Fabrication of carbide-particle-reinforced titanium aluminide-matrix composites by laser-engineered net shaping

TiAl-based titanium aluminide alloys and their composites reinforced with ceramic particles are considered to be important candidate materials for high-temperature structural applications. Laser-engineered net shaping (LENS) is a layered manufacturing process, which involves laser processing fine powders into three-dimensional components directly from a computer-aided design (CAD) model. In this work, the LENS process was employed to fabricate carbide-particle-reinforced titanium aluminide-matrix composites using TiC and gas-atomized Ti-48Al-2Cr-2Nb powders as the feedstock materials. The composites deposited by the LENS process were susceptible to solid-state cracking due to high thermal stresses. The microstructures of the laser-deposited monolithic and composite titanium aluminide materials were characterized using light optical microscopy (LOM), scanning electron microscopy (SEM), X-ray energy-dispersive spectroscopy (EDS) analysis, electron-probe microanalysis (EPMA), and X-ray diffraction (XRD) techniques. Effects of the LENS processing parameters on the cracking susceptibility and microstructure were studied. Crack-free deposits were fabricated by preheating the substrate to 450 °C to 500 °C during LENS processing. The fabricated composite deposits exhibit a hardness of more than twice the value of the Ti-6Al-4V alloy.     

Fabrication of carbide-particle-reinforced titanium aluminide-matrix composites by laser-engineered net shaping

TiAl-based titanium aluminide alloys and their composites reinforced with ceramic particles are considered to be important candidate materials for high-temperature structural applications. Laser-engineered net shaping (LENS) is a layered manufacturing process, which involves laser processing fine powders into three-dimensional components directly from a computer-aided design (CAD) model. In this work, the LENS process was employed to fabricate carbide-particle-reinforced titanium aluminide-matrix composites using Tic and gas-atomized Ti−48Al−2Cr−2Nb powders as the feedstock materials. The composites deposited by the LENS process were susceptible to solid-state cracking due to high thermal stresses. The microstructures of the laser-deposited monolithic and composite titanium aluminide materials were characterized using light optical microscopy (LOM), scanning electron microscopy (SEM), X-ray energy-dispersive spectroscopy (EDS) analysis, electron-probe microanalysis (EPMA), and X-ray diffraction (XRD) techniques. Effects of the LENS processing parameters on the cracking susceptibility and microstructure were studied. Crack-free deposits were fabricated by preheating the substrate to 450 °C to 500 °C during LENS processing. The fabricated composite deposits exhibit a hardness of more than twice the value of the Ti−6Al−4V alloy.     

Texture and residual strain in two SiC/Ti-6-2-4-2 titanium composites

Residual strain and texture variations were measured in two titanium matrix composites reinforced with silicon carbide fibers (Ti/SiC) of similar composition but fabricated by different processing routes. Each composite comprised a Ti-6242 α/β matrix alloy containing vol 35 pct continuous SiC fibers. In one, the matrix was produced by a plasma sprayed (PS) route, and in the other by a wiredrawn (WD) process. The PS and WD composites were reinforced with SCS-6 (SiC) and Trimarc (SiC) fibers, respectively. The texture in the titanium matrices differed significantly. The titanium matrix for the PS material exhibited random texture pre and post fabrication of the composite. For the WD material, the starting texture of the monolithic titanium matrix was ≈17 times random, but after consolidation into composite form, it was ≈6 times random. No significant differences were noted in the fiber-induced matrix residual strains between the composites prepared by the two procedures. However, the Trimarc (WD) fibers recorded higher (≈1.3 times) compressive strains than the SCS-6 (PS) fibers. Stresses and stress balance results are reported. Plane-specific elastic moduli, measured in load tests on the unreinforced matrices, showed little difference. This article is based on a presentation made in the Symposium “Mechanisms and Mechanics of Composites Fracture” held October 11–15, 1998, at the TMS Fall Meeting in Rosemont, Illinois, under the auspices of the TMS-SMD/ASM-MSCTS Composite Materials Committee.     

