Comparison between microwave and conventional sintering on the properties and microstructural evolution of tetragonal zirconia

In this research, the comparison between microwave sintering and conventional sintering on the mechanical properties and microstructural evolution of 3?mol% yttria-stabilised zirconia were studied. Green bodies were compacted and sintered at various temperatures ranging from 1200?°C to 1500?°C. The results showed that microwave assisted sintering was beneficial in enhancing the densification and mechanical properties of zirconia, particularly when sintered at 1200?°C. It was revealed that as the sintering temperature was increased to 1400?°C and beyond, the grain size and mechanical properties for both microwave- and conventional-sintered ceramics were comparable thus suggesting that the sintering temperature where densification mechanism was activated, grain size was strongly influenced by the sintering temperature and not the sintering mode.     

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.     

A new Li-based ceramic of Li4MgSn2O7: Synthesis,phase evolution and microwave dielectric properties

A pure-phase Li₄MgSn₂O₇ (L₄MS) was successfully synthesized through optimizing the calcination condition. Microwave dielectric properties of the L₄MS ceramic with the phase evolution were investigated together with its low-temperature sintering. The sample maintains a single L₄MS phase as sintered below 1200?°C, such that τ_f remains a constant value of ～12.4?ppm/°C. Accompanied by the appearance of impurity phases (Li₂SnO₃)_ss and especially (MgO)_ss at higher sintering temperatures, excellent microwave dielectric properties of ε_r?=?13.1–13.5, Q?×?f?=?106,800–126,810?GHz and τ_f ?=?0–?4.2?ppm/°C are obtained in samples sintered at 1215–1260?°C for 4?h. Reduction of sintering temperature using LiF sintering aid also helps achieve pure-phase dense L₄MS ceramic. The L₄MS?+?x wt.% LiF ceramic exhibits ε_r～13.7, Qxf～97,000?GHz (x?≤?3) and τ_f ～8–13?ppm/°C sintered at 850?°C for potential LTCC applications, and ε_r ～13.9, Qxf～146,000?GHz and τ_f ～1.5–6?ppm/°C (x?≥?4) as sintered 1000?°C, exhibiting large potentials for microwave dielectric candidates.     

Effect of microwave sintering on the properties of copper oxide doped Y-TZP ceramics

The effect of various amounts of copper oxide (CuO) up to 1?wt% on the densification behaviour and mechanical properties of 3?mol% yttria-tetragonal zirconia polycrystal (Y-TZP) were studied by using microwave (MW) sintering method. The MW sintering was performed at temperatures between 1100?°C and 1400?°C, with a heating rate of 30?°C/min. and holding time of 5?min. The beneficial effect of MW in enhancing densification was also compared for the undoped and 0.2?wt% CuO-doped Y-TZP when subjected to conventional sintering (CS) method. The results showed that significant enhancement in the relative density and Vickers hardness were observed for the undoped Y-TZP when MW-sintered between 1100?°C and 1250?°C. It was revealed that the 0.2?wt% CuO-doped Y-TZP and MW sintered at 1250–1300?°C could attain ≥?99.8% of theoretical density, Vickers hardness of about 14.4?GPa, fracture toughness of 7.8 MPam^1/2 and exhibited fine equiaxed tetragonal grain size of below 0.25?µm. In contrast, the addition of 1?wt% CuO was detrimental and the samples exhibited about 50% monoclinic phase upon sintering coupled with poor bulk density and mechanical properties. The study also revealed that the addition of 0.2?wt% CuO and subjected to conventional sintering produced similar densification as that obtained for microwave sintering, thus indicating that the dopant played a more significant role than the sintering method.     

