Optically transparent ceramics by spark plasma sintering of oxide nanoparticles

Optical transparency in polycrystalline ceramic oxides can be achieved if the material is fully densified. Spark plasma sintering (SPS) of oxide nanoparticles leads to immediate densification with final-stage sintering. Further densification by annihilation of the isolated pores is associated with diffusional processes, regardless of the densification mechanism during the intermediate stage. Densification equations in conjunction with the concept of grain boundary free volume were used to derive the pore size–grain size–temperature map for designing the nanopowder and SPS process parameters to obtain transparent oxides

Proto-TGO formation in TBC systems fabricated by spark plasma sintering

Thermal barrier coatings (TBC) are commonly used in modern gas turbines for aeronautic and energy production applications. The conventional methods to fabricate such TBCs are EB-PVD or plasma spray deposition. Recently, the spark plasma sintering (SPS) technique was used to prepare new multilayered coatings. In this study, complete thermal barrier systems were fabricated on single crystal Ni-based superalloy (AM1®) substrate in a one-step SPS process. The lifetime of TBC systems is highly dependent on its ability to form during service a dense, continuous, slow-growing alumina layer (TGO) between an underlying bond coating and a ceramic top coat. In the present paper, we show that such kind of layer (called proto-TGO in the following) can be in situ formed during the SPS fabrication of TBC systems. This proto-TGO is continuous, dense and its nature has been determined using TEM-EDS-SAD and Raman spectroscopy. This amorphous oxide layer in the as-fabricated samples transforms to α-Al2O3 during thermal treatment under laboratory air at 1100 °C. Oxidation kinetics during annealing are in good agreement with the formation of a protective α-Al2O3 laye

Sintering and densification of nanocrystalline ceramic oxide powders: a review

Observation of the unconventional properties and material behaviour expected in the nanometre grain size range necessitates the fabrication of fully dense bulk nanostructured ceramics. This is achieved by the application of ceramic nanoparticles and suitable densification conditions, both for the green and sintered compacts. Various sintering and densification strategies were adopted, including pressureless sintering, hot pressing, hot isostatic pressing, microwave sintering, sinter forging, and spark plasma sintering. The theoretical aspects and characteristics of these processing techniques, in conjunction with densification mechanisms in the nanocrystalline oxides, were discussed. Spherical nanoparticles with narrow size distribution are crucial to obtain homogeneous density and low pore-to-particle-size ratio in the green compacts, and to preserve the nanograin size at full densification. High applied pressure is beneficial via the densification mechanisms of nanoparticle rearrangement and sliding, plastic deformation, and pore shrinkage. Low temperature mass transport by surface diffusion during the spark plasma sintering of nanoparticles can lead to rapid densification kinetics with negligible grain growth

High-temperature transport properties of complex antimonides with anti-Th3P4 structure

Polycrystalline samples of R4Sb3 (R = La, Ce, Smand Yb) and Yb4-xR¢xSb3 (R¢ = Sm and La) have been quantitatively synthesized by high-temperature reaction. They crystallize in the anti-Th3P4 structure type (I ¯43d, no. 220). Structural and chemical characterizations have been performed by X-ray diffraction and electron microscopy with energy dispersive X-ray analysis. Powders have been densified by spark plasma sintering (SPS) at 1300 ◦C under 50 MPa of pressure. Transport property measurements show that these compounds are n-type with low Seebeck coefficient except for Yb4Sb3 that shows a typical metallic behavior with hole conduction. By partially substituting Yb by a trivalent rare earth we successfully improved the thermoelectric figure of merit of Yb4-xR¢xSb3 up to 0.75 at 1000 ◦C

Spark plasma sintered carbon electrodes for electrical double layer capacitor applications

The spark plasma sintering (SPS) is an emerging process for shaping any type of materials (metals, ceramic, polymers and their composites). The advantage of such a process is to prepare densified ceramic materials in a very short time, while keeping the materials internal porosity. In the present work, we have used the SPS technique to prepare activated carbon-based electrodes for Electrochemical Double Layer Capacitor applications (EDLC). Self-supported 600 and 300µm-thick electrodes were prepared and characterized using of Electrochemical Impedance Spectroscopy and galvanostatic cycling in a non-aqueous 1.5MNEt4BF4 in acetonitrile electrolyte. Electrochemical performance of these sintered electrodes were found to be in the same range – or even slightly better – than the conventional tape-casted activated carbon electrodes. Although organic liquid electrolyte was used to characterize the electrochemical performance of the sintered electrodes, these results demonstrate that the SPS technique could be worth of interest in the ultimate goal of designing solid-state supercapacitors

