Enhancement of the wettability and solder joint reliability at the Sn–9Zn–0.5Ag lead-free solder alloy–Cu interface by Ag precoating

The enhancement of the wettability and solder joint reliability at the Sn–9Zn–0.5Ag solder alloy–Cu interface by Ag precoating has been investigated. The wettability of the Sn–9Zn–0.5Ag solder alloy–Cu interface has been improved by Ag precoating. The adhesion strength of the solder alloy–Ag precoated Cu interface increases from 4.11±0.56 to 6.92±0.85 MPa as dipped at 250 °C for 10 s. When the dipping time is prolonged from 10 to 30 s, the interfacial adhesion strength increases from 6.92±0.85 to 13.62±0.73 MPa. The interfacial adhesion strength is enhanced by the rod-like Cu–Zn intermetallic compound (IMC) formed close to the interface. The diffusion coefficients of Sn and Zn in the IMC layer are determined as 5.76×10⁻¹⁰ and 9.50×10⁻¹¹ cm²/s at the Sn–9Zn–0.5Ag–Cu and Sn–9Zn–0.5Ag–Ag precoated Cu interfaces, respectively.     

Investigations of interfacial reactions of Sn–Zn based and Sn–Ag–Cu lead-free solder alloys as replacement for Sn–Pb solder

The interfacial reactions of Sn–Zn based solders and a Sn–Ag–Cu solder have been compared with a eutectic Sn–Pb solder. During reflow soldering different types of intermetallic compounds (IMCs) are found at the interface. The morphologies of these IMCs are quite different for different solder compositions. As-reflowed, the growth rates of IMCs in the Sn–Zn based solder are higher than in the Sn–Ag–Cu and Sn–Pb solders. Different types of IMCs such as γ-Cu₅Zn₈, β-CuZn and a thin unknown Cu–Zn layer are formed in the Sn–Zn based solder but in the cases of Cu/Sn–Pb and Cu/Sn–Ag–Cu solder systems Cu₆Sn₅ IMC layers are formed at the interface. Cu₆Sn₅ and Cu₃Sn interfacial IMCs are formed in the early stages of 10 min reflow due to the limited supply of Sn from the Sn–Pb solder. The spalling of Cu–Sn IMCs is observed only in the Sn–Ag–Cu solder. The size of Zn platelets is increased with an increase of reflow time for the Cu/Sn–Zn solder system. In the case of the Sn–Zn–Bi solder, there is no significant increase in the Zn-rich phases with extended reflow time. Also, Bi offers significant effects on the wetting, the growth rate of IMCs as well as on the size and distribution of Zn-rich phases in the β-Sn matrix. No Cu–Sn IMCs are found in the Sn–Zn based solder during 20 min reflow. The consumption of Cu by the solders are ranked as Sn–Zn–Bi > Sn–Ag–Cu > Sn–Zn > Sn–Pb. Despite the higher Cu-consumption rate, Bi-containing solder may be a promising candidate for a lead-free solder in modern electronic packaging taking into account its lower soldering temperature and material costs.     

Phase transformation and morphology of the intermetallic compounds formed at the Sn–9Zn–3.5Ag/Cu interface in aging

The morphology and phase transformation of the intermetallic compounds (IMCs) formed at the Sn–9Zn–3.5Ag/Cu interface in a solid-state reaction have been investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), electron diffraction (ED), scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS). The monoclinic η′-Cu₆Sn₅ transforms to the hexagonal η-Cu₆Sn₅ and the orthorhombic Cu₅Zn₈ transforms to the body-centered cubic (bcc) γ-Cu₅Zn₈ as aged at 180 °C. The scallop-shaped Cu₆Sn₅ layer is retained after aging at 180 °C for 1000 h. In the solid-state reaction, Ag is repelled from η′-Cu₆Sn₅ and reacts with Sn to form Ag₃Sn, and the Cu₅Zn₈ layer decomposes. Kirkendall voids are not observed at the Sn–9Zn–3.5Ag/Cu interface even after aging at 180 °C for 1000 h.     

