Effects of composition and cooling rate on the microstructure of?Sn–3.7Ag–0.9Zn–Bi solders

The effects of Bi addition, of less than 3 wt.%, and applied cooling rate on the solidified microstructure of the eutectic Sn–3.7Ag–0.9Zn (weight percent, hereafter) solder were investigated. As observed by microstructural analysis, the increase of Bi content favors the separation of the β-Sn and AgZn intermetallic compounds (IMCs) in the eutectic Sn–Ag–Zn solder. And there are some Bi precipitates formed along with the primary β-Sn dendrites as the concentration of Bi exceeds 2%. As the applied cooling rate increases, the microstructure of the Sn–3.7Ag–0.9Zn–Bi solder is refined, and the segregation of Bi is restrained. By increasing the amount of Bi, the microhardness of the solder increases.     

Effects of N and B on continuous cooling transformation diagrams of Mo–V–Ti micro-alloyed steels

Effects of the single addition of nitrogen (N) and boron (B) and the combined addition of N and B on continuous cooling transformation (CCT) diagrams and properties of the three Mo–V–Ti micro-alloyed steels were investigated by means of a combined method of dilatometry and metallography. Microstructures observed in continuous cooled specimens were composed of pearlite (P), quasi-polygonal ferrite (QPF), granular bainite (GB), acicular ferrite (AF), lath-like bainite (LB) and martensite (M) depending on the cooling rates and transformation temperatures. Single addition of 12?ppm B effectively reduced the formation of QPF and broadened the cooling rate region for LB and M. Added N makes the action of B invalid and the QPF region was prominently broadened, and even though the cooling rate is higher than 50°C?s^?1, it cannot obtain full bainite.     

Low-temperature STM/STS investigation of nanostructures created by an STM tip on Au(111) surfaces

The structural stability of rapidly solidified (about 10⁴ K/s) Sn–3.7Ag–0.9Zn eutectic solder was explored by high-temperature annealing. For the as-cast solders, the applied fast cooling rate had a significant influence on the microstructure of the solders. The faster the applied cooling rates, the smaller the β-Sn dendrites. After annealing at 473 K for 20 and 50 h, β-Sn dendrites congregated together into bulk ones for minimizing the interfacial energy, and Ag₃Sn intermetallic compounds (IMCs) as well as ternary Ag–Zn–Sn IMCs segregated on the grain boundary of the β-Sn dendrites. It seems that the coarsening of the β-Sn dendrites in the rapidly solidified specimen brought a significant softening during annealing of the explored Sn–Ag–Zn alloy. Finally, the β-Sn dendrites vanished gradually with increase of the annealing period, which leads to a kind of softening.     

Preparation and characteristics of?a?BaO–Al2O3–B2O3–SiO2–La2O3 glass ceramic via spray pyrolysis

The characteristics of a BaO–Al₂O₃–B₂O₃–SiO₂–La₂O₃ glass ceramic prepared by spray pyrolysis were studied. Glass powders with spherical shape and amorphous phase were prepared by complete melting at a preparation temperature of 1 500°C. The mean size and geometric standard deviation of the powders prepared at the temperature of 1 500°C were 0.6 μm and 1.3. The glass powders had similar composition to that of the spray solution. The glass transition temperature (T _g) of the glass powders was 600.3°C. Two crystallization exothermic peaks were observed at 769.3 and 837.8°C. Densification of the specimen started at a sintering temperature of 600°C, in which Ba₄La₆O(SiO₄)₆ as main crystal structure was observed. Complete densification of the specimen occurred at a sintering temperature of 800°C. The specimens sintered at temperatures above 800°C had main crystal structure of BaAl₂Si₂O₈.     

