Effect of preparation conditions on mechanical,dielectric and microwave absorption properties of SiC fiber/mullite matrix composite

Silicon carbide fiber-reinforced mullite matrix (SiC_f/Mu) composites were fabricated via an infiltration and sintering method. Effects of sintering parameters on microstructure, mechanical, dielectric and microwave absorption properties of SiC_f/Mu composites have been investigated. The flexural strength is significantly improved with increasing sintering temperature, and the highest flexural strength of 213?MPa is obtained in vacuum at 1000?°C for 2?h. The performances of composites with different holding time are further studied at 1000?°C. The flexural strengths of composites sintered at 1000?°C for 2 and 4?h reach 213 and 219?MPa, respectively. The failure displacement of the composite sintered at 1000?°C for 4?h reaches 0.39?mm. The excellent microwave absorption properties are achieved for the composite sintered at 1000?°C for 2?h. The minimum reflection loss (RL) reaches ?38?dB with a thickness of 2.9?mm?at 12?GHz and the effective absorbing bandwidth (RL?≤??10?dB) with a thickness of 3.4?mm covers the whole X?band, which indicate that SiC_f/Mu composite is a good candidate for microwave absorbing materials. These results provide valuable solutions to obtaining structural-functional materials for microwave absorption applications in civil and military areas.     

Characterization of 3Y-TZP/TiO2 hybrid experimental dental ceramics

The addition of titania to zirconia dental implants has been considered a promising choice to improve its bioactivity. This study aimed to evaluate the effect of different sintering conditions on the microstructure, density, optical properties and flexural strength of a 3Y-TZP/TiO₂ dental ceramic based on zirconia with two different titania contents (7.5 mol% and 12.5 mol%). 3Y-TZP/TiO₂ ceramic powders were synthesized by coprecipitation, uniaxially pressed and sintered at six different sintering conditions. Microstructural analysis of the sintered samples was performed by scanning electron microscopy and X-ray diffraction. Optical properties were measured using a spectrophotometer. The density was determined by Archimedes principle. Flexural strength was estimated by the biaxial flexure device. The microstructure and flexural strength of the 3Y-TZP/TiO₂ dental ceramic with 7.5% and 12.5 mol% were affected by the sintering conditions. Sintering the specimens at 1460 °C for 2 h increased the grain size and significantly decreased the flexural strength of 3Y-TZP/TiO₂ dental ceramic. The interaction (titania content x sintering conditions) affected the relative density and optical properties. A relative density greater than 98% was achieved for the T7.5 groups (sintered at 1260 °C/1 h, 1300 °C/1 h and 1300 °C/2 h) and for the T12.5 groups (sintered at 1260 °C/1 h, 1260 °C/4 h, 1300 °C/1 h and 1300 °C/2 h). The highest values of L*, a* and b* were respectively 87.2 (T7.5 group sintered at 1460 °C/2hs), 4.3 (T12.5 group sintered at 1300 °C/2hs) and 15.8 (T12.5 group sintered at 1300 °C/1 h). The material developed with 12.5 mol% of titania and sintered at 1300 °C/2 h showed high densification, flexural strength of 670 MPa and has good potential to be used in dentistry.     

Effect of two-step sintering on the hydrothermal ageing resistance of tetragonal zirconia polycrystals

The effects of two-step sintering (TSS) on the mechanical properties and hydrothermal ageing resistance of yttria-stabilized tetragonal zirconia polycrystals (Y-TZP) were investigated. In TSS, the first step involved heating the samples up to 1400 °C at a heating rate of 10 °C/min and holding the samples at this temperature for 1 min. The second step involved sintering by cooling the samples down to 1200 °C and holding the samples at this temperature for various holding times (t) ranging from 0 to 30 h before cooling to room temperature. Moreover, TSS promoted densification with increasing holding time without sacrificing the mechanical properties of the sintered body and causing abnormal grain growth. The average grain size was found not to be affected by the long holding times, and the final microstructure composed of a uniformly distributed tetragonal grain having sizes ranging from 0.24 to 0.26 µm. The beneficial effect of TSS in suppressing the hydrothermal ageing of Y-TZP has been revealed in the present work. In particular, samples sintered at t=20 and 30 h exhibited excellent resistance to low-temperature degradation when exposed to superheated steam at 180 °C, attributed mainly to the enhance densification of the sintered bodies.     

