The effects of metal coating on the diffusion bonding in Al2O3/Inconel 600 and the modulus of rupture strength of alumina

Alumina with a sputter-deposited metal film was diffusion bonded to Inconel 600. A higher bonding strength and lower joining temperature were obtained with titanium coating compared to that for the non-coated sample. The improved joining behaviour was attributed to an enhanced interface reaction and reduction in the thermal stress. Also, the effect of various coatings of 3 m thickness on the mechanical property of alumina after heat treatment at 1000 °C for 30 min under 10^–6 torr vacuum was evaluated in terms of modulus of rupture (MOR) using a Weibull plot. While the Cu coating did not change MOR strength of alumina, the reactive Ti and Zr metal coatings caused a noticeable reduction in averaged MOR strength. The effect of co-sputtering of Ti-Cu, and bilayer coatings of Cu/Ti and Ti/Cu was also investigated.     

Ceramic joining IV. effects of processing conditions on the properties of alumina joined via Cu/Nb/Cu interlayers

Multilayer copper/niobium/copper interlayers consisting of 3 m thick cladding layers of copper on a 125 m thick niobium core layer were used to join aluminum oxides at 1150°C or 1400°C, or both. Three microstructurally distinct aluminum oxides were joined—a 25 m grain size 99.5% pure alumina, a submicron grain size 99.9% pure alumina, and single crystal sapphire. Two-phase interlayer microstructures containing both copper-rich and niobium-rich phases developed during bonding. In some cases, the initially continuous copper film evolved via Rayleigh instabilities into an array of discrete copper-rich particles along the interlayer/alumina interface with concurrent increases in the niobium/alumina contact area. Processing conditions (temperature and applied load) and the alumina microstructure (grain size) impacted the extent of film breakup, the morphologies of the copper-rich and niobium-rich phases, the interlayer/alumina interfacial microstructure, and thereby the strength characteristics. Joints possessing a large copper/alumina interfacial area fraction were comparatively weak. Increases in bonding pressure and especially bonding temperature yielded interfaces with higher fractional niobium/alumina contact area. For joined polycrystals, such microstructures resulted in higher and more consistent room temperature fracture strengths. Joined 99.9% alumina polycrystals retained strengths >200 MPa to 1200°C. Relationships between processing conditions, interlayer and ceramic microstructure, and joint strength are discussed.     

Diffusion bonding of zirconia to silicon nitride using nickel interlayers

The possibilities of diffusion bonding of zirconia to silicon nitride using a nickel interlayer were studied by carrying out bonding experiments under various processing conditions. The process parameters considered were temperature, bonding pressure and interlayer thickness. The optimal process conditions were determined by evaluating the mechanical strength using shear strength testing. It was found that the bonding is optimal in the temperature range 1000–1100°C. The bond strength appears to be independent of the bonding pressure and interlayer thickness if threshold values are exceeded (bonding pressure >14 MPa, interlayer thickness >0.2 mm). At the Si3N4 Ni interface, Si3N4 decomposes, forming a solid solution of silicon in nickel. At the ZrO2–Ni interface, no reaction was observed. © 1998 Kluwer Academic Publishers     

Analysis of interfacial fracture in ceramic–metal assemblies under effect of thermal residual stresses

In this study, the finite element method is used to analyze the behavior of interface cracks in ceramic–metal assemblies under the effect of thermal residual stresses. These stresses are due to the elaboration process of the bimaterial junctions. The stress intensity factor is used as fracture criterion. The effects of the temperature of elaboration and the metal thickness on the variations of the thermal SIF are highlighted. The obtained results show that the mode of fracture under thermal residual stresses for all ceramic–metal couples is the mixed mode (opening + sliding). The mode II (the sliding mode) is the dominant mode.     

