Thermoluminescent and stuctural properties of BaAl2O4:Eu,Nd,Gdphosphors prepared by combustion method

BaAl₂O₄:Eu²⁺,Nd³⁺,Gd³⁺ phosphors were prepared by a combustion method at different initiating temperatures (400–1200 °C), using urea as a comburent. The powders were annealed at different temperatures in the range of 400–1100 °C for 3 h. X-ray diffraction data show that the crystallinity of the BaAl₂O₄ structure greatly improved with increasing annealing temperature. Blue-green photoluminescence, with persistent/long afterglow, was observed at 498 nm. This emission was attributed to the 4f⁶5d¹–4f⁷ transitions of Eu²⁺ ions. The phosphorescence decay curves were obtained by irradiating the samples with a 365 nm UV light. The glow curves of the as-prepared and the annealed samples were investigated in this study. The thermoluminescent (TL) glow peaks of the samples prepared at 600 °C and 1200 °C were both stable at ∼72 °C suggesting that the traps responsible for the bands were fixed at this position irrespective of annealing temperature. These bands are at a similar position, which suggests that the traps responsible for these bands are similar. The rate of decay of the sample annealed at 600 °C was faster than that of the sample prepared at 1200 °C.     

Lanthanide absorption spectral probe in titania nanoparticles synthesized by ultrasonic assistant sol-gel method

Titania nanoparticles were obtained by an ultrasonic assistant sol-gel method. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermal analysis. The optical absorption of the samples has been measured by photoacoustic (PA) spectroscopy, which is powerful for detecting small amount of strongly scattering materials. The structural variations of the sample during the phase transitions were firstly studied using Nd³⁺ as an absorption spectral probe. The PA results show that the TiO₂ gel heated at 50 °C is basically amorphous and still contains abundant trapped water and ethanol, which makes the environment around Nd³⁺ similar with that of its aqueous ion. For the sample calcined at higher temperature, the f-f transitions of Nd³⁺ exhibit a continuous red shift along with the gel-to-anatase transformation, indicating an increase of the “degree of covalency” for Nd³⁺ bonding. For the sample calcined at 1100 °C, however, the f-f transitions of Nd³⁺ show blue shifts and the hypersensitive transition intensities of Nd³⁺ decrease, indicating an increase of ionicity for Nd³⁺ bonding. This can be attributed to the segregation of Nd³⁺ ions to the external surface, forming Nd₄Ti₉O₂₄ during the anatase-to-rutile transition.     

Conducting antimony-doped tin oxide films derived from stannous oxalate by aqueous sol-gel method

Nanocrystalline SnO₂:Sb films were prepared by a sol-gel route using C₆H₈O₇-triethanolamine (TEA) mixing aqueous solution with pH 6.5-7.0. Stannous oxalate and antimony trichloride were used as tin and antimony sources. IR, XRD FESEM, FETEM, UV-vis and four-point probe measurement were used to characterize sol-gel chemistry, structure, morphologies, optical and electrical properties. Mechanism of sol-gel reaction illuminated that existence of TEA supplied large numbers of active tin hydrate and ionized state carboxyl groups for tin and antimony chelation through the amido association with the ionized H⁺ on -COOH of H₃L and H₂C₂O₄. The 6 at.% Sb-doped films with film thickness of 600 nm had sheet resistance as low as 42.85 Ω/ when annealed at 450 °C for 10 min. Annealing temperature intensively altered sheet resistance and optimum was in the range of 450-500 °C. The longer annealing time caused Sb volatilization which led to the optimum doping level shifted from 6 to 12 at.%.     

VPO catalysts synthesized on substrates with modified activated carbons

VPO catalysts were prepared on oxidized and unoxidized activated carbons differing in initial porous structure. Carbons were oxidized under relatively soft (30% H₂O₂, 200 °C) and hard (50% H₂O₂, 350 °C) conditions. Carbon modification was carried out hydrothermally in a traditional autoclave (HTT) or a microwave reactor (MWT). The synthesis was also carried out under hydrothermal (HTS or MWS) conditions. V₂O₅ and NH₄VO₃ were used as precursors. The samples are characterized by diversified porous structure at S_BET = 732-1617 m²/g and V_por = 0.44-0.90 cm³/g, as well as various degree of VPO crystallinity. Possibility of preparation of the VPO catalysts under ecologically appropriate conditions, i.e. in aqueous solutions, was shown.     