Mechanical characterisation and hydrothermal degradation of Al2O3-15 vol% ZrO2 nanocomposites consolidated by two-step sintering

The objective of this work was to study two-step sintering as a means of controlling the microstructure of Al₂O₃ matrix nanocomposites containing nanometric inclusions of ZrO₂ 15% by volume and evaluate its hydrothermal degradation as function of time and its mechanical properties. Powders of Al₂O₃ and ZrO₂ were prepared and compacted by means of isostatic pressing and sintering in different heating cycles. The results showed that two-step sintering allowed a more efficient microstructural control than single-step sintering, resulting in good mechanical properties. The studied nanocomposites showed excellent resistance to hydrothermal degradation compared to commercial ZrO₂ and ZrO₂ TZ-3Y-E.     

Effect of Glass Addition on the Microwave Dielectric Properties of CaMgSi2O6 Ceramics

CaMgSi₂O₆ (CMS) ceramics prepared by the solid-state ceramic route have a sintering temperature of 1300°C/2 h. The sintering temperature of CMS was reduced below the melting point of Ag using low-melting LBS and LMZBS glasses. In the case of CMS+15 wt% LMZBS sintered at 900°C/2 h, the dielectric properties obtained were ɛ_r=8.2, Q_u×f=32,000 GHz (10.15 GHz), and τ_f=–48 ppm/°C. The CMS+15 wt% LBS composite, sintered at 925°C/2 h, showed ɛ_r=8, Q_u×f=15,000 GHz (10.17 GHz), and τ_f=–49 ppm/°C. The chemical compatibility of Ag with the ceramic–glass composites was also investigated for low-temperature co-fired ceramic applications.     

Fabrication and characterization of Nb2O5-doped 3Y-TZP materials sintered by microwave technology

The purpose of this research is focused on the manufacture and characterization of a partially stabilized zirconia ceramic with 3 mol% of Yttria and doped with .5 and 1.5 mol% of Nb₂O₅ to analyze the influence of doping, with the purpose of improving the properties before hydrothermal degradation. In the first instance, the microwave sintering process was used for the consolidation of this material, then the physical and mechanical properties were characterized. Together, the results obtained by the conventional sintering process were compared. A low hydrothermal degradation study (LTD) is presented at low temperatures in which possible changes in the mechanical properties of the ceramic materials are analyzed and its influence on the phase transformation that zirconia may present is observed. The mechanical properties were evaluated through hardness, fracture toughness, and Young's modulus tests. Likewise, their density was analyzed, and microstructure was characterized by FESEM. It was found that the microwave-sintered samples at 1200°C exhibited superior properties of toughness than even samples sintered by conventional methods at higher temperatures (1400°C). The sample of 3Y-TZP with 1.5 mol% Nb₂O₅ sintered by microwave with <.2% of porosity achieved a maximum fracture toughness value around 40% higher than the dense monolithic 3Y-TZP material.     

Development and evaluation of TiB2–AlN ceramic composites sintered by spark plasma

Titanium diboride (TiB₂) is a ceramic material with high mechanical resistance, chemical stability, and hardness at high temperatures. Sintering this material requires high temperatures and long sintering times. Non-conventional sintering techniques such as spark plasma sintering (SPS) can densify materials considered difficult to sinter. In this study, TiB₂–AIN (aluminum nitride) composites were sintered by using the SPS technique at different sintering temperatures (1500 °C, 1600 °C, 1700 °C, 1800 °C, and 1900 °C). x-ray diffraction was used to identify the phases in the composites. mechanical properties such as hardness and indentation fracture toughness was obtained using a vickers indenter. Different toughening mechanisms were identified, and good densification results were obtained using shorter times and lower temperatures than those previously reported.     