Effect of particles and interface conditions on fibrous tissue interposition between bone and implant. A particle challenge model in rabbit

Interposed fibrous tissue at bone–implant interfaces was quantitatively measured in the presence or absence of polyethylene (PE) or alumina particles. Three different conditions of the interface were designed by implanting a pre-polymerized polymethylmethacrylate (PMMA) plug (plug group), a doughy PMMA (injection group) and a hydroxyapatite (HA) plug (HA group) in the hole drilled at the intercondylar notch of rabbit knees. PE (170±18 m) or alumina particles (88±26 m) were repeatedly administered into the knee joints at one month intervals (six times). All animals were sacrificed seven months after the implantation. The bone–implant interface was histomorphometrically examined using undecalcified ground sections. In the plug group, the PE particles significantly increased the extent of the interposed fibrous tissue (p < 0.05), while the alumina particles showed no effect. In contrast, both particles showed no significant effects in the injection and the HA groups. These results indicate that both particle characteristics and conditions of the bone–implant interface affected particle-induced fibrous tissue interposition. The loose PMMA plug with PE particles induced the greatest amount of fibrous tissue interposition. ©2000 Kluwer Academic Publishers     

Effect of loading rate on the monotonic tensile behavior and tensile strength of an oxide–oxide ceramic composite at 1200 °C

The influence of loading rate on monotonic tensile behavior and tensile properties of an oxide–oxide ceramic composite was evaluated in laboratory air at 1200 °C. The composite consists of a porous alumina matrix reinforced with woven mullite/alumina (Nextel™720) fibers, has no interface between the fiber and matrix, and relies on the porous matrix for flaw tolerance. Tensile tests conducted at loading rates of 0.0025 and 25 MPa/s revealed a strong effect of rate on the stress–strain behavior as well as on the ultimate tensile strength (UTS), elastic modulus and failure strain. At 0.0025 MPa/s, increase in stress results in non-monotonic change in strain, with the rate of change of strain reversing its sign at stresses 25 MPa/s. Several samples were subjected to additional heat treatments prior to testing in order to determine whether this unusual stress–strain behavior was an artifact of incomplete processing of fibers in the as-received material. The unusual material response in the 0–30 MPa stress range was further investigated in creep tests conducted with the applied stresses ≤26 MPa. Negative creep (i.e. decrease in strain under constant stress) was observed. Porosity measurements indicate that a decrease in matrix porosity and matrix densification may be taking place in the N720/A composite exposed to 1200 °C at stresses <30 MPa for prolonged periods of time.     

Adherence-fracture energy of a glass-bonded thick-film conductor: effect of firing conditions

The effect of firing conditions on the adherence of a glass-bonded Pt-Au printed thick film conductor to a 96 wt % Al₂O₃ substrate was determined by a fracture mechanics measurement of the critical fracture energy for catastrophic thick film-substrate separation. The technique also demonstrated that separation by slow crack growth (delayed failure) occurred in this system. Analysis of the thick film microstructure and fracture surfaces showed that optimum adherence was primarily a result of a mechanically interlocked interface formed between the conductor metal and the glass bonding layer which, in turn, was strongly bonded to the alumina substrate. The two step decrease observed in _IC (from 3.7 to 0.2 J m^–2) with firing temperatures over 860° C resulted from the removal of this interlocking metal-glass interface brought on by metal sintering and glass migration to the substrate. Thus, at 860° C firing temperatures, adherence is controlled by cohesive fracture in the glass bonding phase while above 1000° C it is controlled by adhesive failure of the weak chemical-physical bond at the metal-glass interface.     

