Oxidation behavior of single-crystal Al2O3-fiber-reinforced Ni3Al-based composites

A series of single-crystal Al₂O₃-fiber-reinforced Ni3Al-based intermetallic matrix composites were fabricated by pressure casting. The matrices employed were binary Ni₃Al, Ni₃Al-0.5 at. pct Cr, and Ni₃Al-0.34 at. pct Zr. The development of microstructure upon oxidation in air at either 1100 °C or 1200 °C was investigated by optical, scanning, and transmission electron microscopy. In air-oxidized binary Ni₃Al, some of the fibers were fully or partially covered with a layer of oxide. A weak fiber/matrix bond in this system, which led to fiber debonding during composite processing, is believed to be responsible for the ingress of O into the composite and oxidation of the matrix in the debonded regions at the fiber/matrix interface. Addition of Cr to Ni₃Al resulted in an almost threefold increase in fiber/matrix bond strength. No oxidation of the interface was observed. A thick layer of oxide was formed around all the fibers when the composite was thermally cycled prior to isothermal annealing. Addition of Zr to Ni₃Al resulted in the formation of a layer of ZrO₂ on the surface of the fibers during composite processing. The ZrO₂ layer provided a fast path for the diffusion of O, which led to the formation of a rootlike oxide structure around the fibers. The rootlike structure consisted of a network of Al₂O₃-covered ZrO₂.     

Interface nanochemistry effects on stainless steel diffusion bonding

The diffusion-bonding behavior of single-phase austenitic stainless steel depends strongly on the chemistry of the surfaces to be bounded. We found that very smooth (0.5 nm root-mean-square (RMS) roughness), mechanically polished and lapped substrates would bond completely in ultrahigh vacuum (UHV) in 1 hour at 1000 °C under 3.5 MPa uniaxial pressure, if the native oxide on the substrates was removed by ion-beam cleaning, as shown by in-situ Auger analysis. No voids were observed in these bonded interfaces by transmission electron microscopy (TEM), and the strength was equal to that of the unbounded bare material. No bond formed between the substrates if in-situ ion cleaning was not used. The rougher cleaned substrates partially bonded, indicating that roughness, as well as native oxides, reduced the bonding kinetics.     

Microstructural and mechanical assessment of transient liquid phase bonded commercially pure titanium

Diffusion joining of commercially pure titanium was successfully prepared via transient liquid phase bonding in vacuum environment. The process was carried out using AMS 4772 silver-based filler alloy at 900–1000°C for various holding time under the vacuum of 6?×?10^?7?Torr. Optical and scanning electron microscopy equipped with an EDS analyzer was conducted for microstructural evaluations. Mechanical properties were also investigated by shear test, fractographic assessment and X-ray diffraction analyses. The tendency to achieve isothermally solidified joint increased by increasing bonding time. No sign of athermal solidification was detected of sample bonded at 1000°C for 90?min. Consequently, the bonding condition of a high quality joint was obtained. Elemental analyses revealed that filler alloy’s elements (Ag, Cu) distributed more uniformly in fully isothermal solidified bond, whereas the aggregation of these elements is considerable in athermally solidified bond. Shear test results represented that the highest shear strength attributed to the sample bonded in isothermal solidified condition (bonded at 1000°C for 90?min).     

Microstructural control of toughness in aluminium-lithium alloys

Investigation of the deformation behaviour of AlLi based alloys containing zirconium as a grain-refining addition shows that the poor toughness properties are attributed to the intense coplanar slip associated with δ' (Al₃Li) precipitation being unimpeded by the grain structure as a result of the pronounced deformation texture present in the sheet product; fracture proceeds via a transgranular shear failure mode which limits toughness. Changes in composition and thermomechanical treatment have been utilised in order to encourage the formation of additional precipitate phases, and, whilst δ' confers the major increment of strength to all AlLi based alloys, widespread precipitation of S phase (Al₂CuMg) within AlLiMgCuZr alloys is shown to influence strongly the deformation behaviour; in particular the propensity towards slip coplanarity is reduced, and significant improvements in toughness are obtained. Additionally, by promoting homogeneous deformation within the grain structure, the presence of S phase causes the material to display isotropic properties even though a strong texture remains in the zirconium-refined sheet product.     

