Authors: Fei Zhang, Kim Vanmeensel, Masanao Inokoshi, Bart van Meerbeek, Ignace Naert, Jef Vleugels
Abstract: The influence of the addition of 0.25, 2 and 5 wt.% alumina on the mechanical properties and low temperature degradation (LTD) behaviour of 3 mol% yttria-coated ZrO2 powder based Y-TZP ceramics was investigated, and compared to commercial powder based co-precipitated 3Y-TZPs with 0-0.25 wt.% Al2O3 addition. The ceramics were subjected to accelerated hydrothermal degradation in an autoclave in H2O at 134°C up to 40 hrs. X-ray diffraction and Raman spectroscopy were used to assess the LTD behaviour. Incorporating the Y2O3 stabilizer by means of a coating method resulted in a higher LTD resistance without compromising the higher fracture toughness, compared to the co-precipitation method. Alumina addition did not significantly influence the mechanical properties of all Y-TZPs but significantly increased the LTD resistance of the Y-TZP ceramics. The LTD resistance of 0.25 wt% Al2O3 doped TZPs was substantially higher than that of ceramics containing 2 or 5 wt.% Al2O3, which had a comparable susceptibility. The highest LTD resistance for the 0.25 wt.% alumina doped ceramics could be correlated to the solubility limit of alumina in zirconia.
139
Authors: Jef Vleugels, Olivier Malek, Kim Vanmeensel, Shui Gen Huang, Song Lin Ran, Omer Van der Biest, Bert Lauwers
Abstract: Pulsed electric current sintering allows densifying most ceramics at high heating and
cooling rates within very short times at elevated temperature, allowing to minimise grain growth. In
order to fully explore the PECS potential, it is beneficial to flow the current through the powder
compact by either using conductive powder or a powder compact that becomes conductive during
densification. Although in-situ Joule heating of the powder compact allows very fast heating rates, it
does not necessarily result in a homogeneous temperature distribution. The influence of the current
flow on densification and the impact of electrical conductivity on the temperature distribution
during PECS are illustrated. The PECS technology at present is limited to the fabrication of simple
geometrical shapes. Electrical Discharge Machining (EDM) on the contrary allows production of
complex shapes, providing the ceramic has a minimum electrical conductivity. Although EDM has
no mechanical impact, the thermal impact is high and the EDM parameters should be carefully
selected in order to optimise surface quality and component strength. During wire-EDM, the fast
and rough initial cut has to be followed by a sequence of lower energy finishing cuts to optimise the
surface quality. The case studies presented are B4C-TiB2 ceramics and ZrO2-based composites with
electrically conductive phase addition.
175
Authors: Melis Arin, Jef Vleugels, Kim Vanmeensel, G. Göller
Abstract: Fully dense ZrO2-TiN composites containing 1.75-2 mol %Y2O3, 1 mol% Y2O3 and 1
mol% Nd2O3 stabilizers, small amounts of Al2O3, and electrical conductive TiN particles (40-70
vol%) have been produced by hot pressing and spark plasma sintering at 1550°C. Although the
intrinsic hardness of TiN (1400 kg/mm²) is higher than that of t-ZrO2 (1200 kg/mm²), the
decreasing hardness trend can be attributed to the larger TiN grain size with the higher TiN content.
Since TiN is more brittle, the fracture toughness decreases with increasing TiN content.
Transformation toughening has been attributed as the main toughening mechanism as a result of
fracture toughness decreasing with the transformability. Spark Plasma sintering temperature was too
high for mechanical properties and hydrothermal stability of the mixed stabilized composites. The
transformability decreases so hydrothermal stability increases linearly with increasing TiN content
as a result of smaller volume fraction of t-ZrO2 grains becoming susceptible to hydrothermal
transformation due to the shielding effect of the present TiN grains.
