Sn–In–Ag phase equilibria and Sn–In–(Ag)/Ag interfacial reactions

Experimental verifications of the Sn–In and Sn–In–Ag phase equilibria have been conducted. The experimental measurements of phase equilibria and thermodynamic properties are used for thermodynamic modeling by the CALPHAD approach. The calculated results are in good agreement with experimental results. Interfacial reactions in the Sn–In–(Ag)/Ag couples have been examined. Both Ag₂In and AgIn₂ phases are formed in the Sn–51.0 wt%In/Ag couples reacted at 100 and 150 °C, and only the Ag₂In phase is formed when reacted at 25, 50 and 75 °C. Due to the different growth rates of different reaction phases, the reaction layer at 100 °C is thinner than those at 25 °C, 50 °C, and 75 °C. In the Sn–20.0 wt%In/Ag couples, the ζ phase is formed at 250 °C and ζ/AgIn₂ phases are formed at 125 °C. Compared with the Sn–20 wt%In/Ag couples, faster interfacial reactions are observed in the Sn–20.0 wt%In–2.8 wt%Ag/Ag couples, and minor Ag addition to Sn–20 wt%In solder increases the growth rates of the reaction phases.     

Interfacial microstructure and mechanical properties of In–Bi–Sn lead-free solder

The interfacial microstructure and mechanical properties of a low melting temperature lead-free solder of In-18.75Bi-22.15Sn (in at.%) (In–Bi–Sn) were investigated. The microstructure analysis of bulk In–Bi–Sn revealed that irregular lamellar γ-Sn phases distributed in the In₂Bi matrix. There was only a single endothermic peak with an onset temperature of 62 °C on the DSC curve, indicating that In–Bi–Sn is close to a ternary eutectic solder. The ultimate tensile strength of the bulk In–Bi–Sn was 21.76 MP at a strain rate of 10^?2s^?1 at 25 °C. The elongation of the bulk In–Bi–Sn solder reached 87 %, indicating an excellent ductility of the In–Bi–Sn solder. Two intermetallic compounds (IMCs), needle-like Cu(In,Sn)₂ and laminar Cu₆(In,Sn)₅, formed at the In–Bi–Sn/Cu interface. An IMC layer of polyhedral crystallites of InNi formed at the In–Bi–Sn/Ni interface. The shear strength of Cu/In–Bi–Sn/Cu solder joints was 21.15 MP, and the shear fractograph showed that the ductile fracture with dimples appearance occurred in the solder.     

In vitro degradation behavior and cytocompatibility of Mg–Zn–Zr alloys

Zinc and zirconium were selected as the alloying elements in biodegradable magnesium alloys, considering their strengthening effect and good biocompatibility. The degradation rate, hydrogen evolution, ion release, surface layer and in vitro cytotoxicity of two Mg–Zn–Zr alloys, i.e. ZK30 and ZK60, and a WE-type alloy (Mg–Y–RE–Zr) were investigated by means of long-term static immersion testing in Hank’s solution, non-static immersion testing in Hank’s solution and cell-material interaction analysis. It was found that, among these three magnesium alloys, ZK30 had the lowest degradation rate and the least hydrogen evolution. A magnesium calcium phosphate layer was formed on the surface of ZK30 sample during non-static immersion and its degradation caused minute changes in the ion concentrations and pH value of Hank’s solution. In addition, the ZK30 alloy showed insignificant cytotoxicity against bone marrow stromal cells as compared with biocompatible hydroxyapatite (HA) and the WE-type alloy. After prolonged incubation for 7 days, a stimulatory effect on cell proliferation was observed. The results of the present study suggested that ZK30 could be a promising material for biodegradable orthopedic implants and worth further investigation to evaluate its in vitro and in vivo degradation behavior.     

