Microstructure and flexural strength of the Y:TZP/BG composite

The addition of bioactive glasses to a Y:TZP matrix represents a feasible alternative to provide bioactivity to this material and optimize osseointegration. This work evaluated the effect of the BG concentration (0 and 10 wt%) and the sintering temperature (1200°C and 1300°C) on the microstructure, relative density, and flexural strength of the composite Y:TZP/BG. The Y:TZP and Y:TZP/BG powders were uniaxially pressed and sintered at 1200°C or 1300°C for 1 h. The microstructure was characterized by X-ray diffraction analysis, scanning electron microscopy, and energy-dispersive X-ray Spectroscopy. Relative density was calculated from density values obtained using the Archimedes’ principle. For the flexural strength, specimens (n = 6) were fractured in a biaxial flexural setup using a piston-on-three-balls fixture in a universal testing machine. Bioactivity test was performed in simulated body fluid solution. The results suggested that BG addition decreased the grain size of the composite, increased porosity and caused a significant decrease in the relative density and flexural strength. Crystalline phases of calcium stabilized cubic zirconia and sodium zirconium silicate were formed after the addition of BG. Finally, it was concluded that composite specimens sintered at 1300°C showed the highest density values and larger grains compared to those sintered at 1200°C.     

Hydrothermal Degradation Behavior of Y‐TZP Ceramics Sintered by Nonconventional Microwave Technology

Different factors such as the characteristics of starting powders, their processing, the sintering technique and the final sintering temperature were assessed with the goal to improve the low‐temperature degradation (LTD) resistance of 3Y‐TZP materials without compromising on the mechanical properties. The degradation of hydrothermally treated specimens was studied by AFM, nanoindentation technique, micro‐Raman spectroscopy, and electron microscopy. 3Y‐TZP previously prepared in laboratory by colloidal processing, and sintered by microwave method at low temperature (1200°C) led to excellent mechanical and LTD resistance, as compared to dental restorations based on Y‐TZP commercial material. In the former, the presence of m‐phase was almost nonexistent even after 200 h of exposure to LTD conditions and the initial mechanical properties were maintained, giving 16 and 250 GPa mean values for hardness and Young's modulus, respectively. The influence of the fast‐technology by microwave heating is presented with a nonconventional sintering method to fabricate 3Y‐TZP ceramics for dental application with very high resistance against LTD and optimized mechanical properties.     

Effect of surface treatments and aging on phase transformation and flexural strength of different Y-TZP ceramics

This study aimed to evaluate the influence of surface treatments and artificial aging on surface roughness (Ra), phase transformation, and flexural strength of yttria-stabilized tetragonal zirconia polycrystalline (Y-TZP) ceramics. Two-hundred and eighty specimens from four types of Y-TZP were divided into seven groups, according to the surface treatments and aging used: control, air-abrasion, air-abrasion + aging, grinding, grinding + aging, erbium: yttrium-aluminum-garnet (Er:YAG) laser, Er:YAG laser + aging. The Ra values were measured using a profilometer. X-ray diffraction (XRD) analysis was performed to determine phase transformation. Specimens were subjected to a three-point bending test and loaded until fracture. Scanning electron microscope (SEM) and atomic force microscope (AFM) analyses were performed on one specimen per group. Grinding and air-abrasion groups exhibited higher Ra values than the others (P < 0.05). The differences in the roughness and flexural strength values between the laser and control groups were not significant. For all materials, the highest amount of monoclinic phase was found after air-abrasion. Grinding groups showed lower flexural strength values compared with the control groups (P < 0.05), while there was no significant difference between the control and air-abrasion groups. Aging did not affect the roughness and flexural strength (P > 0.05). The grinding process is not recommended in clinical usage for Y-TZP because of the remarkable decrease in flexural strength and reliability.     

