High-throughput Microstructural Characterization of xSi-BN Coated SiC Fibers by Combining Scanning Electron Microscopy and Laser Scanning Confocal Microscopy

doi:10.15541/jim20250457

Abstract

Abstract: BN interphase serves as a key component of SiC_f/SiC composite materials. Optimizing its composition and microstructure is essential for enhancing the comprehensive performance and reliability of ceramic matrix composites. In this investigation, we developed an optoelectric combination technology by combining scanning electron microscopy and laser scanning confocal microscopy through calibration and intelligent positioning, which can characterize the same area of the fiber at multiple scales. Key information, such as the surface roughness, micromorphology, and elemental distribution of BN interphase, was obtained. By establishing a unified planar coordinate system, it increased the measurement speed by about 1.1 times, and allowed high-throughput analysis of 20 component sample areas in one hour. The research indicates that the input flow rate of Si precursor increased during preparation, the Si content in the xSi-BN interphase increased while the B content decreased. The introduction of Si leads to a decrease in the crystallinity of BN and an enhancement in its surface activity, thereby facilitating the absorption of oxygen from the air and the formation of protruding particles on the surface. Si doping significantly influences the layered structure and mechanical properties of BN. As the Si content reaches 8%, the “pop-in” phenomenon associated with interlayer sliding disappears, and the hardness of the xSi-BN interphase markedly decreases from 14.91 GPa to 8.06 GPa. At the Si content reaches 11%, the interfacial shear strength increases significantly from 32.76 MPa to 109.07 MPa. This technology provides an effective approach for the microstructural characterization of the compositional design, structural regulation, and performance optimization of the interphase in SiC_f/SiC composites.

Key words: scanning electron microscopy, laser scanning confocal microscopy, optoelectric combination high-throughput characterization, BN interphase

CLC Number:

TQ174

XU Jialong, QIN Hao, LUO Xinyi, XING Juanjuan, ZHANG Xiangyu, GU Hui. High-throughput Microstructural Characterization of xSi-BN Coated SiC Fibers by Combining Scanning Electron Microscopy and Laser Scanning Confocal Microscopy[J]. Journal of Inorganic Materials, DOI: 10.15541/jim20250457.

