Phase and microstructural evolution in lithium silicate glass-ceramics with externally added nucleating agent

Development of lithium disilicate-based glass-ceramics critically depends on use of nucleating agent in the glass matrix. The present study reports the effect of externally added nucleating agent Li₃PO₄ in Li₂O–K₂O–MgO–ZnO–ZrO₂–Al₂O₃–SiO₂ system which is compared with a reference composition (GC1) (SiO₂:Li₂O = 2.16:1) prepared with in situ formed Li₃PO₄. For externally added Li₃PO₄, two compositions were studied. In one case (GC2) before addition of Li₃PO₄, SiO₂:Li₂O ratio in glass was maintained as 2.87:1 and in another case (GC3) SiO₂:Li₂O ratio in glass was maintained same as reference GC1 that is, 2.16:1. The glasses were characterized by using MAS-NMR spectroscopy. Sintering and crystallization behavior of the glass-ceramics was characterized by using XRD, SEM, DTA. Due to in situ formation of Li₃PO₄, GC1 resulted in a dense sample with finer crystals of lithium disilicate. In GC2 and GC3, externally added lithium phosphate, which was in the form of ultrafine aggregated particles, formed flower-like colonies of radially outward crystals. Higher SiO₂:Li₂O ratio in GC2 resulted in lithium disilicate crystals and high viscous glass causing large air entrapment and so less densification. GC3 with higher lithia in glass showed higher densification than GC2 but only lithium metasilicate crystals were formed.     

Preparation and characterization of alkali-free glass substrates with enhanced properties for TFT–LCDs applications

To obtain an alkali-free glass substrate with enhanced properties for thin-film transistor–liquid crystal displays (TFT–LCDs) applications, we chose a base glass composed of 3B₂O₃-15Al₂O₃-58SiO₂-22MgO-0.5SrO-1.5MgF₂ (mol%) for nucleation–crystallization. The results show that when the nucleation–crystallization processes of the base glass are 810 °C/6 h + 880 °C/6–9 h, the prepared GC/6–GC/9 glass-ceramics exhibit enhanced properties because of the precipitation of nano-sized cordierite. The transmittances in the visible range of the GC/6–GC/9 glass-ceramics exceed 85%, the densities are 2.564–2.567 g/cm³, thermal expansion coefficients are 2.934–3.059 × 10^-6/°C (25–300 °C), compressive strengths are 417–589 MPa, bending strengths are 141–259 MPa, Vickers hardnesses are 6.8–7.8 GPa, and strain points are approximately 735 °C. Considering these properties, the prepared GC/6–GC/9 glass-ceramics have good potential as candidate materials for alkali-free glass substrates. Additionally, these results demonstrate that it is feasible to improve the properties of alkali-free glass substrates by nucleation–crystallization.     

Crystallization of LiNbO3 and NaNbO3 in niobiosilicate glass–ceramics

Although glass–ceramics have been widely explored for their thermal stability and mechanical properties, they also offer unique symmetry-dependent properties such as piezoelectricity and pyroelectricity through controlled crystallization of a polar phase. This work examines crystallization of LiNbO₃ in a 35SiO₂–30Nb₂O₅–35Li₂O mol% composition and crystallization of LiNbO₃ and NaNbO₃ in a 35SiO₂–30Nb₂O₅–25Li₂O–10Na₂O mol% composition. Crystallization kinetics are examined using the Johnson–Mehl–Avrami–Kolmogorov (JMAK) theory where the Avrami exponent, n, is calculated to be 1.0–1.5. Microscopical analysis shows dendritic morphology, which when combined with the JMAK analysis, suggests diffusion-controlled one-dimensional growth. Adding Na₂O to the glass composition increases the inter-diffusivity of ions which causes LiNbO₃ to crystallize faster and lowers the activation energy of transformation from 1054 ± 217 kJ/mol in the ternary composition to 882 ± 212 kJ/mol. Time-temperature-transformation diagrams are presented which show that the temperature for maximum rate of transformation for LiNbO₃ is ∼650°C and for NaNbO₃ is ∼715°C.     