Effect of High‐Temperature Aging on the Fracture Toughness of 40 mol% Ceria‐Stabilized Zirconia

The 40 mol% CeO₂‐stabilized ZrO₂ ceramic was synthesized by the sol‐spray pyrolysis method and aged at 1400°C–1600°C. The effects of high‐temperature aging on its fracture toughness were investigated after heat treatments at 1500°C for 6–150 h in air. Characterization results indicated that the activation energy for grain growth of 40 mol% CeO₂‐stabilized ZrO₂ was 593 ± 47 kJ/mol. The average grain size of this ceramic varied from 1.4 to 5.6 μm within the aging condition of 1500°C for 6–150 h. The Ce‐lean tetragonal phase has a constant tetragonality (ratio of the c‐axis to a‐axis of the crystal lattice) of 1.0178 during the aging process. It was found that the fracture toughness of 40 mol% CeO₂‐stabilized ZrO₂ was determined to be 2.0 ± 0.1 MPa·m^1/2, which did not vary significantly with prolonging aging time. Since no monoclinic zirconia was detected in the regions around the indentation crack‐middle and crack‐tip, the high fracture toughness maintained after high‐temperature aging can be attributed to the remarkable stability of the tetragonal phase in 40 mol% CeO₂‐stabilized ZrO₂ composition.     

Rapid Grain Growth in 3Y‐TZP Nanoceramics by Pressure‐Assisted and Pressure‐Less SPS

Pressure‐less spark plasma sintering (SPS) is a new approach during which rapid densification of ceramic nanopowder green bodies is accompanied by rapid grain growth. Although the origin of this phenomenon has not yet been fully understood significant, difference in grain growth between pressure‐less and pressure‐assisted SPS was expected. In this work 3Y‐TZP nanopowder with average particle size of 12 nm was consolidated using two‐step approach: (1) at an intermediate temperature (600°C to 1000°C) SPS warm pressing followed by (2) high temperature (1400°C to 1600°C) pressure‐less SPS. The standard one step pressure‐assisted SPS experiments were quoted as references. Rapid grain growth was observed during both pressure‐less and standard SPS. The samples prepared by both approaches at the same sintering temperature (1400°C–1600°C) achieved identical grain size and grain size distribution, if large pores were eliminated in early stage by SPS warm pressing. The electric current, electromagnetic field, and mechanical pressure is proven to have a negligible direct influence on grain growth in 3Y‐TZP ceramics at temperatures above 1000°C under standard SPS conditions.     

Preparation of Transparent 3Y‐TZP Nanoceramics with No Low‐Temperature Degradation

The progresses of the relative density, average grain size (GS), and maximum pore size entering into the final sintering stage are investigated in 3 mol% yttria‐stabilized tetragonal zirconia polycrystals (3Y‐TZP) compacts in the range of 87%~99% theoretical density. It is found that during conventional pressureless sintering, the pores in the compact enlarged dramatically, which appears to be the major obstacle for preparing fully dense nanoceramics. Transparent 3Y‐TZP nanoceramics with an average GS of 87 nm were prepared by exploiting microstructural refinement on nanoscale. The yields a maximal optical transmittance of 67% and shows no noticeable low‐temperature degradation after 100 h aging at 134°C under a hydrothermal pressure of two bars.     

3Y-TZP材料的液相烧结

通过在3Y-TZP(Tetragonal Zirconia Polycrystals stabilized with 3mol% Y2O3)中加入适当含量的硅酸盐玻璃添加剂,使其烧结温度明显降低,并且制备出具有细晶粒、高强度的四方相氧化锆增韧陶瓷材料.本文分析了添加剂对3Y-TZP材料烧结特性及显微结构的影响.发现液相烧结的3Y-TZP具有良好的抗弯强度,但韧性有待于提高.     

Effect of filler addition and weathering conditions on the performance of PVC/CaCO3 composites

This study deals with the effects of calcium carbonate (CaCO₃) fillers and hygrothermal aging on the performance of polyvinylchloride (PVC). The properties of the PVC/CaCO₃ composite were studied before and after aging in water up to 3 months at 24°C ± 3°C, 70°C, and 90°C. In terms of fillers effect, it was found that the incorporation of fillers in PVC induces an increase in both T_g value and storage modulus; however, it had no significant effect on the water absorption. However, the addition of fillers has resulted in an improvement in the elastic modulus, whereas it has shown harmful effect on the tensile strength and elongation at break. Concerning flexural properties, an important filler percentage, that is, 35 wt%, is proved to be the optimum content to achieve maximum strength and modulus as well as wear properties. In terms of aging impact, it was found that shift in color on aging occurs noticeably. Elastic modulus, tensile strength, flexural strength, and flexural modulus increase with increasing temperature from ambient to 70°C, whereas they decrease at 90°C. Dynamic mechanical thermal analysis confirmed that at high temperature, the absorbed water affects the PVC matrix during aging. As a result, a loss in strength and stiffness but a gain of ductility was observed. The great quantity of absorbed water acts as a barrier layer and, thus, minimizes the wear. POLYM. COMPOS., 37:2171–2183, 2016. © 2015 Society of Plastics Engineers     