Texture and residual strain in two SiC/Ti-6-2-4-2 titanium composites

Residual strain and texture variations were measured in two titanium matrix composites reinforced with silicon carbide fibers (Ti/SiC) of similar composition but fabricated by different processing routes. Each composite comprised a Ti-6242 α/β matrix alloy containing vol 35 pct continuous SiC fibers. In one, the matrix was produced by a plasma sprayed (PS) route, and in the other by a wiredrawn (WD) process. The PS and WD composites were reinforced with SCS-6 (SiC) and Trimarc (SiC) fibers, respectively. The texture in the titanium matrices differed significantly. The titanium matrix for the PS material exhibited random texture pre and post fabrication of the composite. For the WD material, the starting texture of the monolithic titanium matrix was ≈17 times random, but after consolidation into composite form, it was ≈6 times random. No significant differences were noted in the fiber-induced matrix residual strains between the composites prepared by the two procedures. However, the Trimarc (WD) fibers recorded higher (≈1.3 times) compressive strains than the SCS-6 (PS) fibers. Stresses and stress balance results are reported. Plane-specific elastic moduli, measured in load tests on the unreinforced matrices, showed little difference. This article is based on a presentation made in the Symposium “Mechanisms and Mechanics of Composites Fracture” held October 11–15, 1998, at the TMS Fall Meeting in Rosemont, Illinois, under the auspices of the TMS-SMD/ASM-MSCTS Composite Materials Committee.     

Interface-controlled fatigue cracking of SCS-6/Ti-22Al-23Nb “orthorhombic” titanium aluminide composite

The effect of aging at elevated temperature on interfacial stability and fatigue behavior of a SCS-6/Ti-22Al-23Nb “orthorhombic” (O) titanium aluminide composite is investigated. The composite was heat treated in vacuum at 900 °C for up to 250 hours to change the microstructural characteristics. The stability of the matrix alloy and interfacial reaction zone after extended thermal exposure was analyzed. The effect of interface on fatigue behavior, including stiffness degradation, evolution of fatigue damage, and crack growth rates, was characterized. Finally, a modified shear-lag model was used to predict the saturated matrix crack spacing in the composite under fatigue loading. The results demonstrate that aging at elevated temperature affects the stability of the interfacial reaction zone, which, in turn, degrades the fatigue properties of the composite. However, fatigue crack will not develop from the ruptured interfacial reaction layer until the thickness of the reaction zone or the maximum applied stress exceeds a critical value.     

Role of matrix microstructure on room-temperature tensile properties and fiber-strength utilization of an orthorhombic ti-alloy-based composite

Microstructure-property understanding obtained for a nominally Ti-25Al-17Nb (at. pct) monolithic sheet alloy was used to heat treat a unidirectional four-ply SCS-6/Ti-25Al-17Nb metal-matrix composite (MMC) and a fiberless “neat” material of the same alloy for enhancing mechanical properties. The unreinforced alloy and [0]₄ composite recorded significant improvements in ductility and strength, which were related to the microstructural condition. Modeling of the tensile strength based on fiber fracture statistics helped in understanding how improved matrix microstructure provided more efficient utilization of fiber strength. In comparison to the [0]₄ MMC, improvement of the [90]₄ response was negligible, which was related to an α₂ stabilized zone around the fiber. A Nb coating on the fiber was used to modify the local microstructure, and it produced a modest improvement in strength and ductility in the transverse direction. Structure-property relations of the matrix under different heat-treatment conditions are described in terms of deformation and failure mechanisms of the constituent phases; α₂ (ordered hexagonal close-packed), B2 (ordered body-centered cubic), and O (ordered orthorhombic based on Ti₂AlNb).     

Transverse behavior and acoustic-emission analysis of titanium metal-matrix composites under tensile loading

The transverse behavior of 1140+/Ti-6-4 and SCS-6/Ti-β21s composites has been investigated using conventional tensile testing in air. Acoustic emission (AE) has also been used to assess and to locate the position of damage. Few AE events can be detected in 1140+/Ti-6-4 composites below the stress of ∼250 MPa, whereas for SCS-6/Ti-β21s composites, AE events are found almost immediately on loading. Many AE events of high energy were detected over a range of stresses, which appear to be associated with debonding. Continuous AE events are obtained with an increase of stress, and this suggests that debonding is an incremental process: a ring crack (formed by premature debonding at the surface) penetrates into the depth along interface “tubes.” The peak energy of AE events obtained in SCS-6/Ti-β21s composites is ∼650 arbitrary units, which is approximately 4 times that obtained in 1140+/Ti-6-4 composites. Distinct AE events have also been deduced to correspond to cracking of carbon coating layers and fiber/matrix reaction products. A change of fiber volume fraction from 8 to 21 pct for the 1140+/Ti-6-4 composites has no effect on the characteristics or distribution of AE events received.     