Magnetic and bioactivity evaluation of ferrimagnetic ZnFe2O4 containing glass ceramics for the hyperthermia treatment of cancer

Glass ceramics of the composition xZnO·25Fe₂O₃·(40−x)SiO₂·25CaO·7P₂O₅·3Na₂O were prepared by the melt-quench method using oxy-acetylene flame. Glass-powder compacts were sintered at 1100 °C for 3 h and then rapidly cooled at −10 °C. X-ray diffraction (XRD) revealed 3 prominent crystalline phases: ZnFe₂O₄, CaSiO₃ and Ca₁₀(PO₄)₆(OH)₂. Vibrating sample magnetometer (VSM) data at 10 KOe and 500 Oe showed that saturation magnetization, coercivity and hence hysteresis area increased with the increase in ZnO content. Nano-sized ZnFe₂O₄ crystallites were of pseudo-single domain structure and thus coercivity increased with the increase in crystallite size. ZnFe₂O₄ exhibited ferrimagnetism due to the random distribution of Zn²⁺ and Fe³⁺ cations at tetrahedral A sites and octahedral B sites. This inversion/random distribution of cations was probably due to the surface effects of nano-ZnFe₂O₄ and rapid cooling of the material from 1100 °C (thus preserving the high temperature state of the random distribution of cations). Calorimetric measurements were carried out using magnetic induction furnace at 500 Oe magnetic field and 400 KHz frequency. The data showed that maximum specific power loss and temperature increase after 2 min were 26 W/g and 37 °C, respectively for the sample containing 10% ZnO. The samples were immersed in simulated body fluid (SBF) for 3 weeks. Scanning electron microscope (SEM), energy dispersive spectroscopy (EDX) and XRD results confirmed the growth of precipitated hydroxyapatite phase after immersion in SBF, suggesting that the ferrimagnetic glass ceramics were bioactive and could bond to the living tissues in physiological environment.     

Low-temperature synthesis of BaMgAl10O17:Eu blue phosphors

Using H₃BO₃ as the flux, pure BaMgAl₁₀O₁₇:Eu²⁺ (BAM) blue phosphors were successfully prepared via a solid-state reaction. By this approach, well-crystallized submicron BAM particles were obtained at temperatures as low as 1100 °C with a sintering duration of 2 h. The sintering temperature required by this approach was at least 400 °C lower than that required by the conventional solid-state approach for preparing BAM; moreover, the sintering time required by the former approach was also considerably shorter than that required by the latter approach. These factors are expected to lower the cost for large-scale production of BAM phosphors. Crystal structures and luminescence properties of the synthesized samples were characterized by XRD and TG–DTA, and photoluminescence spectroscopy, respectively. The reactivity of an intermediate, BaAl₂O₄, is thought to be the key factor influencing the synthesis temperature for BAM.     

Structural,magnetic and electrical properties of Co1−xZnxFe2O4 synthesized by co-precipitation method

Nanoparticles of Co_1−xZn_xFe₂O₄ with stoichiometric proportion (x) varying from 0.0 to 0.6 were prepared by the chemical co-precipitation method. The samples were sintered at 600 °C for 2 h and were characterized by X-ray diffraction (XRD), low field AC magnetic susceptibility, DC electrical resistivity and dielectric constant measurements. From the analysis of XRD patterns, the nanocrystalline ferrite had been obtained at pH=12.5–13 and reaction time of 45 min. The particle size was calculated from the most intense peak (3 1 1) using the Scherrer formula. The size of precipitated particles lies within the range 12–16 nm, obtained at reaction temperature of 70 °C. The Curie temperature was obtained from AC magnetic susceptibility measurements in the range 77–850 K. It is observed that Curie temperature decreases with the increase of Zn concentration. DC electrical resistivity measurements were carried out by two-probe method from 370 to 580 K. Temperature-dependent DC electrical resistivity decreases with increase in temperature ensuring the semiconductor nature of the samples. DC electrical resistivity results are discussed in terms of polaron hopping model. Activation energy calculated from the DC electrical resistivity versus temperature for all the samples ranges from 0.658 to 0.849 eV. The drift mobility increases by increasing temperature due to decrease in DC electrical resisitivity. The dielectric constants are studied as a function of frequency in the range 100 Hz–1 MHz at room temperature. The dielectric constant decreases with increasing frequency for all the samples and follow the Maxwell–Wagner's interfacial polarization.     