Effect of manganese addition on sintering behavior and mechanical properties of alumina toughened zirconia

The effect of MnO₂ additives on the sintering behavior and mechanical properties of alumina-toughened zirconia (ATZ, with 10 vol% alumina) composites was investigated by incorporating different amounts of MnO₂ (0, 0.5, 1.0, and 1.5 wt%) and sintering at various temperatures ranging from 1300 to 1450 °C. The addition of MnO₂ up to 1.0 wt% improved the sintered density, hardness, flexural strength, and fracture toughness of the composite. However, the addition of 1.5 wt% MnO₂ degraded the relative density, hardness, and flexural strength of the composite due to the transformation of the ZrO₂ phase from tetragonal to monoclinic and grain coarsening. Optimal results were obtained with 1.0 wt% MnO₂ and sintering at 1450 °C, which improved the mechanical properties (hardness: 13.5 GPa, flexural strength: 1.2 GPa, fracture toughness: 8.5 MPa m^1/2) and lowered the sintering temperature compared to the conventional sintering temperature of ATZ composites (1550 °C). Thus, the ATZ composite doped with MnO₂ is a promising material for structural engineering ceramics owing to its improved mechanical properties and lower sintering temperature.     

In-situ formation of Al2O3/Al core-shell from waste material: Production of porous composite improved by graphene

Aluminum dross produced from aluminum industry was used to fabricate Al₂O₃/Al porous composites. The dross was milled for 20?h to obtain nano powder. The milled material was examined by TEM and XRD. Graphene (up to 4?wt%) was mixed with the dross and utilized to reinforce sintered composites. The milled powders were compacted then fired at various temperatures up to 700?°C. Physical properties in terms of bulk density and apparent porosity for sintered composites were tested using Archimedes method. SEM attached by energy dispersive spectrometer (EDS) was used to inspect microstructure and elemental analysis of sintered composites. Microhardness and compressive strength were also measured. Ultrasonic nondestructive technique was utilized to examine the elastic moduli. Electrical conductivity of sintered composite was also studied. During milling up to 20?h, Al₂O₃/Al core-shell was in-situ formed with size of 65.9 and 23.8?nm, respectively. The apparent porosity of sintered composites was improved with rising graphene percent while it decreased with increasing sintering temperature. Increasing of graphene mass percent and firing temperature led to remarkable increase in all mechanical properties and electrical conductivity. The maximum compressive strength, hardness, elastic modulus and electrical conductivity were 200?MPa, 1200?MPa, 215?GPa and 1.42?×?10^?5 S/m, respectively, obtained for composite sintered at 700?°C having 4?wt% graphene.     

Improvement of wetability,sinterability, mechanical and electrical properties of Al2O3-Ni nanocomposites prepared by mechanical alloying

The wetability improvement and particle size reduction of alumina/Ni composites through mechanical alloying were addressed. Their effect on the sinterability (at high temperature), mechanical and electrical properties were studied. Al₂O₃ matrix nanocomposites reinforced with different volume fractions of Ni up to 10 vol% were prepared by mechanical alloying. The milled powders were cold pressed and sintered at different firing temperatures up to 1600 °C. The morphology of powders and the microstructure of sintered bodies were investigated by transmission electron microscopy (TEM) and scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS), respectively. Furthermore, relative density, apparent porosity, mechanical properties and electrical resistivity of the sintered composites were investigated. The results revealed that Al₂O₃ matrix was successfully coated with Ni thin film through mechanical alloying; the thickness of coat was increased with increasing the Ni content. Moreover, the increasing of both Ni content and sintering temperature up 1600 °C, led to a remarkable increase in the relative density and facture toughness of the sintered specimen. On the other hand, microhardness and elastic modulus were decreased with increasing of Ni content, while they increased significantly with the increase of sintering temperature. The electrical resistivity was decreased with increasing Ni content and sintering temperature.     

