Preparation method of ZrSiO4 anti-oxidation coating on surface of SiC fiber
An anti-oxidation coating and fiber surface technology, which is applied in the field of ceramic matrix composite materials to achieve the effect of improving anti-oxidation performance, reducing thermal damage and reducing synthesis temperature
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[0029] refer to Figure 1-Figure 8 , a preferred embodiment of the present invention, a SiC fiber surface ZrSiO 4 The preparation method of anti-oxidation coating comprises the following steps:
[0030] (1) ZrSiO 4 Preparation, reaction and aging of the precursor impregnating solution: tetraethyl silicate and zirconium chloride were used as silicon source and zirconium source, lithium fluoride was used as mineralizer, and absolute ethanol was used as solvent. Reflux in an oil bath to obtain ZrSiO 4 Precursor impregnation solution;
[0031] (2) SiC fiber surface degumming treatment: the SiC fiber used is the commercially available domestic second-generation SiC fiber, the specification is 1K;
[0032] (3) Use ZrSiO 4 Precursor impregnation solution dip coating SiC fiber: place the SiC fiber after surface degumming on ZrSiO 4 Ultrasonic impregnation in the precursor impregnation solution, and then pull the SiC fiber out of the impregnation solution at a speed of 50mm / min; ...
Embodiment 1
[0041] A kind of SiC fiber surface ZrSiO of the present invention 4 The preparation method of anti-oxidation coating comprises the following steps:
[0042] (1) ZrSiO 4 Preparation, reaction and aging of precursor impregnating solution: take TEOS and ZrCl with Si, Zr molar ratio of 1.2:1 4 ; LiF with a molar ratio of Li and Si of 3:10 is formulated into a precursor solution with a concentration of 0.2mol / L, and the specific operation is as follows: ZrCl 4 Mix with ethanol and filter, mix with LiF and TEOS, and filter again, reflux the filtered mixture at 118°C for 30 hours for non-hydrolytic polycondensation reaction, and age for 50 hours to obtain ZrSiO 4 Precursor impregnation sol;
[0043] (2) Degumming treatment on the surface of SiC fiber: place the SiC fiber in a tube furnace under high-purity Ar atmosphere at 600°C for 1h;
[0044] (3) Use ZrSiO 4 Precursor impregnation liquid dip-coating SiC fiber: place the fiber after degumming in step (2) in the impregnation so...
Embodiment 2
[0052] A kind of SiC fiber surface ZrSiO of the present invention 4 The preparation method of anti-oxidation coating comprises the following steps:
[0053] (1) ZrSiO 4 Preparation, reaction and aging of precursor impregnating solution: take TEOS and ZrCl with Si, Zr molar ratio of 1.2:1 4 ; LiF with a molar ratio of Li and Si of 3:10 is formulated into a precursor solution with a concentration of 0.2mol / L, and the specific operation is as follows: ZrCl 4 Mix with ethanol and filter, then mix with LiF and TEOS, then filter again, reflux the filtered mixture at 118°C for 30h for non-hydrolytic polycondensation reaction, and age for 50h to obtain ZrSiO 4 Precursor impregnation sol;
[0054] (2) SiC fiber surface degumming treatment: soak the SiC fiber in acetone at room temperature for 24 hours;
[0055] (3) Use ZrSiO 4 SiC fibers were impregnated with precursor impregnation solution: the fibers after degumming in step (2) were placed in the impregnation sol prepared in ste...
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