Diffusion Bonding of Microduplex Stainless Steel and Ti Alloy with and without Interlayer: Interface Microstructure and Strength Properties

The interface microstructure and strength properties of solid state diffusion bonding of microduplex stainless steel (MDSS) to Ti alloy (TiA) with and without a Ni alloy (NiA) intermediate material were investigated at 1173 K (900 °C) for 0.9 to 5.4 ks in steps of 0.9 ks in vacuum. The effects of bonding time on the microstructure of the bonded joint have been analyzed by light optical microscopy and scanning electron microscopy in the backscattered mode. In the direct bonded joints of MDSS and TiA, the layer-wise σ phase and the λ + FeTi phase mixture were observed at the bond interface when the joint was processed for 2.7 ks and above holding times. However, when NiA was used as an intermediate material, the results indicated that TiNi₃, TiNi, and Ti₂Ni are formed at the NiA-TiA interface, and the irregular shaped particles of Fe₂₂Mo₂₀Ni₄₅Ti₁₃ have been observed within the TiNi₃ intermetallic layer. The stainless steel-NiA interface is free from intermetallics and the layer of austenitic phase was observed at the stainless steel side. A maximum tensile strength of ~520 MPa, shear strength of ~405 MPa, and impact toughness of ~18 J were obtained for the directly bonded joint when processed for 2.7 ks. However, when nickel base alloy was used as an intermediate material in the same materials, the bond tensile and shear strengths increase to ~640 and ~479 MPa, respectively, and the impact toughness to ~21 J when bonding was processed for 4.5 ks. Fracture surface observations in scanning electron microscopy using energy dispersive spectroscopy demonstrate that in MDSS-TiA joints, failure takes place through the FeTi + λ phase when bonding was processed for 2.7 ks; however, failure takes place through σ phase for the diffusion joints processed for 3.6 ks and above processing times. However, in MDSS-NiA-TiA joints, the fracture takes place through NiTi₂ layer at the NiA-TiA interface for all bonding times.     

Diffusion Bonding of 17-4 Precipitation Hardening Stainless Steel to Ti Alloy With and Without Ni Alloy Interlayer: Interface Microstructure and Mechanical Properties

In the present study, the diffusion bonding of 17-4 precipitation hardening stainless steel to Ti alloy with and without nickel alloy as intermediate material was carried out in the temperature range of 1073 K to 1223 K (800 °C to 950 °C) in steps of 298 K (25 °C) for 60 minutes in vacuum. The effects of bonding temperature on interfaces microstructures of bonded joint were analyzed by light optical and scanning electron microscopy. In the case of directly bonded stainless steel and titanium alloy, the layerwise α-Fe + χ, χ, FeTi + λ, FeTi + β-Ti phase, and phase mixture were observed at the bond interface. However, when nickel alloy was used as an interlayer, the interfaces indicate that Ni₃Ti, NiTi, and NiTi₂ are formed at the nickel alloy-titanium alloy interface and the PHSS-nickel alloy interface is free from intermetallics up to 1148 K (875 °C) and above this temperature, intermetallics were formed. The irregular-shaped particles of Fe₅Cr₃₅Ni₄₀Ti₁₅ have been observed within the Ni₃Ti intermetallic layer. The joint tensile and shear strength were measured; a maximum tensile strength of ~477 MPa and shear strength of ~356.9 MPa along with ~4.2 pct elongation were obtained for the direct bonded joint when processed at 1173 K (900 °C). However, when nickel base alloy was used as an interlayer in the same materials at the bonding temperature of 1148 K (875 °C), the bond tensile and shear strengths increase to ~523.6 and ~389.6 MPa, respectively, along with 6.2 pct elongation.     

Structure and mechanism of bonding at a diffusion-bonded Al/SiC interface

Al/SiC interfaces were fabricated by diffusion bonding a pure Al foil between two blocks of SiC for temperatures ranging from 500 to 600°C. For samples bonded below 586°C, the interfacial strength was low and TEM speciments could not be fabricated due to separation of the Al and SiC pieces dring thinning. For samples bonded at and above 586°C, a strong bond was formed and conventional and high-resolution transmission electron microscopy revealed the formation of a thin amorphous phase at the interface. Compositional analysis showed that the interfacial phase contained Al, Si, C and O. Formation of the amorphous phase was demonstrated to occur by a solid state reaction and is discussed on the basis of thermodynamic and kinetic considerations. Lastly, some of the advantages of having an amorphous phase at a metal/ceramic interface are discussed.     