Fabrication and characterization of p-type In–N codoped ZnMgO films

Indium (In) and nitrogen (N) codoped ZnMgO films (ZnMgO:In–N) were fabricated on quartz substrates by radio frequency magnetron sputtering and ion-implantation technique. p-ZnMgO:In–N films were successfully achieved after post-implantation annealing at an appropriate temperature ranging from 570 to 590?°C. X-ray diffraction (XRD) indicates that severe damage in films is introduced by N ion implantation and the damaged lattice can be partially recovered after post-implantation annealing. The analysis of Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) demonstrates that post-implantation annealing can promote a reduction of donor type zinc interstitials (Zn_i) and the formation of In_Zn+2N_O acceptor complex, which mainly contribute to the realization of p-type ZnMgO:In–N films.     

In situ production of Fe–VC and Fe–TiC surface composites by cast-sintering

Using a new cast-sintering technique, iron-base surface composites reinforced by VC and TiC particles which were produced in situ and consisting of self-lubricant graphite and chromium-carbide, were sintered on the surface of cast steel during casting. The structure and composition of the surface composites were studied with the help of a SEM, an electron probe and XRD. From the outside in of the iron-based surface composites, the concentration of V and Ti was relatively stable and consistently retained a high level, while the concentration of Cr and Ni took on a gradient distribution and decreased gradually. The fine particles of VC and TiC measuring between 1 and 3 μm in diameter were uniformly dispersed in their matrices, and there was a perfect metallurgy-bond between the surface composite layer and the master-alloy. Under the condition of dry slipping with a heavy load, the Fe–VC and Fe–TiC surface composites offer virtually unique wear-resistance.     

In situ prepared polypyrrole–Ag nanocomposites: optical properties and morphology

Polypyrrole–silver (PPy–Ag) nanocomposites with various silver contents have been synthesized via a kinetically favorable one-step chemical oxidative polymerization process. The oxidant, ammonium persulfate, was used to oxidize pyrrole monomer for growing chains of PPy. And AgNO₃ was used as a precursor for metallic silver nanoparticles. The detailed characterization techniques, UV–Vis–NIR, fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction spectroscopy, field-emission scanning electron microscopy, and transmission electron microscopy (TEM), have been used to reveal electronic environment, structure, and morphology of composites as well as as-synthesized PPy. The synthesis environment prior to polymerization has also been investigated by absorption spectroscopy. The TEM images of PPy–Ag nanocomposites reveal that silver nanoparticles are deeply embedded into the polymer matrix in addition to surface adsorption. It is observed that the size distribution of inorganic nanoparticles (ca. 4–10 nm, depending on the metal ion concentrations) as well as structural morphology is altered by the initial concentrations of silver ions.     

Annealing Influence on the Microstructure and Magnetic Properties of Ni–Mn–In Alloys Ribbons

We report on the structure, microstructure and inverse magnetocaloric effect associated with the first-order martensitic phase transition, in Heusler Ni_50.0Mn_35.5In_14.5 alloy ribbons. We have studied the short-time vacuum annealing influence at 1048?K, 1073?K, 1098?K, and 1123?K in these properties. At room temperature, an increase in the degree of structural order for ribbons annealed up to 1098 K was observed, corresponding to cubic L2₁ austenite phase. Meanwhile, for the sample annealed at 1123?K a monoclinic 10M martensitic phase was detected. A comparison of magnetic entropy change as a function of the applied field, after using zero-field-cooling thermomagnetic and isothermal magnetization measurements, has been made for the sample annealed at 1073?K.     

