Lead and copper removal from aqueous solutions by porous glass derived calcium hydroxyapatite

A porous glass was prepared by sintering Na₂O-CaO-B₂O₃ glass powder with powdered sodium chloride. Subsequently, the sodium chloride was dissolved in water resulting in a highly porous material. A sample was prepared consisting of 60 vol% glass and 40 vol% salt which both had particle sizes <100 and 400-500 μm, respectively. The sample was sintered at a temperature of 580 °C for 15 min which resulted in an optimum structure with 57.5% porosity and 0.944 MPa compressive strength. Amorphous calcium hydroxyapatite was formed by immersing these materials in 0.1 M K₂HPO₄ solutions at room temperature for 1 day. The porous glass derived hydroxyapatite matrix was then processed for removing lead and copper ions from aqueous solutions. The results showed that the glass derived calcium hydroxyapatite matrix effectively immobilizes lead and copper ions in solution. The adsorption mechanism was investigated by the X-ray Diffraction (XRD) and Scanning Electron Microscopy including Energy Dispersive X-Ray Spectrometry (SEM-EDX).     

Preparation and properties of low-temperature co-fired ceramic of CaO–SiO2–B2O3 system

Low temperature co-fired ceramic (LTCC) was prepared by sintering a glass selected from CaO–SiO₂–B₂O₃ system, in which 0.5 wt% P₂O₅ and 0.5 wt% ZnO were added to optimize the preparation conditions. The glass powder and sintered bodies were characterized by different analytical techniques such as TG-DTA analysis, X-ray diffraction and Scanning electron microscopy. It was found that the optimal sintering temperature was 820°C based on the microstructure and the properties of sintering bodies, and then the major phases of the LTCC were CaSiO₃, CaB₂O₄ and SiO₂. The obtained products, with dielectric constant about 6.5, dielectric loss about 2 × 10⁻³ at 30 MHz and coefficient of thermal expansion about 8 × 10⁻⁶ °C⁻¹ between 20 and 400°C, are supposed to be suitable for application in wireless communications.     

Microstructure and microwave dielectric characteristics of CaO–B2O3–SiO2 glass ceramics

CaO–B₂O₃–SiO₂ (CBS) glass powders are prepared by traditional glass melting method, whose properties and microstructures are characterized by Differential thermal analysis (DTA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). It is found that the pure CBS glass ceramics possess excellent dielectric properties (ε _r = 6.5, tan δ = 5 × 10⁻³ at 10 GHz), but a higher sintering temperature (>900 °C) and a narrow sintering temperature range (about 10 °C). The addition of a low-melting-point CaO–B₂O₃–SiO₂ glass (LG) could greatly decrease the sintering temperature of CBS glass to 820 °C and significantly enlarge the sintering temperature range to 40 °C. The CBS glass ceramic with 30 wt% LG glass addition sintered at 840 °C exhibits better dielectric properties: ε _r ≈ 6, tan δ < 2 × 10⁻³ at 10 GHz, and the major phases of the sample are CaSiO₃, CaB₂O₄ and SiO₂.     

Effect of sintering process on electrical properties and ageing behavior of ZnO–V2O5–MnO2–Nb2O5 varistor ceramics

The effect of sintering process on microstructure, electrical properties, and ageing behavior of ZnO–V₂O₅–MnO₂–Nb₂O₅ (ZVMN) varistor ceramics was investigated at 875–950 °C. The sintered density decreased from 5.52 to 5.44 g/cm³ and the average grain size increased from 4.4 to 9.6 μm with the increase of sintering temperature. The breakdown field (E_{1 mA}) decreased from 6991 to 943 V/cm with the increase of sintering temperature. The ZVMN varistor ceramics sintered at 900 °C led to surprisingly high nonlinear coefficient (α = 50). The donor concentration (N_d) increased from 3.33 × 10¹⁷ cm⁻³ to 7.64 × 10¹⁷ cm⁻³ with the increase of sintering temperature and the barrier height (Φ_b) exhibited the maximum value (1.07 eV) at 900 °C. Concerning stability, the varistors sintered at 925 °C exhibited the most stable accelerated ageing characteristics, with %ΔE_{1 mA} = 1.5% and %Δα = 13.3% for DC accelerated ageing stress of 0.85 E_{1 mA}/85 °C/24 h.     