Phase transformation of Ni/Si thin films induced by nanoindentation and annealing

Thin Ni/Si films are prepared by depositing a Ni layer with a thickness of 100 nm on a Si (100) substrate. The as-deposited thin-film specimens are indented to a maximum depth of 500 nm using a nanoindentation technique and are then annealed at temperatures of 200°C, 300°C, 500°C and 800°C for 2 min. The microstructural changes and phases induced in the various specimens are observed using transmission electron microscopy (TEM) and micro-Raman scattering spectroscopy (RSS). Based on the load-displacement data obtained in the nanoindentation tests, the hardness and Young’s modulus of the as-deposited specimens are found to be 13 GPa and 177 GPa, respectively. The microstructural observations reveal that the nanoindentation process prompts the transformation of the indentation-affected zone of the silicon substrate from a diamond cubic structure to a mixed structure comprising amorphous phase and metastable Si III and Si XII phases. Following annealing at temperatures of 200∼500°C, the indented zone contains either a mixture of amorphous phase and Si III and Si XII phases, or Si III and Si XII phases only, depending on the annealing temperature. In addition, the annealing process prompts the formation of nickel silicide phases at the Ni/Si interface or within the indentation zone. The composition of these phases depends on the annealing temperature. Specifically, Ni₂Si is formed at a temperature of 200°C, NiSi is formed at a temperature of 300°C and 500°C, and NiSi₂ is formed at 800°C.     

Hybrid silicon evanescent approach to optical interconnects

We discuss the recently developed hybrid silicon evanescent platform (HSEP), and its application as a promising candidate for optical interconnects in silicon. A number of key discrete components and a wafer-scale integration process are reviewed. The motivation behind this work is to realize silicon-based photonic integrated circuits possessing unique advantages of III–V materials and silicon-on-insulator waveguides simultaneously through a complementary metal-oxide semiconductor fabrication process. Electrically pumped hybrid silicon distributed feedback and distributed Bragg reflector lasers with integrated hybrid silicon photodetectors are demonstrated coupled to SOI waveguides, serving as the reliable on-chip single-frequency light sources. For the external signal processing, Mach–Zehnder interferometer modulators are demonstrated, showing a resistance-capacitance-limited, 3 dB electrical bandwidth up to 8 GHz and a modulation efficiency of 1.5 V mm. The successful implementation of quantum well intermixing technique opens up the possibility to realize multiple III–V bandgaps in this platform. Sampled grating DBR devices integrated with electroabsorption modulators (EAM) are fabricated, where the bandgaps in gain, mirror, and EAM regions are 1520, 1440 and 1480 nm, respectively. The high-temperature operation characteristics of the HSEP are studied experimentally and theoretically. An overall characteristic temperature (T ₀) of 51°C, an above threshold characteristic temperature (T ₁) of 100°C, and a thermal impedance (Z _T ) of 41.8°C/W, which agrees with the theoretical prediction of 43.5°C/W, are extracted from the Fabry–Perot devices. Scaling this platform to larger dimensions is demonstrated up to 150 mm wafer diameter. A vertical outgassing channel design is developed to accomplish high-quality III–V epitaxial transfer to silicon in a timely and dimension-independent fashion.     

c-axis-textured LiNbO3 thin films on Si (111) substrates

We have successfully prepared highly c-axis-textured LiNbO₃ films on hydrogen-terminated Si (111) substrate using sol-gel spin-coating and rapid thermal annealing. These highly c-axis-textured films were obtained with a preheating at 300 °C for 15 min followed by a rapid thermal annealing at 500–700 °C for 120 s. The c-axis orientation of the LiNbO₃ film is due to a weak effect caused by the 3-fold symmetry match between the film and the Si (111) substrate. The c-axis orientation of LiNbO₃ films is very useful in integrated optics devices and metal–ferroelectric–semiconductor nonvolatile memory applications. Received: 15 September / Accepted: 4 December / Published online: 3 April 2001     

Microwave dielectric properties of the 5.5Li<Subscript>2</Subscript>O–Nb<Subscript>2</Subscript>O<Subscript>5</Subscript>–7TiO<Subscript>2</Subscript> ceramics

A new Li₂O–Nb₂O₅–TiO₂ (LNT) ceramic with the Li₂O:Nb₂O₅:TiO₂ mole ratio of 5.5:1:7 was prepared by solid state reaction route. The phase and structure of the ceramic were characterized by X-ray diffraction and scanning electron microscopy (SEM). The microwave dielectric properties of the ceramics were studied using a network analyzer. The microwave dielectric ceramic has low sintering temperature (∼1075°C) and good microwave dielectric properties of ε _r=42, Q×f=16900 GHz (5.75 GHz), and τ _f =63.7 ppm/°C. The addition of B₂O₃ can effectively lower the sintering temperature from 1075 to 875°C and does not induce degradation of the microwave dielectric properties. Obviously, the LNT ceramics can be applied to microwave low temperature-cofired ceramics (LTCC) devices.     