Effect of MgF2 addition on sinterability and mechanical properties of fluorapatite ceramic composites fabricated by wollastonite and phosphate glass

In this paper, we successfully report the design and synthesis of fluorapatite ceramic composites using phosphate glass and wollastonite as raw materials via a simple sintering method. The effects of MgF₂ additives in phase composition, microstructure, densification, and mechanical properties are investigated at various temperatures from 600 °C to 900 °C, and characterized by SEM/EDS, XRD, FTIR, linear shrinkage and water absorption, flexural strength analysis. It shows that the densification and mechanical behavior of composites increase with both the sintering temperature and MgF₂ content. Especially, the sample SCPF-7 exhibits the highest densification and optimal mechanical properties at 900 °C. At these conditions, the water absorption of fluorapatite ceramic composite is less than 0.20%, and the flexural strength is over 70 MPa. For the microstructure analysis, the formation of fluorapatite with a rod-like microstructure is enhanced with the increase of MgF₂ content. The amelioration of these properties is due to the formation of a new phase which helps to the formation of compact microstructure. The findings in this work provide a feasible strategy for the preparation of fluorapatite ceramic composites from available phosphate glass and wollastonite at a lower temperature.     

3Y‐TZP In‐Depth Phase Transformation by Raman Spectroscopy: A Comparison of Three Methods

Zirconia phase transformation is usually studied on surface. For in‐depth study, three methods were proposed using Raman microspectroscopy quantitative evaluation: direct measurement on sample cross section, confocal Raman spectroscopy (CRS), and progressive pinhole aperture enlargement (PPAE). The aim of this study was to compare transformation profiles obtained with these three methods on the same sample. Three 3Y‐TZP samples were aged, respectively, for 25, 72, and 90 h in artificial saliva. Transformation profiles were determined with cross‐sectional measurement, CRS and PPAE. A transformation profile simulation model based on PPAE measurements is proposed, using the convolution of the excitation intensity profile and the Beer–Lambert law (optical properties of zirconia). The simulation model was validated with the determination of 3Y‐TZP transformation factor, T = 1.15 μm^?1, identical for the three aging durations. Both cross section and PPAE measured similar in‐depth transformation decrease, but with a 10 μm‐shift: transformed zirconia layer is more important in cross‐sectional protocol (36 μm with PPAE and 46 μm with cross‐sectional after 90 h aging). Complementary measurements on a 10 h aged sample, where transformation is initiated by Low‐Temperature Degradation, showed that sample preparation and polishing, necessary in the cross‐sectional method, were responsible for the higher transformation. PPAE method enables noninvasive in‐depth measurements with limited optical and mechanical biases.     

Short‐beam and three‐point‐bending tests for the study of shear and flexural properties in unidirectional‐fiber‐reinforced epoxy composites

The bending properties of composite materials are often characterized with simply supported beams under concentrated loads. The results from such tests are commonly based on homogeneous beam equations. For laminated materials, however, these formulas must be modified to account for the stacking sequence of the individual plies. The horizontal shear test with a short‐beam specimen in three‐point bending appears suitable as a general method of evaluation for the shear properties in fiber‐reinforced composites because of its simplicity. In the experimental part of this work, the shear strength of unidirectional‐glass‐fiber‐reinforced epoxy resin composites was determined in different fiber directions with the short‐beam three‐point‐bending test. Also, the elastic constants and flexural properties of the same materials were determined from bending experiments carried out on specimens in the 0, 15, 30, 45, 60, 75, and 90° fiber directions with high span–thickness ratios. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 63–74, 2004     

Recycling of extracted titanium slag and gold tailings for preparation of self-glazed ceramic foams

Self-glazed ceramic foams were successfully synthesized via powder sintering method, using extracted titanium slag (ETS) and gold tailings (GT) as raw materials without adding any sintering aids and foaming agents. Influence of ETS addition and sintering temperature on crystal phase evolution, physical–mechanical properties, and micro-morphology of ceramic foams was systematically studied. Results indicated that products sintered at 1180 °C with 30 wt% ETS and 70 wt% GT showed the best performance, i.e., bulk density of 1.66 g cm^?3, flexural strength of 20.4 MPa, water absorption of 0.14%, open porosity of 0.23%, and glaze Vickers hardness of 6.5 GPa. Moreover, it was observed that there existed strong correlation between bulk density and bending strength. Self-glazed ceramic foams developed in this study are expected to be used as building envelope materials and provide new ideas for effective reuse of other similar solid wastes.     