Effect of molding pressure on structural and densification behavior of microwave-sintered ceramic tool material

The die-pressed Al₂O₃-based ceramic compacts for microwave sintering were prepared using uniaxial molding pressure. Effect of molding pressure on density distribution, microstructure, and mechanical properties of both green and sintered compacts were studied by simulation and experiments. The results suggested that the density distribution of green compact showed obvious stratification phenomenon as the pressure increased. High pressure could increase the density of green compact but led to large density variation. Cracks were formed within the sintered compact due to the severe stress concentration at high molding pressure. Better mechanical properties were obtained at the pressure of 200-300°MPa. The optimal mechanical properties of Al₂O₃/Ti(C,N) ceramic tool were obtained at 1550°C with the soaking time of 10 minutes, which were as high as that of conventional sintering, but the sintering period was sharply shortened.     

Effect of Ga2O3 on Sintering and Phase Stability of Sc2O3‐Doped Tetragonal Zirconia Prepared via Aqueous Solution Route

The effects of the presence of Ga₂O₃ on low‐temperature sintering and the phase stability of 4, 5, and 6 mol% Sc₂O₃‐doped tetragonal zirconia ceramics (4ScSZ, 5ScSZ, and 6ScSZ, respectively) were investigated. A series of zirconia sintered bodies with compositions (ZrO₂)_0.99?x(Sc₂O₃)_x(Ga₂O₃)_0.01, x = 0.04, 0.05, and 0.06 was fabricated by sintering at 1000°C to 1500°C for 1 h using fine powders that were prepared via the combination of homogeneous precipitation method and hydrolysis technique using monoclinic zirconia sols synthesized through the forced hydrolysis of an aqueous solution of zirconium oxychloride at 100°C for 168 h. The presence of 1 mol% Ga₂O₃ was effective in reducing sintering temperature necessary to fabricate dense bodies and enabled to obtain dense sintered bodies via sintering at 1100°C for 1 h. The phase stability, that is, low‐temperature degradation behavior of the resultant zirconia ceramics was determined under hydrothermal condition. The zirconia ceramics codoped with 1 mol% Ga₂O₃ and 6 mol% Sc₂O₃ (1Ga6ScZ) fabricated via sintering at 1300°C for 1 h showed high phase stability without the appearance of monoclinic zirconia phase, that is the tetragonal‐to‐monoclinic phase transformation was not observed in the 1Ga6ScZ after treatment under hydrothermal condition at 150°C for 30 h.     

Fabrication of Si3N4 ceramics with high thermal conductivity and flexural strength via novel two-step gas-pressure sintering

Si₃N₄ ceramic substrates serving as heat dissipater and supporting component are required to have excellent thermal and mechanical properties. To prepare Si₃N₄ with desirable properties, a novel two-step gas-pressure sintering route including a pre-sintering step followed by a high-temperature sintering step was devised. The effects of pre-sintering temperature (1500 – 1600 °C) on the phase transformation, microstructure, thermal and mechanical properties of the samples were studied. The pre-sintering temperature played an important role in adjusting the Si₃N₄ particles’ rearrangement and α→β transformation rate. Furthermore, the densification process for the Si₃N₄ ceramics prepared via the two-step gas-pressure sintering was revealed. After sintered at 1525 °C for 3 h followed by a high-temperature sintering at 1850 °C for another 3 h, the prepared Si₃N₄ compact with a bimodal microstructure presented the highest thermal conductivity and flexural strength of 79.42 W·m^?1·K^?1 and 801 MPa, respectively, which holds great application prospects as ceramic substrates.     

Two-step sintering of Sm2O3 doped ceria stabilized zirconia

Effect of Sm₂O₃ addition and two-step sintering of Ceria Stabilized Zirconia (CSZ) on microstructure and mechanical properties were investigated in the present work. Samaria doped CSZ (SmCSZ) nanopowders were prepared by co-precipitation synthesis from their respective nitrate salts. Synthesized powders were calcined at 1000?°C for 2?h and then compacted to ?10?mm pellets using a uniaxial hydraulic press. Single step & two-step sintering methods were used to sinter the compacted pellets. Powders and sintered pellets were characterized for phase and microstructure using X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) technique. Rietveld method was used for quantification of obtained phases. The hardness of the sintered samples was evaluated by Vicker's hardness tester, and toughness was estimated by indentation fracture toughness method. Samples sintered using two-step sintering method shown optimum hardness and toughness (up to 1288 HV10 and 5.37?MPa?m^1/2) values compared to conventionally sintered samples because of reduced grain size.     

