The gold technology in Iberia underwent an important development during the Early Iron Age (EIA) following the arrival of new technological skills from the Mediterranean region, including the use of filigree, granulation, and brazing. This work presents the microanalytical study of EIA gold jewels (22 spherical beads and four tongue pendants) recovered from three graves in southern Portugal. The set of jewelry, showing an extraordinary stylistic resemblance, was characterized by optical microscopy, micro energy-dispersive X-ray spectrometry and scanning electron microscopy with X-ray microanalysis to establish the alloy composition and production techniques. The pieces show a close technological relation, making use of artificial gold alloys with different amounts of silver (c. 40 and 25%). The decorative styles include different types of filigree (solid wires and hollow wires), while the joining techniques comprise brazing with Au-Ag-Cu solders and, probably, sintering. In spite of those technological and stylistic features, clearly pointing to a Mediterranean influence, the absence of granulation suggests an indigenous workshop where exogenous technologies/decorations were not yet fully integrated in the manufacture of such luxury items.

AlMgB14–TiB2 ceramic was successfully brazed to TC4 alloy with inactive AgCu filler alloy. X-ray diffractometer, SEM, and energy-dispersive spectrometer were used to study interfacial microstructure and shear strength of the joints under different brazing temperatures. The results indicated that the typical microstructure of the TC4/AlMgB14–TiB2 joint was TC4/Ti(s.s) + Ti2Cu/Ti2Cu/TiCu/TiCu2Al/Ag(s.s) + Cu(s.s)/TiB whiskers/TiB2 reaction layer/AMBT. By increasing the brazing temperature, the thickness of the TC4 diffusion layer was improved, whereas that of the brazing seam decreased remarkably. When the brazing temperature was increased to 880 °C, the brazing seam was composed of Ti–Cu intermetallic Ag(s.s) with a few Cu(s.s), TiCu2Al distributed. Meanwhile, the formation of a continuous TiB2 reaction layer at the interface of the AMBT and brazing filler facilitated the improvement of joint shear strength. The joint with the maximum shear strength of 46.7 MPa was obtained while brazing at 880 °C for 10 min.

Based on wettability and reaction interfaces previously reported, as well as on thermodynamic considerations, a likely mechanism has been proposed for the chemical interaction taking place at the metal/ceramic interface during wettability experiments carried out by the so-called “sessile drop” method. The experiments involved three Ag-Cu-based brazing alloys [Cusil (Ag-28wt.%Cu), Cusil-ABA (Ag-34.6wt.%Cu-1.58wt.%Ti) and Incusil-ABA (Ag-26.6wt.%Cu-12.4wt.%In-0.89wt.%Ti)] and as polished and pre-oxidized pressure-less sintered silicon carbide (PLS-SiC), with a total holding time of 90 minutes at 850 °C, under a Zr sponge-gettered vacuum of 10-4/10-5 Torr.

An old procedure used to carry out a graphical derivation of curves, which is based on the optical properties of plane mirrors, has been adapted for the measurement of the contact angle (θ) formed between a liquid drop and a flat solid substrate in wettability experiments carried out by the so-called “sessile drop” method. The method was tested for mercury on soda-lime glass at room temperature in air as well as for Cusil (Ag-28wt.%Cu) and Incusil-ABA (Ag-27wt.%Cu-12wt.%In-2wt.%Ti) brazing alloys on pressureless-sintered silicon carbide (PLS-SiC) at 850 °C, under a vacuum of 10-4/10-5 Torr. The proposed method is fast, simple and accurate enough from high (∼140°) to relatively low (∼10°) contact angles. Although the proposed method has been tested for metal-ceramic systems, it is of general application, so that it would be useful for any liquid-solid system. The method is applicable for any temperature, pressure and atmospheric experimental conditions employed, as well as for any chemical composition of liquid and solid. It is also useful for both low and high contact angles, as well as for reactive and non-reactive systems, as long as a photograph of a liquid drop resting on a flat solid surface is available for the studied system.