Electrohydrodynamic micropatterning of silver ink using near-field electrohydrodynamic jet printing with tilted-outlet nozzle

This paper introduces for the first time near-field electrohydrodynamic jet printing with tilted-outlet nozzle to obtain the fine and highly conductive patterns of silver (Ag) ink. Line widths produced by near-field electrohydrodynamic jet printing are less than 6 μm, which is approximately twenty times smaller than that of inkjet printing. Under optimized Ag ink annealing ranges 3–9 min for 30 wt% at 150°C, we observed Ag line pattern resistivities as low as 7×10⁻⁶ Ω⋅cm. Ag ink conduction mechanisms were brought to light from microstructure analysis and post-thermal-annealing examination of electrical characteristics.     

Structural, electrical, and surface characteristics of La0.5Sr0.5CoO3 thin films prepared by pulsed-laser deposition

A parametric study of the growth of La_0.5Sr_0.5CoO₃ (LSCO) thin films on (100) MgO substrates by pulsed-laser deposition (PLD) is reported. Films are grown under a wide range of substrate temperature (450–800 °C), oxygen pressure (0.1–0.9 mbar), and incident laser fluence (0.8–2.6 J/cm²). The optimum ranges of temperature, oxygen pressure, and laser fluence to produce c-axis oriented films with smooth surface morphology and high metallic conductivity are identified. Films deposited at low temperature (500 °C) and post-annealed in situ at higher temperatures (600–800 °C) are also investigated with respect to their structure, surface morphology, and electrical conductivity. Received: 20 November 1998 / Accepted: 6 July 1999 / Published online: 21 October 1999     

Structure and electrical properties of HfO<Subscript>2</Subscript> high-<Emphasis Type="Italic">k</Emphasis> films prepared by pulsed laser deposition on Si (100)

High-k gate dielectric hafnium dioxide films were grown on Si (100) substrate by pulsed laser deposition at room temperature. The as-deposited films were amorphous and that were monoclinic and orthorhombic after annealed at 500°C in air and N₂ atmosphere, respectively. After annealed, the accumulation capacitance values increase rapidly and the flat-band voltage shifts from −1.34 V to 0.449 V due to the generation of negative charges via post-annealing. The dielectric constant is in the range of 8–40 depending on the microstructure. The I–V curve indicates that the films possess of a promising low leakage current density of 4.2×10⁻⁸ A/cm² at the applied voltage of −1.5 V.     

Consideration of the growth mode in isochronal austenite-ferrite transformation of ultra-low-carbon Fe–C alloy

The three cooling rates of 10, 100, 200 K/min dilatometry experiments are used to investigate the kinetics of the isochronal austenite (γ) to ferrite (α) transformation of Fe–0.0036wt.%C alloy. “Normal transformation” and “abnormal transformation” have both been observed for transformations at different cooling rates. In accordance with the thermodynamic characteristics of the γ→α transformation investigated here and previous kinetic considerations, a JMAK-like approach for the kinetics of isochronal phase transformations was developed that incorporates three overlapping processes: site saturation nucleation, alternate growth modes (from interface-controlled to diffusion-controlled to interface-controlled growth), as well as impingement for random distribution nuclei. The JMAK-like approach has been employed to fit the experimental results, and the fitting results show that for the γ→α transformation of the Fe–C alloy at all applied cooling rates, the growth mode evolves in the corresponding order: from interface-controlled to diffusion-controlled growth; from interface-controlled to diffusion-controlled to interface-controlled growth; and interface-controlled growth.     