Liquid–solid interfacial reactions of Sn–Ag and Sn–Ag–In solders with Cu under bump metallization

Intermetallic compounds formed during the liquid–solid interfacial reaction of Sn–Ag and Sn–Ag–In solder bumps on Cu under bump metallization at temperatures ranging from 240 to 300 °C were investigated. Two types of intermetallic compounds layer, η Cu₆Sn₅ type and ε Cu₃Sn type, were formed between solder and Cu. It was found that indium addition was effective in suppressing the formation of large Ag₃Sn plate in Sn–Ag solder. During interfacial reaction, Cu consumption rate was mainly influenced by superheat of solder, contact area between solder and Cu and morphology of intermetallic compounds. The growth of η intermetallic compounds was governed by a kinetic relation: ΔX = tⁿ, where the exponent n values for Sn–Ag/Cu and Sn–Ag–In/Cu samples at 240 °C were 0.35 ± 0.01 and 0.34 ± 0.02, respectively. The n values increased with reaction temperature, and it was higher for Sn–Ag/Cu than that for Sn–Ag–In/Cu sample at the same temperature. After Cu was exhausted, ε intermetallic compound was converted to η intermetallic compound. The mechanisms for such growth of interfacial intermetallic compounds during the liquid–solid reaction were investigated.     

In vitro degradation behavior and biocompatibility of Mg–Nd–Zn–Zr alloy by hydrofluoric acid treatment

In this paper, Mg–Nd–Zn–Zr alloy (denoted as JDBM) coated with hydrofluoric acid (HF) chemical conversion film (MgF₂) was researched as a potential biodegradable cardiovascular stent material. The microstructures, in vitro degradation and biocompatibility were investigated. The field emission scanning electron microscopy (FE-SEM) and X-ray photoelectron spectroscopy (XPS) showed that a compact MgF₂ film was formed on the surface of JDBM. The corrosion rate decreased in artificial plasma from 0.337 to 0.253 mm·y^? 1 and the electrochemical measurement demonstrated that the corrosion resistance of JDBM alloy could be obviously improved due to the protective MgF₂ film on the surface of the substrate. Meanwhile, the hemolysis ratio of JDBM decreased from 52.0% to 10.1% and the cytotoxicity met the requirement of cellular application after HF treatment. In addition, JDBM and MgF₂ film showed good anti-platelet adhesion, which is a very favorable property for implant material in contact with blood directly.     

In vitro biocompatibility of modified potassium fluorrichterite and potassium fluorrichterite-fluorapatite glass–ceramics

Potassium fluorrichterite (KNaCaMg₅Si₈O₂₂F₂) glass–ceramics were modified by either increasing the concentration of calcium in the glass (GC5), or by the addition of P₂O₅ to produce potassium fluorrichterite-fluorapatite (GP2). The solubility of the stoichiometric composition (GST), GC5 and GP2 were measured using the standard test described in ISO 6872:1995 (Dental Ceramics). Ion release profiles were determined for Si, Ca, Mg, Na, K and P using inductively coupled plasma mass spectrometry and fluoride ion (F⁻) concentration was measured using an ion-selective electrode. The cytotoxicity of all compositions was assessed using cultured rat osteosarcoma cells (ROS, 17/2.8). Cell response was qualitatively assessed using scanning electron microscopy (SEM) and quantitatively using the Alamar blue assay. GST was the least soluble and also released the lowest concentration of ions following immersion in water. Of the modified compositions, GC5 demonstrated intermediate solubility but the greatest ion release while GP2 exhibited the highest solubility. This was most likely due to GC5 having the greatest proportion of residual glass following crystallisation. The mass loss exhibited by GP2 may have been due in part to the partial disintegration of the surface of specimens during solubility testing. SEM demonstrated that all compositions supported the growth of healthy ROS cells on their surfaces, and this data was further supported by the quantitative Alamar blue assay.     

In situ high-temperature X-ray and neutron diffraction of Cu–Mn oxide phases

Copper–manganese oxides were analyzed by in situ high-temperature powder neutron and X-ray diffraction to investigate their crystal structure. Cu–Mn spinel was found to form a continuous solid solution with cubic symmetry between Mn₃O₄ and Cu₂MnO₄. A high-temperature phase with approximate composition Cu₅Mn₄O₉ was shown to have hexagonal symmetry. The cation distribution and lattice parameters of Cu–Mn spinel were resolved through Rietveld refinement of in situ neutron diffraction data. The results demonstrated that the Cu ion has a lower octahedral site preference than manganese ions, and quenching is not a reliable method to determine the equilibrium structure in the system.     

