Matrix/Interface/Fiber Integrated Oxidation Mechanism of Mini-SiCf/BN/SiC in Water-oxygen Environment at 1100 ℃

doi:10.15541/jim20250249

Abstract

Abstract:

SiC_f/SiC composites exhibit advantages such as high-temperature resistance, oxidation resistance and high strength, making them a “star” candidate material in the field of aerospace thermal protection. Under operational conditions, these materials are subjected to prolonged multiple coupled fields such as heat, water and oxygen, exhibiting complex failure mechanisms and damage evolution patterns. This study investigated the integrated oxidation mechanism of the matrix/interface/fiber in Mini-SiC_f/BN/SiC composites under cyclic oxidation at 1100 ℃ in a water-oxygen coupled environment by using multi-scale macro/micro characterization techniques. The results showed that during the initial oxidation stage, an amorphous SiO₂ glass layer with relatively smooth morphology formed on the material surface. However, with an increase in crystallinity, localized spallation occurred in the oxide layer, causing the surface roughness to initial decrease and subsequent increase. X-ray microscope results showed that numerous micro-defects were generated within the material after cyclic oxidation, and the number of defects increased by orders of magnitude (about 107 fold). Majority of these micro-defects were mainly distributed on the matrix surface, and the oxidation products played a certain filling role in these defects. The tensile strength showed no significant variation before ((328.47±32.84) MPa) and after ((343.27±35.71) MPa) cyclic oxidation, indicating continued effectiveness of the synergistic toughening mechanism of “strong matrix-weak interface”. These observations indicate that an integrated oxidation protection mechanism involving matrix, interface and fiber exists in the Mini-SiC_f/BN/SiC, which is predicated on the filling of defects by SiO₂ and borosilicate glass generated by its interface layer and adjacent matrix with fibers in the direction parallel to the fiber axis. Dynamic “outer porous sacrificial layer-middle dense SiO₂-inner SiC matrix” is a three-dimensional protective barrier of the matrix in the direction perpendicular to the fiber axis. This dual-protection system substantially alleviates material degradation under cyclic thermal water oxidative conditions.

Key words: Mini-SiC_f/BN/SiC, cyclic oxidation, high-temperature water-oxygen environment, multi-scale representation, oxidation mechanism

CLC Number:

TB332

QI Fang, LIU Hui, WU Zhengmin, LU Yi, WU Wenwen, WANG Zhen. Matrix/Interface/Fiber Integrated Oxidation Mechanism of Mini-SiC_f/BN/SiC in Water-oxygen Environment at 1100 ℃[J]. Journal of Inorganic Materials, 2026, 41(3): 340-348.

Figures/Tables 14

Fig. 1 Schematic diagrams of the test for Mini-SiCf/BN/SiC (a) Location of SEM test; (b) Tensile test specimen

Fig. 2 SEM images (a, b) and EDS pattern (c) of the original Mini-SiCf/BN/SiC composite

Fig. 3 Relationship between mass change and cyclic oxidation time of Mini-SiCf/BN/SiC

Fig. 4 SEM images of Mini-SiCf/BN/SiC surface after cyclic oxidation for different time (a) 0 h; (b) 20 h; (c) 40 h; (d) 60 h; (e) 80 h; (f) 100 h

Fig. 5 Surface morphologies, 3D images and roughnesses of Mini-SiCf/BN/SiC after cyclic oxidation for different time (a, b) 0 h; (c, d) 20 h; (e, f) 40 h; (g, h) 60 h; (i, j) 80 h; (k, l) 100 h

Fig. 6 XRD patterns of Mini-SiCf/BN/SiC surface after cyclic oxidation for different time

Fig. 7 SEM images of the middle part of Mini-SiCf/BN/SiC (10 mm from the end) after cyclic oxidation for different time (a) 0 h; (b) 20 h; (c) 40 h; (d) 60 h; (e) 80 h; (f) 100 h

Fig. 8 SEM images and EDS patterns of Mini-SiCf/BN/SiC near the tip (1 mm away from the tip) after oxidation for 100 h (a, b) SEM images; (c) EDS-spot 1; (d) EDS-spot 2

Fig. 9 XRM analyses of Mini-SiCf/BN/SiC before oxidation (a) Overall diagram; (b-d) Slice diagrams; (e, f) Defect distribution diagrams; (g) Defect statistical diagram

Fig. 10 XRM analyses of Mini-SiCf/BN/SiC after oxidation for 100 h (a) Overall diagram; (b-d) Slice diagrams; (e, f) Defect distribution diagrams; (g) Defect statistical diagram

Fig. 11 Analysis of the proportion of defect volume with different sizes in Mini-SiCf/BN/SiC after oxidation for 0 and 100 h

Fig. 12 Oxidation mechanism of Mini-SiCf/BN/SiC in 1100 ℃ water oxygen environment

Fig. 13 Tensile strength histogram of Mini-SiCf/BN/SiC before and after oxidation

Fig. 14 Tensile fracture morphologies and EDS analyses of Mini-SiCf/BN/SiC before and after oxidation (a, b) 0 h; (c-f) 100 h

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