Contribution of some transition metal oxides to crystallization and electro-thermal properties of glass-ceramics

Lithium di-silicate (LS₂) glass-ceramics modified with copper oxide using the formula: 34.83Li₂O–xCuO–(65.17-x)SiO₂ (where; x = 1, 2, 4 and 6 mol%) were prepared by melt-quenching followed by controlling heat-treatment. 6 mol% of MnO or Fe₂O₃ transition metal oxides was added instead of SiO₂ in the high CuO-content composition. The effect of the transition cations on phase formation, microstructure, density, thermal expansion, and electrical conductivity was investigated as a function of the controlled crystallization. Results show that up to 4 mol%, Cu⁺² was hosted in stable Li₂Si₂O₅ structure. This enhanced the crystal formation, including Li₂Si₂O₅ and its solid solution (ss), Li₂SiO₃, Li₂Cu₅(Si₂O₇)₂, CuMn₆SiO₁₂, LiFeSi₂O₆ (ss), and the orthosilicate Li₂FeSiO₄ (ss). The prepared materials had different density values ranged from 2.35 to 2.79 g/cm³ for glass and varied from 2.43 to 3.15 g/cm³ for glass–ceramics, whereas the α-values of glass-ceramics ranged in the 95–165 × 10⁻⁷/°C. The progress of electrical properties in glass-ceramics, as a function of composition, was studied. It was markedly improved by adding different transition cations especially, Fe⁺³. The study reveals that the incorporation of transition metal ions in LS₂ composition has a positive effect on the physical-chemical properties of the prepared glass-ceramics. Therefore, it constitutes to prepare future glass-ceramic applications as hermetic seals of metals as well solid electrolyte materials.     

Influence of Al2O3/SiO2 ratio in multicomponent LNAS glasses and glass-ceramics on the crystallization behavior,microstructure and mechanical performance

Transparent glass-ceramics containing eucryptite and nepheline crystalline phases were prepared from alkali (Li, Na) aluminosilicate glasses with various mole substitutions of Al₂O₃ for SiO₂. The relationships between glass network structure and crystallization behavior of Li₂O–Na₂O–Al₂O₃–SiO₂ (LNAS) glasses were investigated. It was found that the crystallization of the eucryptite and nepheline in LNAS glasses significantly depended on the concentration of Al₂O₃. LNAS glasses with the addition of Al₂O₃ from 16 to 18 mol% exhibited increasing Q⁴ (mAl) structural units confirmed by NMR and Raman spectroscopy, which promoted the formation of eucryptite and nepheline crystalline phases. With the Al₂O₃ content increasing to 19–20 mol%, the formation of highly disordered (Li, Na)₃PO₄ phase which can serve as nucleation sites was inhibited and the crystallization mechanism of glass became surface crystallization. Glass-ceramics containing 18 mol% Al₂O₃ showed high transparency ～84% at 550 nm. Moreover, the microhardness, elastic modulus and fracture toughness are 8.56 GPa, 95.7 GPa and 0.78 MPa m^1/2 respectively. The transparent glass-ceramics with good mechanical properties show high potential in the applications of protective cover of displays.     

Mechanical property and adhesion strength of carbon nanofillers reinforced alumina single splats using in-situ picoindentation and nanoscratch test

Current study deals with the effect of carbon nanotube (CNTs) and graphene nanoplatelets (GNPs) reinforcement on the mechanical properties and the adhesion strength of plasma sprayed alumina (Al₂O₃) single splats, using in-situ picoindentation and nanoscratch test, respectively. The hardness of the Al₂O₃ splat was measured as 18 ± 5.3 GPa which increased to 34.22 ± 8.44 GPa on 1 wt% CNTs addition and to 42.5 ± 9.06 GPa on 0.5 wt% GNPs addition. Hybrid addition of CNTs and GNPs provided the maximum hardness value of 51.25 ± 8.76 GPa to the Al₂O₃ splat. Similar trend in the elastic modulus has been reported with a minimum value for Al₂O₃ splat, i.e. 159 ± 35.40 GPa, and maximum for the Al₂O₃ splat mixed synergistically with CNTs and GNPs (269 ± 43.12 GPa). Adhesion strength of the Al₂O₃ splat (0.21 ± 0.11 MPa) also showed a nearly 5-fold increase on hybrid addition of CNTs and GNPs with a maximum value of 1.08 ± 0.38 MPa. This improvement in the properties were due to the extremely high mechanical properties of CNTs and GNPs and better melting of the splats, which not only improved the densification but also provided a better interlocking between the splat and the substrate.     

