Solidification and interfacial interactions in gold–tin system during eutectic or thermo-compression bonding for 200 mm MEMS wafer level hermetic packaging

In this work, Au–Sn eutectic bonding and Au–Sn thermo-compression bonding are studied for applications in hermetic packaging at wafer level. Eutectic bonding experiments were performed under vacuum or pure nitrogen at temperatures between 300 and 350 °C while thermo-compression bonding experiments were performed under vacuum at 270 °C. During these experiments, the solidification of electrodeposited Au–Sn alloy as well as the interaction of this alloy with W₂N layers are studied. Some supplementary specific brazing experiments were performed using commercial sheets of eutectic Au–Sn alloy in order to understand the mechanisms of interactions between the Au–Sn alloy and the W₂N layer and of solidification of the Au–Sn eutectic alloy. The melting and solidification process of eutectic Au–Sn alloy were studied by differential scanning calorimetry under different geometrical configurations such as commercial eutectic Au–Sn sheets alone, brazing joints performed by commercial eutectic Au–Sn alloy and samples made by thermo-compression bonding. Bonded wafers with good mechanical properties were characterized by cross-section scanning electron microscopy using energy dispersive X-ray mode. Some samples were characterized by transmission electron microscopy. The mechanical strength of the seal was checked by shear tests.     

Graphene sheets decorated with ZnO nanoparticles as anode materials for lithium ion batteries

ZnO/graphene composites were synthesized using a facile solution-based method. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction, thermogravimetric analysis, and Raman spectra revealed that ZnO nanoparticles with a particle size of around 4 nm were densely and homogeneously deposited on graphene sheets. As the anode material for the lithium ion batteries, the ZnO/graphene composites delivered a stable capacity of 404 mAh/g after 100 cycles at a current rate of 0.5 C, which is much superior to bare ZnO nanoparticles. The battery performance result indicates the presence of graphene sheets in the composites effectively enhance the conductivity and accommodate the volume change.     

Transparent conductive and infrared reflective AZO/Cu/AZO multilayer film prepared by RF magnetron sputtering

AZO/Cu/AZO multilayer films were prepared on glass substrate by radio frequency magnetron sputtering technology. The prepared films were investigated by a four-point probe system, X-ray diffraction, optical transmittance spectra, scanning electron microscope, atomic force microscopy and Fourier transform infrared spectroscopy. The results showed that Cu inner layer started forming a continuous film at the thickness around 11 nm. The prepared AZO/Cu/AZO samples exhibited the visible transmittance of 60–80 % and sample with 15 nm Cu inner layer showed the highest infrared reflection rate of 67 % in FIR region and the lowest sheet resistance of 16.6 Ω/sq. The proper visible transmittance and infrared reflection property of the AZO/Cu/AZO multilayer film make it a promising candidate for future energy conservation materials.     

Synthesis and characterization of electrochemically-reduced graphene

Graphene has superior electrical conductivity than graphite and other allotropes of carbon because of its high surface area and chemical tolerance. Electrochemically processed graphene sheets were obtained through the reduction of graphene oxide from hydrazine hydrate. The prepared samples were heated to different temperatures such as 673 and 873 K. X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDXS), transmission electron microscopy (TEM), Raman spectra and conductivity measurements were made for as-prepared and heat-treated graphene samples. XRD pattern of graphene shows a sharp and intensive peak centred at a diffraction angle (2θ) of 26·350. FTIR spectra of as-prepared and heated graphene were used to confirm the oxidation of graphite. TEM results indicated that the defect density and number of layers of graphene sheets were varied with heating temperature. The hexagonal sheet morphology and purity of as-prepared and heat treated samples were confirmed by SEM–EDX and Raman spectroscopy. The conductivity measurements revealed that the conductivity of graphene was decreased with an increase in heating temperature. The present study explains that graphene with enhanced functional properties can be achieved from the as-prepared sample.     

Growth of TiO2 nanowire bundle arrays and their application in dye-sensitized solar cells

Highly oriented single-crystalline TiO₂ nanowire bundle arrays on transparent conductive fluorine-doped tin oxide substrates are prepared by hydrothermal method using the precursors of titanium butoxide, deionized water and hydrochloric acid. The structure and morphology characteristics of all the samples have been analyzed by X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy. Results show that the diameter, length, and density of the nanowire bundle arrays can be varied by changing the growth parameters, such as growth time, initial reactant concentration and acidity. The enhanced (002) peak in XRD patterns indicate that the nanowire is well crystallized and grow perpendicular to the substrate. The high resolution transmission electron microscope images and selected-area electron diffraction patterns confirm that there are approximately 10–30 nanowires in each bundle. The nanowire is single crystalline. Dye-sensitized solar cells assembled from oriented TiO₂ nanowire bundle arrays as the photoanode are studied. The light-to-electricity conversion efficiency is about 2.17 %.     