Effect of replacement of MgO by CaO on sintering,crystallization and properties of MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript> system glass-ceramics

The effects of replacement of MgO by CaO on the sintering and crystallization behavior of MgO–Al₂O₃–SiO₂ system glass-ceramics were investigated. The results show that with increasing CaO content, the glass transition temperature firstly increased and then decreased, the melting temperature was lowered and the crystallization temperature of the glass-ceramics shifted clearly towards higher temperatures. With the replacement of MgO by less than 3 wt.% CaO, the predominant crystalline phase in the glass-ceramics fired at 900 °C was found to be α-cordierite and the secondary crystalline phase to be μ-cordierite. When the replacement was increased to 10 wt.%, the predominant crystalline phase was found to be anorthite and the secondary phase to be α-cordierite. Both thermal expansion coefficient (TCE) and dielectric constant of samples increases with the replacement of MgO by CaO. The dielectric loss of sample with 5 wt.% CaO fired at 900 °C has the lowest value of 0.08%. Only the sample containing 5 wt.% and10 wt.% CaO (abbreviated as sample C5 and C10) can be fully sintered before 900 °C. Therefore, a dense and low dielectric loss glass-ceramic with predominant crystal phase of α-cordierite and some amount of anorthite was achieved by using fine glass powders (D₅₀ = 3 μm) fired at 875–900 °C. The as-sintered density approaches 98% theoretical density. The flexural strength of sample C5 firstly increases and then decreases with sintering temperature, which closely corresponds to its relative density. The TCE of sample C5 increases with increasing temperature. The dielectric property of sample C5 sintered at different temperatures depends on not only its relative density but also its crystalline phases. The dense and crystallized glass-ceramic C5 exhibits a low sintering temperature (≤900 °C), a fairly low dielectric constant (5.2–5.3), a low dielectric loss (≤10⁻³) at 1 MHz, a low TCE (4.0–4.25 × 10⁻⁶ K⁻¹), very close to that of Si (∼3.5 × 10⁻⁶ K⁻¹), and a higher flexural strength (≥134 MPa), suggesting that it would be a promising material in the electronic packaging field.     

Fabrication of transparent silica glass by powder sintering

Transparent silica glasses were obtained by sintering a green compact (fabricated by slip-casting methods for high-purity silica glass powder) in diverse atmospheres. The relationships between sintering atmosphere and sintering temperature that result in transparent, sintered silica glass were shown. The results indicate that there are four forming phases for each sintering atmosphere and temperature: (1) nontransparent glass resulting from an overabundance of pores (2) crystal, such as cristobalite or β-quartz, (3) moganite, and (4) transparent glass. Optimum sintering temperature for fabricating transparent silica glass was above 1673 K in a high-vacuum (10^–4 Pa: p(O₂) = 10^–14) atmosphere. We investigate the fabrication of transparent and hydroxyl-free silica glass by a powder-sintered method. After studying the effect of sintering schedule on residual [OH^–] concentration for transparent, sintered silica glasses, we sintered a green compact prepared by silica powders with a mean particle size of 1.6 µm, first heating it to 1523 K for dehydration and then to 1873 K for densification. This typical fabricated condition resulted in a transparent, sintered silica glass with <1 ppm [OH^–] concentration.     

The effect of glass addition on the dielectric properties of barium strontium titanate

Ba_0.7Sr_0.3TiO₃ (BST) ceramics were prepared by the conventional solid state ceramic route. Different weight percentages of twelve different glasses were added to the calcined BST ceramics and sintered. The structure and microstructure of the sintered materials were investigated by X-ray diffraction and Scanning Electron Microscopic techniques. The low frequency dielectric properties of the glass-ceramic composites were measured using LCR meter. Some of the glasses improved the dielectric properties and considerably lowered the sintering temperature. The glasses were prepared and characterized under identical conditions. Among the different glasses, 1.5 wt% addition of 71ZnO–29B₂O₃ lowered the sintering temperature of BST to 975 °C with a dielectric loss of 9 × 10⁻³ and dielectric constant of 875 at 1 MHz. The curie temperature of BST ceramics was found to shift towards lower temperature with glass addition.     

