Crystallization and microstructural evolution of MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript>–TiO<Subscript>2</Subscript>–La<Subscript>2</Subscript>O<Subscript>3</Subscript> glass-ceramics

Crystallization and microstructure of glasses with the molar compositions 1MgO·1.2Al₂O₃·2.8SiO₂·1.2TiO₂·xLa₂O₃ (x = 0.1 and 0.4) were thermally treated at different temperatures in the range from 950 to 1250 °C and then analyzed by X-ray diffraction and scanning electron microscopy, in combination with energy-dispersive X-ray spectroscopy and electron backscatter diffraction. It was found that the microstructure is first homogeneous with the precipitation of randomly distributed crystals and then indialite domains with embedded perrierite and rutile crystals are formed. For higher temperatures or prolonged times, more domains appear and expand into the bulk of the sample. Finally, the entire sample consists of the indialite domains and the boundaries that are enriched in rutile, perrierite, and magnesium aluminotitanate. Nevertheless, very distinct differences are observed between the samples with different La₂O₃ concentrations. For the sample with x = 0.4, the domains were detected at lower temperatures, while the quantity and size of the domains increase faster due to the promoted precipitation of indialite. For the sample with x = 0.1, in addition to the domain boundaries, secondary boundaries between the “regions” (assemblages of the domains) are observed in a larger length scale. The average size of the crystalline phases found between the “regions” is larger than that typically observed at the domain boundaries. The sizes of the crystals at the boundaries decrease with higher concentrations of La₂O₃, and the crystals (especially perrierite) within the domains become larger, resulting in a more homogeneous microstructure. This results in better dielectric properties, i.e., much higher quality factor for the sample with x = 0.4 in comparison to that with x = 0.1 after heat-treatment at 1150 or 1250 °C.     

Spectroscopic characterisation of local structure in Y<Subscript>2</Subscript>O<Subscript>3</Subscript>–B<Subscript>2</Subscript>O<Subscript>3</Subscript>–Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> glasses doped with gadolinium

Gadolinium doped bismuth borate glasses containing up to 30 mol% Y₂O₃ were prepared by fast melt quenching method. The effect of yttrium on the local order in 3B₂O₃ · Bi₂O₃ and B₂O₃ · Bi₂O₃ glass matrices, particularly on the bismuth sites, was investigated by infrared (IR) spectroscopy and electron paramagnetic resonance (EPR) of Gd³⁺ ions. The IR results show that the local structure is more ordered in the glass system with higher bismuth content and the progressive addition of yttrium increases the local disorder in both bismuth–borate glass matrices. The EPR results indicate that Gd³⁺ ions occupy both bismuth and yttrium sites and reflect the same structural disorder like that suggested by IR results.     

In vitro dissolution behavior of SiO<Subscript>2</Subscript>–MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–K<Subscript>2</Subscript>O–B<Subscript>2</Subscript>O<Subscript>3</Subscript>–F glass–ceramic system

Herein, we report the results of the in vitro dissolution tests, which were carried out by immersing the selected glass-ceramic samples in artificial saliva (AS) for various time periods of up to 42 days. In our experiments, the SiO(2)-MgO-Al(2)O(3)-K(2)O-B(2)O(3)-F glass ceramics with different crystal morphology and crystal content were used and a comparison is also made with the baseline glass samples (without any crystals). The bioactivity of the samples was probed by measuring the changes in pH, ionic conductivity and ionic concentration of AS following in vitro dissolution experiments. High resistance of the selected glass-ceramic samples against in vitro leaching has been demonstrated by minimal weight loss (<1%) and insignificant density change, even after 6 weeks of dissolution in artificial saliva. While XRD analysis reveals the change in surface texture of the crystalline phase, FT-IR analysis weakly indicated the Ca-P compound formation on the leached surface. The experimental measurements further indicate that the leaching of F(-), Mg(2+) ions from the sample surface commonly causes the change in the surface chemistry. Furthermore, the presence of (Ca, P, O)-rich mineralized deposits on the leached glass-ceramic surface as well as the decrease in Ca(2+) ion concentrations in the leaching solutions (compared to that in the initial AS solution) provide evidences of the moderate bioactive or mild biomineralisation behaviour of investigated glass-ceramics.     