Surface modification and enhanced multiferroic behavior of BiFe<Subscript>0.25</Subscript>Cr<Subscript>0.75</Subscript>O<Subscript>3</Subscript> films with different thickness over Pt(111)/Ti/SiO<Subscript>2</Subscript>/Si substrate

Polycrystalline BiFe_0.25Cr_0.75O₃ thin films have been fabricated via a chemical deposition technique at various thicknesses (60-, 130-, 190-, 240 nm). The effect of Cr substitution on BiFeO₃ structures have been briefly discussed by performing X-ray diffraction and SAED pattern. The nature of the films surface at different thicknesses were briefly discussed using scanning electron microscope and transmission electron microscope. Roughness and other amplitude parameters of the film at different thickness are studied through atomic force microscopy. The result indicates that, when changing the thickness of the film, the average bond length gets changed causing difference in electrical and magnetic properties. Electrical and dielectric study reveals thickness dependent property and is deeply understood from space charge, oxygen vacancies and super-exchange interaction. Film at 60 nm shows higher magnetization with 8.5042 emu/cm³ and with a retentivity of 3.852 emu/cm³ than the thick film. Further, the spin-cooling behavior and magnetization below room temperature from 2 to 300 K were analyzed briefly for spintronics applications.     

Structural, magnetic and electromagnetic wave absorption properties of SrFe12O19/ZnO nanocomposites

Microwave absorption of nanocomposites of strontium ferrite and zinc oxide has been investigated. M-type strontium ferrite powders synthesized by a sol–gel method were combined with different concentrations of ZnO using a new method. The samples were characterized by various experimental techniques including TGA/DTA, X-ray diffraction, transmission electron microscopy, vibrating sample magnetometer and vector network analyzer. Reflection loss of nanocomposites has been measured in two frequency ranges of 8–12 GHz (X-band) and 12–18 GHz (Ku-band). The saturation magnetization of the nanocomposites decreased with increasing concentration of ZnO, but reflection loss in the Ku frequency band is enhanced by up to 5 dB for 15 % of ZnO in the nanocomposites.     

Synthesis, structural and optical properties of Ni-doped ZnO micro-spheres

Ni doped ZnO nanoparticles were synthesized by a simple chemical method at low temperature with Ni:Zn atomic ratio from 0 to 5 %. The synthesis process is based on the hydrolysis of zinc acetate dihydrate and nickel acetate tetrahydrate followed by heat treatment at 65 °C under refluxing using methanol as a solvent. X-ray diffraction analysis reveals that the Ni-doped ZnO crystallizes in a wurtzite structure with crystal size of 4–11 nm. These nanocrystals self-aggregated themselves into hollow spheres of size of 600–170 nm. High resolution transmission electron microscopy image shows that each sphere is made up of numerous nanoparticles of average diameter 4 nm. The XRD patterns, Scanning electron microscopy and transmission electron microscopy micrographs of doping of Ni in ZnO are confirmed the formation of micro-spheres. Furthermore, the UV–vis. spectra and photoluminescence spectra of the Ni-doped ZnO nanoparticles were also investigated. The band gap of the nanoparticles can be tuned in the range of 3.55–3.36 eV by the use of the dopants. The observed red shift in the band gap from UV–visible analysis and near band edge UV emission with Ni doping may be considered to be related to the incorporation of Ni ions into the Zn site of the ZnO lattice.     

Few-layer graphene films prepared from commercial copper foil tape

We present a facile, versatile and cost-effective method for the synthesis of mono- and bilayer graphene films on copper substrate using as carbon feedstock the pyrolysis products of the conductive adhesive polymer of a commercial copper tape commonly used in electron microscopy. A copper tape with adhesive on both sides is subjected to a heat treatment during 15 min at temperatures of 900, 1000, and 1050 °C under the flow of an Ar + 3%H₂ gas mixture. With this treatment, the tape adhesive polymer is pyrolized and the interaction of its decomposition products with the copper substrate gives rise to a graphene film of good structural quality mixed with amorphous carbon residues of the pyrolysis. For a temperature of 1050 °C (few degrees below the melting point of Cu), mono- and bilayer coexisting domains of graphene are obtained with almost 100% area coverage of the Cu substrate. For lower heat treatment temperatures, area coverage is reduced to 60–70% and the graphene film becomes predominantly bilayer. The treatment at the lowest temperature of 900 °C results in isolated hexagonal domains of graphene intermixed with a large amount of amorphous carbon residues and large uncovered areas of oxidized copper substrate. These results indicate that the number of active species for the formation of graphene films increases with increasing temperature, nevertheless limited by the copper melting point. Characterization of the obtained samples was performed with scanning electron microscopy, Raman scattering, and high-resolution transmission electron microscopy.     