Effect of 1 wt% LiF additive on the densification of nanocrystalline Y2O3 ceramics by spark plasma sintering

Densification of nanocrystalline cubic yttria (nc-Y2O3) powder, with 18 nm crystal size and 1 wt% LiF as a sintering additive was investigated. Specimens were fabricated by spark plasma sintering at 100 MPa, within the temperature range of 700–1500 °C. Sintering at 700 °C for 5 and 20 min resulted in 95% and 99.7% dense specimens, with an average grain size of 84 and 130 nm, respectively. nc-Y2O3 without additive was only 65% dense at 700 °C for 5 min. The presence of LiF at low sintering temperatures facilitated rapid densification by particle sliding and jamming release. Sintering at high temperatures resulted in segregation of LiF to the grain boundaries and its entrapment as globular phase within the fast growing Y2O3 grains. The sintering enhancement advantage of LiF was lost at high SPS temperatures

Synthesis, Sintering, and Electrical Properties of BaCe0.9−xZrxY0.1O3−δ

BaCe0.9−xZrxY0.1O3−δ powders were synthesized by a solid-state reaction. Different contents of cerium and zirconium were studied. Pellets were sintered using either conventional sintering in air at 1700◦C or the Spark Plasma Sintering (SPS) technique. The density of the samples sintered by SPS is much higher than by conventional sintering. Higher values of ionic conductivity were obtained for the SPS sample

Reactivity and microstructure evolution of a CoNiCrAlY/Talc cermet prepared by spark plasma sintering

A mixture of CoNiCrAlY and talc powders is considered as a new candidate composition for abradable seal coating applications. Dense specimen having the composition of 1:20 weight ratio of talc with respect to CoNiCrAlY was prepared using the Spark Plasma Sintering (SPS) technique. The aim of the present article is to investigate the reactivity and microstructure evolution of the β/γ-CoNiCrAlY based cermet. The resulting microstructures were analysed and their compositions determined using standard analytical techniques such as SEM, TEM and X-ray diffraction. After fabrication, the bulk of the material is shown to contain a continuous oxide layer of MgAl2O4 at the periphery of metallic particles, resulting from the reaction between aluminium, which has diffused from the bulk of CoNiCrAlY grains, with magnesium and oxygen delivered during the high temperature decomposition of the talc phase. Thermodynamic calculations results are found to be consistent with the experimental observations. The oxidation behaviour at a high temperature of this cermet was also investigated. It was shown that at its external surface a continuous double layer is formed — one external film at the surface of the sample made of MgAl2O4 and the second one more internal in between the later and the cermet made of α-Al2O3. The oxide scale is protective with low oxidation kinetics typical of alpha alumina growth (kP = 1.8 10 − 7mg2 cm − 4 s − 1 at 1050 °C in flowing dry air)

Densification and polymorphic transition of multiphase Y2O3 nanoparticles during spark plasma sintering

Multiphase (MP) monoclinic and cubic Y2O3 nanoparticles, 40 nm in diameter, were densified by spark plasma sintering for 5–15 min and100 MPa at 1000 °C, 1100 °C, and 1500 °C. Densification started with pressure increase at room temperature. Densification stagnated during heating compared to the high shrinkage rate in cubic single-phase reference nanopowder. The limited densification of the MP nanopowder originated from the vermicular structure (skeleton) formed during the heating. Interface controlled monoclinic to cubic polymorphic transformation above 980 °C led to the formation of large spherical cubic grains within the vermicular matrix. This resulted in the loss of the nanocrystalline character and low final density

Constitutive modelling and mechanical characterization of aluminium-based metal matrix composites produced by spark plasma sintering

Spark plasma sintering has been applied to the production of aluminium-based functionally graded material systems to be used in abrasive and high temperature conditions. The overall mechanical properties of these metal matrix composites were determined during the optimization phases of the production process by a fast and reliable identification procedure based on instrumented indentation, which can be easily performed on small specimens. The experimental information gathered from conical (Rockwell) indentation was used as input data for the calibration of the material parameters entering the elastic–plastic Drucker–Prager constitutive model. Eventually, the so identified material parameters were used to predict the result of pyramidal (Vickers) indentation, in order to validate the model selection and the output of the identification procedure. The good matching between modelling and experimental results for the different test configurations confirmed the soundness of the considered approach, especially evidenced on the light of the strong influence on the overall mechanical characteristics of the material microstructure and defectiveness resulting from the production process, which prevent the use of classical homogenization rules to evaluate the macroscopic material properties