Evaluation of transient liquid phase bonding between nickel-based superalloys

Induction brazing of Inconel 718 to Inconel X-750 using Ni-7Cr-3Fe-3.2B-4.5Si (wt.-%) foil as brazing filler metal was investigated in this paper. Brazing was conducted at the temperature range 1373–1473 K for 0–300 s in a flow argon environment. Both interfacial microstructures and mechanical properties of brazed joints were investigated to evaluate joint quality. The optical and scanning electron microscopic results indicate that good wetting existed between the brazing alloy and both Inconel 718 and Inconel X-750. Microstructures at joint interfaces of all samples show distinct multilayered structures that were mainly formed by isothermal solidification and following solid-state interdiffusion during joining. The diffusion of boron and silicon from brazing filler metal into base metal at the brazing temperature is the main controlling factor pertaining to the microstructural evolution of the joint interface. The element area distribution of Cr, Fe, Si, Ni and Ti was examined by energy dispersive X-ray analysis. It was found that silicon and chromium remain in the center of brazed region and form brittle eutectic phases; boron distribution is uniform across joint area as it readily diffuses from brazing filler metal into base metal. The influence of heating cycle on the microstructures of base material and holding time on the mechanical properties of brazed joint were also investigated.     

Microstructure of diffusional zirconia–titanium and zirconia–(Ti–6 wt% Al–4 wt% V) alloy joints

Zirconia–titanium and zirconia–titanium alloy joints were made by diffusion bonding under an inert atmosphere at temperatures in the 1162–1494°C range. To inhibit the strong oxygen uptake by the titanium member a platinum insert was alternatively used. The microstructures and elemental profiles across the joints were investigated by scanning electron microscopy imaging and energy-dispersive spectroscopy or wavelength-dispersive spectroscopy microanalysis. It was found that direct ZrO2–Ti joining produces oxygen saturation in the Ti member and the formation of (Ti,Zr)2O at the interface. ZrO2/Pt/Ti joints present a complex layer sequence which at lower temperatures can be described on the basis of the Pt–Ti binary, except near the ceramic where a (Pt,Zr)-rich layer forms; at higher temperatures these joints develop an oxide layer of composition Ti2O3, this oxide probably resulting from local decomposition of the ceramic and reaction of oxygen with the incoming titanium. When Ti is replaced by the Ti–6 wt% Al–4 wt% V alloy in joints where Pt is present, the main consequences are the presence of liquid at lower joining temperatures and the earlier development of the oxide layer, now of nominal composition TiO. In all Pt-containing joints a phase of nominal composition Ti3Pt2 forms; it is advanced that this may be an equilibrium phase not predicted by the Pt–Ti diagrams available. All joints are weak, the fracture path running through the metal in the case of direct ZrO2–Ti joints and through the interface between the ceramic and the (Pt,Zr)-rich layer in joints where Pt is present.     

Development of a copper-based filler alloy for brazing stainless steels

The filler alloy of nominal composition Cu–40Mn–10Ni (all in wt%) was prepared in the form of ribbon of 40 μm thick by melt spinning technique. The ribbon exhibits narrow melting zone and comprise single phase of Cu–Mn–Ni solid solution. The melt spun ribbon successfully brazed 304 stainless steel butt joints. The formation of solid solution in the joining area without any intermetallics is observed. The bonding strength of filler alloy is achieved around 456 MPa.     

Bond strength and interfacial structure of silicon nitride joints brazed with aluminium-silicon and aluminium-magnesium alloys

From the results of the bending strength and Weibull modulus of the joints of silicon nitride ceramics brazed using aluminium-silicon and aluminium-magnesium alloy filler metals at a temperature of 1073 K for 0.9 ksec in a vacuum of 1.3 × 10^–3 Pa, silicon, especially, present in a small amount in the filler metals, was found to be effective in improving the bond strength, while magnesium in the filler metals was harmful to the joining. This can result in the formation of a thick stable alumina layer on the surfaces of the filler metals containing magnesium during brazing which prevented contact of the filler metals with the silicon nitride ceramics.     

