Effect of BiFeO3 addition on Bi2O3–ZnO–Nb2O5 based ceramics

In this paper, low temperature sintering of the Bi₂(Zn_1/3Nb_2/3)₂O₇ (β-BZN) dielectric ceramics was studied with the use of BiFeO₃ as a sintering aid. The effects of BiFeO₃ contents and the sintering temperature on the phase structure, density and dielectric properties were investigated. The results showed that the sintering temperature could be decreased and the dielectric properties could be retained by the addition of BiFeO₃. The structure of BiFeO₃ doped β-BZN was still the monoclinic pyrochlore phase. The sintering temperature of BiFeO₃ doped β-BZN ceramics was reduced from 1000 °C to 920 °C. In the case of 0.15 wt.% BiFeO₃ addition, the β-BZN ceramics sintered at 920 °C exhibited good dielectric properties, which were listed as follows: ε_r = 79 and tan δ = 0.00086 at a frequency of 1 MHz. The obtained properties make this composition to be a good candidate for the LTCC application.     

Effects of nano-carbon doping and sintering temperature on microstructure and properties of MgB2

We fabricated nano-carbon (NC) doped MgB₂ bulks using an in situ process in order to improve the critical current density (J_c) under a high magnetic field and evaluated the correlated effects of the doped carbon content and sintering temperature on the phase formation, microstructure and critical properties. MgB_2−xC_x bulks with x = 0 and 0.05 were fabricated by pressing the powder into pellets and sintering at 800 °C, 900 °C, or 1000 °C for 30 min.We observed that NC was an effective dopant for MgB₂ and that part of it was incorporated into the MgB₂ while the other part remained (undoped), which reduced the grain size. The actual C content was estimated to be 68–90% of the nominal content. The NC doped samples exhibited lower T_c values and better J_c(B) behavior than the undoped samples. The doped sample sintered at 900 °C showed the highest J_c value due to its high doping level, small amount of second phase, and fine grains. On the other hand, the J_c was decreased at a sintering temperature of 1000 °C as a result of the formation of MgB₄ phase.     

Anneal temperature dependence of Si/SiO2 superlattices photoluminescence

Photoluminescence spectroscopy, Fourier transform infrared spectroscopy, X-ray reflectometry and high resolution electron microscopy have been used to interpret the photoluminescence properties of annealed (3/19 nm) Si/SiO₂ multilayers grown by reactive magnetron sputtering. The multilayers show an emission in the visible and near-infrared range after heat treatment from 900°C which tends to decrease from 1200°C. Three different origins for the photoluminescence activity have been found. An anneal temperature of 1200°C is necessary to optimise the silicon crystallisation within the silicon sublayers.     

Anodization of aluminium thin films on pSi and annihilation of strong luminescence from Al2O3

Photoluminescence (PL) of Al₂O₃ films obtained by anodization of thermally evaporated and annealed thin Al films on p⁺⁺Si in 0.3 M oxalic acid has been investigated. Thermal annealing at 200–950 °C under the dry nitrogen atmosphere was used for deactivation of luminescence centres. Luminescence from as grown films was broad and located at 425 nm. This luminescence reached to highest level after annealing at 600 °C. Maximum 10 min was required for full optical activation and prolonged annealing up to 4 h did not change the luminescence intensity. Because of deep levels, absorption band edge of as grown films was shifted to the lower energy which is 3.25 eV. Annealing above 800 °C reduced the PL intensity and this observation was correlated with the blue shift of band edge as the defects annealed out. Disappearing PL intensity and blue shift of band edge absorption after annealing at 950 °C was mainly attributed to the oxygen-related defects and partly to impurities that may be originated from oxalic acid. AFM results did not show any hexagonally ordered holes but uniformly distributed nanosized Al₂O₃ clusters that were clearly seen. XRD measurements on as grown Al₂O₃ showed only [1 1 0] direction of α phase. Debye–Scherer calculation for this line indicates that cluster size is 35.7 nm. XRD and AFM pictures suggest that nanocrystalline Al₂O₃ are embedded in amorphous Al₂O₃.     