795
Authors: Shui Gen Huang, Omer Van der Biest, Jef Vleugels, Kim Vanmeensel, Lin Li
Abstract: In this study, 2 mol% Y2O3 (2Y), 1 mol% Y2O3+6 mol% CeO2 (1Y6Ce) and 12 mol%
CeO2 (12Ce)-doped tetragonal ZrO2 ceramics were made by spark plasma sintering (SPS) for 2 min
at 1450°C under a pressure of 60 MPa. The influence of stabilizers on microstructure, phase and
mechanical properties of the ZrO2 ceramics was investigated. After sintering, the 2Y and 1Y6Ce
were intact, containing full tetragonal ZrO2 phase on the polished cross-sectioned surface, whereas
the 12Ce exhibited macro-cracks, corresponding to a large amount of monoclinic ZrO2 phase.
Graded microstructure and mechanical properties were observed in the 1Y6Ce, showing a gradually
decreased fracture toughness from sample edge towards centre, together with the slight decreased
hardness. The 2Y had a uniform microstructure and mechanical properties. The formation of the
graded structure and toughness profile was explained in terms of the gradual CeO2 reduction to
Ce2O3 in the Y2O3+CeO2 doped ZrO2 ceramics.
231
Authors: Guy Anné, Kim Vanmeensel, Jef Vleugels, Omer Van der Biest
Abstract: Due to their excellent properties of high strength, biocompatibility and stability in
physiological environments, ceramics are investigated as bone substitute materials. In this way
ceramic components have been used for total hip replacement components since the early 1970s.
Alumina and zirconia monoliths are mainly used for these components. However, zirconia can
undergo low temperature degradation in aqueous environment and alumina is brittle.
To increase the strength, functionally graded Al2O3/ZrO2 ball-heads and acetabular cup inserts were
made in this work 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 thermal residual
stresses at the surface after sintering.
Experimental work revealed that a sequence of counter-electrodes was necessary to EPD complex
shaped functionally graded material (FGM) components. To obtain deposits with a shape different
from the deposition electrode, the deposit was grown up to the counter-electrode and the design of
the counter-electrodes was supported by electrical field calculations to generate a constant electric
field at the surface of the deposition electrode
213
Authors: Guy Anné, Bram Neirinck, Kim Vanmeensel, Omer Van der Biest, Jef Vleugels
Abstract: 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.
187
Authors: Guy Anné, Bram Neirinck, Kim Vanmeensel, Omer Van der Biest, Jef Vleugels
Abstract: 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.
181
Authors: Guy Anné, Bram Neirinck, Kim Vanmeensel, Omer Van der Biest, Jef Vleugels
Abstract: The electrical field drop over a deposit during electrophoretic deposition (EPD)
determines the deposition rate and the uniformity of the deposit when a non-uniform electrical field
is present. Due to the large practical consequences of a potential drop over the deposit, a procedure
was developed to calculate the electrical field strength at the deposition front from currentconductivity
measurements during EPD. The evolution of the electrical field strength during EPD
was calculated for MEK and ethanol based suspensions. It was found that the suspension
composition determines whether a potential drop over the deposit is present or not. EPD
experiments on a membrane revealed that the extra potential drop is over the deposit and not caused
by electrode polarization for the ethanol-acid based suspensions.
13
Authors: Kim Vanmeensel, K.Y. Sastry, J. Hennicke, Guy Anné, Dongtao Jiang, A.I. Laptev, Jef Vleugels, Omer Van der Biest
Abstract: Future materials for wear resistant components require a combination of excellent mechanical properties such as hardness and toughness, short processing times and good electrical conductivity to facilitate shaping by electro discharge machining (EDM). In this work, the hardness and fracture toughness of t-ZrO2 based electro conductive composites was optimised, while short processing times below 20 minutes using spark plasma sintering were sufficient to obtain near fully dense materials. The influence of powder processing technique using TiC0.5N0.5 as the starting powder and yttria as a stabiliser on the mechanical properties of ZrO2-TiC0.5N0.5-Al2O3 based composites was investigated. Fully dense Y-TZP based composites possessed an excellent toughness of 9.2 MPa.m1/2 and an increased Vickers hardness of 1397 kg/mm².
153
Authors: Kim Vanmeensel, Guy Anné, Dongtao Jiang, Jef Vleugels, Omer Van der Biest
Abstract: 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.
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