Chemical and microstructural characterisation of HfO2-Y2O3 ceramics with high amount of Y2O3 (33, 40 and 50 mol. %) manufactured using spark plasma sintering

Hafnia based ceramics are potential promising candidates to be used as thermal barrier coatings (TBC) for applications in the field of propulsion. In this study, Spark Plasma Sintering (SPS) of fully stabilised hafnia with yttrium oxide (yttria) was investigated to provide a better understanding of the effect of manufacturing parameters, on the crystallography, chemistry and microstructure of the material. Several hafnia powders, containing different amounts of yttria (33 mol. %, 40 mol. % or 50 mol. %), were sintered by SPS at different temperature levels ranging from 1600 °C to 1850 °C. On these materials, X-ray diffraction patterns associated with scanning electron micrographs have highlighted the influence of both the sintering temperature and the amount of yttria on the final composition, the lattice parameter and the microstructure of hafnia-based materials. In the end, it is established that, for all quantities of yttrium employed, the main phase is Y₂Hf₂O₇ with very high densification levels.     

Preparation of anorthite ceramics using SPS

A mixture of kaolin (92 wt.% of kaolinite) and laboratory-grade CaCO₃ was used for anorthite preparation using the spark plasma sintering (SPS) technique. The powder was heated up to the maximum temperature (850 °C–1100 °C with a step of 50 °C, heating rate 50 °C/min) using the SPS device. The as-prepared samples were compared with a reference sample produced by dry pressing and conventional firing. Rietveld refinement performed on the X-ray diffraction data revealed that before anorthite formation, gehlenite and Ca-feldspar appeared, which gradually transformed into anorthite with increasing temperature. The sample prepared by SPS at 1100 °C contained 90 wt.% of anorthite, while the anorthite content in the reference sample reached only 47 wt.%. The porosity of the samples prepared by SPS reached significantly lower values compared to that of the reference sample. Therefore, SPS can be considered as a promising technique in the preparation of anorthite ceramics at lower temperatures.     

Fabrication of transparent Y2O3 ceramics by two-step spark plasma sintering

Transparent Y₂O₃ ceramics were successfully fabricated by spark plasma sintering applying a two-step pressure and heating profile. Through the shrinkage curve of the single-step SPS profile, it was confirmed that shrinkage occurred at 800°C–1250°C, and it was selected as the two-step pressure profile. After the first-step SPS stage at 1250°C, the second-step SPS stage, which had the highest real in-line transmittance, was completed at 1500°C. The two-step SPS profile improved the shrinkage behavior and was able to achieve sufficient densification without excessive coarsening. As a result, the normalized real in-line transmittance to 1 mm was 80.6% at 1100 nm, which is close to the theoretical transmittance of 81.6%. The two-step pressure and heating profile in the SPS process was a significant advantage in manufacturing ceramics that were transparent and had sufficient densification.     

Yb doped MgO transparent ceramics generated through the SPS method

Yb doped (0, 0.02, 0.1 and 0.5 at%) MgO transparent ceramics were synthesized through spark plasma sintering (SPS) at the relatively low temperature of 1100 °C for 5–60 min under a pressure of 105 MPa. The effects of dopant concentration and sintering holding time on the densification and microstructure evolution of MgO ceramics were investigated. All ceramics reached a relative density greater than 99.20%. The 0.02% Yb-doped MgO ceramic sintered at 1100 °C for 60 min showed the highest in-line transmittance, of 80% at 1030 nm, a value close to that of MgO single crystals. Yb dopant improved the transmittance, degree of densification and control of grain growth. Herein, the influence of Yb doping on the crystalline phase and microstructure was explored, and the photoluminescence properties of Yb in transparent MgO ceramics were investigated.     

Effects of oxidation temperature on microstructure and EMI shielding performance of layered SiC/PyC porous ceramics

Herein, the influence of oxidation temperature on the oxidation behavior, microstructure and electromagnetic shielding performance of layered porous ceramics has been systematically investigated. Layered SiC/PyC porous ceramics were prepared by using low-pressure chemical vapor infiltration (LPCVI) method. The oxidized SiC/PyC layered porous ceramics exhibited a negligible mass reduction of 11.94 mg·cm^?3, which indicates the excellent high-temperature oxidation resistance of porous ceramics. The electromagnetic shielding performance of SiC/PyC porous ceramics did not exhibit any obvious change even after oxidation at high temperature from 900 to 1300 °C for 10 h. The SE_T of the layered SiC/PyC porous ceramics was 24.1, 20.0, 19.5, 19.0, 19.8 dB after oxidation at 25 °C, 900 °C, 1000 °C, 1100 °C and 1300 °C, which corresponds to a decrease of 17.01%, 19.09%, 21.16% and 17.84%, respectively. The high-temperature oxidation has rendered a more significant influence on the reflection efficiency of the layered SiC/PyC porous ceramics.     