Investigation of the formation of silicon nanocrystals by annealing of amorphous SiCx/c-Si structures

In this work, we study the changes in the optical properties of 300-nm-thick hydrogenated amorphous silicon carbide layers after an annealing process. Both intrinsic and phosphorus-doped amorphous silicon carbide layers (a-SiC_x:H) were deposited on silicon wafers by plasma enhanced chemical vapour deposition (PECVD) at 400 °C and annealed in a quartz furnace at 800 °C. The presence of randomly oriented silicon nanocrystals was confirmed by X-ray diffraction (XRD) measurements after the partial recrystallization process only in the doped layers. The presence or the absence of the nanocrystals clearly changes the Fourier transform infrared (FTIR) spectra. From the fitting of the experimental curves with the model of Lorentz oscillators, the refractive index and the extinction coefficient of the different layers were obtained.     

Pore formation in in situ processed MgB2 superconductors

MgB₂ bulks were prepared by an in situ process which utilizes the reaction between boron and magnesium powder. The reaction time was fixed at 0.5 h and the temperature was changed from 600 °C to 1000 °C. The density decrease due to pore formation and mass (mainly magnesium) loss during the formation reaction of MgB₂ was observed in all samples. In addition to the pore formation, a pellet expansion which can be explained by the outgrowth of MgB₂ grains was also observed. Two different mechanisms were adopted to explain the pore formation; Kirkendall pores formed at a temperature below the melting point (m.p.) of magnesium by a difference in the diffusivity between magnesium and boron, and the pores formed at a temperature above the m.p. by melting of magnesium and a capillary movement. The density, T_c and J_c results suggest that the current carrying capacity can be improved by a careful control of the process parameters regarding a pore evolution.     

Si-nanostructures formation in amorphous silicon nitride SiNx:H deposited by remote PECVD

The formation of silicon nanoclusters embedded in amorphous silicon nitride (SiN_x:H) can be of great interest for optoelectronic devices such as solar cells. Here amorphous SiN_x:H layers have been deposited by remote microwave-assisted chemical vapor deposition at 300 °C substrate temperature and with different ammonia [NH₃]/silane [SiH₄] gas flow ratios (R=0.5−5). Post-thermal annealing was carried out at 700 °C during 30 min to form the silicon nanoclusters. The composition of the layers was determined by Rutherford back scattering (RBS) and elastic recoil detection analysis (ERDA). Fourier transform infrared spectroscopy (FTIR) showed that the densities of SiH (2160 cm⁻¹) and NH (3330 cm⁻¹) molecules are reduced after thermal annealing for SiN:H films deposited at flow gas ratio R>1.5. Breaking the SiH bonding provide Si atoms in excess in the bulk of the layer, which can nucleate and form Si nanostructures. The analysis of the photoluminescence (PL) spectra for different stoichiometric layers showed a strong dependence of the peak characteristics (position, intensity, etc.) on the gas flow ratio. On the other hand, transmission electron microscopy (TEM) analysis proves the presence of silicon nanoclusters embedded in the films deposited at a gas flow ratio of R=2 and annealed at 700 °C (30 min).     

Epitaxial growth of highly transparent and conducting Sc-doped ZnO films on c-plane sapphire by sol–gel process without buffer

Highly transparent and conductive scandium doped zinc oxide (ZnO:Sc) films were deposited on c-plane sapphire substrates by sol–gel technique using zinc acetate dihydrate [Zn(CH₃COO)₂·2H₂O] as precursor, 2-methoxyethanol as solvent and monoethanolamine as a stabilizer. The doping with scandium is achieved by adding 0.5 wt% of scandium nitrate hexahydrate [(ScNO₃·6H₂O)] in the solution. The influence of annealing temperature (300–550 °C) on the structural, optical and electrical properties was investigated. X-ray Diffraction study revealed that highly c-axis oriented films with full-width half maximum of 0.16° are obtained at an annealing temperature of 400 °C. The surface morphology of the films was judged by SEM and AFM images which indicated formation of grains. The average transmittance was found to be above 92% in the visible region. ZnO:Sc film, annealed at 400 °C exhibited minimum resistivity of 1.91 × 10⁻⁴ Ω cm. Room-temperature photoluminescence measurements of the ZnO:Sc films annealed at 400 °C showed ultraviolet peak at 3.31eV with a FWHM of 11.2 meV, which are comparable to those found in high-quality ZnO films. Reflection high-energy electron diffraction pattern confirmed the epitaxial nature of the films even without introducing any buffer layer.     