Effect of zirconia content on mechanical and thermal properties of mullite–zirconia composite

Abstract

Mullite–zirconia composites were prepared by adding various zirconia contents in the mullite ranging from 0 to 30 wt-% and sintering at 1400–1600°C for 2 h. The phase composition examined by X-ray diffraction showed that mullite was the major phase combined with developed t-ZrO₂ and m-ZrO₂ phase as a function of zirconia content, especially at 1600°C, wherein m-ZrO₂ predominated. Density increased when the zirconia content and sintering temperature were increased ranging from 2·2 to 3·53 g cm^?3. The morphology of mullite grain showed elongated grains, whereas dispersed zirconia showed equiaxed and intergranular grains. Flexural strength was continuously improved by adding zirconia during the sintering temperature ranging from 1400 to 1500°C, whereas flexural strength was initially improved up to 5 wt-% of zirconia addition and deteriorated with more than 5 wt-% of zirconia content during sintering between 1550 and 1600°C. The maximum strength, 190 MPa, was obtained when sintering mullite with 30 wt-% of zirconia content at 1500°C. The degradation of strength at high sintering temperature may be a result from more occurrence of m-ZrO₂ phase. Thermal expansion of sintered specimens indicated linear change and hysteresis loop change. The hysteresis loop obtained with increased zirconia content resulted in the t–m phase transformation. Martensitic start temperature M_s was determined to be 530°C for 15 wt-% zirconia sintered at 1500°C, implying that the t–m phase transformation occurred.     

Fine grained Al2O3/SiC composite ceramic tool material prepared by two-step microwave sintering

Fine-grained Al₂O₃/SiC composite ceramic tool materials were synthesized by two-step microwave sintering. The effects of first-step sintering temperature (T1), content and particle size of SiC on the microstructure and mechanical properties were studied. It was found that the sample with higher content of SiC was achieved with finer grains, and the incorporation of SiC particles could bridge, branch and deflect the cracks, thus improving the fracture toughness. Higher T1 was required for the densification of the samples with higher content of SiC (>5?wt%). The sample containing 3?wt% SiC particles with the mean particle size of 100?nm, which was sintered at 1600?°C (T1) and 1100?°C (T2) for 5?min had the fine microstructure and optimal properties. Its relative density, grain size, Vickers hardness and fracture toughness obtained were 98.37%, 0.78?±?0.31?μm, 18.40?±?0.24?GPa and 4.97?±?0.30?MPa?m^1/2, respectively. Compared to the sample prepared by single-step microwave sintering, although near full densification can be achieved in both two methods, the grain size was reduced by 36% and the fracture toughness was improved by 28% in two-step microwave sintering.     

Two-step sintering technique for enhancing mechanical and oxygen permeation properties of dual-phase oxygen transport membranes

The present work involved the application of a two-step sintering (TSS) technique for typical Ce_0.9Gd_0.1O_2?δ–La_0.6Sr_0.4Co_0.2Fe_0.8O_3–δ (GDC–LSCF) composites and its effect on the microstructure and resultantly mechanical and O₂-permeating properties. The samples obtained by conventional sintering (CS) performed at 1100, 1250, and 1400 °C for 3 h exhibited maximum flexural strength and hardness values of 142 MPa and 8.71 GPa, respectively. However, the application of a TSS procedure produced fine-grained microstructures with improved mechanical properties. In particular, with the use of a typical 1250/1200 TSS protocol, increases of approximately 31 % and 7% in the flexural strength and hardness values, respectively, were observed compared to those obtained using the CS method. Moreover, thick-film (～ 60 μm) GDC–LSCF membrane prepared by tape casting and the TSS technique showed remarkably 1.5–2 times higher oxygen permeation flux than membrane sintered by CS method. The results are discussed and explained in detail.     

