Optoelectric Combining High-throughput Microstructural Characterization of xSi-BN/SiC Fibers

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, and 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. When 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. The datasets in this article are listed in Science Data Bank at http://doi.org/10.57760/sciencedb.jim.00028.

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

CLC Number:

TQ174

XU Jialong, QIN Hao, LUO Xinyi, XING Juanjuan, ZHANG Xiangyu, GU Hui. Optoelectric Combining High-throughput Microstructural Characterization of xSi-BN/SiC Fibers[J]. Journal of Inorganic Materials, 2026, 41(9): 1319-1329.

Figures/Tables 11

Fig. 1 Schematic diagrams of optoelectric combination high-throughput characterization technology (a) Sample stage; (b) Sample placement diagram; (c) Schematic of the optoelectric combination. Colorful figures are available on website

Fig. 2 Monte Carlo simulation of the intensity distribution at BN interphase surface under 5 kV electron beam irradiation

Fig. 3 SEM (odd rows) and LSCM (even rows) images of the xSi-BN/SiC fibers

Fig. 4 High magnification SEM and LSCM roughness images of xSi-BN/SiC fibers Colorful figures are available on website

Fig. 5 (a) EDS mapping analysis, (b) EDS line scanning analysis and (c) SEM image of cross section for xSi-BN/SiC fibers Colorful figures are available on website

Table 1 Elemental content (atomic percent) of xSi-BN/SiC fibers

Sample	B/%	N/%	C/%	O/%	Si/%
1	/	/	57.70±0.73	1.84±0.11	40.46±0.83
2	40.12±0.79	47.97±0.37	8.69±0.39	2.63±0.11	0.58±0.15
3	39.71±0.65	46.11±0.93	10.00±0.01	3.13±0.46	1.05±0.18
4	37.37±0.15	44.90±0.41	11.98±0.57	4.30±0.18	1.45±0.11
5	39.91±0.42	45.44±0.52	10.03±0.14	3.13±0.18	1.49±0.10
6	37.37±0.64	43.99±0.28	10.84±0.21	5.47±0.25	2.31±0.10
7	34.20±0.53	36.41±0.86	16.92±1.61	10.08±0.08	2.39±0.08
8	38.27±0.37	43.30±0.32	11.18±0.27	4.29±0.05	2.95±0.10
9	36.10±1.31	42.57±0.90	10.21±0.69	8.13±0.14	2.98±0.06
10	36.06±1.01	42.07±0.66	10.76±0.38	7.87±0.35	3.26±0.12
11	36.28±0.53	41.56±0.39	12.12±0.79	6.75±0.18	3.28±0.13
12	36.91±1.04	40.99±1.45	12.05±0.31	5.71±0.23	4.34±0.19
13	33.68±0.45	42.06±0.53	11.62±0.51	7.93±0.58	4.72±0.01
14	33.53±0.71	35.59±0.84	12.61±0.11	13.50±0.38	4.77±0.21
15	31.52±0.81	36.99±0.33	13.07±0.42	12.17±0.90	6.26±0.44
16	31.54±0.22	36.71±0.26	10.66±0.24	14.52±0.30	6.57±0.27
17	32.02±0.81	38.51±0.83	11.20±0.35	11.41±0.32	6.87±0.06
18	30.70±0.45	38.21±0.50	11.52±0.36	12.38±0.44	7.19±0.39
19	32.72±0.81	42.95±0.24	8.83±0.11	8.08±0.39	7.42±0.12
20	30.05±0.58	44.08±0.38	8.82±0.31	8.37±0.46	8.68±0.28

Fig. 6 TEM images of xSi-BN interphase (a, b) Si0; (c, d) Si17

Fig. 7 Comparison before and after the optoelectric combination

Fig. 8 Load-displacement curves of Si0, Si8, Si11 and Si17 Colorful figure is available on website

Fig. 9 (a) Typical SPM image of Si8 ( the green area is designated as the nanoindentation test area); (b) Hardness of Si0, Si8, Si11 and Si17 measured by nanoindentation Colorful figures are available on website

Fig. 10 (a, c) Strength-displacement curves of fibers pull out tests, (b, d) surface LSCM 3D images and (e) ISS of (a, b) Si0 CMC and (c, d) Si11 CMC Colorful figures are available on website

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