Synthesis and luminescence properties of needle-like SrAl2O4:Eu, Dy phosphor via a hydrothermal co-precipitation method

Needle-like SrAl₂O₄:Eu²⁺, Dy³⁺ phosphors had been prepared by calcining the precursors obtained from hydrothermal process at the temperature of 1100 °C in a weak reductive atmosphere of active carbon. The crystal structure, morphology and optical properties of the composites were characterized. X-ray diffraction (XRD) patterns illustrated that the single-phase SrAl₂O₄ was formed at 1100 °C, which is much lower than that prepared by the traditional method. The transmission electron microscope (TEM) observation revealed the precursors and the resulted SrAl₂O₄:Eu²⁺, Dy³⁺ phosphors had well-dispersed distribution and needle-like morphology with an average diameter about 150 nm at the center and the length up to 1 μm. After irradiation by ultraviolet radiation with 350 nm for 5 min, the phosphors emit green color long-lasting phosphorescence corresponding to the typical emission of Eu²⁺ ion, both the PL spectra and luminance decay revealed that the phosphors had efficient luminescent and long lasting properties.     

Synthesis and photoluminescence of aligned straight silica nanowires on Si substrate

Aligned straight silica nanowires (NWs) have been synthesized on Si wafer by thermal evaporation of mixed powders of zinc carbonate hydroxide and graphite at 1100 °C and condensation on Si substrate without using any catalyst. The straight silica NWs have diameters ranging from 50 to 100 nm, and lengths of several micrometers, with cone-shaped tips at their ends. High deposition temperature and relatively high SiO_x vapor concentration near the growth substrate would be beneficial to the formation of the aligned straight silica NWs. Different morphologies of silica nanostructures have also been obtained by varying the deposition temperature and the vapor concentration of the SiO_x molecules. Room temperature photoluminescence measurements on the oriented silica NWs show that two green emission bands at 510 and 560 nm, respectively, revealing that the aligned straight silica NWs might have potential applications in the future optoelectronic devices.     

Magnetic properties in Fe-doped NiO synthesized by co-precipitation

The magnetic properties of 1.5 at% Fe-doped NiO bulk samples were investigated. The samples were prepared by sintering the corresponding precursor in air at temperatures between 400 and 800 °C for 6 h. The synthesis was by a chemical co-precipitation and post-thermal decomposition method. In order to allow a comparison, a NiO/0.76 at% NiFe₂O₄ mixture was also prepared. The X-ray diffraction pattern shows that the samples that were sintered at 400 and 600 °C remain single phase. As the sintering temperature increased to 800 °C, however, the sample becomes a mixture of NiO and NiFe₂O₄ ferrite phases. The samples were investigated by measuring their magnetization as a function of magnetic field. The samples sintered between 400 and 800 °C and the one mixed directly with NiFe₂O₄ nanoparticles show a coercivity value of H_c≈200, 325, 350 and 110 Oe, respectively. The magnetic properties of the samples depend strongly on the sintering temperature. Simultaneously, the field-cooling hysteresis loop shift also observed after cooling the sample sintered at 600 °C to low temperature suggests the possibility of the existence of a ferromagnetic/antiferromagnetic exchange coupling.     

Thermal stability of alumina thin films containing γ-Al2O3 phase prepared by reactive magnetron sputtering

The paper reports on thermal stability of alumina thin films containing γ-Al₂O₃ phase and its conversion to a thermodynamically stable α-Al₂O₃ phase during a post-deposition equilibrium thermal annealing. The films were prepared by reactive magnetron sputtering and subsequently post-deposition annealing was carried out in air at temperatures ranging from 700 °C to 1150 °C and annealing times up to 5 h using a thermogravimetric system. The evolution of the structure was investigated by means of X-ray diffraction after cooling down of the films. It was found that (1) the nanocrystalline γ-Al₂O₃ phase in the films is thermally stable up to 1000 °C even after 5 h of annealing, (2) the nanocrystalline θ-Al₂O₃ phase was observed in a narrow time and temperature region at ≥1050 °C, and (3) annealing at 1100 °C for 2 h resulted in a dominance of the α-Al₂O₃ phase only in the films with a sufficient thickness.     