C60 and C70 pressure-and-temperature transformations into fullerene-related forms

A two-stage pressure-and-temperature treatment of the C₆₀ and C₇₀ fullerites was carried out. C₆₀ and C₇₀ molecules collapsed at the first-stage hot-isostatic-pressing (HIP; 220 MPa, argon) and transformed into some fullerene-related form in the 900–1750°C temperature range. These materials were used at the second stage of the high-pressure-high-temperature (HPHT; 7.7 GPa/1400°C) treatment to produce the bulk samples that had: a specific weight of about 2.0 g/cm³, 40/110 GPa Young modulus, 6.0/12.5 GPa, and elastic recovery above 81%. Transformations under the treatments were investigated with the X-ray and transmission electron microscopy techniques. The mechanism of the pressure-and-temperature transformations is discussed.     

Synthesis and characterization of copper sulfide nanocrystal with three-dimensional flower-shape

New copper sulfide nanocrystals with three-dimensional (3D) flower-shape were synthesized by using copper acetate (Cu(ac)₂) and citric acid (cit) and thiourea (Tu) as precursors at 160 °C in an anhydrous ethanol by a solvothermal route. The structure and properties of as-prepared products were characterized by X-ray powder diffraction, transmission electron microscopy, field emission scanning electron microscope and scanning electron microscope. The optical properties of copper sulfide nanocrystals were examined by UV–vis and FTIR. The crystal growth mechanism was also proposed.     

Effect of microwave sintering on the structural, optical and electrical properties of BaTiO3 nanoparticles

BaTiO₃ nanoparticles were prepared by high energy ball milling and subjected to conventional and microwave post sintering at 1,000 °C. From the powder X-ray diffraction results, the synthesized material exhibits strong tetragonality with large c/a ratio. Scanning electron microscope results show the formation of tetragonal shaped BaTiO₃ crystals in the nanometer scale and a significant reduction in the particle size for the microwave sintered sample. The reduced d-spacing of 1.741 Å with high crystallinity for the microwave sintered material is revealed by high resolution transmission electron microscopy analysis. Ultraviolet–visible spectroscopy studies confirm the higher optical band gap (E_g) of 4.157 eV for the microwave sintered sample. Microwave sintered sample shows a very high dielectric constant of ε_r = 4,445 with a low dielectric loss as tan δ = 0.0961. Microwave sintered sample exhibit a high polarization maximum of 73 μC/mm² with reduced coercivity to be 0.293 kV/mm.     

Structural,optical and electrical properties of Zn-doped SnO2 nanoparticles synthesized by the co-precipitation technique

Nanometric size Zn-doped SnO₂ particles with Zn concentration varying from 1 to 6 % were prepared using the co-precipitation method. X-ray diffraction patterns show for all samples a typical rutile-type tetragonal structure of SnO₂ without any additional peaks from spurious phases. These results together with transmission electron microscopy analyses have shown that the size of the nanoparticles decreases with Zn doping down to 4 nm. According to UV–visible absorption measurements this decrease of particle size is accompanied by a decrease of the band gap value from 3.34 eV for SnO₂ down to 3.28 eV for 6 % Zn doping. The electrical conductivity of the system has been investigated between 473 and 718 K, in the 200 Hz–5 MHz frequency range, by means of impedance spectroscopy. The temperature dependence of the bulk conductivity was found to obey the Arrhenius law with activation energies of 0.74 eV for SnO₂ and 0.69 eV for 6 % Zn doping.     

A comparative study of ZnNb2O6 nanoceramics synthesized by high energy ball milling and subsequent conventional and microwave annealing

Ball-milling and subsequent conventional and microwave assisted heating processes have been applied to synthesize ZnNb₂O₆ nanoceramic. X-ray diffraction, simultaneous thermal analysis, scanning electron microscope (SEM), transmission electron microscope (TEM) and BET techniques were utilized to characterize the as-milled and annealed samples. Characterization of synthesized powders revealed that in spite of the very short heating time in the microwave process without soaking time, the powder heated at 550 °C had all physical properties similar to powders synthesized in conventional heating at the 650 °C temperature with a heating rate of 10 °C/min and a soaking time of 1 h. In addition, SEM, TEM and BET observations of synthesized powders showed that the particle size of powders lies in the nano meter range.     

The preparation of novel hollow tetragonal starlike polyaniline and its electrochemical performance

Novel hollow tetragonal starlike polyaniline (HTS-PANI) doped with citric acid has been successfully synthesized by hydrothermal method for the first time. Scanning electron microscopy, transmission electron microscopy, UV–visible spectroscopy, Fourier transmission infrared spectroscopy, and X-ray diffraction were employed to analysis the morphology and structure of the obtained PANI. The results show that the HTS-PANI is in semi redox state and highly crystallized, accompanied with good thermal stability. According to the galvanostatic charge–discharge analysis, the specific capacitance of the sample is up to 460 F g^?1 at a current density of 0.2 A g^?1 in 1 M KCl electrolyte, and retains about 58 % after 1,000 charge–discharge processes at a current density of 5 A g^?1.     