Tough,strong, hard,and chemically durable enstatite-zirconia glass-ceramic

Strong glass-ceramics (GCs) have been envisaged and widely researched for various applications, including large architectural panels, ballistic impact protection, bioactive medical implants, and odontological prostheses. Here, we report on the development and characterization of a novel hard, strong and tough enstatite-zirconia (MgSiO₃-ZrO₂) glass-ceramic derived from a 51SiO₂–35MgO–6Na₂O–4ZrO₂–4TiO₂ (mol%) glass. The best GC was developed by treating glass samples for nucleation at 700°C for 12 hours, followed by crystal growth at 1090°C for 3 minutes. It was characterized by X-ray fluorescence (XRF), differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HR-TEM), and contained plate-like enstatite, zirconia, and Ti-containing crystals. We investigated the nucleating ability of ZrO₂ and TiO₂ in inducing internal nucleation. In the early stage of crystallization, enstatite spherulites were observed, which were precipitated by heterogeneous nucleation on previously nucleated ZrO₂ nano-crystals. At more advanced stages, at high temperatures, they transformed into plate-like crystals. The ball-on-three-balls strength, elastic modulus, and Vickers micro-hardness of the GC are 323 ± 26 MPa, 146 ± 13 GPa, and 6.9 ± 0.1 GPa (load = 5N), respectively. The indentation (K_C), single-edge notched beam bending (K_IC), and crack tip (K_tip) fracture toughness are 2.8 ± 0.6 MP.m^0.5, 2.2 ± 0.3 MP.m^0.5, 1.9 ± 0.3 MP.m^0.5, respectively. The crack propagation profile after a controlled Vickers indentation was quite intricate. The enstatite and zirconia crystals enhanced crack deflection, bridging and branching, hindering crack propagation. According to the ISO 6872 for dental materials, the chemical solubility of our GC is 80 ± 5 μg/cm². Due to this positive combination of high strength, toughness, hardness, and chemical durability, this new glass-ceramic is envisioned as a candidate for several applications and could be further developed for memory disc substrates, architectural cladding and tiles, ceramic glazes, and dental materials.     

Role of MgO in lowering glass transition temperature and increasing hardness of lithium silicate glass and glass-ceramics

The effect of variation of MgO (1.5, 4.5 and 7.5 mol%) content on glass structure, crystallization behavior, microstructure and mechanical properties in a Li₂O–K₂O–Na₂O–CaO–MgO–ZrO₂–Al₂O₃–P₂O₅–SiO₂ glass system has been reported here. Increased amount of MgO enhanced the participation of Al₂O₃ as a glass network former along with [SiO₄] tetrahedra, reducing the amount of non-bridging oxygen (NBO) and increasing bridging oxygen (BO) amount in glass. The increased BO in glass resulted in a polymerized glass structure which suppressed the crystallization and subsequently increased the crystallization temperature, bulk density, nano hardness, elastic modulus in the glasses as well as the corresponding glass-ceramics. MgO addition caused phase separation in higher MgO (7.5 mol%) containing glass system which resulted in larger crystals. The nano hardness (～10 GPa) and elastic modulus (～127 GPa) values were found to be on a much higher side in 7.5 mol% MgO containing glass-ceramics as compared to lower MgO containing glass-ceramics.     