Structure and luminescent properties of LaNbO4 synthesized by sol-gel process

The luminescence properties of LaNbO₄ synthesized by the citric gel process were investigated. The crystallized orthorhombic and monoclinic biphasic structure forms at temperatures below 1100 °C and well-crystallized monoclinic LaNbO₄ is obtained by heat treatment at a temperature of 1200 °C for 3 h. All of LaNbO₄ phosphors derived from the citric gel method exhibit red-shifted excitation spectra as the calcining temperature increased from 700 to 1200 °C. The effect of the heat treatment conditions on the peak shape and the peak positions of the photoluminescence (PL) emission are undetectable, and the PL spectra excited at 260 nm have a blue emission band maximum at 408 nm, corresponding to the self-activated luminescence center of LaNbO₄. The sample heat treated at 1100 °C for 3 h showed the highest absorption and fluorescence intensities among the prepared samples.     

On the thermal stability of Co2Z hexagonal ferrites for low-temperature ceramic cofiring technologies

Co₂Z hexaferrite Ba₃Co₂Fe₂₄O₄₁ was prepared by a mixed oxalate co-precipitation route and the standard ceramic technology. XRD studies show that at T<1300 °C different ferrite phases coexist with the M-type hexaferrite as majority phase between 1000 and 1100 °C and the Y-type ferrite at 1230 °C. The Z-type material has its stability interval between 1300 and 1350 °C. Both synthesis routes result in almost single-phase Z-type ferrites after calcination at 1330 °C, intermediate grinding and sintering at 1330 °C. The permeability of Co₂Z-type ferrite of about μ=20 is stable up to several 100 MHz, with maximum losses μ′′ around 700 MHz. Addition of 3 wt% Bi₂O₃ as sintering aid shifts the temperature of maximum shrinkage down to 950 °C and enables sintering of Z-type ferrite powders at 950 °C. However, the permeability is reduced to μ=3. It is shown here for the first time that Co₂Z ferrite is not stable under these conditions; partial thermal decomposition into other hexagonal ferrites is found by XRD studies. This is accompanied by a significant decrease of permeability. This shows that Co₂Z hexagonal ferrite is not suitable for the fabrication of multilayer inductors for high-frequency applications via the low-temperature ceramic cofiring technology since the material is not compatible with the typical process cofiring temperature of 950 °C.     

Highly thermal stable transparent conducting SnO2:Sb epitaxial films prepared on α-Al2O3 (0 0 0 1) by MOCVD

Antimony-doped tin oxide (SnO₂:Sb) single crystalline films have been prepared on α-Al₂O₃ (0 0 0 1) substrates by metal organic chemical vapor deposition (MOCVD). The antimony doping was varied from 2% to 7% (atomic ratio). Post-deposition annealing of the SnO₂:Sb films was carried out at 700-1100 °C for 30 min in atmosphere ambient. The effect of annealing on the structural, electrical and optical properties of the films was investigated in detail. All the SnO₂:Sb films had good thermal stability under 900 °C, and the 5% Sb-doped SnO₂ film exhibited the best opto-electrical properties. Annealed above 900 °C, the 7% Sb-doped SnO₂ film still kept high thermal stability and showed good electrical and optical properties even at 1100 °C.     

Atomically controlled surfaces with step and terrace of β-Ga2O3 single crystal substrates for thin film growth

The surface of β-Ga₂O₃ (1 0 0) single crystal grown with floating zone method was treated by chemical-mechanical-polishing (CMP) for 30-120 min followed by annealing in oxygen atmosphere at temperature 600-1100 °C for 3-6 h. The evolution of the step arrangement was investigated with reflection high energy electron diffraction and atomic force microscopy. Atomically smooth surfaces with atomic step and terrace structure of β-Ga₂O₃ substrates were successfully obtained after just CMP treatment as well as CMP treatment and post annealing at 1100 °C for 3 h. The uniform step height was 0.57 nm, and smooth terrace width was 100 nm, where the misorientation angle was about 0.36°. The obtained atomically smooth surface provides a potential application for the high-quality epitaxial film growth.     

Surface evolution of a gradient structured Ti in hydrogen peroxide solution

In this work, the interaction between hydrogen peroxide (H₂O₂) and a gradient structured Ti was investigated extensively. The gradient structured Ti (SMAT Ti) was produced by surface mechanical attrition treatment (SMAT), and then it was immersed in H₂O₂ solution for different time until 48 h at room temperature (25 °C). The structure and surface morphology evolution were examined by Raman spectra and scanning electron microscopy (SEM). The formation mechanism of nanoporous titania was discussed based on above results.     