Effect of Bonding Temperature on Interfacial Reaction and Mechanical Properties of Diffusion-Bonded Joint Between Ti-6Al-4V and 304 Stainless Steel Using Nickel as an Intermediate Material

An investigation was carried out on the solid-state diffusion bonding between Ti-6Al-4V (TiA) and 304 stainless steel (SS) using pure nickel (Ni) of 200-μm thickness as an intermediate material prepared in vacuum in the temperature range from 973 K to 1073 K (700 °C to 800 °C) in steps of 298 K (25 °C) using uniaxial compressive pressure of 3 MPa and 60 minutes as bonding time. Scanning electron microscopy images, in backscattered electron mode, had revealed existence of layerwise Ti-Ni-based intermetallics such as either Ni₃Ti or both Ni₃Ti and NiTi at titanium alloy-nickel (TiA/Ni) interface, whereas nickel-stainless steel (Ni/SS) diffusion zone was free from intermetallic phases for all joints processed. Chemical composition of the reaction layers was determined in atomic percentage by energy dispersive spectroscopy and confirmed by X-ray diffraction study. Room-temperature properties of the bonded joints were characterized using microhardness evaluation and tensile testing. The maximum hardness value of ~800 HV was observed at TiA/Ni interface for the bond processed at 1073 K (800 °C). The hardness value at Ni/SS interface for all the bonds was found to be ~330 HV. Maximum tensile strength of ~206 MPa along with ~2.9 pct ductility was obtained for the joint processed at 1023 K (750 °C). It was observed from the activation study that the diffusion rate at TiA/Ni interface is lesser than that at the Ni/SS interface. From microhardness profile, fractured surfaces and fracture path, it was demonstrated that failure of the joints was initiated and propagated apparently at the TiA/Ni interface near Ni₃Ti intermetallic phase.     

The diffusion bonding of Zr-2.5 pct Nb to steel

The diffusion bonding of zirconium-2.5 pct niobium to carbon steel with an interlayer of platinum has been investigated. Bonds were produced by heating samples in a furnace under compressive loading. Metallography of the bonds revealed that at both the Fe-Pt and the Pt-Zr/Nb interfaces, interdiffusion and the formation of thin bands of intermetallic phases occurred during bonding. The presence of FePt₃ was detected at the former interface and several intermetallics including Pt₃Zr at the latter. In both cases, intermetallic compound formation resulted in an increase in microhardness in the bond region; this was particularly severe at the Pt-Zr/Nb interface where cracking was observed to occur during, metallographic sample preparation. Bonding at temperatures above 1150 °C caused eutectic melting at the Pt-Zr/Nb interface.     

Effect of Bonding Temperature on Microstructure and Mechanical Properties of WC–Co/Steel Diffusion Brazed Joint

In this work, the diffusion brazing of AISI 4145 steel to WC–Co cemented carbide using RBCuZn-D interlayer with bonding temperature values of 930, 960, 990 and 1020 °C was studied. The microstructure of the joint zone was evaluated by scanning electron microscope (SEM) and X-ray diffraction (XRD). Vickers microhardness and shear strength tests were performed to investigate mechanical behaviors of the brazed joints. The XRD and SEM results indicated that with increase of bonding temperature, the elements readily diffused along the interface and formed various compounds such as γ, α and β and Co₃W₃C. The results also showed that with the increase of bonding temperature from 930 to 960 °C, a sound metallurgical bond was produced, however in higher bonding temperatures (990 and 1020 °C) a decrease in mechanical properties of the joints was observed which could be due to the excessive zinc evaporation, interface heterogeneity and voids formation. The maximum shear strength of 425 MPa was obtained for the bond made at 960 °C.     

Effect of reaction products on mechanical properties of diffusion bonded of titanium to 304 stainless steel with Cu interlayer joints

In present study, pure copper was used as an interlayer of the diffusion bonded joints between commercially pure titanium and 304 stainless steel. The process was carried out at 900°C for 30–150 minutes in steps of 30 minutes under 3MPa uniaxial load in vacuum. Microstructures of the bonded assemblies were observed in optical and scanning electron microscopes. The study exhibits the presence of different reaction layers in the diffusion zone and their chemical compositions were determined by energy dispersive spectroscopy. Formation of reaction products in diffusion interfaces were confirmed by xray diffraction technique. The maximum tensile strength of ∼322MPa (∼101% of Ti) and shear strength of ∼254MPa (∼86% of Ti) along with 8.4 % ductility were obtained for the couple bonded for 60 minutes and due to the rise in bonding time up to 90 minutes, bond strength drops marginally. With a further increase in joining time, the bond strength drops gradually due to the increase in the width of Fe-Ti base reaction products. Observation of fracture surfaces in SEM using EDS indicated that fracture takes place through the SS-Cu interface for all bonded samples.     