In vitro and in vivo biocompatibility of graded hydroxyapatite–zirconia composite bioceramic

To obtain bioceramics with good osteoinductive ability and mechanical strength, graded hydroxyapatite–zirconia (HA–ZrO₂) composite bioceramics were prepared in this work. The biocompatibility of the bioceramics was investigated in vitro based on acute toxicity and cytotoxicity tests and hemolysis assay. Results showed the studied graded HA–ZrO₂ had little toxicity to mouse and L929 mouse fibroblasts. Also, hemolysis assay indicated a good blood compatibility of the bioceramics. Based on the results of in vitro tests, animal experiments were performed on white New Zealand rabbits by implantation into hip muscles and femur. It was found that the graded HA–ZrO₂ composite bioceramics exhibited superior osteoinductive ability, which may be a promising bioceramics implant.     

Experimental investigation and thermodynamic calculation of phase equilibria in the In–Sb–Zn ternary system

Binary thermodynamic data, successfully used for phase diagram calculations of binary systems In–Sb, In–Zn, and Sb–Zn, were used for prediction of phase equilibria in ternary In–Sb–Zn system. The liquidus projection, invariant equilibria and several vertical sections were calculated using the CALPHAD method. Alloys, situated along three calculated vertical sections, were investigated by differential thermal analysis (DTA). The experimentally determined phase transition temperatures were compared with predicted results. Phase identification of selected samples was done using scanning electron microscopy (SEM) with energy dispersive X-ray microanalysis (EDS).     

Precipitation behavior of Ag–Pd–In dental alloys

Age-hardening characteristics and precipitation behavior of Ag–25%Pd–3%In–1%Zn–0.5%Ir alloy were investigated in detail by means of hardness testing, X-ray diffraction, electron microscopy and resistivity measurement. The solution treating could be accomplished at 980 °C and the aging in the temperature range from 950 to 850 °C occurred by continuous precipitation. The aging in the temperature range from 850 to 450 °C occurred first, forming GP-zones with a hardness increase and then in overaging stage by forming discontinuous precipitation, which consisted of lamellae of solute (Pd, In, Zn) depleted Ag-rich phase and (Pd,Ag)₃(In,Zn) intermetallic phase. The hardness increased very fast to its peak in 10 min during aging at temperatures between 450 and 550 °C.     

Luminescence and energy transfer in Er3+/Nd3+ ion-codoped Ge–In–S–CsBr chalcohalide glasses

This study investigates the emission properties of the Er³⁺/Nd³⁺ ions codoped 70GeS₂–10In₂S₃–20CsBr chalcohalide glasses. The vacuumed melt-quenching technique is employed to synthesize the glasses. The absorption spectra, upconversion and near-IR emission spectra as well as fluorescence decay curves are collected. With the increasing concentration of Er³⁺ ions, the lifetimes at 1073 nm for Nd³⁺ ions decrease from 538 to 420 μs under 808 nm excitation. Meanwhile, the lifetimes at 1540 nm for Er³⁺ ions decrease from 245 to 214 μs with the increasing concentration of Nd³⁺ ions. The emission spectra and lifetimes show that energy transfer exists between the Nd³⁺ and Er³⁺ ions. The luminescence and detailed energy transfer mechanisms are schematically proposed.     