Dolomite,wollastonite and calcite as different CaO sources in anorthite-based porcelain

Anorthite-based porcelain was fabricated by using ball clay, quartz, alumina, feldspar and three different sources of CaO as raw materials. The effect of CaO sources such as dolomite, wollastonite and calcite on the mechanical, thermal and aesthetical properties of anorthite-based porcelain was investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies were also carried out to analyze the microstructure. Anorthite was formed as major phase in all the samples fired at their optimum sintering temperatures (1200, 1215 and 1230 °C). The sample with dolomite had the highest bulk density but the smallest flexural strength due to formation of substantial glassy phase. The maximum flexural strength (～110 MPa) was reached in the sample containing wollastonite, which was mainly attributed to the favorable microstructure. Anorthite as the single crystalline phase was found in the sample with calcite and the sample showed the lowest thermal expansion coefficient and the highest whiteness, which was similar to bone china in appearance.     

Mechanical properties of solid oxide fuel cell glass-ceramic sealants in the system BaO/SrO-MgO-B2O3-SiO2

Planar solid oxide fuel cells (p-SOFCs) require materials that can satisfy the high mechanical demands related to their utilization in stationary and, especially, in mobile applications. Two suitable glass-ceramic sealants based on the system BaO/SrO-MgO-B₂O₃-SiO₂ have been characterized with respect to their mechanical properties such as hardness, Young’s modulus, flexural strength at room and elevated temperature, fracture toughness as well as creep behavior at relevant operation temperatures (800 °C). Fracture toughness was calculated from crack opening displacements (COD) and the results were compared with fracture toughness measured by bending tests of notched bar samples. The mechanical behavior has been discussed regarding different thermal aging times of the glass-ceramics and their microstructural evolution. The glass-ceramics containing SrO revealed a better mechanical behavior than glass-ceramics with BaO. In particular, several superior properties were found in comparison to previously reported materials for this application.     

Autonomous high‐temperature healing of surface cracks in Al2O3 containing Ti2AlC particles

In this work, the oxidation‐induced crack healing of Al₂O₃ containing 20 vol.% of Ti₂AlC MAX phase inclusions as healing particles was studied. The oxidation kinetics of the Ti₂AlC particles having an average diameter of about 10 μm was studied via thermogravimetry and/or differential thermal analysis. Surface cracks of about 80 μm long and 0.5 μm wide were introduced into the composite by Vickers indentation. After annealing in air at high temperatures, the cracks were filled with stable oxides of Ti and Al as a result of the decomposition of the Ti₂AlC particles. Crack healing was studied at 800, 900, and 1000°C for 0.25, 1, 4, and 16 hours, and the strength recovery was measured by 4‐point bending. Upon indentation, the bending strength of the samples dropped by about 50% from 402 ± 35 to 229 ± 14 MPa. This bending strength increased to about 90% of the undamaged material after annealing at 1000°C for just 15 minutes, while full strength was recovered after annealing for 1 hour. As the healing temperature was reduced to 900 and 800°C, the time required for full‐strength recovery increased to 4 and 16 hours, respectively. The initial bending strength and the fracture toughness of the composite material were found to be about 19% lower and 20% higher than monolithic alumina, respectively, making this material an attractive substitute for monolithic alumina used in high‐temperature applications.     

Ytterbia–neodymia–costabilized TZP—Breaking the limits of strength–toughness correlations for zirconia?

TZP ceramics were manufactured by hot pressing of pyrogenic zirconia nanopowder which was costabilized by 1 mol% ytterbia and 2 mol% neodymia (1Yb–2Nd–TZP) via the nitrate route. The evolution of microstructure, phase composition and mechanical properties with variation of sintering temperature from 1200 °C to 1400 °C was investigated. 1Yb–2Nd–TZP consists of a bimodal microstructure of small very transformable tetragonal grains and large cubic grains. At intermediate sintering temperature the materials combine a bending strength of 1250 MPa with a fracture resistance >13 MPa √m. The high threshold stress intensity of 7 MPa √m indicates high resistance to subcritical crack growth. An increase in fracture resistance before the crack tip induced by compressive residual stress shifts the strength–toughness correlations to higher values than previously considered possible.     