Joining of zirconia to metal with Cu–Ga–Ti and Cu–Sn–Pb–Ti fillers

The method of brazing by capillary impregnation of Cu–Ga melt through a titanium powder layer situated between brazed details is elaborated. Samples of ZrO₂ ceramic/metal brazed joints using Cu–Ga–Ti filler and Cu–Sn–Pb–Ti filler were fabricated. The joints’ shear strength was 277±37 MPa for the Cu–Ga–Ti and 156±25 MPa for the Cu–Sn–Pb–Ti.     

采用Ag-Cu-In-Ti焊料连接碳化硅陶瓷

采用四元Ag-Cu-In-Ti焊料成功地连接了常压烧结SiC陶瓷. 研究了钎焊温度和保温时间对碳化硅连接强度的影响, 同时通过EPMA和TEM分析连接界面的微观结构, 并且探讨了连接的原理. 试验结果表明, 在700～780℃试验温度范围内, 碳化硅的连接强度存在峰值, 最高四点弯曲强度达到了234MPa, 但是连接强度随着保温时间的增加呈现单调下降趋势. 接头微观结构由基体SiC、反应层和焊料三部分组成, 连续致密的反应层紧密连接基体和焊料, 反应层由带状层、TiC层和Ti5Si3层组成, 带状层宽度约20nm, 由Ag、In、Si和少量的Ti、Cu组成. 元素线扫描结果显示焊料中的活性元素Ti含量在反应层内形成峰值, 活性元素Ti与SiC发生反应生成新的反应层是连接的主要因素.     

Active vacuum brazing of CNT films to metal substrates for superior electron field emission performance

The joining of macroscopic films of vertically aligned multiwalled carbon nanotubes (CNTs) to titanium substrates is demonstrated by active vacuum brazing at 820 °C with a Ag–Cu–Ti alloy and at 880 °C with a Cu–Sn–Ti–Zr alloy. The brazing methodology was elaborated in order to enable the production of highly electrically and thermally conductive CNT/metal substrate contacts. The interfacial electrical resistances of the joints were measured to be as low as 0.35 Ω. The improved interfacial transport properties in the brazed films lead to superior electron field-emission properties when compared to the as-grown films. An emission current of 150 μA was drawn from the brazed nanotubes at an applied electric field of 0.6 V μm⁻¹. The improvement in electron field-emission is mainly attributed to the reduction of the contact resistance between the nanotubes and the substrate. The joints have high re-melting temperatures up to the solidus temperatures of the alloys; far greater than what is achievable with standard solders, thus expanding the application potential of CNT films to high-current and high-power applications where substantial frictional or resistive heating is expected.     

Interaction of Si3N4 with Ni–Cr alloy under N2 or Ar atmosphere

In relation to the joining of silicon nitride ceramics to metal, the interaction of Si3N4 with Ni–Cr alloy was investigated at temperatures from 1073 to 1573 K under N2 or Ar atmosphere.Reaction rates were determined by thermogravimetry and reaction products were examined by X-ray diffraction. CrN, Ni3Si,Ni5Si2, Ni2Si and (Cr, Si)3Ni2Si were produced under N2 atmosphere. In addition to these products, Ni3Si2,Cr3Si and Cr5Si3 also were produced under Ar atmosphere. The reaction products were considered from the standpoint of thermodynamics. While the incubation period was observed under Ar atmosphere, it was not observed under N2 atmosphere. The initial rates obeyed a linear rate equation. The rates at the later stage of reaction described a parabolic rate equation. The reaction mechanism model was proposed.     

The study of metal ion release and cytotoxicity in Co–Cr–Mo and Ti–Al–V alloy in total knee prosthesis – scanning electron microscopic observation

We surgically retrieved two cobalt(Co)–chromium(Cr)–molybdenum(Mo) and five titanium(Ti)–aluminum(Al)–vanadium(V) alloy knee prostheses from patients because of mechanical failure and pain. We examined the distribution of the small particles which were released from the Co–Cr–Mo and Ti–Al–V alloys using a backscattered scanning electron microscopy (SEM). In addition we analyzed the metals in the artificial knee joints and the tissues adjacent to them using energy dispersive X-ray spectroscopy (EDS). We demonstrated that a myriad of fine particles, produced by the abrasion of both Co–Cr–Mo and Ti–Al–V alloys, accumulated in the synovial cells. As Co–Cr–Mo alloys disintegrate easily in the cells, Co dissolves from the peripheral areas of them, although Cr remains within the cells. In contrast Ti–Al–V alloys are very stable in the synovial cells. From these findings we conclude that the Co–Cr–Mo alloys are hazardous to the body as the alloys release Co which enters the body. In contrast the Ti–Al–V alloys are very stable and are patently safer. Artificial joints, however, are still in considerable need of improvement.     