Nanocrystalline CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> powder by PVA sol–gel route: synthesis,characterization and its giant dielectric constant

Nanocrystalline CaCu₃Ti₄O₁₂ powders were synthesized by a simple PVA sol–gel route and calcined at 700 and 800°C in air for 8 h. The diameter of the powders ranges from 40–100 nm. The calcined CaCu₃Ti₄O₁₂ powders were characterized by TG-DTA, XRD, FTIR, SEM, and TEM. Sintering of the powders was conducted in air at 1100°C for 16 h. The XRD results indicated that all sintered samples had a typical perovskite CaCu₃Ti₄O₁₂ structure although the sintered samples contained some amount of CaTiO₃. SEM of the sintered CaCu₃Ti₄O₁₂ ceramics showed the average grain sizes of 13–15 μm. The samples exhibit a giant dielectric constant, ε′∼10⁵ at 150 to 200°C with weak temperature dependence below 1 kHz in the sample sintered using the powders calcined at 700°C. The Maxwell–Wagner polarization mechanism is used to explain the high permittivity in these ceramics. It is also found that all sintered samples have the same activation energy of grains, which is ∼0.122 eV.     

Microstructure changes in two phase β+ γ Co-Ni-Al ferromagnetic shape memory alloys in relation to Al/Co ratio

The microstructure of Co_{35 + x}-Ni_{40 - x}-Al₂₅ (x = 0, 2.5, 5.0) ferromagnetic shape memory alloys annealed at 1200 °C and water quenched has been investigated by optical (OM) and analytical transmission electron microscopy (TEM). The microstructure consists of elongated grains of martensite and γ phase. Annealing twins were found frequently in the γ phase. The volume fraction of γ phase has been determined to be about 40%. TEM observations show twinned L1₀ martensite with {111}-type twinning plane and tetragonality c/a = 0.85 in all investigated alloys. Determination of the composition of β phase, allows to calculate Al/Co and e/a ratio in the range 7.68–8.40 in correlation with its Ms temperatures between 66 and 167 °C, respectively. An increase in the Al/Co ratio together with a decrease of Ni content in β phase causes a decrease of the e/a ratio, which promotes a decrease of martensitic transformation temperatures.     

Transparence and electrical properties of ZnO-based multilayer electrode

Three-layered ZnO/Ag–Ti/ZnO structures were prepared using both the sol-gel technique and DC magnetron sputtering. This study focuses on the electrical and optical properties of the ZnO/Ag–Ti/ZnO multilayers with various thicknesses of the Ag–Ti layer. The ZnO thin film prepared by the sol–gel method was dried at 300°C for 3 minutes, and a fixed thickness of 20 nm was obtained. The thickness of the Ag–Ti thin film was controlled by varying the sputtering time. The Ag–Ti layer substantially reduced the electrical resistivity of the sol–gel-sprayed ZnO thin films. The sheet resistance of the Ag–Ti layer decreased dramatically and then became steady beyond a sputtering time of 60 s. The sputtering time of Ag–Ti thin film deposition was determined to be 60 s, taking into account the optical transmittance. Consequently, the transmittance of the ZnO/Ag–Ti/ZnO multilayer films was 71% at 550 nm and 60% at 350 nm. The sheet resistance was 4.2 Ω/sq.     

Secondary defects in low-energy As-implanted Si

14 /cm² dose of As ions followed by both isochronal and isothermal annealing. The elementary defects generated first during solid-phase epitaxial recovery of implantation-induced amorphous layers at temperatures of 550 °C and/or 600 °C are {311} defects 2–3 nm long. They are considered to be transformed into {111} and {100} defects after annealing at temperatures higher than 750 °C. These secondary defects show the opposite annealing behavior to the dissolution and growth by the difference of their depth positions at 800 °C. This phenomenon is explained by the diffusion of self-interstitials contained in defects. With regard to the formation and dissolution of defects, there is no significant difference between the effects of rapid thermal annealing (950 °C for 10 s) and furnace annealing (800 °C for 10 min). Received: 14 November 1997/Accepted: 16 November 1997     