Phase development and sintering behaviour of biphasic HA-TCP calcium phosphate materials prepared from hydroxyapatite and bioactive glass

The composites of hydroxyapatite (HA) with 2.5 and 5 wt% of a double oxide (50 mol% CaO and 50 mol% P₂O₅) glass were prepared using the conventional powder mixing and sintering method. The addition of the glass significantly enhanced the decomposition process of HA into alpha tricalcium phosphate (α-TCP) for bodies sintered at 1,300 and 1,350 °C and β-TCP phases for the ones sintered at 1,200, 1,250 and 1,300 °C. Microstructural characteristics, phase development and thermal behaviour were studied by SEM, XRD and STA. The effects of TCP phase content and phase transformation from β-TCP to α-TCP on the sintering are discussed. The characterizations revealed considerable content of TCP in the form of large semi-islands due to important reactions between the fine HA and the glass mixed powders.     

The effect of polymeric chain-like structure on the degradation and cellular biocompatibility of calcium polyphosphate

Three-dimensional porous calcium polyphosphate (CPP) scaffolds were fabricated in the present work. We investigated the degradation mechanism of CPP from the viewpoint of polymeric structure and the effects of different polymeric structure on cell viability. By controlling the sintering temperature and altering the proportion of hydrolytic groups (Q¹ groups) in polyphosphate chain, CPP can be obtained respectively with different degradation rate. The results suggested that with increasing sintering temperature, the proportion of Q¹ groups in polyphosphate chain decreased. CPP sintered at 550 °C had 15.1% Q¹ groups in polyphosphate chain, while CPP sintered at 650 °C and 750 °C exhibited 10.5 and 8.3%, respectively. During immersion in simulated body fluid (SBF) for 30 days, the weight loss of CPP sintered at 550 °C was about 80%, while CPP sintered at 650 °C and 750 °C degraded by only 8% and 5%. Cell viability test results showed that the porous CPP did not exert cytotoxicity effect on the cells after being cultured 6 days. Due to the lower degradation rate, CPP sintered at 750 °C showed better cell attachment and proliferation as well as higher cell density. These findings may provide an approach to study and achieve controllable degradation of CPP, and explore more biomedical applications.     

Effect of sintering temperature on structural and electrical properties of gadolinium doped ceria (Ce<Subscript>0·9</Subscript>Gd<Subscript>0·1</Subscript>O<Subscript>1·95</Subscript>)

Gadolinium doped ceria oxide is one of the promising materials as an electrolyte for IT-SOFCs. Ce_0·9Gd_0·1O_1·95 (GDC10) powder was prepared by solid state reaction and sintered at 1473 K, 1573 K, 1673 K and 1773 K. All samples were studied using X-ray diffraction, scanning electron micrograph and d.c. conductivity measurement. The crystallinity and surface morphology of the samples improved with sintering temperature. Further, the electrical conductivity measurement indicated that the conduction mechanism is mainly ionic. The conductivity of samples sintered at 1673 K and 1773 K at 800°C are of the order of 0·1 S-cm⁻¹. The activation energies decreased from 1·25–0·82 eV with increase in sintering temperature.     

Sintering, crystallization, and properties of a low-viscosity SnO–MgO–P2O5 glass

A lead-free, low-viscosity SnO–MgO–P₂O₅ glass powder was fabricated. Sinterability, wetting, flowability, crystallization, and the resulting properties of the glass powder were investigated. It is shown that the powder compact can be fully densified above 362 °C and show good wet to the substrate above 417 °C. The properties (coefficient of thermal expansion and chemical durability) of the sintered glass depend on the sintering temperature and are discussed in terms of the development of crystalline phases during sintering.     

Specific contact resistance and metallurgical process of the silver-based paste for making ohmic contact structure on the porous silicon/p-Si surface of the silicon solar cell

Porous silicon has been considered as a promising optoelectronic material for developing a variety of optoelectronic devices and sensors. In the present study, the electrical properties and metallurgical process of the screen-printed Ag metallization formed on the porous silicon surface of the silicon solar cell have been investigated. The contact structure consists of thick-film Ag metal contact patterned on the top of the porous silicon surface. The sintering process consists of a rapid firing step at 750–825 °C in air ambient. It results in the formation of a nearly perfect contact structure between the Ag metal and porous silicon/p-Si structure that forms the top metalization for the screen-printed silicon solar cells. The SEM picture shows that Ag metal firmly coalesces with the silicon surface with a relatively smooth interfacial morphology. This implies that high temperature fire-through step has not introduced any signs of adverse effect of junction puncture or excessive Ag indiffusion, etc. The three-point probe (TPP) method was applied to estimate the specific contact resistance, ρ _c (Ω-cm²) of the contact structure. The TPP measurement shows that contact structure has excellent ohmic properties with ρ _c = 1.2 × 10⁻⁶ Ω-cm² when the metal contact sintered at 825 °C. This value of the specific contact resistance is almost three orders of magnitude lower than the corresponding value of the ρ _c = 7.35 × 10⁻³ Ω-cm² obtained for the contact structure sintered at 750 °C. This improvement in the specific contact resistance indicates that with increase in the sintering temperature, the barrier properties of the contact structure at the interface of the Ag metal and porous silicon structure improved which in turn results a lower specific contact resistance of the contact structure.     