Effects of TiN addition on the properties of hot pressed TiN–Ti/Al2O3 composites

TiN–Ti/Al₂O₃ composites of varying TiN content (0–20?vol%) were prepared by vacuum hot-pressing sintering at different temperatures (1400?°C and 1500?°C) to investigate how TiN affected the mechanical properties and electrical conductivity of the composites. Sintered samples with added TiN exhibited better performance than those without it. The sample with 20?vol% TiN sintered 1500?°C had an optimal relative density of 99.49, Vickers hardness of 14.94?GPa, flexural strength of 321.55?MPa, and electrical resistivity of 1474.7?μΩ?cm. However, this increased temperature did not improve the best sample resistivity of 930.3?μΩ?cm, which was obtained at 1400?°C. Form SEM images and XRD patterns, the positive effect of TiN on composite mechanical properties may be ascribed to its good performance of high hardness and strength, a decrease of the brittle intermetallic phase, the form of AlTi₃N, and the impact of the fine-grained strength of the TiN phase.     

Electrical properties of lead-free 0.98(Na<Subscript>0.5</Subscript>K<Subscript>0.5</Subscript>)NbO<Subscript>3</Subscript>-0.02Ba(Zr<Subscript>0.52</Subscript>Ti<Subscript>0.48</Subscript>)O<Subscript>3</Subscript> piezoelectric ceramics by optimizing sintering temperature

Lead-free 0.98(Na_0.5K_0.5)NbO₃-0.02Ba(Zr_0.52Ti_0.48)O₃ [0.98NKN-0.02BZT] ceramics were fabricated by the conventional mixed oxide method with sintering temperature at 1,080°C to 1,120°C. The results indicate that the sintering temperature obviously influences the structural and electrical properties of the sample. For the 0.98NKN-0.02BZT ceramics sintered at 1,080°C to 1,120°C, the bulk density increased with increasing sintering temperature and showed a maximum value at a sintering temperature of 1,090°C. The dielectric constant, piezoelectric constant [d ₃₃], electromechanical coupling coefficient [k _p], and remnant polarization [P _r] increased with increasing sintering temperature, which might be related to the increase in the relative density. However, the samples would be deteriorated when they are sintered above the optimum temperature. High piezoelectric properties of d ₃₃ = 217 pC/N, k _p = 41%, dielectric constant = 1,951, and ferroelectric properties of P _r = 10.3 μC/cm² were obtained for the 0.98NKN-0.02BZT ceramics sintered at 1,090°C for 4 h.     

Combined role of SiC particles and SiC whiskers on the characteristics of spark plasma sintered ZrB2 ceramics

In this research work, the effects of silicon carbide (SiC) as the most important reinforcement phase on the densification percentage and mechanical characteristics of zirconium diboride (ZrB₂)-matrix composites were studied. In this way, a monolithic ZrB₂ ceramic (as the baseline) and three ZrB₂ matrix specimens each of which contains 25 vol% SiC as reinforcement in various morphologies (SiC particulates, SiC whiskers, and a mixture of SiC particulates/SiC whiskers), have been processed through spark plasma sintering (SPS) technology. The sintering parameters were 1900 °C as sintering temperature, 7 min as the dwell time, and 40 MPa as external pressure in vacuum conditions. After spark plasma sintering, a relative density of ~96% was obtained (using the Archimedes principles and mixture rule for evaluation of relative density) for the unreinforced ZrB₂ specimen, but the porosity of composites containing SiC approached zero. Also, the assessment of sintered materials mechanical properties has shown that the existence of silicon carbide in ZrB₂ matrix ceramics results in fracture toughness and microhardness improvement, compared to those measured for the monolithic one. The simultaneous addition of silicon carbide particulates (SiC_p) and whiskers (SiC_w) showed a synergistic effect on the enhancement of mechanical performance of ZrB₂-based composites.