Kim Vanmeensel

Influence of sintering conditions on low-temperature degradation of dental zirconia

UNLABELLED The effect of sintering conditions and concomitant microstructure of dental zirconia (ZrO2) ceramics on their low-temperature degradation (LTD) behavior remains unclear. OBJECTIVES Therefore, their effect on LTD of dental ZrO2 ceramics was investigated. METHODS Three commercial pre-sintered yttria-stabilized dental zirconia materials were sintered at three temperatures (1450°C, 1550°C and 1650°C) applying three dwell times (1, 2 and 4h). Grain size measurements and LTD tests were performed on polished sample surfaces. LTD tests were performed at 134°C in an autoclave. The amount of monoclinic ZrO2 on the exposed surface was measured by X-ray diffraction (XRD). RESULTS Higher sintering temperatures and elongated dwell times increased the ZrO2 grain size. Simultaneously, a larger fraction of zirconia grains adopted a cubic crystal structure, resulting in a decreased yttria content in the remaining tetragonal grains. Both the larger grain sizes and the lower average stabilizer content made the tetragonal grains more susceptible to LTD. Overall, independent on the commercial dental zirconia grade tested, the specimens sintered at 1450°C for 1h combined good mechanical properties with the best resistance to LTD. SIGNIFICANCE In general, increased sintering temperatures and times result in a higher sensitivity to low-temperature degradation of Y-TZP ceramics.

Highly-translucent, strong and aging-resistant 3Y-TZP ceramics for dental restoration by grain boundary segregation

Latest trends in dental restorative ceramics involve the development of full-contour 3Y-TZP ceramics which can avoid chipping of veneering porcelains. Among the challenges are the low translucency and the hydrothermal stability of 3Y-TZP ceramics. In this work, different trivalent oxides (Al2O3, Sc2O3, Nd2O3 and La2O3) were selected to dope 3Y-TZP ceramics. Results show that dopant segregation was a key factor to design hydrothermally stable and high-translucent 3Y-TZP ceramics and the cation dopant radius could be used as a controlling parameter. A large trivalent dopant, oversized as compared to Zr(4+), exhibiting strong segregation at the ZrO2 grain boundary was preferred. The introduction of 0.2 mol% La2O3 in conventional 0.1-0.25 wt.% Al2O3-doped 3Y-TZP resulted in an excellent combination of high translucency and superior hydrothermal stability, while retaining excellent mechanical properties.

Spark Plasma Sintering As a Solid-State Recycling Technique: The Case of Aluminum Alloy Scrap Consolidation

Recently, “meltless” recycling techniques have been presented for the light metals category, targeting both energy and material savings by bypassing the final recycling step of remelting. In this context, the use of spark plasma sintering (SPS) is proposed in this paper as a novel solid-state recycling technique. The objective is two-fold: (I) to prove the technical feasibility of this approach; and (II) to characterize the recycled samples. Aluminum (Al) alloy scrap was selected to demonstrate the SPS effectiveness in producing fully-dense samples. For this purpose, Al alloy scrap in the form of machining chips was cold pre-compacted and sintered bellow the solidus temperature at 490 °C, under elevated pressure of 200 MPa. The dynamic scrap compaction, combined with electric current-based joule heating, achieved partial fracture of the stable surface oxides, desorption of the entrapped gases and activated the metallic surfaces, resulting in efficient solid-state chip welding eliminating residual porosity. The microhardness, the texture, the mechanical properties, the microstructure and the density of the recycled specimens have been investigated. An X-ray computed tomography (CT) analysis confirmed the density measurements, revealing a void-less bulk material with homogeneously distributed intermetallic compounds and oxides. The oxide content of the chips incorporated within the recycled material slightly increases its elastic properties. Finally, a thermal distribution simulation of the process in different segments illustrates the improved energy efficiency of this approach.

(Nbx, Zr1–x)4AlC3 MAX Phase Solid Solutions: Processing, Mechanical Properties, and Density Functional Theory Calculations

The solubility of zirconium (Zr) in the Nb4AlC3 host lattice was investigated by combining the experimental synthesis of (Nbx, Zr1-x)4AlC3 solid solutions with density functional theory calculations. High-purity solid solutions were prepared by reactive hot pressing of NbH0.89, ZrH2, Al, and C starting powder mixtures. The crystal structure of the produced solid solutions was determined using X-ray and neutron diffraction. The limited Zr solubility (maximum of 18.5% of the Nb content in the host lattice) in Nb4AlC3 observed experimentally is consistent with the calculated minimum in the energy of mixing. The lattice parameters and microstructure were evaluated over the entire solubility range, while the chemical composition of (Nb0.85, Zr0.15)4AlC3 was mapped using atom probe tomography. The hardness, Youngs modulus, and fracture toughness at room temperature as well as the high-temperature flexural strength and E-modulus of (Nb0.85, Zr0.15)4AlC3 were investigated and compared to those of pure Nb4AlC3. Quite remarkably, an appreciable increase in fracture toughness was observed from 6.6 ± 0.1 MPa/m(1/2) for pure Nb4AlC3 to 10.1 ± 0.3 MPa/m(1/2) for the (Nb0.85, Zr0.15)4AlC3 solid solution.