Low temperature sintering and microwave dielectric properties of zinc silicate ceramics

Effects of ZnO–B₂O₃–SiO₂ glass on the sintering behavior, the microstructure, and the microwave dielectric properties of Zn₂SiO₄ ceramics have been investigated. The ZnO–B₂O₃–SiO₂ glass lowered the sintering temperature of Zn₂SiO₄ ceramics effectively from 1300 to 900 °C. The X-ray diffraction results showed that the secondary phase of SiO₂ in the Zn₂SiO₄ ceramics could be dissolved in the glass. The dielectric constant decreased slightly, and the quality factor decreased with increasing glass content. Especially, when the glass content was chosen as 20 wt%, the ceramics sintered at 900 °C for 2 h exhibited a low dielectric constant of 6.85, a high quality factor of 31,690 and the temperature coefficient of the resonant frequency of −28 ppm/°C, which demonstrated a good potential for use in low temperature co-fired ceramics field.     

Effects of glass additions on the dielectric properties and energy storage performance of Pb0.97La0.02(Zr0.56Sn0.35Ti0.09)O3 antiferroelectric ceramics

In this work, CdO–Bi₂O₃–PbO–ZnO–Al₂O₃–B₂O₃–SiO₂ low softening point glass powders were prepared and employed as sintering aid to improve the dielectric breakdown strength and reduce the sintering temperature of Pb_0.97La_0.02(Zr_0.56Sn_0.35Ti_0.09)O₃ antiferroelectric ceramics. The effects of glass content and sintering temperature on the densification, microstructure, dielectric properties and energy storage performance of Pb_0.97La_0.02(Zr_0.56Sn_0.35Ti_0.09)O₃ antiferroelectric ceramics have been investigated. With inclusion of glass, sintered densities comparable to those obtained by conventional sintering are achieved at only 1,050 °C. The breakdown strength of glass-added samples was notably improved due to the reduction of the grain size. The antiferroelectric to ferroelectric switching field and the ferroelectric to antiferroelectric field both increased with increasing glass content. The dielectric constant and dielectric loss decreased gradually with increasing glass content. As a result, the highest recoverable energy density of 3.3 J/cm³ with an energy efficiency of 80 % was achieved in 4 wt% glass-added sample sintered at 1,130 °C.     

Influence of sintering atmosphere on the microstructure and water durability of SnO–MgO–P<Subscript>2</Subscript>O<Subscript>5</Subscript> glass

Effects of sintering atmosphere (Ar, air, and O₂) on the sinterability and crystallization at 380–470 °C of 60SnO, 10MgO, 30P₂O₅ (mol%) glass powder, and the water durability of the sintered glass were investigated. Increasing the oxygen partial pressure (P_\textO2 ) (P_{{{\text{O}}_{2} }} ) in the sintering atmosphere enhanced the oxidation tendency of Sn²⁺ to Sn⁴⁺ near the surface region of the glass particles. Therefore, the glass viscosity was increased, resulting in the increase in both the temperature of densification and the temperature at which crystalline phases developed. Phase assemblage and the amounts of crystalline phases were also affected by P_\textO2 . P_{{{\text{O}}_{2} }} . The water durability of the sintered glasses is discussed in terms of the above microstructural parameters.     

Sintering, densification and crystallization of Ca–Al–B–Si–O glass/Al2O3 composites for LTCC application

Ca–Al–B–Si–O glass/Al₂O₃ composites were prepared based on the borosilicate glass powders (D₅₀ = 2.84) and Al₂O₃ ceramic powders (D₅₀ = 3.26), and the sintering, densification, crystallization of samples were investigated. The shrinkage of sample starts to have a sharp increase at 600 °C. The shrinkage of sample starts to have a further rapid increase after the glass softening temperature of about 713 °C. Glass/Al₂O₃ composites can be sintered at 875 °C/15 min and exhibit better properties of a relative density of 98.4 %, a λ value of 2.89 W/mK, a ε _r value of 7.82 and a tan δ value of 5.3 × 10^?4. The interface between glass and Al₂O₃ grains and the interface between anorthite and glass phase depicts a good compatibility according to transmission electron microcopy test. It is the low sintering temperature, high density and good compatibility with Ag electrodes that, guarantee borosilicate glass/Al₂O₃ composites suitable for low temperature co-fired ceramic materials.     