Effect of heat treatment on the roughness and mechanical properties of dental lithium disilicate glass-ceramics

In dental clinics, it is common to perform small fitting adjustments in dentures using a micro-grinding tool after testing them in the patient's mouth. This procedure increases local roughness and can lead to formation of microcracks on the prosthesis surface. This study aimed to investigate the benefits of a post-finishing heat treatment to surface roughness and crack healing and its effect on the flexural strength of lithium disilicate (LD) dental glass-ceramics. Commercially available lithium metasilicate, Li₂SiO₃, samples were heat treated at 840 °C for 7 min to induce the phase transformation into LD, Li₂Si₂O₅. The LD samples were characterized by X-ray Diffraction, Scanning Electron Microscopy, Vickers hardness, Young’s modulus, and fracture toughness. One of the surfaces of the LD samples was sanded aiming to simulate the denture fitting adjustments performed in the dentist’s laboratory, generating a rough surface, Group 1. Half of the LD samples had their biaxial flexural strength evaluated by the piston-on-three-ball test (P–3B) and the other half were submitted to a second short-term heat treatment (840 °C - 5 min), Group 2, and later assessed by the P–3B. Roughness parameters in both groups were measured by 3D optical profilometry. After the crystallization heat treatment, formation of elongated LD crystals, Li₂Si₂O₅, 35% amorphous phase, and residual Li₃PO₄ was observed. In addition, the following mechanical property values were obtained: Vickers hardness = 5.8 ± 0.1 GPa, fracture toughness = 2.2 ± 0.1 MPa m^1/2, and Young’s modulus = 100.3 ± 0.3 GPa. The samples in Group 1 showed bending strength of 206 ± 30 MPa and the following roughness parameters: Ra = 0.45 ± 0.16 μm, Rz = 22.7 ± 6.7 μm, and PV = 27.7 ± 7.1 μm. In the samples in Group 2, the Ra, Rz and PV roughness parameters were 0.31 ± 0.12 μm, 5.2 ± 2.5 μm, and 9.2 ± 4.7 μm, respectively. With this decrease in roughness, the bending strength increased by 62%, with a mean value of 331 ± 59 MPa. In the need for machine finishing of LD-based glass-ceramic dental prostheses, the use of a second short-term heat treatment at 840 °C for 5 min generates considerable gains in bending strength, increasing the lifecycle of the prosthesis as a result of reduced surface roughness caused by softening of the remaining amorphous phase in the glass-ceramic. These conditions can be adapted to each chemical and crystallographic composition of the glass-ceramic under study.     

A novel high-strength lithium disilicate glass-ceramic featuring a highly intertwined microstructure

To achieve long-term clinical performance and wider application of glass-ceramic dental restorations, it is urged to enhance the mechanical properties of glass-ceramic materials. In this study, a high-strength lithium disilicate glass-ceramic was developed in a SiO₂–Li₂O–Al₂O₃–MgO–P₂O₅–ZrO₂ related glass system, which demonstrates a high flexural strength of 562 ± 107 MPa. In this high-strength glass-ceramic, the microstructure features highly intertwined colonies of lithium disilicate. This novel microstructure effectively contributes to the improvement of flexural strength. The minor crystalline phases (β-quartz, MgAl₂Si₄O₁₂, and Li₃PO₄) embedded within the Li₂Si₂O₅ (LS₂) crystal colonies and residual glass matrix could further strengthen the glass-ceramic. The development process of such a novel microstructure and its possible formation mechanism are proposed. This material could be an excellent candidate for restorative dental applications up to three-unit posterior bridges.     

Low-temperature joining of SiC ceramics with Y2O3-Al2O3 interlayer by SiO2-based liquid phase extrusion strategy

In order to reduce the joining temperature of SiC ceramics by glass-ceramic joining, some oxides were usually introduced into to Y₂O₃–Al₂O₃ for reducing the eutectic temperature. However, the joints might have poor high-temperature resistance due to the low melting point of the joining layer. In the present work, based on novel SiO₂-based liquid phase extrusion strategy, joining of SiC ceramics with Y₂O₃–Al₂O₃ interlayer was carried out by using Y₂O₃–Al₂O₃–SiO₂ as the filler through spark plasma sintering (SPS). The SiO₂-free interlayer of Y₂O₃–Al₂O₃ was used for comparison. It was found that SiC joints using Y₂O₃–Al₂O₃ could be only joined at a high temperature of 1800 °C, and the thickness of the interlayer was about 20 μm. The shear strength of the joint obtained at 1800 °C was 89.62 ± 4.67 MPa and the failure located in the SiC matrix. By contrast, reliable joining of SiC ceramics could be finished at as low as 1550 °C by extrusion of SiO₂-containing liquid phase when using Y₂O₃–Al₂O₃–SiO₂ as the interlayer, alongside the interlayer thickness of only several microns. The joint strengths after joining at 1550 °C was 84.90 ± 3.48 MPa and the failure located in matrix position. The joining mechanism was discussed by combining the detailed microstructure analysis and phase diagram.     