Pressure infiltration of sol/gel processed short fibre ceramic matrix composites

Using pressure infiltration short fibre-reinforced ceramic matrix composites with uniform and dense microstructure can be made. Based upon this processing technique, composites composed of silica sol, alumina particles, and alumina short fibres were fabricated. The related processing parameters studied in this work include infiltration rate, fibre volume fraction Vf, particle size, and infiltrate viscosity. An optimal infiltration rate was 4 mm min-1, at which rate the composite with Vf of 8.1% and particle size of 3 m has the highest green density. An equilibrium between particle packing strength and applied load must be obtained during the infiltration to obtain high green density and composite strength. The influence of fibre volume fraction and particle size on composite green density is in a synergistic manner because it involves particle–fibre interactions, fibre–fibre interactions, and sedimentation. Furthermore, the increase of sol viscosity results in more sedimentation in the infiltrate and lower composite green density. The fracture toughness of composites is 38% higher than that of monolithic alumina. © 1998 Chapman & Hall     

The solid state bonding of nickel,chromium and nichrome sheets to α-Al2O3

This paper describes experiments to measure the interfacial shear strengths of bonds formed between nickel, chromium and nichrome sheets hot pressed on to -Al₂O₃ single crystal plaques. Nickel developed bonds of 8×10³ psi (56 MN. m^–2) in shear when pressing was carried out under non-reducing conditions at 1100° C, 1 tsi (15 MN. m^–2) for 2 h: in the case of chromium, the effect of pressing temperature (1000 to 1300° C) pressing pressure (1/2 to 3 tsi [7.7 to 45 MN. m^–2]) and pressing time (1/2 to 7 h) on the bond was investigated. Nickel-chrome alloys produced from alternate nickel and chromium strips showed bond strengths up to 20×10³ psi (140 MN. m^–2) whilst commercial nickel-chrome (containing a silicon impurity) was not as effective in bonding to alumina. In material prepared from alternate strips of nickel and chromium, the degree of alloy homogenisation was investigated using microprobe analysis and suggestions made as to the mechanism of the interfacial reactions with alumina.     

Diffusion bonding behaviour of austenitic stainless steel containing titanium and alumina

A study has been conducted to identify the function of titanium in 1 Cr18Ni9Ti steel and the effects of fabrication temperature, pressure, time and other variables on the strengths of diffusion-bonded alumina-1Cr18Ni9Ti. At temperatures of 750 to 1200°C, 1Cr18Ni9Ti steel was successfully bonded to alumina, with a maximum tensile strength of 19MPa. By EPMA titanium segregated to the interface of the joint, in contrast to the failure of bonding of 1Cr18Ni9 steel and alumina under the same conditions. Titanium can reduce alumina with the reactants of TiO and compounds of titanium and aluminium thermochemical calculation. Thus it is indicated that titanium is an important go-between element for bonding metal to alumina.     

Thick film adherence fracture energy: influence of alumina substrates

The adherence of a glass bonded Pt-Au thick film conductor to various alumina substrates is degraded by changes in the surface composition of and by the presence of (0001) crystallographic texture in the substrate. Using the critical fracture energy (γ_IC) required to separate the thick film from the substrate, it was found that γ_IC was reduced from a maximum of 3.7 J m⁻² using an as-received 96+ wt% alumina substrate to ∼2J m⁻² using an as-received 99+ wt% alumina. In addition, the thick film adherence γ_IC using (0001) sapphire substrates was less than that using (11ˉ23) sapphire. The 96 wt% substate exhibited essentially a random crystallographic surface texture and a considerable amount of surface silicates. The as-received 99+ wt% Al₂O₃ substrate was charactarized by a high (0001) surface texture and, while exhibiting a similar composition silicate layer as that of the as-received 96 wt% alumina, the total amount of the glass layer is greatly diminished. Fractographic analysis of the separated thick films and substrates showed that changes in the substrate crystallographic texture and the glass layer diminish the interpenetrating nature of the glass—metal interface and weaken the glass—substrate interface. Such changes in thick film microstructure lead to poorer thick film adherence.     