Interfacial microstructure and mechanical properties of diffusion-bonded joints of titanium TC4 (Ti-6Al-4V) and Kovar (Fe-29Ni-17Co) alloys

Diffusion bonding is a near net shape forming process that can join dissimilar materials through atomic diffusion under a high pressure at a high temperature.Titanium alloy TC4(Ti-6 Al-4 V)and 4 J29 Kovar alloy(Fe-29 Ni-17 Co)were diffusely bonded by a vacuum hot-press sintering process in the temperature range of 700-850°C and bonding time of 120 min,under a pressure of 34.66 MPa.Interfacial microstructures and intermetallic compounds of the diffusion-bonded joints were characterized by optical microscopy,scanning electron microscopy,X-ray diffraction(XRD)and energy dispersive spectroscopy(EDS).The elemental diffusion across the interface was revealed by electron probe microanalysis.Mechanical properties of joints were investigated by micro Vickers hardness and tensile strength.Results of EDS and XRD indicated that(Fe,Co,Ni)-Ti,TiNi,Ti_2Ni,TiNi_2,Fe_2 Ti,Ti_(17) Mn_3 and Al_6 Ti_(19) were formed at the interface.When the bonding temperature was raised from 700 to 850°C,the voids of interface were reduced and intermetallic layers were widened.Maximum tensile strength of joints at 53.5 MPa was recorded by the sintering process at 850°C for 120 min.Fracture surface of the joint indicated brittle nature,and failure took place through interface of intermetallic compounds.Based on the mechanical properties and microstructure of the diffusion-bonded joints,diffusion mechanisms between Ti-6 Al-4 Vtitanium and Fe-29 Ni-17 Co Kovar alloys were analyzed in terms of elemental diffusion,nucleation and growth of grains,plastic deformation and formation of intermetallic compounds near the interface.     

Phase composition and mechanical properties of a zirconium dioxide based ceramic obtained by high temperature sintering in a vacuum

Changes in phase composition and mechanical properties of sintered ZrO₂ + 3% (mole) Y₂O₃ specimens were examined after annealing in air and after various mechanical operations. Compacted ceramic specimens containing T and T′ phase were obtained by sintering in a vacuum at 1800°C. Ceramics containing T and T′ phases have excellent toughness (K_1c up to 15 MPa·m^1/2), bend strength up to 800 MPa and HV hardness up to 13 GPa.     

Correlation of mechanical properties with nondestructive evaluation of babbitt metal/bronze composite interface

Interfaces of the babbitt metal-bronze composite were examined ultrasonically and were fractured using the Chalmers test method. It was found that the ultrasonic results correlated with the bond strength, the ductility, and the degree of bonding at the tested interface. Specifically, high ultrasonic reflection percentages were associated with low bond strength, low ductility, and low percentages of bonded regions. The fracture mechanism in the bonded area of the babbitt-bronze interface is related to the presence of the intermetallic compound, Cu₆Sn₅, at the interface. It is suggested that the non-destructive ultrasonic technique can detect the bond integrity of babbitted metals.     

Effect of Y2O3 stabilized ZrO2 coating with tri-model structure on bi-layered thermally grown oxide evolution in nano thermal barrier coating systems at elevated temperatures

Bi-layered thermally grown oxide(TGO) layer plays a major role in the spallation of Y2 O3 stabilized ZrO2(YSZ) layer form the bond coat in the thermal barrier coating(TBC) systems during oxidation. On the other hand, bi-layered TGO formation and growth in the TBC systems with nanostructured YSZ have not been deeply investigated during cyclic oxidation. Hence, Inconel 738/NiCrAlY/normal YSZ and Inconel 738/NiCrAlY/nano YSZ systems were pre-oxidized at 1000 °C and then subjected to cyclic oxidation at 1150 °C. According to microstructural observations, nanostructured YSZ layer over the bond coat should have less micro-cracks and pinholes, due to the compactness of the nanostructure and the presence of nano zones that resulted in lower O infiltration into the nanothermal barrier coating system, formation of thinner and nearly continuous mono-layered thermally grown oxide on the bond coat during pre-oxidation, lower spinels formation at the Al2 O3 /YSZ interface and finally, reduction of bi-layered thermally grown oxide thickness during cyclic oxidation. It was found that pre-heat treatment and particularly coating microstructure could influence microstructural evolution(bi-layered TGO thickness) and durability of thermal barrier coating systems during cyclic oxidation.     