Sintering effect on microstructural evolution and mechanical properties of spark plasma sintered Ti matrix composites reinforced by reduced graphene oxides

Ti matrix composites reinforced with 0.6?wt% reduced graphene oxide (rGO) sheets were fabricated using spark plasma sintering (SPS) technology at different sintering temperatures from 800?°C to 1100?°C. Effects of SPS sintering temperature on microstructural evolution and mechanical properties of rGO/Ti composites were studied. Results showed that with an increase in the sintering temperature, the relative density and densification of the composites were improved. The Ti grains were apparently refined owing to the presence of rGO. The optimum sintering temperature was found to be 1000?°C with a duration of 5?min under a pressure of 45?MPa in vacuum, and the structure of rGO was retained. At the same time, the reaction between Ti matrix and rGO at such high sintering temperatures resulted in uniform distribution of micro/nano TiC particle inside the rGO/Ti composites. The sintered rGO/Ti composites exhibited the best mechanical properties at the sintering temperature of 1000?°C, obtaining the values of micro-hardness, ultimate tensile strength, 0.2% yield strength of 224 HV, 535?MPa and 446?MPa, respectively. These are much higher than the composites sintered at the temperature of 900?°C. The fracture mode of the composites was found to change from a predominate trans-granular mode at low sintering temperatures to a ductile fracture mode with quasi-cleavage at higher temperatures, which is consistent with the theoretical calculations.     

The impact of microwave-assisted sintering on fabrication of cobalt ferrite nanostructure foams for gas-sensing

This study employed the Pechini-type sol-gel method to synthesize single-phase cobalt ferrite nanoparticles with almost spherical morphology and an average size of ～50 nm. The Pechini sol-gel is based on the polysterification reaction between citric acid and ethylene glycol and the formation of colloidal nanoparticles due to the polymerization of an iron-cobalt complex. Foam samples were prepared from the obtained nanoparticles by using urea as the progenic agent and subsequent conventional or microwave sintering. The average grain size values for the microwave and conventionally sintered foam samples were 90 and 280 nm, respectively. Microwave sintering has successfully hindered grain growth regarding the initial ～50 nm size of the cobalt ferrite nanoparticles. The microwave sintered foam sample showed an approximately two-fold increase in the surface area value compared to its conventionally sintered counterpart. The pore volume for the conventionally and microwave sintered samples was measured at 0.007 and 0.026 cc/g, respectively. Also, the pore diameter values were measured to be less than 2.5 nm in both samples. The pore size distribution within the microwave sintered sample was unimodal, while the conventionally sintered sample showed a bimodal one. The gas-sensing properties of the samples were examined in pure ethanol, acetone, and liquefied petroleum gas (LPG) atmospheres at different temperatures. The results indicated that for all the samples and in all the three atmospheres, the best working temperature is 300 °C. The microwave sintered foam sample showed the highest sensitivity and the shortest response time. This sample was more selective towards ethanol than the other two gases.     

Effect of segregation on particle size stability and SPS sintering of Li2O-Doped magnesium aluminate spinel

Magnesium aluminate spinel (MAS) was prepared using the simultaneous precipitation method by varying the concentration of Li₂O from 0 to 5 mol%. No residual chlorine from the LiCl precursor was detected in the final powders while Li achieved the target concentration in all samples and contributed to stabilizing nanoparticles smaller than 10 nm. Li segregation to both interfaces (surfaces and grain boundaries) occurred and tended to be more pronounced at the grain boundaries stabilizing this type of interface during processing rather than surfaces. Spark plasma sintering (SPS) was used to consolidate the nanopowders into fully dense nanostructured pellets. The increase in Li content facilitated the sintering process and pore elimination occurred at 850–900 °C, a much lower temperature range as compared to conventional sintering (1650 °C). Samples containing 5 mol% Li sintered at 850 °C exhibited a medium grain size of ?25 nm, microhardness of ?24 GPa and ?50% in-line optical transmission at the 800 nm.     

Rapid densification of SiC ceramic rollers by microwave sintering

Ultralarge silicon carbide (SiC) ceramic rollers are successfully prepared in a microwave multimode cavity at 2·45 GHz. The length of the rollers is 1220 mm with outer diameter of 62 mm and thickness of 7 mm. The optimised sintering temperature of microwave sintering is ～980°C, which is ～400°C lower than that of conventional sintering. Mullite was detected within microwave sintered samples, rather than conventional sintered ones, which preferentially appeared around SiC as well as inside the residual pores. This might be attributed to the unique features of microwave sintering of ‘hot spot effect’, plasma behaviour and high frequency electromagnetic fields.     