Mechanical and acid-etching properties of Bi<Subscript>2</Subscript>O<Subscript>3</Subscript>–ZnO–B<Subscript>2</Subscript>O<Subscript>3</Subscript> glass-containing ceramic fillers

The properties of the composite, having a complicated microstructure, are decided by many factors such as those of glass matrix, crystal phases, fillers, and holes. We investigated how the addition of ceramic fillers to the glass matrix affects the mechanical and etching properties of the glass composite by forming new crystal phases. Different amounts of two fillers, ZnO and Al₂O₃, were added to a glass frit consisting of Bi₂O₃–ZnO–B₂O₃. It was sintered at 550 °C for 30 min. Based on the results of this study, the porosity and degree of crystallization of the composites could be controlled by adjusting the content of the ZnO and Al₂O₃ fillers. Therefore, porosity and degree of crystallization formed by the reaction between a glass matrix and fillers influence the mechanical and etching properties of the composite.     

Compositional dependence of the structural and dielectric properties of Li<Subscript>2</Subscript>O–GeO<Subscript>2</Subscript>–ZnO–Bi<Subscript>2</Subscript>O<Subscript>3</Subscript>–Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> glasses

(10Li₂O–20GeO₂–30ZnO–(40-x)Bi₂O₃–xFe₂O₃ where x = 0.0, 3, 6, and 9 mol%) glasses were prepared. A number of studies, viz. density, differential thermal analysis, FT-IR spectra, DC and AC conductivities, and dielectric properties (constant ε′, loss tan δ, AC conductivity, σ _ac, over a wide range of frequency and temperature) of these glasses were carried out as a function of iron ion concentration. The analysis of the results indicate that, the density and molar volume decrease with an increasing of iron content indicates structural changes of the glass matrix. The glass transition temperature T _g and onset of crystallization temperature T _x increase with the variation of concentration of Fe₂O₃ referred to the growth in the network connectivity in this concentration range, while glass-forming ability parameter ΔT decrease with increase Fe₂O₃ content, indicates an increasing concentration of iron ions that take part in the network-modifying positions. The FT-IR spectra evidenced that the main structural units are BiO₃, BiO₆, ZnO₄, GeO₄, and GeO₆. The structural changes observed by varying the Fe₂O₃ content in these glasses and evidenced by FTIR investigation suggest that the iron ions play a network modifier role in these glasses while Bi₂O₃, GeO₂, and ZnO play the role of network formers. The temperature dependence of DC and AC conductivities at different frequencies was analyzed using Mott’s small polaron hopping model and, the high temperature activation energies have been estimated and discussed. The dielectric constant and dielectric loss increased with increase in temperature and Fe₂O₃ content.     

Evaluation of CaO–SiO<Subscript>2</Subscript>–P<Subscript>2</Subscript>O<Subscript>5</Subscript>–Na<Subscript>2</Subscript>O–Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> bioglass-ceramics for hyperthermia application

Magnetic bioglass ceramics (MBC) are being considered for use as thermoseeds in hyperthermia treatment of cancer. While the bioactivity in MBCs is attributed to the formation of the bone minerals such as crystalline apatite, wollastonite, etc. in a physiological environment, the magnetic property arises from the magnetite [Fe₃O₄] present in these implant materials. A new set of bioglasses with compositions 41CaO · (52 ? x)SiO₂ · 4P₂O₅  · xFe₂O₃ · 3Na₂O (2 ≤ x ≤ 10 mol% Fe₂O₃) have been prepared by melt quenching method. The as-quenched glasses were then heat treated at 1050°C for 3 h to obtain the glass-ceramics. The structure and microstructure of the samples were characterized using X-ray diffraction and microscopy techniques. X-ray diffraction data revealed the presence of magnetite in the heat treated samples with x ≥ 2 mol% Fe₂O₃. Room temperature magnetic property of the heat treated samples was investigated using a Vibrating Sample Magnetometer. Field scans up to 20 kOe revealed that the glass ceramic samples had a high saturation magnetization and low coercivity. Room temperature hysteresis cycles were also recorded at 500 Oe to ascertain the magnetic properties at clinically amenable field strengths. The area under the magnetic hysteresis loop is a measure of the heat generated by the MBC. The coercivity of the samples is another important factor for hyperthermia applications. The area under the loop increases with an increase in Fe₂O₃ molar concentration and the. coercivity decreases with an increase in Fe₂O₃ molar concentration The evolution of magnetic properties in these MBCs as a function of Fe₂O₃ molar concentration is discussed and correlated with the amount of magnetite present in them.     