Effects of Y2O3 addition on structure and properties of LZAS vitrified bond for CBN grinding tools application

The effects of Y₂O₃ addition on the structure and properties of Li₂O–ZnO–Al₂O₃–SiO₂ (LZAS) vitrified bonds were firstly investigated for CBN grinding tools application. Glasses and glass-ceramics were characterized using differential scanning calorimetry, X-ray diffractometry, scanning electron microscopy and infrared spectroscopy. The thermal expansion coefficient (TEC), microhardness, bending strength and chemical durability of the obtained products were also evaluated. Results showed that Y₂O₃ acted as the network former in the track of SiO₄ tetrahedrals. Introducing Y₂O₃ in the glasses increased the glass transition temperature and crystallization temperature. The crystallization of the main β-quartz_ss phase increased with increase of Y₂O₃ content. The morphology of the crystals was dependent on the Y₂O₃ content. The TEC (5.15×10⁻⁶/°C) of vitrified bond containing 1.0 mol% Y₂O₃ (Y1.0) was very close to the TEC (5.0×10⁻⁶/°C) of CBN grains. Moreover, Y1.0 vitrified bond exhibits a high microhardness (5.98 GPa), a high bending strength (202 MPa) and a good chemical durability (20 days, DR=2.8×10⁻⁹ g/cm² min), suggesting that it would be a promising material for CBN grinding tool.     

Microstructure evolution and mechanical behavior of a mullite fiber heat-treated from 1100 to 1300°C

In this paper, the effect of phase transformation on microstructure evolution and mechanical behaviors of mullite fibers was well investigated from 1100 to 1300°C. In such a narrow temperature range, the microstructure and mechanical properties showed great changes, which were significant to be studied. The temperature of the alumina phase transformation started at below 1100°C. The main phases in fibers were γ-Al₂O₃ and δ-Al₂O₃ with amorphous SiO₂ at 1150°C. The stable α-Al₂O₃ formed at 1200°C. Then the mullite phase reaction occurred. As the alumina phase reaction took place, the tensile strength increased with the increasing temperature. In particular, the filaments achieved the highest strength at 1150°C with 1.98 ± 0.17 GPa, and the Young's modulus was 163.08 ± 4.69 GPa, showing excellent mechanical performance. After 1200°C, the mullite phase reaction went on with the crystallization of orthorhombic mullite. The density of surface defects increased rapidly due to thermal grooving, which led to mechanical properties degrade sharply. The strength at 1200°C was 1.01 ± 0.15 GPa with a strength retention of 63.13%, and the Young's modulus was 184.14 ± 10.36 GPa. While at 1300°C, the tensile strength was 0.64 ± 0.14 GPa with a strength retention of only 40.00%.     

Preparation and characterization of fully waste-based glass-ceramics from incineration fly ash,waste glass and coal fly ash