Oxidation processes for alloys in the Ni - Zr system. III. Oxidation of NiZr

We used the continuous weighing method to study the oxidation kinetics in air for the alloy NiZr at 500–1000°C. We used x-ray diffraction and metallography for layer-by-layer phase analysis of the scale. We have established that the oxidation kinetics is described by a parabolic equation q² = K_pτ (where q is the mass gain per unit area of the sample, K_p is the rate constant, τ is the time). The value of K_p periodically decreased on the kinetic isotherms. In the scale, the phase components are distributed over the layers as follows: top layer, cubic and monoclinic ZrO₂, NiO; inner layer, monoclinic ZrO₂, Ni, and (or) Ni₅Zr. At the boundary with the scale, the alloy layer (underscale) is depleted in zirconium. We have established that oxidation of NiZr is accomplished by predominant diffusion of oxygen through the oxygen vacancies in the lattice of monoclinic ZrO₂. The decrease in q and K_p as the temperature rises from 600°C to 850°C is explained by a reduced concentration of these vacancies and (or) slowdown of their mobility. For T ≥ 850°C, the oxidation mechanism changes: counterdiffusion of Zr⁴⁺ also occurs through interstices in the lattice of monoclinic ZrO₂. The outer layer (NiO), saturated by zirconium dioxide, loses any protective properties and diffusion of oxygen is facilitated. For this reason, both q and K_p increase as the temperature rises to 1000°C.     

Oxidation Processes for Alloys in the Ni – Zr System. Part 2. Phase Composition of Scale Formed on Ni7Zr2

We have used x-ray and metallographic layer-by-layer phase analysis to study the structure and composition of scale formed on the alloy Ni₇Zr₂ during its oxidation in air over a period of 1 h and 10 h in the temperature range 500-1200°C. In the scale we find NiO, the cubic and monoclinic modifications of ZrO₂, and also Ni and Ni₅Zr. The phase components are nonuniformly distributed over the thickness of the scale. The outer scale consists of the oxides NiO and ZrO₂, while the composition of the inner scale includes Ni and Ni₅Zr in addition to monoclinic ZrO₂. Cubic ZrO₂ is formed on the surface of the specimen in the initial stages of its oxidation at 500-700°C. For T ≥ 900°C, on the surface of the scale we find both modifications of ZrO₂, while the nickel phase is itself a solid solution Ni(Zr). We note that the mechanisms for the formation of low-temperature (T ≤ 800°C) and high-temperature (T ≥ 900°C) scales are different. It is hypothesized that these differences are determined mainly by the fact that at high temperatures, diffusion of zirconium ions toward the outer boundary of the scale is superimposed on diffusion of oxygen toward the scale – alloy boundary.     

Characterization of Vacuum Plasma Sprayed Reinforced Hydroxyapatite Coatings on Ti–6Al–4V alloy

Two reinforced hydroxyapatite (HA) coatings with an intermediate layer of zirconia were deposited on Ti–6Al–4V by vacuum plasma spray (VPS) technique. In first coating, HA was reinforced with 10 wt % Al₂O₃ whereas in second coating, HA was reinforced with 10 wt % ZrO₂. The objective of this study was to investigate the microstructure, phase formation and mechanical properties like hardness and bond strength of as-sprayed coatings and the coatings after post coating heat treatment at 700 °C for 1 h. The characterization of the coatings was performed by using SEM/EDAX, XRD, porosity, crystallinity and roughness measurement. The coatings were also evaluated for mechanical properties like hardness and tensile bond strength. It was observed that after post coating heat treatment, crystallinity increased and porosity decreased which indicated recrystallization of amorphous phases of as-sprayed coatings. Heat treatment resulted into improvement in cross-sectional hardness, however sharp decrease in bond strength was observed.     

Wettability and interfacial bonding in AuSi/SiC system

Using the sessile drop method under vacuum, the wettability of monocrystalline α-SiC by AuSi alloys is studied at 1373 K. Additions of Si to Au lead to a strong decrease of the contact angle from θ ⪢ 90° toθ ⪡ 90°. This effect is obtained without significant reactivity and is due to adsorption of Si at the Au/SiC interface, with the formation of a strong chemical bond localised at the interface. Experimental evidence is given showing that oxygen, present in the furnace as an impurity, reinforces the beneficial effect of Si on wetting and can lead to nearly perfect wetting.