Catalytic combustion of methane over Pt and PdO-supported CeO<Subscript>2</Subscript>–ZrO<Subscript>2</Subscript>–Bi<Subscript>2</Subscript>O<Subscript>3</Subscript>/γ-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> catalysts

Catalytic combustion of methane was investigated on Pt and PdO-supported CeO₂–ZrO₂–Bi₂O₃/γ-Al₂O₃ catalysts prepared by a wet impregnation method in the presence of polyvinylpyrrolidone. The catalysts were characterized by X-ray fluorescence analysis, X-ray powder diffraction, X-ray photoelectron spectra, transmission electron microscopy, and BET specific surface area measurements. The Pt/CeO₂–ZrO₂–Bi₂O₃/γ-Al₂O₃ and PdO/CeO₂–ZrO₂–Bi₂O₃/γ-Al₂O₃ catalysts were selective for the total oxidation of methane into carbon dioxide and steam, and no by-products such as HCHO, CO, and H₂ were obtained. The catalytic activities of the PdO/CeO₂–ZrO₂–Bi₂O₃/γ-Al₂O₃ catalysts were relatively higher than those of the Pt-supported catalysts, due to the facile re-oxidation of metallic Pd into PdO based on lattice oxygen supplied from the CeO₂–ZrO₂–Bi₂O₃ bulk. A decrease in the calcination temperature during the preparation process was found to be effective in enhancing the specific surface area of the catalysts, whereby particle agglomeration was inhibited. Optimization of the PdO amount and calcination temperature enabled complete oxidation of methane at temperatures as low as 320 °C on the 11.6 wt% PdO/CeO₂–ZrO₂–Bi₂O₃/γ-Al₂O₃ catalyst prepared at 400 °C.     

Fabrication of Yb<Subscript>2</Subscript>O<Subscript>3</Subscript>–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–P<Subscript>2</Subscript>O<Subscript>5</Subscript>–SiO<Subscript>2</Subscript> Optical Fibers with a Perfect Step-Index Profile by the MCVD Process

An all-vapor phase MCVD process has been proposed for the fabrication of fiber preforms with a Yb₂O₃–Al₂O₃–P₂O₅–SiO₂ multicomponent glass core. We have investigated the tubular preform collapse into a rod and demonstrated approaches capable of preventing P₂O₅ losses in the central part of the core during the collapse process. Preforms with a flat, perfect step-index profile have been fabricated.     

Effect of sintering temperatures on properties of BaO–B<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript>–Al<Subscript>2</Subscript>O<Subscript>3</Subscript> glass/silica composites for CBGA package

BaO–B₂O₃–SiO₂–Al₂O₃ (BBSA) glass/silica composites synthesized by solid-state reaction method were developed for CBGA packages, and the effects of sintering temperature (900–950 °C) on the phase transformation, microstructure, thermal, mechanical and electrical properties were investigated. XRD results show that the major phases quartz and cristobalite, and the minor phase BaSi₂O₅ are detected in BBSA composites. Furthermore, it was found that the quartz phase transforms to cristobalite phase at 930–940 °C. The formation of cristobalite phase with higher coefficient of thermal expansion (CTE) led to the increase of CTE value of BBSA composites. However, excessive cristobalite phase content would degrade the mechanical properties and the linearity of thermal expansion of the ceramics. BBSA composites sintered at 920 °C exhibited excellent properties: low dielectric constant and loss (ε_r = 6.2, tanδ = 10^?4 at 1 MHz), high bending strength (179 MPa), high CTE (12.19 ppm/°C) as well as superior linearity of the thermal expansion.     