The 260 °C phase equilibria of the Sn–Sb–Ag ternary system and interfacial reactions at the Sn–Sb/Ag joints

The isothermal section of the Sn–Sb–Ag ternary system at 260 °C has been determined in this study by experimental examination. Experimental results show no existence of ternary compounds in the Sn–Sb–Ag system. Two extensive regions of mutual solubility have been determined. The one located between the two binary isomorphous phases, Ag₃Sn and Ag₃Sb, is labeled as and the other one located between the two binary isomorphous phases, Ag₄Sn and Ag₄Sb, is labeled as ξ. The phase is a very stable phase and is in equilibrium with ξ, Sb, SbSn, Sb₂Sn₃, and liquid Sn phases. Each of the Sb and SbSn phases has a limited solubility of Ag. Only one stoichiometric compound, Sb₂Sn₃, exists. Besides phase equilibria determination, the interfacial reactions between the Sn–Sb alloys and the Ag substrate were investigated at 260 °C. It was found that the phase formations in the Sn–Sb/Ag couples are very similar to those in the Sn/Ag couples.     

Single-wall carbon nanotube (SWCNT) functionalized Sn–Ag–Cu lead-free composite solders

Sn–3.8Ag–0.7Cu-based composite solders functionalized with single-wall carbon nanotubes (SWCNTs) with various weight proportions ranging from 0.01 to 1 wt% were successfully produced. The microstuctural, melting and mechanical properties of Sn–3.8Ag–0.7Cu-based composite solders were evaluated as a function of different wt% of SWCNT addition. The microstructures of the composite specimens were studied by means of field-emission scanning electron microscope (FE-SEM). It was observed that SWCNTs were homogeneously distributed at the edges of Ag₃Sn compounds that are distributed evenly in the β-Sn solder matrix. Energy dispersion X-ray (EDX) analysis method was employed to reveal the presence of the phases existed in the solder composites. The mechanical properties of the composite solders were evaluated by Vickers-microhardness measurements and tensile tests performed at room temperature. The different wt% and addition of SWCNTs to Sn–3.8Ag–0.7Cu produced a dramatic increase in tensile strength, hardness, and better melting characteristics. A slight decrease in elongation to failure was observed. FE-SEM observations of the fracture surface, revealed the overall failure mechanism as the ductile manner of failure.     

The growth and roughness evolution of intermetallic compounds of Sn–Ag–Cu/Cu interface during soldering reaction

The growth behavior and roughness evolution of intermetallic compounds (IMCs) layer between Sn–3.5Ag, Sn–3.5Ag–0.7Cu, Sn–3.5Ag–1.7Cu and Sn–0.5Ag–4Cu lead-free solder alloys and Cu substrate are investigated during soldering under 250 °C. With the increase of Cu content in Sn–3.5Ag, Sn–3.5Ag–0.7Cu and Sn–3.5Ag–1.7Cu solders, the IMC thickness increases due to the decrease of the dissolution rate of the IMCs. The IMC thickness of Sn–0.5Ag–4Cu is quite thinner in a short soldering time. However, with the increase of soldering time, the IMCs layer grows quickly due to the precipitation effect of the Cu₆Sn₅ in the liquid solder. With the increase of soldering time, the roughness of all the IMC layers increases. The roughness of Sn–3.5Ag–0.7Cu and Sn–3.5Ag–1.7Cu interfaces is larger than that of Sn–3.5Ag while Sn–0.5Ag–4Cu/Cu interface has the smallest roughness value. It is believed that the small IMC roughness of Sn–3.5Ag/Cu interface is caused by the IMCs dissolution, and the large IMC/liquid solder interfacial energy maybe the reason for Sn–0.5Ag–4Cu/Cu interface obtaining the smallest IMC roughness.     