Spark plasma sintering,mechanical and in-vitro behavior of a novel Sr- and Mg-containing bioactive glass for biomedical applications

The so-called BGMS10, a bioactive glass containing 10 mol.% SrO and 10 mol.% MgO, displays a low inclination to crystallize, as confirmed by its high activation energy (538.9 kJ/mol). Such peculiar aspect and the beneficial use of SPS allow for the obtainment of 99.7 % dense and fully amorphous products at 750 °C. The incipient crystallization in the glass is observed when temperature is increased to 850 °C, while 95 wt. % crystallized ceramics are produced at 950 °C. Main crystalline phases are α- and β-CaSiO₃, with grain size of 89 and 97 nm, respectively. Glass crystallization is accompanied by Young’s modulus increase from 90.92 to 98.38 GPa. On the other hand, partially crystallized samples (850 °C) exhibit higher Vickers hardness (718.8) compared to fully crystallized ones (619.8), which show lower density (98.6 %). In-vitro tests in SBF indicate that the silica-gel film preceding apatite nucleation is mostly formed on the amorphous substrate region.     

Facile Fabrication of Highly Transparent Yttria Ceramics with Fine Microstructures by a Hot‐Pressing Method

In this study, we report highly transparent yttria ceramics fabricated by a facile hot‐pressing method with tantalum foil shielding which effectively prevents the ceramic samples from carbon contamination caused by the graphite mold used during the process. The hot‐pressed sample was already highly transparent without a post‐annealing step or hot isostatic pressing. For a 2‐mm‐thick specimen doped with 1 at.% ZrO₂, the in‐line transmittance reaches 74.4% at 400 nm and 81.1% at 1100 nm. The sample shows a very fine microstructure with an average grain size of about 1 μm owing to the low sintering temperature of only 1600°C. The study results indicate that it is possible to produce transparent yttria ceramics with excellent optical transparency using the economical and convenient hot‐pressing method.     

Suppression of carbon contamination in SPSed CaF2 transparent ceramics by Mo foil

Transparent calcium fluoride (CaF₂) ceramics were fabricated by spark plasma sintering (SPS) using Mo foil to separate from graphite die, and the effect of Mo foil on transparency, microstructure and carbon contamination was investigated. The discoloration was removed and the transmittance increased from 8% to 54% at the wavelength of 300 nm and 63% to 86% at 1100 nm by using Mo foil. The average grain size of CaF₂ ceramics SPSed at 1100 °C was 16 μm by using graphite sheet, whereas it was 260 μm by using Mo foil, indicating that ceramics with large grain size are possible to reach high transmittance. Raman spectroscopy and X-ray photoelectron spectroscopy revealed that carbon contamination in the CaF₂ ceramics using Mo foil decreased 78% than that shielded by graphite sheet.     

High‐temperature strength and plastic deformation behavior of niobium diboride consolidated by spark plasma sintering

Bulk niobium diboride ceramics were consolidated by spark plasma sintering (SPS) at 1900°C. SPS resulted in dense specimens with a density of 98% of the theoretical density and a mean grain size of 6 μm. During the SPS consolidation, the hexagonal boron nitride (h‐BN) was formed from B₂O₃ on the powder particle surface and residual adsorbed nitrogen in the raw diboride powder. The room‐temperature strength of these NbB₂ bulks was 420 MPa. The flexural strength of the NbB₂ ceramics remained unchanged up to 1600°C. At 1700°C an increase in strength to 450 MPa was observed, which was accompanied by the disappearance of the secondary h‐BN phase. Finally, at 1800°C signs of plastic deformation were observed. Fractographic analysis revealed a number of etching pits and steplike surfaces suggestive of high‐temperature deformation. The temperature dependence of the flexural strength of NbB₂ bulks prepared by SPS was compared with data for monolithic TiB₂, HfB₂ and ZrB₂. Our analysis suggested that the thermal stresses accumulated during SPS consolidation may lead to additional strengthening at elevated temperatures.     

The effect of SPS parameters on the production of yttria transparent ceramic

In this work, the spark plasma sintering (SPS) of commercial yttria nanopowder is investigated. The SPS parameters such as sintering temperature, applied pressure, and dwell time are varied. Densification without grain growth occurring at occurred up to a sintering temperature of 1400°C and grain growth without further densification taking place at the higher temperature. The optimum sample was obtained at a temperature of 1400°C with a pressure of 70 MPa and dwelling time of 15 minutes. The highest relative density of 99.8% and the average grain size of 1.26 μm were obtained at 1400°C. The yttria ceramic annealed at 1200°C had the in-line transmission of 5%-70% and 70%-82% in the visible and infrared wavelength region, respectively. The measurements of hardness and fracture toughness characteristics of the transparent yttria ceramic showed 9.2 GPa and 2.24 MPa.m^1/2, respectively.     