Wetting behaviour of Cu based alloys on spinel substrates in pyrometallurgical context

Metal droplet losses in slags are an important issue in copper industry. One significant aspect that promotes the entrainment of metal droplets in the slag is their attachment to spinel solids. In the present study, the wetting behaviour of copper alloys on spinel substrates has been investigated in the presence and absence of a slag phase. At first, the attachment was investigated using a synthetic slag containing spinel particles. Microstructural analysis of quenched slag reveals the presence of microdroplets sticking onto a surface of the spinel particles. Second, the metal–spinel interaction was investigated using the sessile drop technique. Wetting angle measurements were performed between Cu–Ag alloys and MgAl2O4 substrates. A non-wetting behaviour between the alloys and substrates was observed. The results suggest that the oxygen partial pressure and the amount of Ag in the alloy both influence the wetting behaviour.

Processing of a Graded Ceramic Cutting Tool in the Al2O3-ZrO2-Ti(C,N) System by Electrophoretic Deposition

In this study, the development of a functionally graded material (FGM) with hard outer surfaces and a tougher inner core was envisaged. The applicability of electrophoretic deposition (EPD) for the processing of FGM materials by continuously changing the suspension composition is shown. Optimisation of the colloidal processing technique was combined with hot pressing experiments on homogeneous composites in the Al2O3-ZrO2-Ti(C,N) system in order to create a very hard functionally graded material with beneficial residual stresses. Finally, the residual stress distribution was briefly discussed using an existing analytical model.

Electrophoretic Deposition as a Novel Near Net Shaping Technique for Functionally Graded Biomaterials

Complex shaped functionally graded alumina and zirconia based femoral ball-heads for biomedical applications were shaped by electrophoretic deposition (EPD). A composition gradient in alumina and zirconia was engineered to obtain a pure alumina surface region and a homogeneous alumina/zirconia core with intermediate continuously graded regions to generate appropriate thermal residual stresses after sintering. The gradient profiles were designed to obtain maximum compressive surface stresses and minimal tensile stresses in the core of the component to increase the strength and wear properties when compared to pure alumina components.

Solid State Recycling of Aluminium Sheet Scrap by Means of Spark Plasma Sintering

Various solid state or ‘meltless’ recycling techniques have recently been developed for light metal scrap in form of chips. Main objective of all approaches is to bypass the need for remelting in order to reduce the overall required energy, and to avoid the material losses that occur during this step. Within this paper, the use of Spark Plasma Sintering (SPS) is proposed as a novel solid state recycling/welding technique for sheet metal scrap. Aluminium 5182 alloy scrap, derived from sheet metal, was successfully consolidated into a fully dense billet via SPS. The use of pulsed electric current heating, in temperatures well below the alloy melting point, combined with mechanical pressure, enchased the densification process resulting into a void-less material. The recycled SPS sample was fully densified and microstructural investigation has been performed in order to confirm effective oxide film breakage. The results illustrate the effectiveness of SPS in aluminium scrap consolidation, also in form of sheet scrap, providing additional means in solid state recycling. The involved mechanisms that contribute to oxide film fracture and scrap consolidation in SPS are being discussed.Keywords: Aluminium, recycling, spark plasma sintering (SPS)

Throwing Power during Electrophoretic Deposition

The deposit can induce an extra potential drop near the electrode, depending on the suspension composition. This can result in a levelling off of the deposition rate in a constant-voltage deposition process. The magnitude of the extra voltage drop determines the uniformity of the deposit as function of the uniformity of the electric field present at the deposition electrode. It was experimentally proven that a uniform Al2O3 coating thickness was obtained in a non-homogeneous electrical field in ethanol with addition of HNO3, while the coating thickness varied uniformly with the E-field strength for a MEK with n-butylamine based suspension. The uniformity of the coating deposited from these suspensions was related to the measured potential drop over the deposit during electrophoretic deposition.

Influence of electrostatic interactions in the deposit on the electrical field strength during electrophoretic deposition

A model was developed to explain the magnitude of the potential drop over the deposit for non-conductive powders during electrophoretic deposition (EPD). The magnitude of the potential drop over the deposit is explained in terms of a reduced ion transport through the deposit, as controlled by the pore potential that is related to the thickness of the electrostatic double layer relative to the pore radius and the magnitude of the surface potential of the powder particles. This model was validated for EPD of Al2O3 powder from ethanol-based suspensions with HNO3 addition. The specific resistivity of the deposit could be related to the calculated potential in the pores of the deposit.