Investigation on the microstructure and mechanical properties of a cast Mg–6Zn–5Al–4RE alloy

Mg–6Zn–5Al–4RE (RE = Mischmetal, mass%) alloy was prepared by metal mould casting method. The microstructure and mechanical properties of the as-cast and heat-treated alloys were investigated. The results show that the phase compositions of the as-cast state alloy are supersaturated solid solution -Mg, lamellar β-Al₁₂Mg₁₇, polygonal Al₃RE and cluster Al₂REZn₂ phases. The mechanical properties, especially the ultimate tensile strength and elongation of the alloy were significantly improved by the heat treatment. Fracture surface of tensile specimens was analyzed by optical microscope and scanning electron microscope.     

Investigation of interfacial reactions between Sn–Zn solder with electrolytic Ni and electroless Ni(P) metallization

In this study, interfacial reactions of electrolytic Ni and electroless Ni(P) metallization of the ball-grid-array (BGA) substrate with the molten Sn–9Zn (wt.%) eutectic solder alloy were investigated, focusing on the shear strengths and the identification of the intermetallic compound (IMC) phases at various reflow periods. Zn-containing Pb-free solder alloys were kept in molten condition (240 °C) on the bond pads for different durations ranging from 1 to 60 min to render the ultimate interfacial reaction and to observe the consecutive shear strength. After the shear test, fracture surfaces were investigated by scanning electron microscopy equipped with an energy dispersive X-ray spectrometer. Cross-sectional studies of the interfaces were also conducted to correlate with the fracture surfaces. The solder ball shear-load for the Ni(P) system during extended reflow increased with the increase of reflow time. The consumption of the electroless Ni(P) layer in Sn–9Zn was also lower than that of the electrolytic Ni. It was evident that the Sn–Zn solder/electrolytic Ni system was more vulnerable than the Sn–Zn solder/electroless Ni(P) system in high temperature long time liquid state annealing. Sn–Zn solder with electroless Ni(P) metallization appeared as a good combination in soldering technology.     

Zinc–nickel alloy coatings electrodeposited from a chloride bath using direct and pulse current

Zinc–nickel alloys were electrodeposited on steel from chloride bath by direct and pulse current. Some electric variables (average current density, pulse frequency, duty cycle) and some important bath conditions (ratio of Ni²⁺/Zn²⁺ in bath, temperature) on chemical compositions, current efficiency, microhardness and surface appearance of coatings were studied. At low current densities, transition from anomalous to normal co-deposition was observed for both direct and pulse current. Pulse current seems to increase brightness of the coating and to decrease the precipitation of zinc hydroxide at the cathode surface. In addition, applied pulse current increases the percentage of nickel in deposits. Pulse frequency and duty cycle had little effect on the chemical composition of deposits. The polarization curve of zinc–nickel deposition with pulse current is shifted to positive potentials in comparison with direct current curves. The temperature of the plating bath had a very strong effect on the composition of the deposits. This is primarily the result of intrinsically slow nickel kinetics. The hardness of Zn–Ni alloy coatings (approx. 220 VHN) was greater than the hardness of zinc coating (approx. 161 VHN). The hydroxide suppression mechanism for Zn–Ni co-deposition has been confirmed.     

Effect of Ag Addition on Microstructure,Mechanical and Corrosion Properties of Mg-Nd-Zn-Zr Alloy for Orthopedic Application

The as-extruded Mg–3Nd–0.2Zn–0.4Zr–xAg (x = 0, 0.2, 0.5, 1 wt%) alloys were prepared for biomedical applications. Scanning electron microscope, electron backscattered diffraction, X-ray diffraction, tensile test machine, electrochemical workstation, and immersion experiments were used to study microstructures, mechanical properties, and corrosion behavior of the as-extruded alloys. The results indicate that the microstructures of all the as-extruded alloys are composed of coarse undynamic recrystallized grains, fine equiaxed recrystallized grains, and precipitated phases. Ag element plays a positive role in promoting dynamic recrystallization and grain refinement. And during the extrusion, all the four alloys generate a $\left\langle {10\overline{1}0} \right\rangle$//ED fiber texture. With the increase of Ag element, the volume fraction of Mg₁₂Nd phase increases and then decreases slightly. By increasing Ag addition, both yield strength and ultimate tensile strength of the as-extruded alloys reduce first and then improve, and the elongation improves gradually from 9.4 to 12.7%. More importantly, the addition of Ag accelerates corrosion of the as-extruded alloys in simulated body fluid, and all the as-extruded alloys show uniform corrosion mode.     