Thermo-compression bonding of alumina ceramics to metal

Alumina ceramics and Kovar with aluminum interlayer are pressed together under vacuum at temperatures around 600°C for joining. This process produces mechanically strong ceramic to metal bonds in one step in an economic manner. In order to arrive at the optimum conditions for solid-state bonding, effects of bonding temperature, pressure and time on the bond strength have been studied. Bonding kinetics is also elucidated. Irradiation of 99% Al₂O₃ ceramics by 4–5 MV X-rays has been found to increase the bond-strength sharply from 33 to 60 MPa with a dose of 15 k Rads for bonding temperatures around 540°C. The apparent activation energy for the bonding process (Q _B) depends strongly on the type of alumina ceramics. Irradiation of alumina ceramics (99%), prior to joining with Kovar, accelerates the solid-state bonding by reducing (Q _B) from 209 to 76 kJ/mole.     

Multiphase composites of tetragonal zirconia agglomerate dispersed into alumina and alumina-zirconia matrices

Multiphase composites of yttria- and ceria-doped tetragonal zirconia agglomerates (10–50 m) dispersed into an alumina or alumina-zirconia matrix were sintered at 1500–1600 °C in air, followed by post-Hot Isostatic Pressing (HIP) at 1450°C and 150 MPa in an Ar gas atmosphere. The relative density of the recovered composites was above 98% of the theoretical density. By chemically etching on the surface of zirconia agglomerates, the sinterability of composites was apparently improved; and no microcracks nor pores were observed at the interface of agglomerate and matrix. According to scanning electron microscopy (SEM) observation, tetragonal and tetragonal-monoclinic zirconia agglomerates were highly dispersed into the alumina or alumina-zirconia matrix. The multiphase composites containing 10 vol% spherical agglomerates demonstrate the relatively low value of bending strength, < 400 MPa, and a high value of fracture toughness, > 11 MPa m^1/2. The crack propagation introduced by Vickers indentation was efficiently suppressed and deflected by the agglomerates.     

Solid-state bonding of alumina to austenitic stainless steel

A low temperature and low pressure bonding process for alumina and 316L austenitic stainless steel has been developed using a titanium/molybdenum laminated interlayer. The intermetallic compounds of Ti₃Al (or Ti₂/Al) and TiAl were formed at the alumina/titanium interface on bonding at above 1273 K. The activation energy of the layer growth was about 142 kJ mol^–1. The construction of Al₂O₃/Ti/Mo/steel gave the most stable joints. The highest tensile strength was above 60 MPa with a titanium 0.4 to 0.6mm thick/molybdenum 0.4 to 0.5 mm thick interlayer on bonding at 1273 K for 3 h under pressure of 12 MPa.     

Substrate/film interactions in thick films of YBaCuO on alumina

The substrate-film interaction in thick films (>10m) of YBa₂Cu₃O_7–x on alumina processed under normal conditions is investigated using electron-probe microanalysis. The formation of a mixture of barium aluminate and alumina over a thickness of about 2m in the interfacial region is established quantitatively using compositional mapping and point-count analysis across the substrate-film interface. Diffusion of aluminium into the film over severalm beyond the reaction layer is also observed. The variation of oxygen composition across the interface has been mapped. Leaching of oxygen from the 1-2-3 phase in the bulk is suggested as the reason for the observed decrease inT _c(0) and increase in T _c in films of YBa₂Cu₃O_7–x on alumina.     

Fatigue-crack propagation behavior in monolithic and composite ceramics and intermetallics