Effects of SrO–B2O3–SiO2 glass additive on densification and energy storage properties of Ba0.4Sr0.6TiO3 ceramics

SrO–B₂O₃–SiO₂ glass powders were prepared and employed as sintering aids to reduce the sintering temperature of Ba_0.4Sr_0.6TiO₃ ceramics. The effects of glass content and sintering temperature on the densification, dielectric properties and energy storage properties of Ba_0.4Sr_0.6TiO₃ ceramics have been investigated. The relative density characterization results indicate that densification of Ba_0.4Sr_0.6TiO₃ ceramics with glass content becomes apparently from sintering temperature of 1,060 °C. XRD results show all Ba_0.4Sr_0.6TiO₃ ceramics exhibit a perovskite structure without the formation of a secondary phase. The dielectric constant and dielectric loss decreased gradually with increasing glass content. The relationship between dielectric constant and breakdown strength was discussed using the thermochemical model. A discharged energy density of 0.44 J/cm³ with an energy efficiency of 67.4% was achieved for Ba_0.4Sr_0.6TiO₃ ceramic with 2.0 wt% glass addition sintered at 1,180 °C.     

Three‐Dimensional Printing of Complex‐Shaped Alumina/Glass Composites

Alumina/glass composites were fabricated by three‐dimensional printing (3DP?) and pressureless infiltration of lanthanum‐alumino‐silicate glass into sintered porous alumina preforms. The preforms were printed using an alumina/dextrin powder blend as a precursor material. They were sintered at 1600 °C for 2 h prior to glass infiltration at 1100 °C for 2 h. The influence of layer thickness and sample orientation within the building chamber of the 3D‐printer on microstructure, porosity, and mechanical properties of the preforms and final composites was investigated. The increase of the layer thickness from 90 to 150 µm resulted in an increase of the total porosity from ～19 to ～39 vol% and thus, in a decrease of the mechanical properties of the sintered preforms. Bending strength and elastic modulus of sintered preforms were found to attain significantly higher values for samples orientated along the Y‐axis of the 3D‐printer compared to those orientated along the X‐ or the Z‐axis, respectively. Fabricated Al₂O₃/glass composites exhibit improved fracture toughness, bending strength, Young's modulus, and Vickers hardness up to 3.6 MPa m^1/2, 175 MPa, 228 GPa, and 12 GPa, respectively. Prototypes were fabricated on the basis of computer tomography data and computer aided design data to show geometric capability of the process.     

Preparation of porous 45S5 Bioglass®-derived glass–ceramic scaffolds by using rice husk as a porogen additive

Bioactive glass is currently regarded as the most biocompatible material in the bone regeneration field because of its bioactivity, osteoconductivity and even osteoinductivity. In the present work porous glass–ceramic scaffolds, which were prepared from the 45S5 Bioglass^® by foaming with rice husks and sintering at 1050°C for 1 h, have been developed. The produced scaffolds were characterized for their morphology, properties and bioactivity. Micrographs taken using a scanning electron microscope (SEM) were used for analysis of macropores, mesopores and micropores, respectively. The bioactivity of the porous glass–ceramic scaffolds was investigated using simulated body fluid (SBF) and characterized by SEM, energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). A great potential scaffold that provides sufficient mechanical support temporarily while maintaining bioactivity, and that can biodegrade at later stages is achievable with the developed 45S5 Bioglass^®-derived scaffolds.     

Development of mixed conducting dense nickel/Ca-doped lanthanum zirconate cermet for gas separation application

La_1.95Ca_0.05Zr₂O_7-δ (LCZ) and Ni–LCZ cermet have been prepared by combustion synthesis and conventional solid state mixing methods respectively. Both the materials are sintered in air and controlled atmosphere (5% H₂ in Ar). The density obtained for the material sintered at 1400 °C in controlled atmosphere is found to be more than 99.5%. This sintering temperature (1400 °C) is considered to be much lower compared to the conventional sintering temperature. The corresponding total conductivity for such Ni–LCZ cermet materials is ～400 S/cm measured at 750 °C having 40 vol% of Ni and 60 vol% LCZ.