Joining of silicon nitride to SUS304 stainless steel using a sputtering method

Silicon nitride with thin sputter-deposited titanium and nickel films was joined to SUS304 stainless steel (18% Cr-8% Ni) using metallic buffers in a series of silicon nitride/nickel/ molybdenum/nickel/SUS304, and the joining strength and microstructures were investigated. Four-point bending tests showed fracture strength of the joints up to 169 MPa. Cracks were formed at the interface between the silicon nitride and its adjacent nickel buffer, and frequently extended into the silicon nitride. Microstructural analyses revealed that the silicon nitride reacted with the sputter-deposited titanium producing titanium nitride and isolated silicon atoms, and that silicon and titanium diffused into the nickel buffer. Calculations using a finite-element method indicated a marked reduction in thermal stress induced in the joined silicon nitride with increasing thickness of the molybdenum buffer. The strong interfacial bond inducing the fracture of the joined silicon nitride was interpreted in terms of a good interfacial reaction, the interdiffusions and the reduction of thermal stress being due to the insertion of the molybdenum buffer.     

Fatigue studies of high-palladium dental casting alloys: Part I. Fatigue limits and fracture characteristics*

The fatigue limits and fracture characteristics for a Pd–Cu–Ga alloy and a Pd–Ga alloy were studied. The alloys were cast into tensile test bars with gauge diameter of 3 mm and gauge length of 15 mm, and the surfaces of the castings were neither air-abraded nor polished after removal from the investment. Specimens were prepared from all-new metal (not previously melted), a combination of 50% new metal and 50% old metal (previously melted one time) and 100% old metal. The cast bars were subjected to heat treatment simulating the complete firing cycles for dental porcelain, and fatigued in air at room temperature under uniaxial tension-compression stress at 10 Hz and a ratio of tensile stress amplitude to compressive stress amplitude (R-ratio) of –1. The alloy microstructures and fracture surfaces were examined with a scanning electron microscope (SEM). Results showed that the fatigue limits at 2 x 10⁶cycles of the Pd–Cu–Ga and Pd–Ga alloys were approximately 0.20 and 0.15 of their 0.1% yield strength (YS) in tension, respectively. The fatigue resistance for specimens from both alloys containing 50% old metal and 50% new metal was comparable to that of specimens containing all-new metal, although this decreased dramatically for Pd–Cu–Ga alloy specimens containing all-old metal. The fatigue resistance of the Pd–Cu–Ga alloy subjected to heat treatment simulating the porcelain firing cycles was not adversely affected by remnants of the original as-cast dendritic microstructure that remained in the relatively large test specimens. A longer heat treatment than recommended by the manufacturer for the porcelain firing cycles is needed to completely eliminate the as-cast dendritic structure in these specimens. The Pd–Cu–Ga alloy exhibited superior fatigue resistance to the Pd–Ga alloy, which has an equiaxed-grain microstructure and lower yield strength.     

Strength of Si3N4/Ni–Cr–Fe alloy joints with test methods: shear, tension, three-point and four-point bending

The experiments were carried out in order to examine the relationship between shear, tension, three-point and four-point bending strengths of Si3N4/Inconel 600 alloy joints. Average values of the shear, tension, and three and four point bending strengths were 178, 233, 321, and 344 MPa, respectively. From the results the strength ratio was 1 : 1.32 : 1.81 : 1.95 in the order of shear, tension, three-point and four-point bend tests. Based on Weibull moduli three-point bend and tension tests showed smaller strength scattering than did the shear and four-point bend tests. As opposed to the behaviour observed for the monolithic ceramic, the average bending strength of Si3N4/Inconel 600 alloy joints decreased as the effective volume of the bend test specimen increased. This revised version was published online in November 2006 with corrections to the Cover Date.     