Microwave hybrid fast sintering of red clay ceramics

This work aimed to examine the performance of the hybrid sintering of clay ceramic in a microwave furnace, compared to the sintering process in a conventional furnace. The raw materials were subjected to X-ray fluorescence, loss on ignition (LOI), X-ray diffraction, particle size distribution, real specific mass, and thermogravimetric analyses. The red clay ceramic mass was prepared, extruded, pre-sintered in a conventional furnace at 600°C/60 min, and sintered at temperatures between 700 °C and 1100 °C. The sintering conventional (resistive oven) was carried out for 60 min with a heating rate of 10°C/min. In the microwave furnace, the sintering times were 5, 10, and 15 min, with a heating rate of 50°C/min, with a sintering chamber coated with silicon carbide (susceptor). The sintered specimens were characterized according to linear shrinkage, water absorption, apparent porosity, apparent specific mass, X-ray diffraction, Raman spectroscopy analysis, spectroscopy analysis in the ultraviolet and visible regions, microhardness, and scanning electron microscopy. The results showed that microwave sintering promoted an increase in the microhardness and apparent specific mass, and reduction in water absorption and apparent porosity values, due to greater densification in the microstructure. The best results occurred for specimens sintered at 1100°C.     

Comparison of a laboratorial scale synthesized and a commercial yttria-tetragonal zirconia polycrystals ceramics submitted to microwave sintering

Conventional sintering techniques of yttria-tetragonal zirconia polycrystals (Y-TZP) ceramics have presented limitations regarding the sintering time and temperature, increasing the cost of the final dental and biomedical products. Herein, microwave sintering comes to be an interesting alternative by providing fast heating, high densification, and grain-size control. The aim of this study was to compare the effect of microwave sintering of Y-TZP dental ceramics prepared from a pre-sintered commercial block and produced from powders synthesized in a laboratorial scale by the precipitation route. The synthetized and commercial discs were submitted to microwave sintering at 1450°C and 1350°C for 15, 30, and 60 minutes. Densification, fracture toughness, grain size, and crystalline phase quantification of the sintered groups were evaluated. Both synthetized and commercial groups sintered at 1450°C for 15 and 30 minutes showed the higher densification results (98% TD). XRD quantitative phase analysis indicates that samples present 89% tetragonal and 11% cubic phases, except for the group prepared from coprecipitated powders sintered at 1450°C for 30 minutes, that presented 79% and 21% of tetragonal and cubic phases. The microwave sintering at 1450°C allows hardness and fracture toughness values comparable to conventional sintering.     

Fabrication of ceramic bioscaffolds from fly ash cenosphere by susceptor-assisted microwave sintering

Cenospheres (CS) are ceramic hollow microspheres and have been used to prepare composite foams for applications such as medical implants. However, its potential standalone application in the biomedical field is not fully explored. Herein, a susceptor-assisted microwave (SMW) sintering approach was used for producing CS foam scaffolds. Owing to the hybrid heating mechanism offered by the SMW process, sintering of the low-dielectric cenospheres was realized. We found that sintering was initiated at a lower temperature (1100 °C) compared to conventional heating (1250 °C) as reported in the literature, probably due to the lower activation energy required by SMW sintering. The physical and compositional properties of the sintered CS specimens were examined, and in vitro studies were performed. The as-fabricated CS foam possessed minimal effect on cell viability. Cells migrated and adhered well within the pores of the specimens, which indicates the potential of the CS as scaffold materials for cell engineering applications.     