Structural, AC, and DC magnetic properties of Zn1−xCoxFe2O4

Structural, AC and DC magnetic properties of polycrystalline Zn_1−xCo_xFe₂O₄ (x=0.2, 0.4) samples sintered at various temperatures (1100-1300 °C), and various dwell times (0.2-15 h) have been investigated thoroughly. The bulk density of the Zn_0.60Co_0.40Fe₂O₄ samples increases as the sintering temperature (T_s) increases from 1100 to 1250 °C, and above 1250 °C the bulk density decreases slightly. The Zn_0.80Co_0.20Fe₂O₄ samples show similar behavior of changes to that of Zn_0.60Co_0.40Fe₂O₄ samples except that the bulk density is found to be highest at 1200 °C. The DC magnetization as a function of temperature curves show that the Zn_0.60Co_0.40Fe₂O₄ sample is ferrimagnetic at room temperature while the Zn_0.80Co_0.20Fe₂O₄ sample is paramagnetic at room temperature. The T_c of Zn_0.80Co_0.20Fe₂O₄ sample is found to be 170 K from DC magnetization measurement. Separate measurement (AC magnetization), initial permeability as a function of temperature shows that the T_c of the Zn_0.60Co_0.40Fe₂O₄ sample is 353 K. Slight variation of T_c is observed depending on sintering condition. The initial permeability for the Zn_0.60Co_0.40Fe₂O₄ composition sintered at 1250 °C is found to be maximum.     

Effect of growth temperature on the morphology and bonded states of SnO2 nanobaskets

The nanobaskets of SnO₂ were grown on in-house fabricated anodized aluminum oxide pores of 80 nm diameter using plasma enhanced chemical vapor deposition at an RF power of 60 W. Hydrated stannic chloride was used as a precursor and O₂ (20 sccm) as a reactant gas. The deposition was carried out from 350 to 500 °C at a pressure of 0.2 Torr for 15 min each. Deposition at 450 °C results in highly crystalline film with basket like (nanosized) structure. Further increase in the growth temperature (500 °C) results in the deterioration of the basket like structure and collapse of the alumina pores. The grown film is of tetragonal rutile structure grown along the [1 1 0] direction. The change in the film composition and bonded states with growth temperature was evident by the changes in the photoelectron peak intensities of the various constituents. In case of the film grown at 450 °C, Sn 3d_5/2 is found built up of Sn⁴⁺ and O-Sn⁴⁺ and the peaks corresponding to Sn²⁺ and O-Sn²⁺ were not detected.     

Enhancement in hydrophobicity of silica films using metal acetylacetonate and heat treatment

Water is one of the most affecting chemicals that can cause damage to the solid surface. To protect the surface due to the action of water, the surface should be made hydrophobic. In the present study, the improvement in hydrophobicity of silica films using metal acetylacetonate (M-acac) by employing heat treatment to methyltrimethoxy silane (MTMS) based silica coatings is reported as a novel attempt. Instead of following the established trends of the surface derivatization or co-precursor method, iron acetylacetonate Fe(acac)₃, copper acetylacetonate Cu(acac)₂ and heat treatment were used to incorporate hydrophobicity with silica coatings. As M-acac is readily soluble in organic solvents, Fe(acac)₃ and Cu(acac)₂ were dissolved in methanol (MeOH) and their concentration was varied from 0 to 0.025 M. The coating solution was prepared by optimizing molar ratio of MTMS:MeOH:basic H₂O to 1:7.15:6.34, respectively. Gelation time (t_g) for Cu(acac)₂ containing silica sol and that containing Fe(acac)₃ were noted to be 30 and 55 min, respectively. The substrates were taken out after gelation and heat treated at 150 °C for 2 h. The heat treated films showed a dramatic increase in the static water contact angle from 82° to as high as 142°.     

Investigations on structural and magnetic properties of cobalt ferrite/silica nanocomposites prepared by the coprecipitation method

Magnetic nanocomposites consisting of cobalt ferrite nanoparticles embedded in silica matrix were prepared by the coprecipitation method using metallic chlorides as precursors for ferrite. Subsequently composites were annealed at 100, 200 and 300 °C for 2 h. The samples were structurally characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). The magnetic properties were measured in the temperature range of 10-300 K using vibrating sample magnetometer (VSM). The effects of thermal treatment on structural and magnetic properties of nanocomposites were investigated. When the samples were annealed, CoFe₂O₄ nanocrystallites were observed in the SiO₂ matrix, whose size increases with increase in annealing temperature. The coercivity and saturation magnetization of nanocomposite (annealed at 300 °C for 2 h) are much higher than that of bulk cobalt ferrite. The realization of adjustable particle sizes and controllable magnetic properties makes the applicability of the CoFe₂O₄ nanocomposite more versatile.