The aim of this study is to evaluate the potential use of titanium foil coated with sputtered silver and copper films as a novel brazing filler for joining TiAl alloys. For this purpose, a detailed microstructural characterization of the resulting brazing interfaces was carried out. The development of brazing fillers that allow the joining of TiAl alloys without compromising the service temperature is a fruitful prospect. Brazing experiments were performed in a vacuum at 900, 950, and 980°C, with a dwell time of 30 min. Microstructural characterization reveals that brazing joints can be obtained successfully at 950 and 980°C. The interface consists of a large central region of α-Ti with an amount of Al and Ti–Ag compound and thin layers, mainly composed of intermetallic compounds, formed close to the base material. A novel brazing filler consisting of Ti foil coated with sputtered Ag and Cu films inhibits the extensive formation of soft (Ag) zones or coarse brittle Ti–Al–(Cu,Ni) particles. Hence, the need for post-brazing heat treatments for the joining of TiAl alloys was avoided.

The wetting of Cu–19Ni–5Al alloy on Ni-coated WC–8Co substrates with different coating thicknesses was investigated, and the brazing of Ni-coated WC–8Co to SAE1045 steel was performed by using the Cu–19Ni–5Al alloy as the filler metal. All the Cu–19Ni–5Al/Ni-coated WC–8Co systems present excellent wettability with a final contact angle of ∼10°. The thicknesses of the β + γ phase enriched with Co, Ni, and Al at the two joint interfaces increase and decrease with the Ni coating thickness, brazing temperature, and holding time increasing, respectively. The joint shear strength increases first and then decreases with the increase of Ni coating thickness, brazing temperature, or holding time. The maximum joint shear strength of ∼328 MPa is obtained while Ni plating for 90 min and brazing at 1210 °C × 5 min.

Diffusion brazing is a potential method to repair parts made from TiAl-alloys. Two different brazing materials with varying contents of titanium, iron and nickel were investigated. The phases present in the brazed zone were identified by high energy X-ray diffraction (HEXRD) at the material science beamline HEMS at the PETRA III synchrotron facility at DESY in Hamburg, Germany, and the microstructure was characterised by scanning electron microscopy (SEM). The braze zone itself is composed of one to two transitional layers from the substrate material to the middle of the joint. Near the substrate material the phase constitution reassembles a TiAl-alloy while the middle of the joint is similar to α/β-titanium alloys. Besides phases commonly encountered in TiAl-alloys such as γ, α2 and β, additional phases, which are related to the presence of nickel or iron as melting point depressing elements are present. The microstructure of the brazed zone changes significantly during a subsequent heat treatment.

Cette étude expérimentale présente de nouveaux matériaux composites développés récemmentpour le brasage de pièces en cuivre. Il s’agit de compositions à base d’agarose quipeuvent être mises en forme par moulage par injection de poudres. Cette facilité de miseen œuvre ouvre comme possibilité d’application la fabrication de préformes de brasage deformes complexes. Deux exemples d’utilisations sont présentés, l’un porte sur le brasagetendre et l’autre concerne le brasage fort. Les brasures finales obtenues permettentd’obtenir une résistance mécanique et une qualité métallurgique similaires à cellesobtenues à partir des matériaux conventionnels (bases SnPb ou CuP) utilisés pour lebrasage manuel de tubes en cuivre.

In order to increase the wettability and capillary forces of the filler metal between micro-cracking and micro-porous on the fracture surfaces of 304 stainless steels, methods of impregnation of Si and growth of Ni nanoparticles were used. These nanoparticles have a role inside the Transient Liquid Phase (TLP) and the substrate when using Brazing process. TLP can react with the nanoparticles previously deposited between micro-cracking and micro-porous and therefore promotes the nucleation and growth sites of phases and decreases the formation of eutectic structures. This method increases the effectiveness of metallic components reparation using Brazing process. Such effectiveness is indicated by an inspection of microstructural failure analysis, as a first stage, in the covered zone by the filler metal.