In-situ observations of titanium metal-matrix composites under transverse tensile loading

The transverse stress-strain behavior of several titanium metal-matrix composites (TiMMCs) has been studied in-situ. Debonding of 1140+/Ti-6-4 composites occurs over a range of stresses. The sharpness of the first “knee” is affected by the fiber volume fraction and by the relative moduli of the matrix regions and the reinforced composite. It has been observed that debonding occurs mainly at the interface between two sublayers of carbon/carbon coatings in 1140+/Ti-6-4 composites and mainly at the interface between the carbon/reaction zone in the as-processed and peak-aged 35 pct SCS-6/Tiβ21s composites. At surface positions, this process starts at very low stresses (≥50 MPa) from the positions with sharp changes of curvatures (or undulations), voids, or debris at the periphery of the interface. Cracking of the outermost carbon sublayer and of the reaction zone in the 1140+/Ti-6-4 composites and the reaction zone in the SCS-6/Tiβ21s composites occurs during elastic deformation of the matrix. This has been directly observed in a field-emission gun (FEG)-scanning electron microscope (SEM) under incremental loading. Although these cracks are arrested and blunted by the matrix material, they cause local stresses and, thus, stimulate local plastic deformation of the matrix and subsequent development of a second knee on the stress-strain curve. The in-situ observations are discussed in terms of the effects of fiber volume fraction and fiber type on the loci and dynamic processes of interfacial debonding, cracking of carbon coatings and reaction zones, and plastic deformation of the matrix.     

Comparison of orthorhombic and alpha-two titanium aluminides as matrices for continuous SiC-reinforced composites

The attributes of an orthorhombic Ti aluminide alloy, Ti-21Al-22Nb (at. pct), and an alpha-two Ti aluminide alloy, Ti-24Al-11Nb (at. pct), for use as a matrix with continuous SiC (SCS-6) fiber reinforcement have been compared. Foil-fiber-foil processing was used to produce both unreinforced (“neat”) and unidirectional “SCS-6” reinforced panels. Microstructure of the Ti-24A1-11Nb matrix consisted of ordered Ti₃Al (α ₂) + disordered beta(β), while the Ti-21 Al-22Nb matrix contained three phases: α₂, ordered beta (β ₀), and ordered orthorhombic(O). Fiber/ matrix interface reaction zone growth kinetics at 982 °C were examined for each composite system. Although both systems exhibited similar interface reaction products(i.e., mixed Ti carbides, silicides, and Ti-Al carbides), growth kinetics in theα ₂ +β matrix composite were much more rapid than in theO +β ₀ +α ₂ matrix composite. Additionally, interfacial reaction in theα ₂ +β} composite resulted in a relatively large brittle matrix zone, depleted of beta phase, which was not present in theO +β ₀+α ₂ matrix composite. Mechanical property measurements included room and elevated temperature tensile, thermal stability, thermal fatigue, thermo-mechanical fatigue (TMF), and creep. The three-phase orthorhombic-based alloy outperformed the α₂+β alloy in all of these mechanical behavioral areas, on both an absolute and a specific(i.e., density corrected) basis.     

Processing and mechanical properties of AI2O3 fiber-reinforced NiAl composites

The mechanical properties of NiAl-matrix composites reinforced with 125-μm diameter single-crystal A1₂O₃ (sapphire) fibers have been examined over the temperature range of 300 to 1200 K. Composites were fabricated with either a strong or weak fiber-matrix interfacial bond strength. During fabrication, a fiber-matrix interaction occurred such that fibers extracted from the NiAl matrix were fragmented and significantly weaker than the as-received fibers. Tensile results of the weakly bonded composite demonstrated that the composite stiffness was greater than the monolithic at both 300 and 1200 K in spite of the weak bond. Room-temperature strengths of the composite were greater than that of the monolithic but below rule-of-mixture predictions (even when the degraded fiber strengths were accounted for). At 1200 K, the ultimate strength of the composite was inferior to that of the monolithic primarily because of the poor fiber properties. No tensile data was obtained on the strongly bonded material because of the occurrence of matrix cracking during fabrication. Primarily because of the fiber strength loss, sapphire-NiAl composite mechanical properties are inferior to conventional high-temperature materials such as superalloys and are currently unsuitable for structural applications.     