We study microstructural mechanisms of fatigue crack growth in advanced monolithic and composite ceramics and intermetallics. Much attention is devoted to the contribution of cycling loading to the hindrance of mechanisms that lead to a considerable increase in toughness (crack-tip shielding) of these materials. For example, in intermetallics with a ductile phase, such as -TiNb-reinforced -TiAl or Nb-reinforced Nb₃Al, a significant increase in toughness caused by the presence of uncracked ductile phase inside a crack is retarded under cyclic loading because ductile particles immediately fail by fatigue. Similarly, in monolithic ceramics, e.g., in alumina (aluminum oxide) or silicon nitride, the significant plasticization appearing under monotonic loading is greatly diminished under cyclic loading due to gradual wear at the grain-matrix interface. In fact, the nature of fatigue in such low-plasticity materials differs essentially from the well-known mechanisms of fatigue in metals and is governed, first of all, by a decrease in shielding, which depends on the loading cycle and time. The susceptibility of intermetallics and ceramics to fatigue degradation under cyclic loading affects seriously the possibility of structural use of these materials in practice. In particular, in this case, it is difficult to apply strength calculation methods that take into account the presence of defects and to implement life-prediction procedures.Center for Advanced Materials, Lawrence Berkeley Laboratory, University of California, USA. Published in Fiziko-Khimicheskaya Mekhanika Materialov, Vol. 30, No. 3, pp. 7–35, May–June, 1994.     

Spallation and transient oxide growth on PWA 1484 superalloy

A multi-layered oxide forms on single crystal PWA 1484 alloy when oxidized at high temperatures, consisting of a spinel ((Ni(Cr,Al,Co)₂O₄) at the air/oxide interface, interspersed with tantalum rich oxide particles (CrTaO₄/NiTa₂O₆), and an inner-most layer of α-alumina (α-Al₂O₃) in contact with the alloy. Observations on rapid cooling after oxidation show that the spallation behavior of this multi-layer oxide depends on time in room temperature laboratory air, the sulfur content of the alloy, and the alloy surface preparation. Time-lapse optical microscopy reveals that spallation of the multi-layer oxide occurs differently on polished surfaces in comparison to ground surfaces. On ground surfaces spallation occurs solely at the metal/alumina interface in both alloys, and follows the grinding scratches’ long axes. The higher S alloy (1.7 ppmw S) almost completely spalls to bare metal (95% oxide spalled), whereas very little spallation (5%) occurs on the lower S alloy (0.2 ppmw S). On polished surfaces spallation occurs along both the alumina/spinel and alumina/alloy interfaces of the higher sulfur containing alloy but only along the alumina/spinel interface of the oxide on the low-sulfur alloy, leaving the alumina in contact with the metal. The lack of significant difference in measured residual stress in the α-alumina combined with the fact that spallation occurred over periods of several hours at room temperature suggests that failure is a time-dependent process likely associated with the presence of moisture, once a critical oxide thickness has been exceeded. The role of sulfur is likely associated with a reduction in fracture toughness of the oxide and oxide/metal interfaces through formation of voids or reduction in bond energy.Re-heating of the alumina-covered, low-sulfur alloy (0.2 ppmw) indicates that outward grain boundary diffusion of aluminum and tantalum occurs through the α-alumina but not nickel. Also, no new Ni-rich oxides reform confirming that they are indeed transient oxides formed during the initial stages of oxidation of the bare alloy.     

Sr effect on the microstructure and tensile properties of A357 aluminum alloy and Al2O3/SiC-A357 cast composites

The effect of strontium as a modifier on the microstructures and tensile properties of two castable particulate metal matrix composites has been studied. The particulate metal matrix composites had similar matrix alloy (A357) but different reinforcing fine particles (silicon carbide and alumina). Results showed that the addition of 0.03% strontium makes a modest improvement to the yield strength, ultimate tensile strength and elongation percentage values, and the scatter of these properties, but makes a significant improvement to minimum strength and elongation results. Microstructural examinations by scanning electron microscope and energy dispersive spectroscopy analysis of metal matrix composites showed segregation of strontium on both the silicon carbide and alumina particles. Further results showed that the addition of higher strontium levels contributes to the over-modification of the eutectic silicon and promotes the formation of an Al–Si–Sr intermetallic compound on the particle/matrix interface.     