Self-assembly,microstructure and photoluminescence properties of nanocomposite mesoporous silica loaded with In2O3 and In2O3–SnO2

Abstract

The mesoporous nanocomposite fabricated by self-assembly has many unique properties compared with the original materials. In₂O₃ (IO) and In₂O₃–SnO₂ (ITO) in mesoporous silica were studied in the present paper. They were self-assembled in a nanoscale mesoporous silica by an adsorption–annealing process. The composite of IO and ITO in mesoporous silica was characterised by transmission electron microscopy, atomic force microscopy and nitrogen sorption isotherms. Photoluminescence spectra of the samples were measured by a fluorescence spectrophotometer. The results show that the composite was synthesised from IO and ITO in a nano-scale mesoporous silica with assembly structure, and bulk mesoporous silica is easier to be loaded by the particles than the sheet one, but the specific surface area decreases with increasing atomic weight of the substances loaded in silica mesoporous. The results also show that the mesoporous composite doped with some substance may enhance the effect of photoluminescence. For instance, the mesoprous composite of IO/SiO₂ has an enhancement in the effect of photoluminescence, and that of the mesoprous nanocomposite of ITO/SiO₂ is greater. Mesoporous nanocomposite is a promising photoluminescence material in the application to industry.     

Effects of Sn/In additions on natural and artificial ageing of Al–Mg–Si alloys

The effect of Sn or In addition on natural ageing and subsequent artificial ageing of Al–Mg–Si alloys was investigated. In addition not only retarded the natural ageing but also improved the T6 hardness. Although Sn addition retarded the natural ageing as well, precipitation kinetics was delayed. In addition, slightly refined the β′′ phase distribution. But β′′ phase was coarse with addition of Sn. During artificial ageing, the vacancies released from binding complexes promote the formation of β′′. The detrimental effects of Sn on artificial ageing could be attributed to the reduction of the amount of Sn solutes and of available Mg solutes forming β′′.     

Power and gas pressure effects on properties of amorphous In–Ga–ZnO films by magnetron sputtering

Amorphous In–Ga–ZnO thin films were deposited on quartz glass substrate at room temperature utilizing radio frequency magnetron sputtering technique. Sputtering power and oxygen flow rate effects on the physical properties of the In–Ga–ZnO films were systematically investigated. It is shown the film deposition rate and the conductivity of the In–Ga–ZnO films increased with the sputtering power. The as-grown In–Ga–ZnO films deposited at 500 W exhibited the Hall mobility of 17.7 cm²/Vs. Average optical transmittance of the In–Ga–ZnO films is greater than 80% in the visible wavelength. The extracted optical band gap of the In–Ga–ZnO films increased from 3.06 to 3.46 eV with increasing the sputtering power. The electrical properties of the In–Ga–ZnO films are greatly dependent on the O₂/Ar gas flow ratio and post-growth annealing process. Increasing oxygen flow rate converted the In–Ga–ZnO films from semiconducting to semi-insulating, but the resistivity of the films was significantly reduced after being annealed in vacuum. Both the as-grown and annealed In–Ga–ZnO films show n-type electrical conductivity.     

Temperature-dependent current–voltage and capacitance–voltage characteristics of the Ag/n-InP/In Schottky diodes

The current–voltage (I–V) and capacitance–voltage (C–V) characteristics of Ag/n-InP/In Schottky diodes have been studied in a wide temperature range by steps of 10 K. A decrease in the apparent barrier height (BH), , an increase in the ideality factor, and a nonlinearity in the activation energy plot with a decrease in temperature have been seen. The experimental values of BH and ideality factor for the devices were calculated as 0.61 eV and 1.18 at 320 K, 0.48 eV and 1.52 at 200 K, and 0.20 eV and 3.89 at 70 K, respectively. An abnormal decrease in the experimental BH and an increase in the ideality factor n with a decrease in temperature have been explained by the barrier inhomogeneities at the metal–semiconductor (MS) interface. From the temperature dependent I–V characteristics of the Ag/n-InP contact, that is, and A* as 0.79 and 0.55 eV, and 7.96 and , respectively, have been calculated from a modified vs. 1/T plot for the two temperature regions. The Richardson constant values are in close agreement with the value of known for n-type InP. Moreover, the difference between the apparent BHs obtained from the I–V and C–V characteristics has been attributed to the existence of Schottky BH inhomogeneity.