase and that the development of transverse cavities is limited for the 30 vol pct composite.     

Fracture toughness of discontinuously reinforced Al-4Cu-1.5Mg/TiB2 composites

The effect of particle size, particle volume fraction, and matrix microstructure on the fracture initiation toughness of a discontinuously reinforced aluminum composite was examined. The composites were Al-4 wt pct Cu-1.5 wt pct Mg reinforced with 0 to 15 vol pct of TiB₂ having an average particle diameter of 1.3 or 0.3μm producedin situ by the XD process. The room-temperature plane-strain toughness measured using compact tension specimens ranged from 19 to 25 MPa . Toughness was adversely affected by increases in TiB₂ volume fraction. The fracture toughness of all composites was affected by changes in the matrix microstructure produced by aging. The response of the composites to artificial aging deviates from that of the matrix. Fractography revealed that these composites failed in a ductile manner, with voids initiating at the reinforcing TiB₂ particles. The experimentally measured plane-strain toughness properties of Al-4Cu-l .5Mg composites with well-dispersed, 1.3-μm TiB² reinforcements agree with the Rice and Johnson model.     

High-temperature environmental embrittlement of thermomechanically processed TiAl-based intermetallic alloys

Thermomechanically processed TiAl-based intermetallic alloys with various alloy compositions and microstructures were tensile tested in various environmental media, including air, water vapor, and a gas mixture of 5 vol pct, H₂ + Ar, as functions of temperature and strain rate. All the TiAl-based intermetallic alloys showed reduced tensile fracture stress (or elongation) in air, in water vapor, and in a gas mixture of 5 vol pct H₂ + Ar, not only at ambient temperature (RT ∼ 600 K), but also at high temperature, from 600 to 1000 K (and sometimes at temperatures higher than 1000 K). The high-temperature environmental embrittlement of TiAl-based intermetallic alloys depended upon the microstructure. The factors causing the high-temperature environmental embrittlement may include hydrogen atoms decomposed from water vapor (H₂O) or hydrogen gas (H₂), similar to those causing the low-temperature environmental embrittlement. Also, it is demonstrated that the oxidized scale is effective in reducing high-temperature environmental embrittlement.     

Effects of TiB2/TiCx ratios on compression properties and abrasive wear resistance of in situ 50 vol.-% (TiB2–TiCx)/Al–Cu composites

Effects of TiB₂/TiC_x ratios on compression properties and abrasive wear resistance of 50?vol.-% (TiB₂–TiC_x)/Al–Cu composites fabricated via the combustion synthesis (CS) method assisted with hot press from the Al–Ti–B₄C system were studied. With decrease in the TiB₂/TiC_x ratio from 3:1 to 1:3, the shape of TiB₂ changed from platelike to clubbed while the size of TiC_x particles increased, which directly led to different mechanical properties. The 50?vol.-% (TiB₂–TiC_x)/Al–Cu composite with the TiB₂/TiC_x ratio of 2:1 exhibited good compression strength without sacrificing the fracture strain, while the composite possessed the highest abrasive wear resistance when the TiB₂/TiC_x ratio was 3:1. The appropriate TiB₂/TiC_x ratio was recommended to be 2:1 in this research.     

An investigation of strain hardening and creep in an AI-6061/AI2O3 metal matrix composite

Experiments were conducted to compare the influence of temperature on the flow and strain-hardening characteristics of an Al-6061 metal matrix composite, reinforced with ∼20 vol pct of Al₂O₃-based microspheres, with the unreinforced monolithic alloy. At room temperature, the yield stresses and the strain-hardening rates are higher in the composite material in the asquenched condition and after aging at 448 K for periods of time up to 300 hours. The 0.2 pct proof stress and the strain-hardening rate decrease with increasing temperature in both materials, but the rate of decrease is faster in the composite so that the unreinforced monolithic alloy exhibits higher yield stresses and strain-hardening rates at temperatures in the vicinity of 600 K. Under conditions of constant stress at high temperatures, the composite exhibits both a higher creep strength than the monolithic alloy and higher values for the stress exponents for creep. Formerly Visiting Scholar, Kyushu University, is Associate Professor, Department of Metallurgy, Xian Institute of Metallurgy and Construction Engineering, Xian 710055, People’s Republic of China.     

The effect of gravity on the combustion synthesis of metal-ceramic composites

The effects of gravity on the combustion characteristics and microstructure of metal-ceramic composites (HfB₂/Al and Ni₃Ti/TiB₂ systems) were studied under both normal and low gravity conditions. Under normal gravity conditions, pellets were ignited in three orientations relative to the gravity vector. Low gravity combustion synthesis (SHS) was carried out on a DC-9 aircraft at the NASA-Lewis Research Center. It was found that under normal gravity conditions, both the combustion temperature and wave velocity were highest when the pellet was ignited from the bottom orientation; i.e., the wave propagation direction was directly opposed to the gravitational force. The SHS of 70 vol pct Al (in the Al-HfB₂ system) was changed from unstable, slow, and incomplete when ignited from the top to unstable, faster, and complete combustion when ignited from the bottom. The hydrostatic force (height × density × gravity) in the liquid aluminum was thought to be the cause of formation of aluminum nodules at the surface of the pellet. The aluminum nodules that were observed on the surface of the pellet when reacted under normal gravity were totally absent for reactions conducted under low gravity. Buoyancy of the TiB₂ particles and sedimentation of the Ni₃Ti phase were observed for the Ni₃Ti/TiB₂ system. The possibility of liquid convective flow at the combustion front was also discussed. Under low gravity conditions, both the combustion temperature and wave velocity were lower than those under normal gravity. The distribution of the ceramic phase, i.e., TiB₂ or HfB₂, in the intermetallic (Ni₃Ti) or reactive (Al) matrix was more uniform.     