Thermally activated diffusion of magnesium from bioapatite crystals

We have attempted to use heat treatment followed by ultrasonic treatment to separate the apatite from the non-apatite components of bone mineral in samples from different animals. The Mg content and the Ca/P ratio in the temperature range 560°C–720°C in the samples before and after ultrasonic treatment were determined by electron-probe x-ray microanalysis. Furthermore, we used atomic absorption spectrometry to measure the Mg content in powdered bone samples only after annealing and in distilled water, which was the “sonication” medium. We obtained evidence for thermally activated transition of Mg from a structurally bound state to a labile state at 680°C–720°C. At the same temperature, the Ca-deficient apatite is transformed to stoichiometric apatite. The data presented are evidence that crystals of Ca-deficient bioapatite are surrounded by Ca-enriched surface layers. As a result of thermal transformations at 680°C-720°C, all the Mg in the biomineral is found in the non-apatite environment surrounding the crystals and is removed by ultrasonic treatment, while the surface-localized Ca penetrates into the apatite lattice, restoring its stoichiometry. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 73, No. 3, pp. 385–391, May–June, 2006.     

Low-temperature tempering kinetics of hardened steel 38KhN3MFA

Diffraction electron microscopy was used in a study of the decay kinetics of the α-iron solid solution and the growth kinetics of cementite particles in steel 38KhN3MFA after tempering at 200–550°C. Growth equations are written for cementite particles formed in lamellar high-temperature martensite crystals. Tomsk Structural Engineering Institute, Tomsk. Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 2, pp. 39–44, February, 1993.     

Trap characterization for Bi4Ti3O12 thin films by thermally stimulated currents

Thermally stimulated current (TSC) measurements performed in the 100 K–400 K temperature range on Bi₄Ti₃O₁₂ (BiT) thin films annealed at 550 °C and 700 °C had revealed two trapping levels having activation energies of 0.55 eV and 0.6 eV. The total trap concentration was estimated at 10¹⁵ cm⁻³ for the samples annealed at 550 °C and 3×10¹⁵ cm⁻³ for a 700 °C annealing and the trap capture cross-section was estimated about 10⁻¹⁸ cm². From the temperature dependence of the dark current in the temperature range 20 °C–120 °C the conduction mechanism activation energy was found to be about 0.956–0.978 eV. The electrical conductivity depends not only on the sample annealing temperature but also whether the measurement is performed in vacuum or air. The results on the dark conductivity are discussed considering the influence of oxygen atoms and oxygen vacancies. Received: 28 January 1998 / Accepted: 8 January 1999 / Published online: 5 May 1999     

Production of biologically inert Teflon thin layers on the surface of allergenic metal objects by pulsed laser deposition technology

Allergic-type diseases are current nowadays, and they are frequently caused by certain metals. We demonstrated that the metal objects can be covered by Teflon protective thin layers using a pulsed laser deposition procedure. An ArF excimer laser beam was focused onto the surface of pressed PTFE powder pellets; the applied fluences were 7.5–7.7 J/cm². Teflon films were deposited on fourteen-carat gold, silver and titanium plates. The number of ablating pulses was 10000. Post-annealing of the films was carried out in atmospheric air at oven temperatures between 320 and 500 °C. The thickness of the thin layers was around 5 μm. The prepared films were granular without heat treatment or after annealing at a temperature below 340 °C. At 360 °C a crystalline, contiguous, smooth, very compact and pinhole-free thin layer was produced; a melted and re-solidified morphology was observed above 420 °C. The adhesion strength between the Teflon films and the metal substrates was determined. This could exceed 1–4 MPa depending on the treatment temperature. It was proved that the prepared Teflon layers can be suitable for prevention of contact between the human body and allergen metals and so for avoidance of metal allergy. Received: 12 June 2002 / Accepted: 13 June 2002 / Published online: 4 November 2002 RID="*" ID="*"Corresponding author. E-mail: bhopp@physx.u-szeged.hu