This article reports on low (below 800 °C) melting temperature characteristics of a Zr-Ti-Ni-Cu alloy system, designed by adding a small amount of Cu to a Zr-Ti-Ni eutectic alloy system in the Zr-rich corner of the Zr-Ti-Ni system. A series of Zr-Ti-Ni-Cu-based alloy buttons of varying Cu content was fabricated by an arc melting machine. The melting temperature ranges of the quaternary alloys were systematically examined by differential thermal analysis (DTA). As a result, a quaternary eutectic alloy of composition Zr54Ti22Ni16Cu8 with a low melting temperature range from 774 °C to 783 °C was found. In addition, structural and chemical analysis results for the slowly solidified, quaternary eutectic alloy sample revealed equivalent quaternary eutectic structure and phases to those of the ternary eutectic Zr50Ti26Ni24 alloy, except for a small amount of Cu dissolved in individual constituent phases. The wetting angle tested at 800 °C for 60 s on the commercially pure titanium was about 25°.

As potential substitutes for traditional Ti(Zr)–Cu–Ni-based brazing metals for high strength Ti alloys as well as a study for metallic glass, Zr–Ti–Ni-based alloys have been attracting much attention recently. In this study, the melting temperatures and microstructures of the Zr(Ti)-rich Zr–Ti–Ni alloys with Ni content below 33.3 at.% were systematically studied. A ternary deep eutectic alloy consisting of three phases was found at the composition of Zr50Ti26Ni24 with a solidus temperature of 798 °C and a liquidus temperature of 809 °C, which are significantly lower than the Zr2Ni–(Zr,Ti)2Ni pseudobinary eutectic melting temperature of 850 °C. This ternary eutectic reaction can be presented as L → α-(Zr/Ti) solid solution + Zr2Ni + ternary Laves (Zr,Ti)2Ni.

A new powder metallurgy technique for creating porous NiTi is demonstrated, combining liquid phase sintering of prealloyed NiTi powders by Nb additions and pore creation by NaCl space-holders. The resulting foams exhibit well-densified NiTi–Nb walls surrounding interconnected pores created by the space-holder, with controlled fraction, size, and shape. Only small amounts of Nb (3 at.%) are needed to produce a eutectic liquid that considerably improves the otherwise poor densification of NiTi powders. NiTi–Nb foams with 34–44% porosity exhibit high compressive failure stress (>1,500 MPa), ductile behavior (>50% compressive strain), low stiffness (10–20 GPa), and large shape-memory recovery strains. These thermomechanical properties, together with the known biocompatibility of the alloy, make these open-cell foams attractive for bone implant applications.

This paper focuses on manufacturing process of regular Metallic Hollow Sphere Structures (MHSS) through brazing technique. As a large stress level is generally confined into the necks formed by brazed spheres, the influence of the filler material on mechanical behavior of cellular metal has been studied. The microstructures of joints resulting from nickel hollow spheres brazing with different commercial fillers “MBF 30” and “MBF 1006” were compared by Scanning Electron Microscopy (SEM) and microhardness testing. These studies revealed a wide boron diffusion into nickel shells through grain boundaries for “MBF 30” brazing, with the formation of borides in a fine brittle eutectic structure. Conversely it was observed that the eutectic structure concentrates at the necks for “MBF 1006” and can be completely eliminated by diffusion-brazing, despite of the shells thinness. The uniaxial compressive tests of HSP specimens have shown two different strain mechanisms depending on brazing process.

The microstructures, interfacial reactions, and bonding strength properties of the Ti–Cu dissimilar joints using a commercially available Ag–28Cu–2Ti filler were studied, particularly as they relate to the role of an Ag barrier layer at the Ti interface. A joint microstructure and interfacial reactions closely related to the formation of brittle interfacial Ti–Cu intermetallics were fully dominated by the presence of the Ag layer at the Ti interface. Reliable Ti(base)/TiAg/Ag/Ag–Cu eutectic/Cu(base) joints without any detrimental Ti–Cu intermetallics were achieved at low brazing temperatures below 810 °C by applying an Ag interlayer of suitable thickness. It was notable that their bonding strengths were strong enough to exceed the strength of a Cu bulk base metal. This research demonstrates the potential application of an Ag interlayer for the reliable Ti–Cu dissimilar joints.