Effects of the amount of γ′ and oxide content on the secondary recrystallization temperature of nickel-base superalloys

The effects of the amount of γ′ and yttria (Y₂O₃) content on the secondary recrystallization (SRx) temperature of as-extruded material of the mechanically alloyed nickel-base superalloys based on a superalloy TMO-2 were investigated. It was observed that (1) the primarily recrystallized grain size of the as-extruded material decreased with increasing the γ′ and the yttria content in the material; (2) the SRx temperature decreased with decreasing the yttria content and with increasing the amount of theγ′ up to about 55 vol pct, while (3) the temperature increased for the material containing more than 65 vol pctγ′; and (4) the SRx temperatures of the material containing 75 vol pctγ′ phase with 1.1 wt pct yttria and 55 vol pctγ′ phase with no yttria were identical to theirγ′ solvus. From these results, the following conclusions are drawn: (1) dissolution of theγ′ particles is a necessary, but not a sufficient, condition for the occurrence of secondary recrystallization; (2) secondary recrystallization of a material with sufficiently smaller grain size occurs at a temperature higher than theγ′ solvus and the temperature at which the yttria particles lose their ability to prevent rapid growth of the primarily recrystallized grains; and (3) the SRx temperature of a material with larger grain size depends on grain size. Formerly Assistant Researcher with NRIM     

Strength and plastic flow in “in situ” TiC reinforced aluminum composites

The deformation behavior of TiC particulate-reinforced aluminum composites (Al-TiC _p ) was investigated in this work using pure aluminum as the reference matrix material. Uniaxial compression tests were carried out at 293 and 623 K and at two strain rates (3.7×10⁻⁴ and 3.7×10⁻³ s⁻¹). Yield strengths of up to 127 MPa were found in composites containing 10 vol pct TiC particulates, which were almost 4 times the yield strength of pure Al. In addition, at 623 K, relatively small reductions in yield strength were found, suggesting that this property was rather insensitive to temperature for the temperatures investigated in this work. Nevertheless, at 623 K, increasing the rate of straining from 3.7×10⁻⁴ s⁻¹ to 3.7×10⁻³ s⁻¹ lowered the yield strength, particularly in 10 vol pct TiC _p -Al composites. Two stages of work hardening were identified in pure Al and a 10 vol pct TiC _p composite during plastic flow through the modified version of the Hollomon equation (σ = Kɛ ⁿ ± Δ). In particular, the work-hardening exponents found in pure Al shifted from high to low values as the extent of plastic strain was increased while the opposite was true for the 10 vol pct TiC _p composite. Finally, at 623 K, dynamic recovery mechanisms became dominant at plastic strain levels >0.2 in 10 vol pct TiC _p -Al composites, with the effect being minor at room temperature.     

Kinetics of biaxial dome formation by transformation superplasticity of titanium alloys and composites

By thermally cycling through their transformation temperature range, coarse-grained polymorphic materials can be deformed superplastically, owing to the emergence of transformation mismatch plasticity (or transformation superplasticity) as a deformation mechanism. This mechanism is presently investigated under biaxial stress conditions during thermal cycling of unalloyed titanium, Ti-6Al-4V, and their composites (Ti/10 vol. pct TiC _p , Ti-6Al-4V/10 vol. pct TiC _p , and Ti-6Al-4V/5 vol. pct TiB _w ). During gas-pressure dome bulging experiments, the dome height was measured as a function of forming time. Adapting existing models of biaxial doming to the case of transformation superplasticity where the strain-rate sensitivity is unity, we verify the operation of this deformation mechanism in all experimental materials and compare the biaxial results directly to new uniaxial thermal cycling results on the same materials. Finally, existing thickness distribution models are compared with experimentally measured profiles.     

Reaction synthesis of Ni-Al-based particle composite coatings

Electrodeposited metal matrix/metal particle composite (EMMC) coatings were produced with a nickel matrix and aluminum particles. By optimizing the process parameters, coatings were deposited with 20 vol pct aluminum particles. Coating morphology and composition were characterized using light optical microscopy (LOM), scanning electron microscopy (SEM), and electron probe microanalysis (EPMA). Differential thermal analysis (DTA) was employed to study reactive phase formation. The effect of heat treatment on coating phase formation was studied in the temperature range 415 °C to 1000 °C. Long-time exposure at low temperature results in the formation of several intermetallic phases at the Ni matrix/Al particle interfaces and concentrically around the original Al particles. Upon heating to the 500 °C to 600 °C range, the aluminum particles react with the nickel matrix to form NiAl islands within the Ni matrix. When exposed to higher temperatures (600 °C to 1000 °C), diffusional reaction between NiAl and nickel produces (γ′)Ni₃Al. The final equilibrium microstructure consists of blocks of (γ′)Ni₃Al in a γ(Ni) solid solution matrix, with small pores also present. Pore formation is explained based on local density changes during intermetallic phase formation, and microstructural development is discussed with reference to reaction synthesis of bulk nickel aluminides.