Broadband dielectric characterization of TiO2 ceramics sintered through microwave and conventional processes

In this work the microwave sintering (MW) of pure submicron rutile TiO₂ powder has been conducted in complete electric field using a single mode cavity of 2.45 GHz and without any susceptor. The sintering conditions were varied and similar sintering cycles were also done using a conventional furnace (CV), in carefully measuring the temperature in both processes. The dielectric properties, from kHz to GHz were determined and a comparison analysis was made between microwaved and conventional sintered specimens. It is shown that microwave sintering allows to obtain dense material (>95%) in a very short time (10–15 min) at a sintering temperature ranging from 1000 °C to 1300 °C. Some samples are fully dense (>99% theoretical density) after being microwave heated for ～10 min at ～1300 °C. Using the microwave heating, the processing temperature to get high dense material (i.e. >94%) is lowered by ～150–175 °C compared to conventionally sintered samples. It is also shown that an annealing in air at ～800 °C for ～4 h, leads to very low loss TiO₂ ceramic in the entire frequency range investigated. Owing to the lowest sintering temperature provided by microwaves, the low frequency dielectric losses are smaller for MW samples than for CV sintered samples. Among the highest reported microwave Q factors (～7350) have been measured on pure TiO₂ samples exhibiting the largest grain size (～1.5 μm) and density (>96%).     

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).     

The effects of Cu2+ and La3+ doping on the sintering ability of sol-gel derived high silica bioglasses

This paper reports the hierarchical influence of co-doping copper and lanthanum in a sol–gel derived quaternary (Si, Ca, Na, P) bioactive glass on its sintering ability. The mutual effects of Cu & La on density, crystallisation and sinterability were investigated using Taguchi analysis. Thermal properties of bioglasses were assessed by DTA/TGA and dilatometry, while crystallisation phase evolution of was monitored by X–ray diffraction. Ten glass compositions were sintered at two temperatures (800 and 900?°C). The glass structure was analysed by MAS–NMR, the sintered density measured, and sintered microstructures observed by SEM/EDS. Results revealed that Cu promotes early densification, enhancing density at lower sintering temperatures. Oppositely, beneficial sintering effects of La might be observed at higher sintering temperatures (>1000?°C). These differences are induced by the distinct roles of doping elements on devitrification upon increasing their concentrations: crystallisation is promoted by Cu and is inhibited by La.     

Microwave-assisted sintering and improved dielectric,ferroelectric properties of 0.5[(Ba0.7Ca0.3)TiO3]–0.5[Ba(Zr0.2Ti0.8)O3] lead-free ceramics

0.5[(Ba_0.7Ca_0.3)TiO₃]–0.5[Ba(Zr_0.2Ti_0.8)O₃] lead-free ceramics were synthesised by coprecipitation method and sintered by fast microwave sintering (MWS) and by conventional sintering (CS) at 1200°C. After being sintered with the two different methods, the materials were characterised for structural, microstructural, frequency and temperature-dependent dielectric properties, Raman spectroscopy, and ferroelectric measurements. Results are compared and discussed in the present paper. X-ray diffraction confirms the presence of the tetragonal and rhombohedral phases in the composites sintered by both methods. The ferroelectric to paraelectric transition temperature (Tc) is increased in microwave-sintered composite. Diffuse constant (γ) values show BCT–BZT ceramics to be neither normal ferroelectrics nor relaxor ferroelectrics. Raman spectra confirm phase transition in the ceramic samples. Saturation polarisation (Ps) values are 7.62 and 4.28?µC?cm^?2 and nearly equal remanant polarisation (Pr) values were observed for BCT–BZT composite sintered with MWS and CS, respectively.     

Preliminary investigation of hydroxyapatite microstructures prepared by flash sintering

Flash sintering is a novel and emerging route for sintering ceramics within a few seconds, even under pressure-less conditions. In the current study, hydroxyapatite (HA) was fully densified by flash sintering at a furnace temperature of 1020°C. Flash sintering with constant electric fields of 750 and 1000?V?cm^?1 reduced the grain growth rate significantly compared to that sintered in the absence of an electric field at 1400°C. The microstructure of HA consolidated by flash sintering was compared with that of the without electric field sintered samples. The flash-sintered samples showed smaller grains (160?～?320?nm) than the without electric field sintered samples (～15?µm). The samples with a higher applied electric field showed slightly better densification than those with the lower field by flash sintering. Overall, the electric flash reduces the sintering temperature effectively and decreases the holding time to densify highly insulating ceramics, such as HA.     