Microwave Sintering of Zirconia Materials: Mechanical and Microstructural Properties

Commercially, 3 mol% Y₂O₃‐stabilized tetragonal zirconia (70–90 nm) compacts were fabricated using a conventional and a nonconventional sintering technique; microwave heating in a resonant mono‐mode cavity at 2.45 GHz, at temperatures in the 1100–1400°C range. A considerable difference in the densification behavior between conventional (CS) and microwave (MW) sintered materials was observed. The MW materials attain a full density of 99.9% of the theoretical density (t.d.) at 1400°C/10 min, whereas the CS reach only 98.0% t.d. at the same temperature and 1 h of dwelling time. Therefore, the MW materials exhibit superior Vickers hardness values (16.0 GPa) when compared with CS (13.4 GPa).     

Mechanical behavior of SiC joints brazed using an active Ag‐Cu‐In‐Ti braze at elevated temperatures

The behavior of SiC ceramic joints brazed with commercially available Incusil ABA (Ag‐32.25Cu‐12.5In‐1.25Ti, in wt.%) was characterized especially with respect to the mechanical performance at temperatures up to 550°C using four‐point bending and torsional shear tests. The failure mechanisms with changing temperature were investigated with the aid of fractography. Additionally, the microstructure of brazed specimens was characterized in detail by high resolution scanning electron microscopy. The test geometry and setup for the high temperature torsional shear test is presented. The change in mechanical behavior of the joints as a function of temperature is shown and discussed. The brazed joints interestingly showed that flexural bending strength was maintained with only a small decrease up to 300°C. Above 300°C, the bending strength decreased much faster. For the first time, this joint system was characterized in torsional shear test at temperatures up to 550°C to achieve the intrinsic shear strength values. Very strong joints were achieved, resulting in failure through the ceramic base materials up to (torsional shear) testing temperatures of 400°C. The results indicate that SiC joints brazed with Incusil ABA exhibit excellent mechanical performance for applications up to 300°C.     

Influence of bonding phases on properties of in-situ bonded porous SiC membrane supports

Porous SiC ceramic membrane supports are widely employed in a wide variety of high-temperature applications, such as hot flue gas filtration, porous burners and molten metal filters. Herein, SiC supports, with a porosity of ~37%, were prepared by using low-temperature bonding techniques and the influence of different bonding phases, such as mullite, cordierite and glass, on ambient-temperature flexural strength, hot modulus of rupture (HMOR), thermal shock resistance and oxidation resistance were systematically investigated. The results reveal that the glass-bonded SiC (GBSC) support exhibited the highest ambient-temperature flexural strength of 33.6 MPa, whereas the flexural strength of mullite-bonded SiC (MBSC) and cordierite-bonded SiC (CBSC) supports ranged from 22 to 25 MPa. However, the presence of glass phase deteriorated the high-temperature properties of the support. MBSC support rendered superior mechanical strength at high temperature and self-strengthening in a certain temperature range, such as HMOR improved 47.5% at 900 °C, but HMOR of glass-bonded support was only 57.4% of the ambient-temperature strength. Moreover, MBSC and CBSC supports exhibited better thermal shock resistance than GBSC supports and the critical temperature difference of water quenching for MBSC supports was ~200 °C higher than GBSC supports. In addition, MBSC support rendered superior oxidation resistance and exhibited a weight gain rate of ~0.1% at 1150 °C for 24 h, which is 54.4% and 42.2% lower than CBSC and GBSC supports, respectively.     

Properties of magnesium-aluminate spinel derived from bauxite and magnesia

The synthesis of magnesium-aluminate spinel divided from bauxites and magnesias, the starting materials with different molar mass ratios (Al₂O₃: MgO) of 3, 1, and 0.6 were developed using solid-state reaction sintering at 1350-1500°C. The effects of different mass ratios and sintering temperatures on the phase composition, densification behavior, shrinkage, flexural strength, and microstructure of the synthetic materials were studied. It was found that as the relative content of bauxite decreased, the flexural strength first decreased before increasing. When n(Al₂O₃)/n(MgO) was 1, the spinel was the primary phase and the sample was dense. When the temperature became 1450°C, the flexural strength became maximized at 106.48 MPa.