Co-based brazing alloy CoFeNi(Si, B)CrTi was designed for SiC joining. The periodic banded reaction structure that existed at the interface between SiC and the traditional Ni-based or Co-based braze has been eliminated by the new brazing alloy. The maximum room-temperature four-point bend strength of 161 MPa was achieved for SiC/SiC joint under the optimum brazing condition of brazing filler thickness of 120 μm, brazing temperature of 1150 °C, and brazing time of 10 min. The corresponding reaction layer of the SiC/SiC joint is composed of multilayer silicides and TiC band, and many small TiC particles are scattered throughout the matrix of the central part of the joint. The joints thus exhibit stable high-temperature strength. It is believed that the formation of TiC in the joint contributes not only to the elimination of the periodic banded reaction structure, but also to the high joint strength and the high-temperature stability.

The silver-copper oxide–based reactive air brazing technique was developed as a method of joining complex-shaped ceramic parts. To investigate the viability of this approach for high-temperature application, a series of air-brazed alumina joints were independently exposed to either oxidizing or reducing atmosphere at 800 °C for 100 h. Those samples that were thermally aged in air maintained good joint strength, similar to that of the original as-brazed samples. Microstructural analysis revealed no significant change in joint microstructure after long-term oxidation at elevated temperature, indicating excellent stability of the Ag–CuO-based filler metal in this environment. On the other hand, exposure of the air-brazed alumina joints to hydrogen under the same aging conditions resulted in a measurable decrease in joint strength. Scanning electron microscope analysis conducted on the fracture surfaces of the broken hydrogen-exposed specimens indicated that the source of joint failure was debonding along the interface between the filler metal and alumina substrate. This was due in large part to internal reduction of CuO precipitates within the filler metal to copper and accompanied by the simultaneous formation of porosity at these sites, both within the bulk of the joint as well as along the filler metal/substrate interfaces. Pore formation was noticeably present in filler metals prepared with a high concentration of copper oxide.

Gold-tin braze is the preferred material for attaching high-precision MEMS inertial sensors within hermetic ceramic packages. The bonds can be made at relatively low temperatures, are mechanically robust, and outgas at very low rates in vacuum sealed packages. There is one significant limitation to Au-Sn bonds, however. The thermal expansion coefficients of MEMS die and ceramic packages are not perfectly matched and temperature gradients occur when the assembly is cooled after brazing. As a result, there is considerable residual stress in the bonded assembly, which is accommodated to some extent by distortion of the sensor die. Over time, as these stresses relax, the distortion of the die changes, which causes the spacing between elements of the integral MEMS sensor to change as well. An important element of sensor-package design is insuring that stress relaxation effects do not cause the instrument to drift beyond its performance specification limits over a typical lifetime of 20 years.

Even though Au-Sn has been used for decades to attach silicon chips to ceramic substrates, there is little data available, particularly at low temperatures. An oven, with a specially designed window, allowed in-situ measurements to be made as a function of temperature, joint thickness and load stress. Additionally, a MEMS device brazed to a package with Au-Sn has been measured interferometrically over time to quantify die distortion in a packaged application.

We investigated a new method of ceramic-to-metal joining, referred to as reactive air brazing, as a potential method of sealing ceramic components in high-temperature electrochemical devices. Sessile drop wetting experiments and joint strength testing were conducted using yttria stabilized zirconia (YSZ) substrates and CuO–Ag-based air brazes. Results from our studies indicate that the wettability of the braze improves substantially with increasing CuO content, over a compositional range of 1–8 mol% CuO, which is accompanied by an increase in the bend strength of the corresponding brazed YSZ joint. The addition of a small amount of TiO2 (0.5 mol%) to the CuO–Ag braze further improves wettability due to the formation of a titanium zirconate reaction product along the braze/substrate interface. However, with one notable exception, the bend strength of these ternary braze joints remained nearly identical to those measured in comparable binary braze joints. Scanning electron microscopy analysis conducted on the corresponding fracture surfaces indicated that in the binary braze joints, failure occurs primarily at the braze/YSZ interface. Similarly in the case of the ternary, TiO2-doped brazes joint failure occurs predominantly along the interface between the braze filler metal and the underlying titanium zirconate reaction layer.

A commercial aluminum foil was used to braze alumina plates in air. Although the outer surface of the aluminum oxidizes in air, the majority of the aluminum underneath remains unoxidized during brazing, allowing the ceramic pieces to be joined together with adequate strength. Joint strength testing and subsequent examination of the fracture surfaces of the joints indicate that the joints are inherently ductile, even after long-term, high-temperature air exposure.