Preparation of the mullite coating precursor solution
All the materials used for mullite precursor synthesis were of
the AR grade. The mullite coating precursor solution was prepared
by mixing a mullite precursor sol with mullite powder, along with
other ingredients. The processing steps for synthesizing mullite
precursor sol are shown in Fig. 1. Tetraethoxysilane (TEOS) was
mixed with aluminum nitrate nonahydrate (ANN) and aluminum
acetate (2:5 molar ratio of ANN to aluminum acetate) in pure
ethanol medium in the stoichiometric ratio of mullite. Acetic acid
was added (0.1–0.2 mol/L) to promote gelation. After 6 h of refluxing
at 353 K, a milky, viscous monophasic sol was obtained. The
mullite precursor sol and 3/2-mullite powder (70–75 wt.% of the
Fig. 2. Surface XRD spectra of the as-prepared mullite coating on SiC-C/C.
total mixture) were mixed by high energy planetary ball-milling
at 300 rpm, with a crack-sealing agent (polyvinylpyrrolidon, PVP,
average molecular weight of 1.3×106 g/mol, about 0.1–0.25 wt.%)
and oxalic acid (3–5 wt.%) as drying control chemical additive
(DCCA). Ball milling was performed for 4 h after the addition of all
the ingredient and, at the end of the ball-milling process, acetone
was added to reach an optimized solution viscosity. The solid concentration
in the optimized mullite coating precursor solution was
about 20 wt%.
The mullite powder was prepared by a sol–gel process and ANN
and TEOS were used as the starting materials. In short, the source
chemicals were dissolved in absolute ethanol in the molar ratio of
3:1 of ANN: TEOS (3/2-mullite) after which acetic acid was added
as a catalyst and chelating agent. Subsequently, the mixture was
heated in a water bath under reflux at 353K for 12 h to form a gel
which was then oven dried at 393K for 12 h and further fired at