References

[1] WANG P R, LIU F Q, WANG H,et al. A review of third generation SiC fibers and SiC_f/SiC composites. Journal of Materials Science & Technology, 2019, 35(12): 2743.
[2] WANG X L, GAO X D, ZHANG Z H, et al. Advances in modifications and high-temperature applications of silicon carbide ceramic matrix composites in aerospace: a focused review. Journal of the European Ceramic Society, 2021, 41(9): 4671.
[3] MANOHARAN V, TAMILPERUVALATHAN S. Experimental investigation and prediction of ECDM parameters on fiber reinforced SiC composite using hybrid ERNN-based Sparrow Search Optimization. Materials Today Communications, 2023, 36: 106777.
[4] ZHAO G C, JIANG Z H, XI H F, et al. Ultrahigh-temperature mechanical behavior and failure mechanisms of SiC_f/SiC composites. Ceramics International, 2023, 49(23): 39391.
[5] WU S F, CHEN J X, ZHANG X L, et al. Recent advances in interphase engineering for improved behavior of SiC_f/SiC composites. Journal of the European Ceramic Society, 2024, 44(12): 6797.
[6] DING J X, MA X K, FAN X M, et al. Failure behavior of interfacial domain in SiC-matrix based composites. Journal of Materials Science & Technology, 2021, 88: 1.
[7] CHEN Y, QIU H P, CHEN M W,et al. SiC/SiC composite: matrix boron modification and mechanical properties. Journal of Inorganic Materials, 2025, 40(5): 504.
[8] CHEN M L, PAN L, XIA X D, et al. Boron nitride (BN) and BN based multiple-layer interphase for SiC_f/SiC composites: a review. Ceramics International, 2022, 48(23): 34107.
[9] YANG H T, LU Z L, BIE B X, et al. Microstructure and damage evolution of SiC_f/PyC/SiC and SiC_f/BN/SiC mini-composites: a synchrotron X-ray computed microtomography study. Ceramics International, 2019, 45(9): 11395.
[10] WEI J Y, ZHOU N, GAO M X, et al. Laser ablation of SiC/SiC ceramic matrix composites: morphological characterization, component evolution and oxidation mechanisms. Corrosion Science, 2024, 227: 111762.
[11] CHRISTENSEN V L, ZOK F W. Insights into internal[11] CHRISTENSEN V L, ZOK F W. Insights into internal oxidation of SiC/BN/SiC composites. Journal of the American Ceramic Society, 2022, 106(2): 1561-1575.
[12] DETWILER K N, OPILA E J.Oxidation of SiC/BN/SiC ceramic matrix composites in dry and wet oxygen at intermediate temperatures.Journal of the European Ceramic Society, 2022, 42(10): 4110-4120.
[13] CHENG X, ZHANG Q, YE F, et al. Recent progress on wet-oxygen corrosion resistance of SiC_f/SiC composites. Journal of Materials Research and Technology, 2024, 33: 4360-4388.
[14] JACOBSON N S, MORSCHER G N, BRYANT D R, et al. High‐Temperature Oxidation of Boron Nitride: II, Boron Nitride Layers in Composites. Journal of the American Ceramic Society, 2004, 82(6): 1473-1482.
[15] CHRISTENSEN V L, GAVALDA-DIAZ O, SKILLETT R,et al. Influence of BN microstructure on oxidation of SiC/BN/SiC composites. Journal of the American Ceramic Society, 2025, 108(3): e20230.
[16] STÖCKEL S, MARX G, GOEDEL W A. Coating of ceramic SiC, SiBNC, and Al₂O₃ fibers with SiBN using a continuous CVD process-influence of stoichiometry on stability against oxidation and hydrolysis. Chemical Vapor Deposition, 2007, 13(10): 553.
[17] 廖春景, 董绍明, 张翔宇, 等. 一种纤维增强陶瓷基复合材料界面相及其筛选方法: CN1113105257A.2021-07-13
[18] CHRISTENSEN V L, SAMUEL A F, HAN N,et al. Microstructure characterization and process-structure correlations in SiC/BN/SiC minicomposites. Acta Materialia, 2024, 264: 119589.
[19] LIU Y S, CHAI N, LI Z, et al. Effect of deposition temperature on deposition kinetics and mechanism of silicon boron nitride coating deposited from SiCl₄-BCl₃-NH₃-H₂-Ar mixture using low pressure chemical vapor deposition. Surface and Coatings Technology, 2015, 261: 295.
[20] SUN J, LIU W, LV X,et al. Characterization of BN interface and its effect on the mechanical behavior of SiC_f/SiC composites. Vacuum, 2023, 211.
[21] ZHANG Y H, HU J B, ZHOU L,et al. Influence of fiber surface properties of SiC_f/SiC composites on the interfacial debonding behavior. Journal of the European Ceramic Society, 2024, 44(2): 795.
[22] WU X C, ZHENG R X, LI L, et al. Research progress on In-situ monitoring of damage behavior of SiC_f/SiC ceramic matrix composites at high temperature environments. Journal of Inorganic Materials, 2024, 39(6): 609.
[23] Lü X, LI L, SUN J,et al. Microstructure and tensile behavior of (BN/SiC)n coated SiC fibers and SiC/SiC minicomposites. Journal of the European Ceramic Society, 2023, 43(5): 1828-1842.
[24] ISMAIL M Y, PATANEN M, KAUPPINEN S,et al. Surface analysis of tissue paper using laser scanning confocal microscopy and micro-computed topography. Cellulose, 2020, 27(15): 8989-9003.
[25] ZHANG W Y, REN Q, WAN W H, et al. High-throughput microstructure characterization of titanium alloy by a multi-dimensional information strategy. Materials Today Communications, 2024, 38: 108360.
[26] RODRíGUEZ M,GONZáLEZ C,et al. An experimental and numerical study of the influence of local effects on the application of the fibre push-in test. Philosophical Magazine, 2011, 91(7-9): 1293-1307.
[27] MUELLER W M, MOOSBURGER-WILL J, SAUSE M G R,et al. Microscopic analysis of single-fiber push-out tests on ceramic matrix composites performed with Berkovich and flat-end indenter and evaluation of interfacial fracture toughness. Journal of the European Ceramic Society, 2013, 33(2): 441.
[28] DE MEYERE R M G, GALE L, HARRIS S,et al. Optimizing the fiber push‐out method to evaluate interfacial failure in SiC/BN/SiC ceramic matrix composites. Journal of the American Ceramic Society, 2021, 104(6): 2741-2752.
[29] ZHANG S Y, LIU M, LUO Y X,et al. Theoretical prediction on structure evolution and optimal properties of silicon modified hexagonal boron nitride as interphase in SiC_f/SiC composite. Journal of the European Ceramic Society, 2022, 42(13): 5323.