Preparation of F-doped titania nanoparticles with a highly thermally stable anatase phase by alcoholysis of TiCl4

Pure anatase is a metastable phase and inclined to (transform) be transformed into rutile structure under heating over than 500 °C, which limits its suitability for high-temperature applications. Hitherto much research efforts have been made to increase the stability temperature of anatase structure. However, metallic doping usually introduced metallic oxides into titania at high temperature, and many nonmetallic doping are not competent for increasing the stability temperature of anatase structure up to 900 °C. In this study, F-doped anatase TiO₂ nanoparticles were conveniently prepared via the alcoholysis of TiCl₄ and the as-prepared product shows very high stability temperature up to 1000 °C before being transformed into rutile structure phase. On the basis of XPS results of F-doped titania annealed at different temperature, it is learned that the F atoms were anchored on the crystal planes of anatase in favor of decreasing the energy faces of anatase and stabilizing the anatase structure till annealed at 1300 °C all the anatase were transformed into rutile phase.     

Influence of ceramic oxide materials on lithium based potentiometric CO2 sensors

In these potentiometric sensors, a mixed binary carbonate sensing material consisting of 90 mol% Li₂CO₃ and 10 mol% BaCO₃ was modified by adding ceramic oxide materials such as SiO₂, B₂O₃, La₂O₃, Bi₂O₃, CeO₂ and In₂O₃ in different mol% concentrations. Various sensors mixed with these external oxides have shown good performance at operating temperatures below 300 °C. Scanning electron microscopy reveals that a glassy sensing phase is formed in the sensing bi-carbonate by the addition of ceramic oxides and sintered at 600 °C for 1 h. The sensor mixed with SiO₂:B₂O₃:Bi₂O₃ in 1:2:1 mol% showed an excellent response and recovery characteristics and followed a fair Nernstian behavior with a ΔEMF/dec value of −48.18 at as low as 150 °C. The decrease in operating temperature is attributed to the enhanced lithium ion migration through the glassy sensing phase of the sensing electrode.     

Transparent conductive ZnO:Ga films prepared by DC reactive magnetron sputtering at low temperature

Ga-doped ZnO (ZnO:Ga) transparent conductive films were deposited on glass substrates by DC reactive magnetron sputtering. The structural, electrical, and optical properties of ZnO:Ga films were investigated in a wide temperature range from room temperature up to 400 °C. The crystallinity and surface morphology of the films are strongly dependent on the growth temperatures, which in turn exert an influence on the electrical and optical properties of the ZnO:Ga films. The film deposited at 350 °C exhibited the relatively well crystallinity and the lowest resistivity of 3.4 × 10⁻⁴ Ω cm. More importantly, the low-resistance and high-transmittance ZnO:Ga films were also obtained at a low temperature of 150 °C by changing the sputtering powers, having acceptable properties for application as transparent conductive electrodes in LCDs and solar cells.     

Effect of annealing temperature on microstructure, optical and electrical properties of sputtered Ba0.9Sr0.1TiO3 thin films

Ba_0.9Sr_0.1TiO₃ (BST) thin films were deposited on fused quartz and Pt/TiN/Si₃N₄/Si substrates by radio frequency magnetron sputtering technique. Microstructure and chemical bonding states of the BST films annealed at 700 °C were characterized by field emission scanning electron microscopy, X-ray photoelectron spectroscopy, glancing angle X-ray diffraction and Raman spectrum. Optical constants including refractive indices, extinction coefficients and bandgap energies of the as-deposited BST film and the BST films annealed at 650, 700 and 750 °C, respectively, were determined from transmittance spectra by envelope method and Tauc relation. Dielectric constant and remnant polarization for the BST films increase with increasing annealing temperature. Leakage current density-applied voltage (J–V) data indicate that the dominant conduction mechanism for all the BST capacitors is the interface-controlled Schottky emission under the conditions of 14 V < V < 30 V and −30 V < V < −14 V. Furthermore, the inequipotential J–V characteristics for the BST films annealed at various temperatures are mainly attributed to the combined effects of the different thermal histories, relaxed stresses and strains, and varied Schottky barrier heights in the BST/Pt and Pt/BST interfaces.     