Effect of temperature on the structure and mechanical properties of SiC–TiB2 composite ceramics by solid-phase spark plasma sintering

SiC composite ceramics have good mechanical properties. In this study, the effect of temperature on the microstructure and mechanical properties of SiC–TiB₂ composite ceramics by solid-phase spark plasma sintering (SPS) was investigated. SiC–TiB₂ composite ceramics were prepared by SPS method with graphite powder as sintering additive and kept at 1700 °C, 1750 °C, 1800 °C and 50 MPa for 10min.The experimental results show that the proper TiB₂ addition can obviously increase the mechanical properties of SiC–TiB₂ composite ceramics. Higher sintering temperature results in the aggregation and growth of second-phase TiB₂ grains, which decreases the mechanical properties of SiC–TiB₂ composite ceramics. Good mechanical properties were obtained at 1750 °C, with a density of 97.3%, Vickers hardness of 26.68 GPa, bending strength of 380 MPa and fracture toughness of 5.16 MPa m^1/2.     

Bending strength and microstructure of Al2O3 ceramics densified by spark plasma sintering

Al₂O₃ ceramics were superfast densified using spark plasma sintering (SPS) by heating to a sintering temperature between 1350 and 1700°C at a heating rate of 600°C/min, without holding time, and then fast cooling to 600°C within 3 min. High-density Al₂O₃ ceramics could be achieved at lower sintering temperatures by SPS, as compared with that by conventional pressureless sintering (PLS). The bending strength of Al₂O₃ superfast densified by SPS in the range of sintering temperature between 1400 and 1550°C reached values as high as 800 MPa, almost twice that obtained by the PLS. SEM observations indicated that intragranular fracture was the preponderant fracture mode in these samples, resulting in these excellent bending strength values.     

Transparent mullite ceramic from single-phase gel by Spark Plasma Sintering

Monophasic mullite precursors with composition of 3Al₂O₃·2SiO₂ (3:2) were synthesized and then were sintered by Spark Plasma Sintering (SPS) to form transparent mullite ceramics. The precursor powders were calcined at 1100 °C for 2 h. The sintering was carried out by heating the sample to 1450 °C, holding for 10 min. The sintered body obtained a relative bulk density of above 97.5% and an infrared transmittance of 75–82% in wavelength of 2.5–4.3 μm without any additive. When the precursor powders were calcined at below 1100 °C, it was unfavorable for completely eliminating the residual OH, H₂O and organic compound. However, when calcined temperature was too high, it was unfavorable either for full densification due to the absence of viscous flow of amorphous phase. At the same calcined temperature, the transmittance of sintered body was decreased with the increase of the sintering temperature above 1450 °C owing to the elongated grain growth.     

Synthesis of Dense Lead Titanate Ceramics with Submicrometer Grains by Spark Plasma Sintering

Dense PbTiO₃ ceramics consisting of submicrometer-sized grains were prepared using the spark-plasma-sintering (SPS) method. Hydrothermally prepared PbTiO₃ (0.1 μm) was used as a starting powder. The powder was densified to ≳98% of the theoretical X-ray density by the SPS process. The average grain size of the spark-plasma-sintered ceramics (SPS ceramics) was ≲1 μm, even after sintering at 900°–1100°C, because of the short sintering period (1–3 min). The measured permittivity of the SPS ceramics showed almost no frequency dependence over the range 10¹–10⁶ Hz, mainly because pores were absent from the ceramics. The coercive field of the SPS ceramics was somewhat higher than that of conventionally sintered ceramics, which could be attributed to the small-grained microstructures of the SPS ceramics.     

Fabrication,microstructure and spectroscopic properties of Yb:Lu2O3 transparent ceramics from co-precipitated nanopowders

Ytterbium doped lutetium oxide (Yb:Lu₂O₃) transparent ceramics were fabricated by vacuum sintering combined with hot isostatic pressing (HIP) of the powders synthesized by the co-precipitation method. The effects of calcination temperature on the composition and morphology of the powders were investigated. Fine and well dispersed 5?at% Yb:Lu₂O₃ powders with the mean particle size of 67?nm were obtained when calcined at 1100?°C for 4?h. Using the synthesized powders as starting material, we fabricated 5?at% Yb:Lu₂O₃ ceramics by pre-sintering at different temperatures combined with HIP post-treatment. The influence of pre-sintering temperature on the densities, microstructures and optical quality of the 5?at% Yb:Lu₂O₃ ceramics was studied. The ceramic sample pre-sintered at 1500?°C for 2?h with HIP post-treating at 1700?°C for 8?h has the highest in-line transmittance of 78.2% at 1100?nm and the average grain size of 2.6?µm. In addition, the absorption and emission cross sections of the 5?at% Yb:Lu₂O₃ ceramics were also calculated.     