Thermodynamic modeling of the Ce–Zn and Pr–Zn systems

In order to develop the thermodynamic database of phase equilibria in the Mg–Zn–Re (Re: rare earth element) base alloys, the thermodynamic assessments of the Ce–Zn and Pr–Zn systems were carried out by using the calculation of phase diagrams (CALPHAD) method on the basis of the experimental data including thermodynamic properties and phase equilibria. Based on the available experimental data, Gibbs free energies of the solution phases (liquid, bcc, fcc, hcp and dhcp) were modeled by the subregular solution model with the Redlich–Kister formula, and those of the intermetallic compounds were described by the sublattice model. A consistent set of thermodynamic parameters has been derived for describing the Gibbs free energies of each solution phase and intermetallic compound in the Ce–Zn and Pr–Zn binary systems. An agreement between the present calculated results and experimental data is obtained.     

Microstructure,Mechanical Properties and Corrosion Behavior of Extruded Mg–Zn–Ag Alloys with Single-Phase Structure

Mg–Zn–Ag alloys have been extensively studied in recent years for potential biodegradable implants due to their unique mechanical properties,biodegradability and biocompatibility.In the present study,Mg–3Zn-x Ag(wt%,x=0.2,0.5 and0.8)alloys with single-phase crystal structure were prepared by backward extrusion at 340°C.The addition of Ag element into Mg–3Zn slightly influences the ultimate tensile strength and microstructure,but the elongation firstly increases from12%to 19.8%and then decreases from 19.8%to 9.9%with the increment of Ag concentration.The tensile yield strength,ultimate tensile strength and elongation of Mg–3Zn–0.2Ag alloy reach up to 142,234 MPa and 19.8%,respectively,which are the best mechanical performance of Mg–Zn–Ag alloys in the present work.The extruded Mg–3Zn–0.2Ag alloy also possesses the best corrosion behavior with the corresponding corrosion rate of 3.2 mm/year in immersion test,which could be explained by the single-phase and uniformly distributed grain structure,and the fewer twinning.     

Formation of 14H long period stacking ordered structure and profuse stacking faults in Mg–Zn–Gd alloys during isothermal aging at high temperature

This paper proposes a time–temperature-transformation diagram of an Mg–Zn–Gd alloy. An Mg₉₇Zn₁Gd₂ (at.%) alloy shows different precipitation sequences at low, medium and high temperatures. Low-temperature aging at <523 K brings about coherent β′-phase precipitation to a -Mg solid solution, resulting in increase in strength of the alloys. However, aging at medium and high temperatures >623 K led to strengthening of the Mg–Zn–Gd alloy, owing to the formation of profuse stacking faults and 14H long period stacking ordered structure from the supersaturated -Mg matrix, respectively.     

The microstructures and mechanical properties of cast Mg–Zn–Al–RE alloys

The microstructures and mechanical properties of cast Mg–Zn–Al–RE alloys with 4 wt.% RE and variable Zn and Al contents were investigated. The results show that the alloys mainly consist of α-Mg, Al₂REZn₂, Al₄RE and τ-Mg₃₂(Al,Zn)₄₉ phases, and a little amount of the β-Mg₁₇Al₁₂ phase will also be formed with certain Zn and Al contents. When increasing the Zn or Al content, the distribution of the Al₂REZn₂ and Al₄RE phases will be changed from cluster to dispersed, and the content of τ-Mg₃₂(Al,Zn)₄₉ phase increased gradually. The distribution of the Al₂REZn₂ and Al₄RE phases, and the content of β- or τ-phase are critical to the mechanical properties of Mg–Zn–Al–RE alloys. The Mg–6Zn–5Al–4RE alloy with cluster Al₂REZn₂ phase and low content of β-phase, exhibits the optimal mechanical properties, and the ultimate tensile strength, yield strength and elongation are 242 MPa, 140 MPa and 6.4% at room temperature, respectively.     

