Authors: L.K.L. Falk, Yvonne Menke, Stuart Hampshire
Abstract: This paper is focussed on the development of microstructure during crystallisation heat treatment of B-phase parent glasses with composition (e/o) 35R:45Si:20Al:83O:17N, where R = Er, Yb, Y or a mixture of Y and Yb. Extensive high resolution analytical transmission electron microscopy has shown that the lenticular B-phase crystals take up a substantial range of composition. The element R is always clearly anti-correlated with the Si, and a larger R3+ cation radius moves the composition range to lower R contents. It is suggested that a locally increased density in the bi-dimensional network of randomly oriented (Si,Al)(O,N)4 tetrahedra is associated with an increased density of vacancies in the R3+ cation lattice.
103
Authors: L.K.L. Falk, N. Schneider, Yvonne Menke, Stuart Hampshire
Abstract: The intergranular microstructure in a liquid phase sintered silicon nitride based ceramic
may be viewed as an oxynitride glass-ceramic. This work is concerned with the incorporation of
yttrium B-phase, which is a five-component phase, into the intergranular regions of silicon nitride
ceramics. The silicon nitride materials were fabricated with the addition of a powdered B-phase
parent glass with composition (e/o) 35Y:45Si:20Al:83O:17N, or the addition of a mixture of Y2O3,
SiO2 and Al2O3 with cation composition (e/o) 35Y:45Si:20Al. The starting powder mixtures
contained 10 wt% of sintering additives. Sintering for 2 h at 1800°C was followed by a two-step
post-densification heat treatment in order to promote nucleation and growth of yttrium B-phase.
Detailed imaging and elemental analysis of the intergranular regions was carried out by EDX in a
FEGTEM.
113
Authors: L.K.L. Falk, Yvonne Menke, Stuart Hampshire
Abstract: Five-component B-phase may be readily formed through the nucleation and
crystallisation heat treatment of nitrogen-rich parent glasses with composition (e/o)
35R:45Si:20Al:83O:17N. This paper is focussed on the B-phase structure where R stands for
ytterbium, erbium or yttrium. Fine probe EDX analysis in the TEM has shown that the lenticular
B-phase crystals take up a substantial range of composition and that the element R is always
clearly anti-correlated with silicon. A larger R3+ cation radius moves the B-phase composition
range to lower R contents, and as a consequence of the anti-correlation with silicon, the silicon
solid solution range goes to higher values. The EDX results lend support to a B-phase structure
consisting of two-dimensional network of randomly linked (Si,Al)(O,N)4 tetrahedra between
layers of R3+ cations. It is suggested that, in addition to the random substitution of silicon by
aluminium in the (Si,Al)(O,N)4 tetrahedra, a locally increased density in the bi-dimensional
network of randomly oriented tetrahedra is associated with an increased density of vacancies in
the R3+ cation lattice.
30
Authors: E. Dolekcekic, Michael J. Pomeroy, Stuart Hampshire
Abstract: Y-SiAlON glasses of composition 36.5 Y: 42.3 Si: 21.2 Al with different amounts of N
(0, 5, 8, 15 and 22 in e/o) were produced by melting appropriate mixtures of powders under flowing nitrogen at 1715°C. This composition is known to give B-phase (Y2SiAlO5N) on crystallisation at temperatures below 1050°C. In this work, the effect of nitrogen in the starting glass composition on the crystalline phases formed is discussed. High temperature in-situ XRD analysis was performed on powdered glass samples up to 1150°C by using a Philips X’pert PRO MPD (Multi Purpose Diffractometer) with a HTK1200 Oven Camera (Anton Paar, Austria). As expected, the results show that different nitrogen contents affect the crystalline phases formed. In all glasses, yttrium apatite silicate forms first, followed by crystallisation of B-phase. The phase transformation from B-phase to Iw-phase (Y3Si2Al[O,N10] i.e. 10 e/o N) takes place at relatively low temperatures (1050°C) for the lower nitrogen containing samples (5 and 8 e/o), whereas, the transformation does not take place for the glasses with higher nitrogen contents even at the maximum temperature studied (1150°C). This work also confirms that there is a correlation between the temperature where the first crystals appear and the amount of nitrogen in the starting glass.
293
Authors: E. Dolekcekic, Michael J. Pomeroy, Stuart Hampshire
1863
Authors: A. Díaz, E. Dolekcekic, Michael J. Pomeroy, Stuart Hampshire
247
Authors: A. Díaz, Yvonne Menke, Stuart Hampshire
79
Authors: M.F. Gonon, Jean-Claude Descamps, F. Cambier, Derek P. Thompson
325
Authors: W.T. Young, L.K.L. Falk, H. Lemercier, Stuart Hampshire
289