Interface characterization of ceramic fiber-reinforced ti alloy composites manufactured by infrared processing

Interfacial reactions between several ceramic fibers (SCS-0, SCS-6, and carbon fibers) and a liquid titanium-nickel-copper alloy were investigated using electron microscopic analysis. Composite spec-imens were produced using a rapid infrared manufacturing (RIM) process. In SCS-O/Ti alloy com-posites, SiC dissolved in the alloy. The main reaction product was discontinuous agglomerates of titanium carbide which formed from the reaction between dissolved carbon and titanium. Polygonal precipitates of Ti₅Si₃, which are believed to have formed during cooling, were also noticed. Two distinct interface morphologies were observed in these composites: uniform fronts caused by iso-thermal dissolution and scalloped fronts formed as a result of an accelerated dissolution mechanism caused by localized heating. The presence of the accelerated dissolution mechanism suggests that SiC fibers cannot be infiltrated with liquid titanium alloys without applying a coating. In the C/Ti system, carbon fibers reacted with the liquid alloy to form a continuous layer of Ti_xC_1-x. Further growth of this layer occurred by the diffusion of carbon atoms across the reaction product. In SCS-6/Ti alloy composites, free carbon present in the coating formed a discontinuous layer of Ti^C,^, whereas SiC particles dissolved in the alloy. Due to channeled dissolution in the coating, the accel-erated dissolution mechanism was not observed in these composites. As a result, the presence of the carbon-rich coating prevented degradation of the fibers. Although the coating present on SCS-6 fibers moderately retarded reactions in the SiC/Ti alloy composite system during infrared liquid infiltration, it is recommended that the fibers be coated with pure carbon to effectively limit the attack of the fiber by molten titanium. Formaly Postdoctoral Fellow, Department of Materials Science and Engineering, University of Cincinnati     

Interface characterization of duplex metal-coated SiC fiber-reinforced Ti-15-3 matrix composites

The interfacial reaction behavior of duplex metal (Cu/Mo and Cu/W)-coated SiC (SCS-6) fiber-reinforced Ti-15-3 composites, before and after thermal exposure, has been studied. The effect of thermal exposure on the shear sliding resistance of these composites was also obtained using a thin-specimen push-out test. The results are compared to those of an original SiC (SCS-6) fiber-reinforced Ti-15-3 composite. The interfacial reaction behavior is strongly affected by the existence of a coating layer. Both the Cu/Mo and Cu/W coating layers prevent the growth of a reaction layer. However, the coatings could not effectively prevent diffusion of alloying elements; only the W layer exists after the thermal exposure. On the other hand, the interface shear sliding stress minimally depends on the duplex metal coating layers prior to the thermal exposure, and this sliding stress in both the SiC/Cu/Mo/Ti-15-3 and SiC/Cu/W/Ti-15-3 composites decreases slightly relative to that in the SiC/Ti-15-3 composite. After thermal exposure, the interface shear sliding stress increases for the SiC/Ti-15-3 composite. In distinction, the interface shear sliding stress significantly decreases after thermal exposure in both the SiC/Cu/Mo/Ti-15-3 and SiC/Cu/W/Ti-15-3 composites. Theses behaviors are attributed to the decrease of radial clamping stress, which originates from a volume expansion associated with the β → α phase transformation.     

The transverse creep deformation and failure characteristics of SCS-6/Ti-6AI-4V metal matrix composites at 482 °C