AlN ceramics prepared by high-pressure sintering with La2O3 as a sintering aid

The magnetic and dielectric properties of Bi–Zn codoped Y-type hexagonal ferrite was investigated. The samples with composition of Ba_2−xBi_xZn_0.8+xCo_0.8Cu_0.4Fe_12−xO₂₂ (x = 0–0.4) were prepared by the solid-state reaction method. Phase formation was characterized by X-ray diffraction. The microstructure was observed via scanning electron microscopy. The magnetic and dielectric properties were measured using an impedance analyzer. Direct current (dc) electrical resistivity was measured using a pA meter/dc voltage source. Minor Bi doping (x = 0.05–0.25) will not destroy the phase formation of Y-type hexagonal ferrite, but lower the phase formation temperature distinctly. Bi substitution can also promote the sintering process. The Bi-containing samples (x > 0.05) can be sintered well under 900 °C without any other addition. The sintering temperature is about 200 °C lower than that of the Bi-free sample. The Bi–Zn codoped samples exhibit excellent magnetic and dielectric properties in hyper frequency. These materials are suitable for multi-layer chip-inductive components.     

Microstructures and properties of Mg–7Gd alloy containing Y

Mg–7 mass%Gd–x mass%Y (x = 0, 1, 3 and 5) alloys were prepared by casting method, and the microstructures, age hardening behavior and mechanical properties have been investigated. The results show that the addition of Y to the binary Mg–7Gd alloy could reduce the grain size of the as-cast alloys, and enhance the age hardening response and improve mechanical properties during the investigated temperature range. The Mg–7Gd–5Y alloy exhibits maximum ultimate tensile strength and yield strength at peak hardness, and the values are 258 and 167 MPa at room temperature, and 212 and 140 MPa at 250 °C, respectively, which is about 1.8 times as high as the Mg–7Gd binary alloy. When x is more than 3, the amount of Mg₅(Gd,Y) phase is observed at the peak hardness of aged alloys. The significant improvement of the tensile strength at peak hardness is mainly attributed to the fine dispersion of the β-Mg₅(Gd,Y) precipitate.     

Thermoelectric properties of ternary phases of thallium–tin–tellurium system

In this paper, we present the measurements of conductivity and of thermoelectric power. Measurements were taken for the temperature range of 100–330 K for the three ternary phases of Tl–Sn–Te system. The potential of these compounds as thermoelectric materials was studied.     

Constitution, structural chemistry and magnetism in the ternary system Ce–Ag–Si

Phase relations were established for the Ce–Ag–Si system at 850°C by means of X-ray diffraction, light optical microscopy and quantitative electron probe microanalysis. Phase equilibria are characterised by the existence of extended solid solutions starting from the binaries: Ce(Ag_xSi_1−x)_2−y (ThSi₂-type), Ce(Ag_1−xSi_x)_1−y (unknown structure type) and Ce(Ag_1−xSi_x)_2−y (unknown structure type). Three ternary phases were found to exist, CeAg₂Si₂ (ThCr₂Si₂-type), Ce(Ag_xSi_1−x)_2−y (AlB₂-type) and the new ternary compound CeAgSi₂ with unknown structure type. Magnetic behaviour was studied from magnetic susceptibility and magnetisation measurements down to 1.7 K and employing magnetic fields up to 5 T. Soft ferromagnetism is observed for CeAg_xSi_2−x (AlB₂-type) below 5 K. Alloys Ce(Ag_xSi_1−x)_2−y with 0.08<x_Ag<0.30 (ThSi₂-type) encounter ferromagnetic order below 7 K. For x_Ag=0.31 the ferromagnetic interaction changes to antiferromagnetism with T_N=5.7 K. For CeAgSi₂ ferrimagnetic or canted antiferromagnetic order is indicated below 7 K.