Crystallization of amorphous Al-Cu films

Quench-condensed (- 160°C) Al-Cu films in the composition range from 19% to 50% Cu were heated to room temperature and annealed up to 300°C. The temperature dependence of the resistivity and the temperature coefficient of the resistivity were observed during various cycles of temperature changes. The films are amorphous at the condensation temperature. Phase transitions which occur as the temperature is increased initiate sharp decreases in the resistance. Investigations of the film structure and composition were carried out with an electron microscope (transmission electron microscopy, electron diffraction, scanning transmission electron microscopy and X-ray microanalysis). The results could be clearly related to the phase transitions as observed via the resistance changes during annealing. For film compositions below 37.4% Cu the phase transition is determined by a eutectic crystallization into two phases. For larger copper contents, an intermediate single- phase state is produced first during the transition by polymorphous crystallization and is succeeded by a multiphase stable state.     

The growth of unusually large grains in thin Al-Cu films

The recrystallization of Al-Cu films with copper contents greater than 77.8% prepared by evaporation onto glass substrates in an ultrahigh vacuum at temperatures between -160 and 200°C was investigated. The film properties were determined by measuring the resistance change during annealing by transmission electron microscopy and by electron diffraction examination. Films with a copper content of 90%–94% which were condensed at -160°C and subsequently annealed at temperatures up to 200°C were transformed into large-grained samples. Grain diameters (flat single crystals) in excess of 100 μm were observed in films about 50 nm thick. The flat crystals were oriented in the [111] direction.     

Fabrication and evaluation of physical properties and cytotoxicity of zein-based polyurethanes

Polyurethane prepolymer (PUP) was first synthesized from polycaprolactone diol and isophorone diisocyanate; and then a series of zein-based polyurethane (ZEPU) sheets was fabricated from PUP and zein (ZE) using a hot press and moulding process without addition of other additives. Effects of ZE content (W_ZE) on the structure and properties of the resultant ZEPU sheets were investigated by Fourier transform infrared spectroscopy, scanning electron microscopy, dynamic mechanical analysis, tensile testing, and dissolubility testing in alcohol. The results indicated that cross-linking and grafting reactions occurred between ZE and PUP to form new polyurethane showing a higher thermal stability, flexibility, and alcohol-resistance than the neat ZE sheets. For example, the elongation at break of ZEPU with 50 % W_ZE was 211.2 %, which was 47 times higher than that of neat ZE sheet. ZE molecules acted as both cross-linkers and polymer fillers in ZEPU sheets. The cytotoxicity and cytocompatibility of ZEPU sheets were evaluated by cell culture in vitro. The ZEPU sheets showed non- or low-cytotoxicity, and L929 cells grew and expanded well on the surfaces of the sheets with W_ZE over 50 %. Undoubtedly, the fabrication of ZE-based polyurethanes without toxic additives such as catalysts, cross-linkers and chain extenders improved the physical properties and cytocompatibility of zein, thus widening the possible range of applications for zein-based biomaterials.     

Mechanochemical Synthesis and Characterization of Group II-VI Semiconductor Nanoparticles

Synthesis of metal sulfide semiconductor nanoparticles of group II-VI; namely ZnS, PbS, CdS, and CuS; by mechanochemical method was carried out in a high energy ball mill from corresponding metal acetates and sodium sulfide. The samples were continuously milled for 10 h with sample withdrawal at 2 h time interval. Structural properties of nanoparticles were studied by x-ray diffraction (XRD), transmission electron microscope (TEM), and ultraviolet-visible spectra. Particle size distribution and stability of 10 h milled samples were examined using particle size analyzer and Turbiscan. It was found that nanoparticles synthesized by mechanochemical method had mean particle sizes as small as 2–25 nm, low agglomeration, narrow size distribution, and uniformity of particle structure and morphology.     

One-step synthesis of conductive ceria/polypyrrole nanocomposite particles via photo-induced polymerization method

Inorganic–organic nanocomposites of ceria/polypyrrole with core/shell morphology and median diameter about of 150 nm in single nanoparticles were synthesized by a novel one-step photo-polymerization method using cerium (III) nitrate hexahydrate dissolved in acetonitrile and irradiation under UV wavelengths for 2 h. The photo-polymerization products were characterized using high resolution transmission electron microscopy, Fourier-transform infrared spectroscopy, energy-dispersive X-ray spectroscopy, wide-angle X-ray diffraction, particle size analysis, and field emission scanning electron microscope. Crystalline/amorphous structure was detected for the obtained core/shell nanoparticles via selected area electron diffraction pattern. Electrical conductivity of the nanoparticles was measured by four-probe technique.