Municipal solid waste incineration (MSWI) fly ash (FA) is a typical hazardous waste due to its high contents of toxic heavy metals, and hence its disposal has attracted global concern. In this work, it was recycled into environmental-friendly CaO–Al₂O₃–SiO₂ system glass-ceramics via adding coal fly ash (CFA) and waste glass (WG). The effects of CaO/SiO₂ ratios and sintering temperatures on the crystalline phases, morphologies, mechanical and chemical properties, heavy metals leaching and potential ecological risks of glass-ceramics were investigated. The results showed that wollastonite (CaSiO₃), anorthite (CaAl₂Si₂O₈) and gehlenite (Ca₂Al₂SiO₇) were the dominant crystals in the glass-ceramics, which were not affected by CaO/SiO₂ ratio and sintering temperature. The compressive strength increased, while the Vickers hardness and microhardness decreased as increasing the sintering temperatures from 850 to 1050 °C, which reached their maximum values of 660.69 MPa, 6.14 GPa, and 7.43 GPa, respectively. However, the increase of CaO/SiO₂ ratio resulted into the reduction of the three mechanical parameters. As varying CaO/SiO₂ ratio from 0.48 to 0.86, the maximum compressive strength, Vickers hardness and microhardness were 611.80 MPa, 5.43 GPa, and 6.56 GPa, respectively. Besides, all the glass-ceramics exhibited high alkali resistance of >97%. The extremely low heavy metals leaching concentrations and low potential ecological risk of glass-ceramics further revealed its environmentally friendly property and potential application feasibility.     

The effect of electrochemical cycling on the strength of LiCoO2

This work utilizes in situ transmission electron microscopy–based nanopillar compression to investigate the effect of electrochemical cycling on the mechanical properties of LiCoO₂. The ultimate strength of LiCoO₂ in the pristine state, and after 1 and 11 cycles are 5.62 ± 0.22 GPa, 3.91 ± 1.22 GPa, and 2.27 ± 1.07 GPa, respectively. The reduced average yield strengths and the large standard deviations of cycled samples, relative to the pristine powder, are hypothesized to result from nonuniform accumulation of Li⁺ site-point defects during cycling; either H⁺ or Li⁺ vacancies. Density functional theory calculations support our hypothesized link between a nonuniform Li site-point defect distribution in the cathode and reduction in the materials cohesive strength.     

A Complete Solid Solution with Rutile‐Type Structure in SiO2–GeO2 System at 12 GPa and 1600°C

High pressure and temperature synthesis of compositions made of (Si_1?x,Ge_x)O₂ where x is equal to 0, 0.1, 0.2, 0.5, 0.7, and 1 was performed at 7–12 GPa and 1200–1600°C using a Kawai‐type high‐pressure apparatus. At 12 GPa and 1600°C, all the run products were composed of a single phase with a rutile structure. The lattice constants increase linearly with the germanium content (x), which indicates that the rutile‐type phases in the SiO₂–GeO₂ system form a complete series of solid solutions at these pressure and temperature conditions. Our experimental results show that thermodynamic equilibrium state was achieved in this system at 12 GPa and 1600°C, but not at 1200°C. At lower pressures (7 and 9 GPa) and 1600°C, we observed the decomposition of (Si_0.5,Ge_0.5)O₂ into SiO₂‐rich coesite and GeO₂‐rich rutile phases. The silicon content in the rutile structure increases sharply with pressure in the vicinity of the coesite–stishovite phase transition pressure in SiO₂.     

Effect of Sintering Additives on Relative Density and Li‐ion Conductivity of Nb‐Doped Li7La3ZrO12 Solid Electrolyte

Lithium ion conductors with garnet‐type structure are promising candidates for applications in all solid‐state lithium ion batteries, because these materials present a high chemical stability against Li metal and a rather high Li⁺ conductivity (10^?3–10^?4 S/cm). Producing densified Li‐ion conductors by lowering sintering temperature is an important issue, which can achieve high Li conductivity in garnet oxide by preventing the evaporation of lithium and a good Li‐ion conduction in grain boundary between garnet oxides. In this study, we concentrate on the use of sintering additives to enhance densification and microstructure of Li₇La₃ZrNbO₁₂ at sintering temperature of 900°C. Glasses in the LiO₂‐B₂O₃‐SiO₂‐CaO‐Al₂O₃ (LBSCA) and BaO‐B₂O₃‐SiO₂‐CaO‐Al₂O₃ (BBSCA) system with low softening temperature (<700°C) were used to modify the grain‐boundary resistance during sintering process. Lithium compounds with low melting point (<850°C) such as LiF, Li₂CO₃, and LiOH were also studied to improve the rearrangement of grains during the initial and middle stages of sintering. Among these sintering additives, LBSCA and BBSCA were proved to be better sintering additives at reducing the porosity of the pellets and improving connectivity between the grains. Glass additives produced relative densities of 85–92%, whereas those of lithium compounds were 62–77%. Li₇La₃ZrNbO₁₂ sintered with 4 wt% of LBSCA at 900°C for 10 h achieved a rather high relative density of 85% and total Li‐ion conductivity of 0.8 × 10^?4 S/cm at room temperature (30°C).     