Optical properties and crystallization of glasses in the system Bi<Subscript>2</Subscript>O<Subscript>3</Subscript>–MoO<Subscript>3</Subscript>–B<Subscript>2</Subscript>O<Subscript>3</Subscript>

The purpose of this work is to study the optical properties and crystallization of glasses in the ternary system Bi₂O₃–MoO₃–B₂O₃. In order to verify the obtaining of bismuth borate crystal phases several glass compositions have been selected for crystallization. The obtained samples were characterized by X-ray diffraction, scanning electron microscopy and UV–Vis spectroscopy. The UV–Vis spectroscopy showed that the obtained glasses are transparent in the visible region. The values of optical band gap (E _opt) and changes in cut-off (λ_c) depending on composition are reported. It was established that the increase in the MoO₃ content led to decreasing the transmittance of the glasses. Moreover, the absorption edge shifts towards longer wavelength.     

Investigation of solid solution of ZrP<Subscript>2</Subscript>O<Subscript>7</Subscript>–Sr<Subscript>2</Subscript>P<Subscript>2</Subscript>O<Subscript>7</Subscript>

In this study, ZrP₂O₇ was synthesized by the solid state reaction of ZrO₂ and NH₄H₂PO₄ at 900 °C. Then, in set 1; 10, 5, 1, 0.5, 0.1, 0.05, 0.03% previously prepared Sr₂P₂O₇ were doped into ZrP₂O₇, and Sr₂P₂O₇ slightly affect the unit cell parameter of cubic ZrP₂O₇ (a = 8.248(6)–8.233(8) Å). The reverse of this process was also applied to Sr₂P₂O₇ system (set 2). ZrP₂O₇ changes the unit cell parameters of orthorhombic Sr₂P₂O₇ in between a = 8.909(5)–8.877(5) Å, b = 13.163(3)–13.12(1) Å, and c = 5.403(2)–5.386(4) Å. Analysis of the vibrations of the P₂O ₇ ^4? ion and approximate band assignments for IR and Raman spectra are also reported in this work. Some coincidences in infrared and Raman spectra both sets were found and strong P–O–P bands were observed. Surface morphology, EDX analysis, and thermoluminescence properties of both sets were given the first time in this paper.     

Preparation and characterization of Li<Subscript>2</Subscript>O–CaO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–P<Subscript>2</Subscript>O<Subscript>5</Subscript>–SiO<Subscript>2</Subscript> glasses as bioactive material

The aim of the present investigation was to study the role of Al₂O₃ in the Li₂O–CaO–P₂O₅–SiO₂ bioactive glass for improving the bioactivity and other physico-mechanical properties of glass. A comparative study on structural and physico-mechanical properties and bioactivity of glasses were reported. The structural properties of glasses were investigated by X-ray diffraction, Fourier transform infrared spectrometry, scanning electron microscopy and the bioactivity of the glasses was evaluated by in vitro test in simulated body fluid (SBF). Density, compressive strength, Vickers hardness and ultrasonic wave velocity of glass samples were measured to investigate physical and mechanical properties. Results indicated that partial molar replacement of Li₂O by Al₂O₃ resulted in a significant increase in mechanical properties of glasses. In vitro studies of samples in SBF had shown that the pH of the solution increased after immersion of samples during the initial stage and then after reaching maxima it decreased with the increase in the immersion time. In vitro test in SBF indicated that the addition of Al₂O₃ up to 1.5 mol% resulted in an increase in bioactivity where as further addition of Al₂O₃ caused a decrease in bioactivity of the samples. The biocompatibility of these bioactive glass samples was studied using human osteoblast (MG-63) cell lines. The results obtained suggested that Li₂O–CaO–Al₂O₃–P₂O₅–SiO₂-based bioactive glasses containing alumina would be potential materials for biomedical applications.     