Synthesis of wurtzite-phase ZnS nanocrystal and its optical properties

The wurtzite phase of ZnS nanocrystal has been prepared by annealing in 200–600 °C temperature range, its cubic phase of 2–3 nm size, prepared through soft chemical method. Results of isochronal experiments of 2 h at different temperatures indicate that visible transformation to wurtzite from cubic ZnS appears at a temperature of 400 °C, which is about three times smaller than that of bulk ZnS phase transition temperature. The phases, nanostructures, and optical absorption characteristics are obtained through X-ray diffraction, transmission electron microscopy, and UV–visible absorption spectroscopy. A stable and green photoluminescence emission peaked at 518 nm is observed from the 600 °C annealed samples, under ultraviolet light excitation.     

Ion-beam irradiation effect on solid-phase growth of β-FeSi2

Effects of Ar⁺ ion-beam irradiation on solid-phase growth of β-FeSi₂ have been investigated. Fe (10 nm)/Si structures were irradiated with 25 keV Ar⁺ (5.0×10¹⁵ cm⁻²) at a temperature of 25°C (sample A) or 400°C (sample B), and subsequently annealed at 800°C. A reference was obtained after annealing without irradiation (sample C). X-ray diffraction results indicated that β-FeSi₂ was formed after annealing at 800°C for 5 h, and the formation rate was the fastest for sample A and the slowest for sample C, i.e., A>BC. However, Auger electron spectroscopy measurements showed that atomic mixing at Fe/Si interface before annealing was B>AC. These results suggested that amorphization of Si substrate, in addition to atomic mixing, enhanced the solid-phase growth of β-FeSi₂, which was confirmed experimentally. Moreover, a direct band gap of 0.89 eV was observed for the sample with pre-amorphization by the Fourier-transform infrared (FT-IR) spectroscopy measurements. These enhancement effects were attributed to that the phase transition to β-FeSi₂ was accelerated by atomic arrangement induced during annihilation of excess vacancies. These enhancement effects can be utilized for nano-fabrication of β-FeSi₂ by using focused ion-beam irradiation.     

Transport properties and defect analysis of La1.9Sr0.1NiO4 + δ

The oxygen flux through La_1.9Sr_0.1NiO_4 + δ has been measured as a function of oxygen activity gradient and temperature (750–1000 °C). The oxygen nonstoichiometry was determined by thermogravimetry in the temperature range of 400–1000 °C and oxygen partial pressures of 0.0002–1 atm. The total conductivity was measured over a similar range of conditions. The oxide ion partial conductivity derived from the oxygen flux data is approximately 4 orders of magnitude lower than the total, mainly p-type electronic conductivity. The defect structure was derived based on the data. Combining the oxygen flux and oxygen nonstoichiometry, the self diffusion coefficient of oxygen interstitials was evaluated.     

The effect of Si surface nitridation on the interfacial structure and electrical properties of (La2O3)0.5(SiO2)0.5 high-k gate dielectric films

Thermal stability, interfacial structures and electrical properties of amorphous (La₂O₃)_0.5(SiO₂)_0.5 (LSO) films deposited by using pulsed laser deposition (PLD) on Si (1 0 0) and NH₃ nitrided Si (1 0 0) substrates were comparatively investigated. The LSO films keep the amorphous state up to a high annealing temperature of 900 °C. HRTEM observations and XPS analyses showed that the surface nitridation of silicon wafer using NH₃ can result in the formation of the passivation layer, which effectively suppresses the excessive growth of the interfacial layer between LSO film and silicon wafer after high-temperature annealing process. The Pt/LSO/nitrided Si capacitors annealed at high temperature exhibit smaller CET and EOT, a less flatband voltage shift, a negligible hysteresis loop, a smaller equivalent dielectric charge density, and a much lower gate leakage current density as compared with that of the Pt/LSO/Si capacitors without Si surface nitridation.     