On the fabrication and mechanical properties of Si3N4 ceramics with low content sintering additives

Si₃N₄ ceramics were prepared by hot pressing (HP) and spark plasma sintering (SPS) methods using low content (5 mol%) Al₂O₃–RE₂O₃(RE = Y, Yb, and La)–SiO₂/TiN as sintering additives/secondary additives. The effects of sintering additives and sintering methods on the composition, microstructures, and mechanical properties (hardness and fracture toughness) were investigated. The results show that fully density Si₃N₄ ceramics could be fabricated by rational tailoring of sintering additives and sintering method, and TiN secondary additive could promote the density during HP and SPS. Besides, SN-AYS-SPS possesses the most competitive mechanical properties among all the as-prepared ceramics with the Vickers hardness as 17.31 ± .43 GPa and fracture toughness as 11.07 ± .48 MPa m^1/2.     

Synthesis and characterization of Li-type EDI zeolite

A Li-type EDI zeolite (Li-EDI) was successfully synthesized in the Li₂O–Al₂O₃–SiO₂–H₂O system using a silica–alumina mixed sol as the starting material in the absence of other chemical species. The characterization of the obtained Li-EDI was compared with that of the Li-exchanged Linde F zeolite (K-type EDI zeolite). Starting gels with the batch composition of xLi₂O·Al₂O₃·2SiO₂·275H₂O (x = 2–5) were prepared by adding a LiOH solution to a silica–alumina mixed sol. A hydrothermal reaction of the gels was carried out at various temperatures. Li-EDI formed from all of the batches in the range of 60–100 °C. However, the ABW-type zeolite co-crystallized in the composition of Li₂O/Al₂O₃ of 2.0–3.0 above 90 °C. The crystal morphology of Li-EDI was a prism shape. The average particle size of Li-EDI is 0.69 μm in length and 0.23 μm in width. The crystal structure of the Li-EDI collapsed at 300 °C, which indicated that the thermal stability of Li-EDI is significantly lower than that of the Linde F zeolite, which is stable up to 1000 °C.     

Crystal structure and microwave dielectric properties of Li2Mg0.6− xCoxZn0.4SiO4 ceramic for LTCC applications

In this work, Li₂Mg_0.6−xCo_xZn_0.4SiO₄ ceramics (x = 0–0.4) added with 3 wt% Li₂O–B₂O₃–Bi₂O₃–SiO₂ (LBBS) glass were synthesised using the solid-state reaction method. The effects of substituting Co²⁺ for Mg²⁺in Li₂Mg_0.6−xCo_xZn_0.4SiO₄ ceramics on crystal structure, microstructure, densification, crystallisation and microwave dielectric properties were investigated. X-ray diffraction patterns showed that monoclinic Li₂MgSiO₄, monoclinic Li₂ZnSiO₄ and orthorhombic Li₂CoSiO₄ formed finite solid solution in Li₂Mg_0.6−xCo_xZn_0.4SiO₄ ceramics. Clear grain boundaries were observed via scanning electron microscopy. The substitution of Co²⁺ for Mg²⁺ increased grain size, densification, crystallinity degree and dielectric constant; it also reduced the dielectric loss of the ceramics to a certain extent. The absolute values of τ_f were positively related to the crystallinity degree. Li₂Mg_0.55Co_0.05Zn_0.4SiO₄ ceramic added with 3 wt% LBBS and sintered at 900 °C exhibited considerable microwave dielectric properties of ε_r = 5.8, Q × f = 47,518 GHz and τ_f = −74.8 ppm/°C. Therefore, the ceramic is considered a candidate low-temperature co-fired ceramic material for substrate and filter applications.