Low‐Temperature Sintering of β‐Spodumene Ceramics Using Li2O–GeO2 as a Sintering Additive

Low‐temperature sintering of β‐spodumene ceramics with low coefficient of thermal expansion (CTE) was attained using Li₂O–GeO₂ sintering additive. Single‐phase β‐spodumene ceramics could be synthesized by heat treatment at 1000°C using highly pure and fine amorphous silica, α‐alumina, and lithium carbonate powders mixture via the solid‐state reaction route. The mixture was calcined at 950°C, finely pulverized, compacted, and finally sintered with or without the sintering additive at 800°C–1400°C for 2 h. The relative density reached 98% for the sample sintered with 3 mass% Li₂O–GeO₂ additive at 1000°C. Its Young's modulus was 167 GPa and flexural strength was 115 MPa. Its CTE (from R.T. to 800°C) was 0.7 × 10^?6 K^?1 and dielectric constant was 6.8 with loss tangent of 0.9% at 5 MHz. These properties were excellent or comparative compared with those previously reported for the samples sintered at around 1300°C–1400°C via melt‐quenching routes. As a result, β‐spodumene ceramics with single phase and sufficient properties were obtained at about 300°C lower sintering temperature by adding Li₂O–GeO₂ sintering additive via the conventional solid‐state reaction route. These results suggest that β‐spodumene ceramics sintered with Li₂O–GeO₂ sintering additive has a potential use as LTCC for multichip modules.     

Impact of microwave processing on porcelain microstructure

Microstructural evolution on sintering of porcelain powder compacts using microwave radiation was compared with that in conventionally sintered samples. Using microwaves sintering temperature was reduced by ~ 75 °C and dwell time from 15 min to 5 min while retaining comparable physical properties i.e. apparent bulk density, water absorption to conventionally sintered porcelain. Porcelain powder absorbed microwave energy above 600 °C due to a rapid increase in its loss tangent. Mullite and glass were used as indicators of the microwave effect: mullite produced using microwaves had a nanofibre morphology with high aspect ratio (~ 32 ± 3:1) believed associated with a vapour-liquid-solid (VLS) formation mechanism not previously reported. Microwaves also produced mullite with different chemistry having ~ 63 mol% alumina content compared to ~ 60 mol% alumina in conventional sintered porcelain. This was likely due to accelerated Al⁺³ diffusion in mullite under microwave radiation. Liquid glass was observed to form at relatively low temperature (~ 900–1000 °C) using microwaves when compared to conventional sintering which promoted the porcelains ability to absorb them.     

The effect of pre-annealing and post-annealing on the transparency of MgAl2O4, prepared by slip casting and spark plasma sintering (SPS)

The aim of this paper is to investigate the effect of slip casting process and the annealing before and after sintering to achieve a transparent MgAl₂O₄. To remove contaminants such as carbon from the structure of shaped spinel bodies, at first, the samples were annealed at temperature of 800?°C, 900?°C and 1000?°C for 2?h and then sintered at 1400?°C. By annealing the sample before sintering at 900?°C, the transmission increased (15% at IR region and 10% at visible region). Although by annealing the samples, the amount of carbon contamination reduced. Annealing the samples after sintering also had some desirable results. The samples annealed at temperature of 1200?°C for a time of 3, 5 and 10?h. The darkness of samples reduced due to the removal of carbon impurities and the sample was annealed at 1200?°C for 5?h had the most transparency in the visible and infrared regions.     

Densification behaviour and physico-mechanical properties of porcelains prepared using spark plasma sintering

Porcelain powder was consolidated using spark plasma sintering (SPS) at a constant heating rate of 100°C?min^?1 to peak temperatures ranging from 1000 to 1200°C and was observed to sinter at relatively low temperature ～920°C under the SPS conditions while conventional sintering requires ～1050°C. SPS produced densification rates about 10 times greater than conventional sintering. The dwelling step at the optimal peak temperature was negligible due to rapid flow of the molten glass assisted by applied pressure. SPSed samples exhibited denser microstructures, resulting in improved physico-mechanical properties compared with conventionally sintered samples such as apparent bulk density improved from 2.38 to 2.48?g?cm^?3, Vickers hardness improved from 3–5 to 6–7?GPa, and fracture toughness improved from 2–3 to 4–6?MPa?m^1/2.