While continuous fiber, unidirectional composites are primarily evaluated for their longitudinal properties, the behavior transverse to the fibers often limits their application. In this study, the tensile and creep behaviors of SCS-6/Ti-6Al-4V composites in the transverse direction at 482 °C were evaluated. Creep tests were performed in air and argon environments over the stress range of 103 to 276 MPa. The composite was less creep resistant than the matrix when tested at stress values larger than 150 MPa. Below 150 MPa, the composite was more creep resistant than the unreinforced matrix. Failure of the composite occurred by the ductile propagation of cracks emanating from separated fiber interfaces. The environment in which the test was performed affected the creep behavior. At 103 MPa, the creep rate in argon was 4 times slower than the creep rate in air. The SCS-6 silicon-carbide fiber’s graphite coating oxidized in the air environment and encouraged the separation of the fiber-matrix interface. However, at higher stress levels, the difference in behavior between air- and argon-tested specimens was small. At these stresses, separation of the interface occurred during the initial loading of the composite and the subsequent degradation of the interface did not affect the creep behavior. Finally, the enrichment of the composite’s surface by molybdenum during fabrication resulted in an alloyed surface layer that failed in a brittle fashion during specimen elongation. Although this embrittled layer did not appear to degrade the properties of the composite, the existence of a similar layer on a composite with a more brittle matrix might be very detrimental.     

Effect of interfacial debonding and sliding on matrix crack initiation during isothermal fatigue of SCS-6/Ti-15-3 composites

Direct observation of initial damage-evolution processes occurring during cyclic testing of an unnotched SCS-6 fiber-reinforced Ti-15-3 composite has been carried out. The aligned fibers break at an early stage, followed by debonding and subsequent sliding along the interface between the reaction layer (RL) and Ti-15-3 alloy matrix. Matrix cracking initiation from the initial broken fiber and RL was avoided. This fracture behavior during cyclic loading is modeled and analyzed by the finite-element method, with plastic deformation of the matrix being considered. The plastic strain in the matrix at the initial crack and at the deflected crack tips, when the interface crack is deflected into the RL after extensive interface debonding propagation, is characterized. The effects of interfacial debond lengths and test temperatures on the matrix cracking mechanism are discussed, based on a fatigue-damage summation rule under low-cycle fatigue conditions. The numerical results provide a rationale for experimental observations regarding the avoidance and occurrence of the matrix cracking found in fiber-reinforced titanium composites.     

Materials characterization of silicon carbide reinforced titanium (Ti/SCS-6) metal matrix composites: Part I. Tensile and fatigue behavior

Flexural fatigue behavior was investigated on titanium (Ti-15V-3Cr) metal matrix composites reinforced with cross-ply, continuous silicon carbide (SiC) fibers. The titanium composites had an eightply (0, 90, +45, -45 deg) symmetric layup. Fatigue life was found to be sensitive to fiber layup sequence. Increasing the test temperature from 24 °C to 427 °C decreased fatigue life. Interface debonding and matrix and fiber fracture were characteristic of tensile behavior regardless of test temperature. In the tensile fracture process, interface debonding between SiC and the graphite coating and between the graphite coating and the carbon core could occur. A greater amount of coating degradation at 427 °C than at 24 °C reduced the Ti/SiC interface bonding integrity, which resulted in lower tensile properties at 427 °C. During tensile testing, a crack could initiate from the debonded Ti/SiC interface and extend to the debonded interface of the neighboring fiber. The crack tended to propagate through the matrix and the interface. Dimpled fracture was the prime mode of matrix fracture. During fatigue testing, four stages of flexural deflection behavior were observed. The deflection at stage I increased slightly with fatigue cycling, while that at stage II increased significantly with cycling. Interestingly, the deflection at stage III increased negligibly with fatigue cycling. Stage IV was associated with final failure, and the deflection increased abruptly. Interface debonding, matrix cracking, and fiber bridging were identified as the prime modes of fatigue mechanisms. To a lesser extent, fiber fracture was observed during fatigue. However, fiber fracture was believed to occur near the final stage of fatigue failure. In fatigued specimens, facet-type fracture appearance was characteristic of matrix fracture morphology. Theoretical modeling of the fatigue behavior of Ti/SCS-6 composites is presented in Part II of this series of articles. This article is based on a presentation made in the symposium entitled “Creep and Fatigue in Metal Matrix Composites” at the 1994 TMS/ASM Spring meeting, held February 28–March 3, 1994, in San Francisco, California, under the auspices of the Joint TMS-SMD/ASM-MSD Composite Materials Committee.     