Thermal and dielectric properties of the LTCC composites based on the eutectic system BaO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript>–B<Subscript>2</Subscript>O<Subscript>3</Subscript>

The low-temperature co-fired ceramic (LTCC) composites containing quartz based on the eutectic system BaO–Al₂O₃–SiO₂–B₂O₃ are fabricated at the sintering temperature below 980 °C. Preparation process and sintering mechanism were described and discussed, respectively. The results indicated that the addition of quartz to the eutectic system can availably improve dielectric properties of the LTCC composites. In addition, The LTCC composites with optimum compositions, which were obtained by the regulation of an Al₂O₃ content in the composite, can express excellent dielectric properties (permittivity: 5.94, 5.48; loss: 7 × 10⁻⁴, 5 × 10⁻⁴), considerable CTE values (11.7 ppm. °C⁻¹, 10.6 ppm. °C⁻¹) and good mechanical properties (128 MPa,133 MPa).     

Mechanochemical behavior of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>–Al–Fe powder mixtures to produce Fe<Subscript>3</Subscript>Al–Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocomposite powder

Mechanical treatment of Fe₂O₃, Al and Fe powder mixtures was carried out in a high energy ball mill to synthesize Fe₃Al–Al₂O₃ intermetallic matrix nanocomposite. Different compositions including 3Fe + Al, Fe₂O₃ + 2Al, 3Fe₂O₃ + 8Al and Fe₂O₃ + 3Al+Fe were chosen in this study. Phase development and structural changes occurring during ball milling were investigated by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The results showed that during MA, Fe₂O₃, Al, and Fe react to give a nanocrystalline Fe₃Al intermetallic compound matrix. The presence of pure Fe in initial powder mixture changed the modality of mechanochemical process from sudden to gradual reaction. The Fe₃Al–Al₂O₃ compound had a finer microstructure and particles size compared to the Fe₃Al compound.     

Frequency dependence of dielectric properties of CaO–SrO–Li<Subscript>2</Subscript>O–Ln<Subscript>2</Subscript>O<Subscript>3</Subscript>–TiO<Subscript>2</Subscript> ceramics

CaO–SrO–Li₂O–Ln₂O₃–TiO₂ ceramics were prepared by solid state reaction method, where Ln₂O₃ consists of equal proportions of Nd₂O₃ and Sm₂O₃. Dielectric properties and crystal structure were investigated with respect to the content of TiO₂. Single phase with an orthorhombic perovskites structure was formed within the composition range of investigation. The frequency dependence of dielectric properties of the present ceramics was extensively investigated. Dielectric constant was less sensitive to frequency. However, dielectric loss and temperature coefficients were both very sensitive to frequency and gradually decreased with increasing frequency, such as the variation was more than ten times between 1 MHz and several GHz. The relationship between the temperature coefficient and dielectric loss was also discussed at different frequencies. And the mechanism of the frequency dependence was discussed in term of the role of Li ions.     

The effect of Fe contents on the local structure and crystallization behavior of SiO<Subscript>2</Subscript>–CaO–P<Subscript>2</Subscript>O<Subscript>5</Subscript>–Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> glasses

The glass and glass ceramics containing SiO₂–CaO–Fe₂O₃–P₂O₅ were prepared by sol–gel method. The influence of the Fe contents on the crystallization and local structure of the glass and glass ceramics was systematically investigated. The crystal structure of the glass ceramics was identified by XRD characterization. Hematite phase can be precipitated from the glass matrix in all glass ceramics with various Fe contents, and the crystallographic parameters of hematite were determined by XRD Rietveld refinement. The crystallization kinetics of the glasses was investigated in detail. Relative low activation energies were obtained at low Fe contents. The local structure evolution of the glass and glass ceramics has been studied in-depth by means of FTIR and Mössbauer spectroscopy. Fe element is present both as network former and network modifier which significantly influenced the crystallization activation energies of the glasses. The results of this work may be of great significance for the material design and practical applications of bioactive magnetic glass ceramics for hyperthermia.     