Bending property and phase transformation of Ti–Ni–Cu alloy dental castings for orthodontic application

Bending property of Ti–Ni–Cu alloy castings was investigated in a three-point bending test for orthodontic application in relation to the phase transformation. The compositions of the alloys were Ti–50.8Ni and Ti–40.8Ni–10.0Cu (mol %), and four cross-sectional shapes of the specimens were selected. Heat treatment was performed at 713, 753 or 793 K for 1.8 ks. The bending load changed by the cross-sectional size and shape mainly because of the difference in the moment of inertia of area, but the load–deflection relation did not differ proportionally in the unloading process. The difference between the load values in the loading and the unloading processes was relatively small for Ti–Ni–Cu alloy. With respect to the residual deflection, there was no significant difference between Ti–Ni and Ti–Ni–Cu alloys with the same treatment condition. The load values in the loading and the unloading processes decreased by each heat treatment for Ti–Ni alloy; however, the decrease in the load values for Ti–Ni–Cu alloy was not distinct. It is proved that Ti–Ni–Cu alloy castings produce effective orthodontic force as well as stable low residual deflection, which is likely to be caused by the high and sharp thermal peaks during phase transformation.     

Interfacial reactions between lithium silicate glass-ceramics and Ni-based superalloys and the effect of heat treatment at elevated temperatures

Two lithium silicate glasses (S- and BPS-glass) were sealed to four different Ni-based superalloys (Inconel 600, Inconel 718, Haynes 230, and Hastelloy C-276) and the effects of long-term heating at 700–900°C on the chemical, microstructural, and mechanical properties of sealed interfaces were studied. The presence of a small amount of ZnO in the BPS-glass leads to the formation of a thin interfacial second phase layer and a less rough alloy interface compared to the ZnO-free S-glass. Inconel 718 was found to be the most reactive of the alloys, with Cr and Nb diffusing into the glass and forming a coarse glass-ceramic microstructure at the interface. Heat treatment of all the reaction assemblies at 900°C for 100 h in air resulted in degradation of the seals and their spontaneous failure. Heat treatments at 700 or 800°C did not cause any interfacial coarsening in BPS sealed to Inconel 600, Haynes 230, and Hastelloy C-276 alloys and did not alter the bond strength of Haynes 230 bars, sealed with a thin layer of BPS-glass, demonstrating the potential of these material combinations for applications up to 800°C.     

Effect of active metal coatings on the mechanical properties of silicon nitride-based ceramics

The effects of titanium, zirconium, hafnium and tantalum coatings on the mechanical properties of three silicon nitride ceramics were studied. The titanium coatings was found to cause a 50% decrease in the four-point bend strength of one of the silicon nitride ceramics while the effects of the zirconium, hafnium and tantalum coatings on all three silicon nitride ceramics were moderate. The reactions at a high temperature (940–980°C) between titanium and the grain-boundary glassy phase was the major cause for the degradation of the ceramic properties by the titanium coating. Residual tensile stress developed at the reaction interface replaced the glassy grain-boundary phase. Analytical electron microscopy showed the formation of a 180 nm thick Ti₅Si₃ layer and the crystallization of the amorphous grain-boundary phase. An indentation technique was used to measure qualitatively the residual stress developed at the reaction interface.     

Brazing of titanium to steel with different filler metals: analysis and comparison

Evaluations of vacuum brazed commercially pure titanium and low-carbon steel joints using one copper-based alloy (Cu–12Mn–2Ni) and two silver-based braze alloys (Ag–34Cu–2Ti, Ag–27.25Cu–12.5In–1.25Ti) have been studied. Both the interfacial microstructures and mechanical properties of brazed joints were investigated to evaluate the joint quality. The optical and scanning electron microscopic results showed that all the filler metals interact metallurgically with steel and titanium, forming different kinds of intermetallic compounds (IMC) such as CuTi, Cu2Ti, Cu4Ti3, and FeTi. The presence of IMC (interfacial reaction layers) at the interfacial regions strongly affects the shear strength of the joints. Furthermore, it was found that the shear strength of brazed joints and the fracture path strongly depend on the thickness of the IMC. The maximum shear strength of the joints was 113 MPa for the specimen brazed at 750 °C using an Ag–27.25Cu–12.5In–1.25Ti filler alloy.     