Degradation of residual strength in SCS-6/Ti-15-3 Due to fully reversed fatigue

Little attention has been given to residual strength degradation in titanium matrix composites (TMCs) after exposure to fatigue loading. To address this problem, fatigue tests on SCS-6/Ti-15-3 were performed to investigate the fatigue life and residual strength behavior of TMCs with different fiber volume fractions. Results indicate that fiber volume fraction seems to have an effect on both of these quantities. Lower fiber percentages result in a material where the characteristics of the matrix, such as hardening or cracking, play a much larger role in the composite response. Fatigue lives were not affected by fiber volume fraction at higher strain ranges, but lower fiber volume fractions resulted in shorter fatigue lives at lower strain values. Also, a slight increase in residual strength occurred up to 75 pct of fatigue life, for the lower-fiber volume fraction material. Despite these distinctions between specimens with different fiber contents, all specimens tested retained the majority of their strength prior to failure. This article is based on a presentation made in the symposium “Fatigue and Creep of Composite Materials” presented at the TMS Fall Meeting in Indianapolis, Indiana, September 14–18, 1997, under the auspices of the TMS/ASM Composite Materials Committee.     

Infrared transient-liquid-phase joining of SCS-6/β21S titanium matrix composite

Fiber-reinforced titanium matrix composites (TMCs) are among the advanced materials being considered for use in the aerospace industry due to their light weight, high strength, and high modulus. A rapid infrared joining process has been developed for the joining of composites and advanced materials. Rapid infrared joining has been shown not to have many of the problems associated with conventional joining methods. Two models were utilized to predict the joint evolution and fiber reaction zone growth. Titanium matrix composite, 16-ply SCS-6/β21S, has been successfully joined with total processing times of approximately 2 minutes, utilizing the rapid infrared joining technique. The process utilizes a 50 °C/s ramping rate, 17-μm Ti-15Cu-15Ni wt pct filler material between the faying surfaces; a joining temperature of 1100 °C; and 120 seconds of time to join the composite material. Joint shear-strength testing of the rapid infrared joints at temperatures as high as 800 °C has revealed no joint failures. Also, due to the rapid cooling of the process, no poststabilization of the matrix material is necessary to prevent the formation of a brittle omega phase during subsequent use of the TMC at intermediate temperatures, 270 °C to 430 °C, for up to 20 hours.     

A comparison of the mechanical properties and microstructures of intermetallic matrix composites fabricated by two different methods

The tensile properties of SCS-6 SiC fiber-reinforced Ti-24Al-11Nb (at. pct) have been measured over the past several years by a number of investigators. These composites have been fabricated by different techniques and tend to exhibit a large amount of scatter in the longitudinal tensile properties. To date, it is not known if one optimized fabrication method provides composites with improved mechanical properties over those produced by other optimized methods, since carefully controlled experiments have not been performed to determine this. Thus, the purpose of the present study was to compare the longitudinal tensile strengths of SCS-6 SiC/ Ti-24Al-11Nb composites that had been fabricated by the powder-cloth method and the lowpressure plasma spray (LPPS) method. In this study, the same lots of matrix powder and reinforcing fiber were used for fabricating the composites. It was determined that the powder-cloth and plasma spray methods produced composites having very similar tensile properties. Both fabrication methods induced damage in a small percentage of fibers, which manifested itself in the form of bimodal Weibull distributions of extracted fiber strengths. It appeared that the particular lot of SCS-6 fiber used in fabricating both types of composites was more susceptible to fabrication damage than those used in previous studies. This article also shows the dramatic effect that different handling and testing techniques can have on measured fiber strengths.     

Fatigue crack growth in Ti-matrix composites with spatially varied interfaces

Spatially varied interfaces (SVIs) is a design concept for composite materials where the interface mechanical properties are varied along the length and circumference of the fiber/matrix interface. These engineered interfaces can be used to modify critical titanium matrix composite properties such as transverse tensile strength and fatigue crack growth resistance in ways that produce a balanced set of properties. The SVI approach may also be used to probe interface failure mechanisms for the purpose of understanding complex mechanical phenomena. Single lamina Ti-6Al-4V matrix composites containing strongly bonded SiC fibers were fabricated both in the as-received condition and with a weak longitudinal stripe along the sides of the fibers. The striped SVI composites exhibited an increase in the overall fatigue crack growth life of the specimens compared to the unmodified specimens. This improvement was caused by an increased extent of debonding and crack bridging in SVI composites. This article is based on a presentation made in the symposium “Fatigue and Creep of Composite Materials” presented at the TMS Fall Meeting in Indianapolis, Indiana, September 14–18, 1997, under the auspices of the TMS/ASM Composite Materials Committee.