Effect of annealing upon the structure and adhesion properties of sputtered bio-glass/titanium coatings

Bio-glass films were deposited by radio-frequency magnetron sputtering technique onto medical grade Ti6Al7Nb alloy substrates from prepared silica based bio-glass target. A low deposition temperature was used (150 °C) and three different working pressures, followed by annealing in air at 550 and 750 °C. A quasi-stoichiometric target to substrate atomic transfer was found for Si, Ca and P, along with strong enrichment in Na and depletion in K and Mg, as evidenced by the energy dispersive microanalysis. The best results, taking into account stoichiometry and surface roughness, were obtained for the BG layers deposited at 0.3 Pa argon working pressure. The infrared spectroscopy of the as-sputtered and of the annealed films evidenced the characteristic molecular vibrations of silicate, phosphate and carbonate functional groups. The as-deposited films are amorphous and became partly crystalline after annealing at 750 °C, as evidenced by X-ray diffraction. The pull-out measurements, performed with a certified pull-test machine, gave very strong film–substrate adhesion strength values. For the non-crystalline layers, the pull-out strength is higher than 85 MPa, and decreases after annealing at 750 °C to 72.9 ± 7.1 MPa. The main objective of this work was to establish the influence of the working pressure upon the composition and morphology of the as-deposited films, and of the annealing temperature upon structure and film–substrate adhesion.     

Laser assisted thermoluminescence dosimetry using temperature controlled linear heating

We have developed a non-contact laser–fiberoptic system for thermoluminescence dosimetry (TLD) measurements. The system is based on: (i) linear heating of a TLD sample by a CO₂ laser beam; (ii) measuring the sample's temperature, using infrared thermometry and (iii) using a feedback loop, for controlling the heating rate. The infrared thermometry was carried out, using infrared transmitting AgClBr fibers. The system made it possible to obtain linear heating at slow rates (e.g. 5 °C/s), or fast rates (up to 60 °C/s), or even to obtain non-linear heating. Measurements on LiF TLD samples revealed excellent linearity between the doses, to which the samples had been exposed, and the amplitudes of the measured glow curve peaks, over a wide range of doses. Our results were highly reproducible, which clearly demonstrated the potential of laser heated thermoluminescence for accurate dosimetry.     

Effects of deposition temperature on the structural and morphological properties of thin ZnO films fabricated by pulsed laser deposition

ZnO thin films were grown on Si(1 0 0) substrates using pulsed laser deposition in O₂ gas ambient (10 Pa) and at different substrate temperatures (25, 150, 300 and 400 °C). The influence of the substrate temperature on the structural and morphological properties of the films was investigated using XRD, AFM and SEM. At substrate temperature of T=150 °C, a good quality ZnO film was fabricated that exhibits an average grain size of 15.1 nm with an average RMS roughness of 3.4 nm. The refractive index and the thickness of the thin films determined by the ellipsometry data are also presented and discussed.     

Influence on the long afterglow properties by the environmental temperature

Sr₂MgSi₂O₇:Eu²⁺, Dy³⁺ (SMED) and Ba₂MgSi₂O₇:Eu²⁺, Dy³⁺ (BMED) were synthesized with the solid-state reaction. The SMED shows long afterglow while the afterglow of BMED is not visible at room temperature. When the environmental temperature is 150 °C, the afterglow of SMED is not obvious while the BMED shows the long afterglow. The decay curves measured at different temperatures conform to this phenomenon. It ascribes to the different trap depths of different samples. The thermoluminescence (TL) curves of SMED peaks at 80 °C. BMED has two TL peaks peaking at about 80 and 175 °C respectively. The low temperature peak is weak and its density is small. The high-temperature peak reveals that one trap of BMED is deeper than the one of SMED. The afterglows of the phosphors strongly depend on the environmental temperature since the lifetime of the trapping carriers is temperature-dependence. BMED is a potential optimum long afterglow phosphor for the purpose of high-temperature application.