xSi-BN/SiC纤维光电联用高通量表征

doi:10.15541/jim20250457

无机材料学报 ›› 2026, Vol. 41 ›› Issue (9): 1319-1329.DOI: 10.15541/jim20250457

xSi-BN/SiC纤维光电联用高通量表征

许嘉垅¹(), 秦浩², 罗昕沂¹, 邢娟娟¹(), 张翔宇²(), 顾辉³

¹ 上海大学材料科学与工程学院, 上海 200444
² 中国科学院上海硅酸盐研究所, 上海 201899
³ 北京高压科学中心, 北京 100094

收稿日期:2025-11-12 修回日期:2026-02-02 出版日期:2026-09-20 网络出版日期:2026-02-05
通讯作者: 邢娟娟, 副教授. E-mail: xingjuanjuan@shu.edu.cn;
张翔宇, 研究员. E-mail: xyzhang@mail.sic.ac.cn
作者简介:许嘉垅(2001-), 女, 硕士研究生. E-mail: xjlong_23@shu.edu.cn
基金资助:
国家重点研发计划(2022YFB3707700)

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

XU Jialong¹(), QIN Hao², LUO Xinyi¹, XING Juanjuan¹(), ZHANG Xiangyu²(), GU Hui³

¹ School of Materials Science and Engineering, Shanghai University, Shanghai 200444, China
² Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China
³ Center of High Pressure Science & Technology Advanced Research, Beijing 100094, China

Received:2025-11-12 Revised:2026-02-02 Published:2026-09-20 Online:2026-02-05
Contact: XING Juanjuan, associate professor. E-mail:xingjuanjuan@shu.edu.cn;ZHANG Xiangyu, professor. E-mail:xyzhang@mail.sic.ac.cn
About author:XU Jialong (2001-), female, Master candidate. E-mail: xjlong_23@shu.edu.cn
Supported by:
National Key R&D Program of China(2022YFB3707700)

摘要/Abstract

摘要：

BN界面相是SiC_f/SiC复合材料的关键组元, 优化成分与微观结构对改善其综合性能与可靠性至关重要。本研究开发了一种基于扫描电子显微镜和激光共聚焦显微镜的智能定位光电联用高通量表征技术, 能够对纤维表面同一区域实现多尺度表征, 获取BN界面相的表面粗糙度、微观形貌及元素组成等关键信息。该技术通过建立统一坐标系实现快速定位, 可在1 h内完成20个组分区域的多尺度分析, 整体表征效率提升约1.1倍。研究表明, 随着制备过程中Si前驱体的输入流量升高, xSi-BN界面相中Si含量增加, B含量相应降低。引入Si导致BN结晶度降低, 表面活性增强, 促使BN吸附空气中的氧并在表面形成凸起颗粒。Si掺杂对BN层状结构及其力学性能具有显著影响。随着Si含量增至8%, 与层间滑移相关的“pop-in”现象消失, 界面层硬度从14.91 GPa显著降低至8.06 GPa; 当Si含量达到11%时, 界面剪切强度从32.76 MPa大幅提升至109.07 MPa。该技术为SiC_f/SiC复合材料界面相的成分设计、结构调控与性能优化提供了有效的方法支撑。本文数据集可在 https://www.doi.org/10.57760/sciencedb.jim.00028中访问获取。

关键词: 扫描电子显微镜, 激光共聚焦显微镜, 光电联用高通量表征, BN界面相

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

中图分类号:

TQ174

许嘉垅, 秦浩, 罗昕沂, 邢娟娟, 张翔宇, 顾辉. xSi-BN/SiC纤维光电联用高通量表征[J]. 无机材料学报, 2026, 41(9): 1319-1329.

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.

图/表 11

图1 光电联用高通量表征技术示意图

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

图2 5 kV电压下电子束在BN界面相表面强度分布的蒙特卡洛模拟

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

图3 xSi-BN/SiC纤维的SEM照片(单数行)和LSCM照片(偶数行)

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

图4 xSi-BN/SiC纤维的高倍SEM照片和LSCM表面粗糙度图像

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

图5 xSi-BN/SiC纤维的(a) EDS面分布、(b) EDS线扫描及(c)截面SEM照片

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

表1 xSi-BN/SiC纤维的元素含量(原子百分比)

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

图6 xSi-BN界面相的TEM照片

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

图7 光电联用技术前后对比

Fig. 7 Comparison before and after the optoelectric combination

图8 样品Si0、Si8、Si11和Si17的载荷-位移曲线

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

图9 (a) Si8纳米压痕SPM图像(绿色区域为纳米压痕测试区); (b) 由纳米压痕测得的Si0、Si8、Si11和Si17的硬度

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

图10 (a, b) Si0 CMC和(c, d) Si11 CMC的(a, c)纤维推出强度-位移曲线、(b, d) LSCM表面3D视图和(e)界面剪切强度

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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xSi-BN/SiC纤维光电联用高通量表征

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

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