Structure and properties of CaF<Subscript>2</Subscript>–B<Subscript>2</Subscript>O<Subscript>3</Subscript> glasses

FTIR spectroscopy has been employed to investigate the structure of CaF₂–B₂O₃ glasses. It is proposed that CaF₂ partially modifies the borate network forming \textCa _{1 / 2} ²⁺ [\textBO _{3 / 2} \textF] ^- {\text{Ca}}_{ 1 / 2}^{ 2+ } [{\text{BO}}_{ 3 / 2} {\text{F]}}^{ - } units. The rest of CaF₂ is assumed to build an amorphous network formed of CaF₄ tetrahedra. Analysis of density and molar volume revealed that the volume of CaF₄ tetrahedron in the studied glasses is slightly greater than that in the crystalline form. Data of density, molar volume, and electric conductivity have been correlated with the glass structure. As far as the authors know, CaF₂–B₂O₃ glasses are investigated for the first time.     

Enhanced antibacterial performance of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>–Ag and MnFe<Subscript>2</Subscript>O<Subscript>4</Subscript>–Ag nanocomposites

In this work, we have described the antibacterial activities of Fe₃O₄ nanoparticles with different organic parts, including Humic acid (HA), Nicotinic acid (Nico) and Histidine (His), and the antibacterial activity of MnFe₂O₄ nanoparticles coated with PANI and SiO₂ against different bacteria and some standard antibacterial drugs. The present study revealed that the newly fabricated various Fe₃O₄ and MnFe₂O₄ nanocomposites, when combined with some different organic parts, are superiour antibacterial agents. Also, the synthesized nanocomposites can be easily separated from aqueous solution by magnetic filtration without any contamination of the medium.     

Hardness properties and microscopic investigation of crack–crystal interaction in SiO<Subscript>2</Subscript>–MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–K<Subscript>2</Subscript>O–B<Subscript>2</Subscript>O<Subscript>3</Subscript>–F glass ceramic system

In view of the potential engineering applications requiring machinability and wear resistance, the present work focuses to evaluate hardness property and to understand the damage behavior of some selected glass–ceramics having different crystal morphologies with SiO₂–MgO–Al₂O₃–K₂O–B₂O₃–F composition, using static micro-indentation tests as well as dynamic scratch tests, respectively. Vickers hardness of up to 5.5 GPa has been measured in glass–ceramics containing plate like mica crystals. Scratch tests at a high load of 50 N in artificial saliva were carried out in order to simulate the crack–microstructure interaction during real-time abrasion wear and machining operation. The experimental observations indicate that the novel “spherulitic-dendritic” shaped crystals, similar to the plate like crystals, have the potential to hinder the scratching induced crack propagation. In particular, such potential of the ‘spherulitic-dendritic’ crystals become more effective due to the larger interfacial area with the glass matrix as well as the dendritic structure of each mica plate, which helps in crack deflection and crack blunting, to a larger extent. While modest damage tolerant behavior is observed in case of ‘spherulitic-dendritic’ crystal containing material, severe brittle fracture of plate like crystals were noted, when both were scratched at 50 N load.     

Characterization of microstructure and properties of Al–Al<Subscript>3</Subscript>Zr–Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite

Aluminium-based metal matrix composite strengthened by in situ Al₂O₃ and Al₃Zr particles were synthesized by powder metallurgy route. Phase analysis by X-ray diffraction and scanning electron microscopy revealed that the reaction between Al and ZrO₂ produced Al₂O₃ and Al₃Zr phases in the sintered composites. The hardness of the composite is a strong function of sintering temperature as well as the volume fraction of reinforcements. The dry sliding wear test results clearly indicated that increasing the volume fraction of zirconia particles in the composite improved the wear resistance. Microcutting, ploughing, delamination and oxidation were the main mechanisms of wear.