Mechanical properties and corrosion resistance of Ti–6Al–7Nb alloy dental castings

With the aim of applying a novel titanium alloy, Ti–6Al–7Nb, to a dental casting material, a comprehensive research work was carried out on its characteristics, such as castability, mechanical properties and corrosion resistance in the present study. As a result, Ti–6Al–7Nb alloy exhibited sufficient castability by a dental casting method for titanium alloys and enough mechanical properties for dental application. It is also showed excellent corrosion resistance through an immersion test in 1.0% lactic acid and an anodic polarization test in 0.9% NaCl solution. From these results, it is concluded that this Ti–6Al–7Nb alloy is applicable as a dental material in place of Ti–6Al–4V alloy, which includes cytotoxic vanadium.     

Reaction kinetics and mechanical properties in the reactive brazing of copper to aluminum nitride

Aluminum nitride (AlN) is an attractive substrate material for electronic packaging applications because of its high thermal conductivity and electrical resistivity. However, improved metallization of aluminum nitride is required for reliable conductivity and good adhesion to the ceramic substrate. In this study, the kinetics, microstructure, and mechanical strength of Ag–Cu–Ti/AlN reaction couples have been studied in the temperature range of 900–1,050 °C and hold time range of 0–1.44 × 10⁴ s using a eutectic silver–copper filler alloy containing titanium within the range of 2–8 wt%. The product layer thickening kinetics has been observed to change from a linear to non-linear thickening mechanism with the increase in holding time and temperature. At shorter hold times at a fixed temperature, the interfacial product layer followed a linear thickening kinetics. With the increase in the hold time, the thickening kinetics of the interface followed a non-linear thickening behavior. The non-linear thickening mechanism has been approximated as a parabolic thickening mechanism. The interface has been found to be rich in the reactive metal (Ti) content. The mechanical strength of the brazed joints has been analyzed using four-point bend tests. The strength of the brazed joints initially increased and then decreased with an increase in the hold time at a fixed temperature. A maximum strength of 196 MPa has been obtained for a brazed joint heated at 1,000 °C for 2,700 s containing 2 wt% Ti in the filler alloy. It was observed that the sample with the maximum strength had a discontinuous interface.     

A study of the wetting,microstructure and bond strength in brazing SiC by Cu-X(X = Ti,V,Nb,Cr) alloys

In the active brazing of SiC by copper-based alloys, the effects of various active elements such as titanium, vanadium, niobium and chromium on the wetting, microstructure and bond strength are investigated. In wetting, Cu-Cr alloys have the lowest wetting angles on SiC of 10°–20° depending on the chromium content. SiC is decomposed on contact with alloy melts during brazing. Carbon and silicon released from this decomposition of SiC react with active elements to produce their carbides and suicides at the interface. The reacted layers have different microstructures depending on the brazing alloys, but Cu-Ti and Cu-Cr alloys show similar microstructure, as do Cu-V and Cu-Nb alloys. In the four-point bend tests, the brazed joints of Cu-5 at % Ti, Cu-5 at % V and Cu-5 at % Nb alloys have similar bend strengths of 86.9, 80.3 and 92.4 MPa, respectively. The brazed joints of Cu-2 at % Nb alloys show a high bend strength of 154 MPa, although the wetting angle is a little higher, at about 60°. Niobium is found as a new active element of copper-based alloys to braze SiC. Cu-Nb alloys are promising for substitution for Cu-Ti alloys.     

TLP bonding of SiCp/2618Al composites using mixed Al–Ag–Cu system powders as interlayers

Mixed Al–Ag–Cu and Al–Ag–Cu–Ti powders were used as interlayers for transient liquid phase diffusion bonding (TLP bonding) of SiC particulate reinforced 2618 aluminum alloy matrix composite (SiCp/2618Al MMC). The results show that by using mixed Al–Ag–Cu powder with the eutectic composition as an interlayer, SiCp/2618Al MMC can be TLP bonded at 540 °C, however, the joining layer is porous. Adding a certain amount of titanium into the Al–Ag–Cu interlayer, the TLP bonding quality can be improved. The titanium added into the Al–Ag–Cu interlayer has an effect of shortening the solidification time of the joining layer, thus decreasing SiC particles from the parent materials entering into the joining layer. The joints bonded using Al–Ag–Cu–Ti interlayers have a maximum shear strength of 101 MPa when 2.1% titanium is added.