Mechanical damping and dynamic modulus measurements in alumina and tungsten fibre-reinforced aluminium composites

Simultaneous measurements of mechanical damping, or internal friction (Q ^–1 ), and dynamic Young's modulus (E) were made near 80 kHz and at strain amplitudes () in the range 10^–8 to 10^–4 on small specimens of continuous or chopped fibre-reinforced metal matrix composites (MMCs): 6061 aluminium reinforced with alumina (Al/Al₂O₃) and 6061 aluminium reinforced with tungsten (Al/W). Baseline experiments were also done on 99.999% aluminium (pure Al). The strain amplitude dependence of damping and the temperature dependence of dynamic modulus were of particular interest in this study. The temperature (T) dependence of the modulus from room temperature up to 475° C was determined for the Al/Al₂O₃ and pure Al specimens and a highly linear decrease in modulus with increasing temperature was observed. The rate of modulus loss (dE/dT –80 M Pa° C^–1 ) was the same for both materials and the reduction in modulus of the Al/Al₂O₃ was attributed to the reduction in modulus of the alu minium matrix, not the alumina fibres. The size, type, and amount of fibre reinforcement were found to have a significant effect on the strain amplitude dependence of the damping in both MMCs. Unreinforced aluminium exhibited classical dislocation damping trends with a region of strain amplitude independent damping at low strains (less than 10^–5) followed by a non linear, strain amplitude dependent region at higher strains. The addition of alumina fibres (chopped or continuous), while increasing stiffness, resulted in a significant reduction in damping capacity for the MMC relative to that for aluminium and near complete suppression of the amplitude dependent response. The damping levels increased as the volume fraction of fibre, and therefore, the amount of fibre/matrix (FM) interface decreased, indicating that the matrix, not factors such as increased dislocation densities at the FM interface, was the dominant influence on the damping. Analysis of the Al/Al₂O₃ results by Granato-Lücke (GL) theory indicated that dislocation densities were increased relative to those in aluminium, but the dis locations were well pinned and unable to increase damping levels effectively. Analysis of the Al/W results by GL theory also revealed high dislocation densities, but, unlike the Al/Al₂O₃ specimens, the Al/W specimens (continuous fibres) exhibited strong amplitude dependent damping (starting near strain levels of 2 × 10^–6) with damping levels approximately twice those of pure aluminium. Trends showed increased damping with increased fibre diameter, not with increased FM interface area. There was some evidence that it was the tungsten fibre itself that dominated the damping behaviour in Al/W composites, not the aluminium matrix or the FM interface.     

Preparation and properties of cast aluminium-ceramic particle composites

A casting technique for preparing aluminium-alumina, aluminium-illite and aluminium-silicon carbide particle composites has been developed. The method essentially consists of stirring uncoated but suitably heat-treated ceramic particles of sizes varying from 10 to 200 m in molten aluminium alloys (above their liquidus temperature) using the vortex method of dispersion of particles, followed by casting of the composite melts. Recoveries and microscopic distribution of variously pretreated ceramic particles in the castings have been reported. Mechanical properties and wear of these composites have been investigated. Ultimate tensile strength (UTS) and hardness of aluminium increased from 75.50 MN m^–2 and 27 Brinell hardness number (BHN) to 93.15 MN m^–2 and 37 BHN respectively due to additions of 3 wt % alumina particles of 100 m size. As a contrast, the tensile strength of aluminium-11.8 wt % Si alloy decreased from 156.89 MN m^–2 to 122.57 MN m^–2 due to the addition of 3 wt % alumina particles of the same size. Adhesive wear rates of aluminium, aluminium-11.8 wt % Si and aluminium-16 wt % Si alloys decreased from 3.62×10^–8, 1.75×10^–8 and 1.59×10^–8 cm³ cm^–1 to 2.0×10^–8, 0.87×10^–8 and 0.70×10^–8 cm³ cm^–1, respectively, due to the additions of 3 wt % alumina particles.Formerly with the Department of Mechanical Engineering, Indian Institute of Science, Bangalore 560 012, India.