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.     

Low-temperature reactive spark plasma sintering of dense SiC-Ti3SiC2 ceramics

SiC-based ceramics are of great interest for various advanced applications. However, its fabrication requires high-temperature treatment at ～2000 – 2100 °С. In this study, we developed an approach based on low-temperature reactive spark plasma sintering to produce dense SiC-based ceramics with superior mechanical properties. It was found that an SPS temperature of 1600 °C and introduction of 10 – 15 wt% of mechanically activated non-oxide Ti–Si–C additive is required to manufacture ceramics with a theoretical density of higher than 90%. Nonetheless, employing 5 – 15 wt% of the additive mixture and an SPS temperature of 1700 °C, the maximum density of ～ 98% was achieved. The controlled formation and decomposition of the in-situ Ti₃SiC₂ MAX phase enables the fabrication of the engineering ceramics with enhanced compressive strength (550 MPa), elastic modulus (485 GPa), and microhardness (32 GPa), which are comparable to the best-reported SiC ceramics. The study has a significant potential for practical application in the production of advanced SiC-based ceramics for various purposes and could be used for further understanding and development of the high-temperature sintering methods.     

Ce3+ doped Lu3Al5O12 ceramics prepared by spark plasma sintering technology using micrometre powders: Microstructure,luminescence, and scintillation properties

Ce³⁺ doped Lu₃Al₅O₁₂ (Ce:LuAG) ceramics were fabricated by the solid-state reaction method through spark plasma sintering (SPS) from 1350 °C to 1700 °C for 5 min at a pressure of 50 MPa using micro powders. The average grain size of the SPSed ceramics gradually grew from 0.42 µm (1400 °C) to 1.55 µm (1700 °C), which is nearly one order of magnitude lower than that of vacuum sintered (VSed) Ce:LuAG ceramics (~24.6 µm). Characteristic Ce³⁺ emission peaking at around 510 nm appeared and 92% photoluminescence intensity of room temperature can be reserved at 200 °C revealing excellent thermal stability. The maximum radioluminescence intensity reached around 3 times of VSed Ce:LuAG ceramics and 7.8 times of BGO crystals. The maximum scintillation light yield under γ-ray (¹³⁷Cs) excitation reached 9634 pho/MeV @ 2 μs. It is concluded that SPS technology is a feasible way to develop Ce:LuAG ceramics and further optical enhancement can be expected.     

Fracture and property relationships in the double diboride ceramic composites by spark plasma sintering of TiB2 and NbB2

Bulk titanium diboride–niobium diboride ceramic composites were consolidated by spark plasma sintering (SPS) at 1950°C. SPS resulted in dense specimens with a density exceeding 98% of the theoretical density and a multimodal grain size ranging from 1 to 10 μm. During the SPS consolidation, the pressure was applied and released at 1950 and 1250°C, respectively. This allowed obtaining a two-phase composite consisting of TiB₂ and NbB₂. For these ceramics composites, we evaluated the flexural strength and fracture toughness and room and elevated temperatures. Room-temperature strength of thus produced bulks was between 300 and 330 MPa, at 1200°C or 1600°C an increase in strength up to 400 MPa was observed. Microstructure after flexure at elevated temperatures revealed the appearance of the needle-shape subgrains of NbB₂, an evidence for ongoing plastic deformation. TiB₂–NbB₂ composites had elastic loading stress curves at 1600°C, and at 1800°C fractured in the plastic manner, and strength was ranged from 300 to 450 MPa. These data were compared with a specimen where a (Ti,Nb)B₂ solid solution was formed during SPS to explain the behavior of TiB₂–NbB₂ ceramic composites at elevated temperatures.     

Recycling photovoltaic silicon waste for fabricating porous mullite ceramics by low-temperature reaction sintering

In this study, porous mullite ceramics with coral-like structures were fabricated at a low temperature of 900 °C by using photovoltaic silicon waste (PSW) as the silicon source directly. The effects of additive content and sintering temperature on the mullitization reaction of green bodies were studied. The results showed that ammonium molybdate tetrahydrate molybdenum (H₂₄Mo₇N₆O₂₄·4H₂O) as an additive could reduce the reaction temperature for mullitization from 1100 °C to 900 °C. The research on the influence of catalyst on material properties showed that porous mullite ceramics with a flexural strength of 52.83 MPa, a 41.78 % porosity, a sintering expansion rate of 0.49 % and an average pore size of 0.23 μm could be fabricated by introducing 7.5 % H₂₄Mo₇N₆O₂₄·4H₂O at the sintering temperature of 1000 °C. This study develops an environment-friendly recycling method of PSW and provides a new idea for the low-cost preparation of porous mullite ceramics with high purity.