碳纤维布表面PyC界面相微观结构及均匀性的工艺调控

doi:10.15541/jim20230512

无机材料学报 ›› 2024, Vol. 39 ›› Issue (4): 399-408.DOI: 10.15541/jim20230512 CSTR: 32189.14.10.15541/jim20230512

碳纤维布表面PyC界面相微观结构及均匀性的工艺调控

薛轶凡¹(), 李玮洁²(), 张中伟¹(), 庞旭¹, 刘愚³

1.北京理工大学先进结构技术研究院, 北京 100081
2.北京交通大学土木建筑工程学院, 北京 100044
3.中南大学粉末冶金研究院, 粉末冶金国家重点实验室, 长沙 410083

收稿日期:2023-11-03 修回日期:2024-01-01 出版日期:2024-04-20 网络出版日期:2024-01-08
通讯作者: 李玮洁, 副教授, E-mail: wj.li@bjtu.edu.cn;
张中伟, 研究员. E-mail: zhangzhongw@163.com
作者简介:薛轶凡(1999-), 男, 硕士研究生. E-mail: 3120211981@bit.edu.cn
基金资助:
国家重点研发计划(2022YFB3706100)

Process Control of PyC Interphases Microstructure and Uniformity in Carbon Fiber Cloth

XUE Yifan¹(), LI Weijie²(), ZHANG Zhongwei¹(), PANG Xu¹, LIU Yu³

1. Institute of Advanced Structure Technology, Beijing Institute of Technology, Beijing 100081, China
2. School of Civil Engneering, Beijing Jiaotong University, Beijing 100044, China
3. State Key Laboratory of Powder Metallurgy, Powder Metallurgy Research Institute, Central South University, Changsha 410083, China

Received:2023-11-03 Revised:2024-01-01 Published:2024-04-20 Online:2024-01-08
Contact: LI Weijie, associate professor. E-mail: wj.li@bjtu.edu.cn;
ZHANG Zhongwei, professor. E-mail: zhangzhongw@163.com
About author:XUE Yifan (1999-), male, Master candidate. E-mail: 3120211981@bit.edu.cn
Supported by:
National Key Research and Development Program of China(2022YFB3706100)

摘要/Abstract

摘要：

陶瓷基复合材料力学性能与界面相的微观结构和均匀性有密切关系。本研究在碳纤维布表面沉积PyC界面相, 探究沉积温度、丙烯分压、滞留时间和氢气分压等工艺参数对PyC界面相微观结构及均匀性的影响规律。使用多种手段对PyC界面相微观形貌、织构进行表征, 并分析了微观结构、均匀性与工艺参数之间的内在关联。结果表明: 界面相织构的规整度随沉积温度和丙烯分压的提高而提高, 随氢气分压的提高而降低, 而受滞留时间影响较小; 沉积温度和丙烯分压升高均导致界面相厚度分布更加不均匀, 且丙烯分压过高会直接产生炭黑, 延长滞留时间有利于提高界面相的均匀性; 对于中织构和高织构, 随着氢气分压提高, 界面相均匀性先降低后增加, 而低织构的界面相均匀性受其影响较小。最后, 阐明了PyC界面相生长模式, 揭示了工艺参数对PyC界面相织构形态及均匀性的影响规律, 为PyC界面相的精细调控提供了基础。

关键词: 陶瓷基复合材料, PyC界面相, 均匀性, 微观结构

Abstract:

Mechanical properties of ceramic matrix composites are highly dependent on the microstructure and homogeneity of the interphase. This study examined the influence of process factors, such as deposition temperature, propylene partial pressure, retention time, and hydrogen partial pressure, on the microstructure and homogeneity of PyC interphase deposited on the surface of carbon fiber cloth. Various characterization techniques were used to characterize the microstructure and texture of the PyC interphase, and the inherent correlation between microstructure, uniformity, and process parameters was analyzed. The results show that increasing temperature and propylene partial pressure lead to a more regular texture in the interphase, while decreasing hydrogen partial pressure has the opposite effect, and retention time has little effects. Additionally, an increase in deposition temperature and propylene partial pressure leads to an uneven distribution of interphase thickness, and overhigh propylene partial pressure directly leads to the production of carbon black. Increasing retention time helps to improve interphase homogeneity. The interphase uniformity of medium and high textures firstly drops and then increases when the hydrogen partial pressure increases, but the interphase uniformity of low texture is less impacted. Ultimately, the study clarified the growth method of the PyC interphase. Furthermore, the research delved into the process factors influencing the texture and uniformity of the PyC interphase, which provided a basis for the fine regulation of PyC interface phase in the future.

Key words: ceramic matrix composite, PyC interphase, uniformity, microstructure

中图分类号:

TQ174

薛轶凡, 李玮洁, 张中伟, 庞旭, 刘愚. 碳纤维布表面PyC界面相微观结构及均匀性的工艺调控[J]. 无机材料学报, 2024, 39(4): 399-408.

XUE Yifan, LI Weijie, ZHANG Zhongwei, PANG Xu, LIU Yu. Process Control of PyC Interphases Microstructure and Uniformity in Carbon Fiber Cloth[J]. Journal of Inorganic Materials, 2024, 39(4): 399-408.

图/表 33

图1 模具示意图

Fig. 1 Schematic diagram of mold

表1 实验设计参数

Table 1 Design parameters for experiment

Group	T/℃	p_C3H6/kPa	τ/s	p_H2/kPa
1	950	5	3	0
2	950	3	3	0
3	950	3	1	0
4	950	1	1	0
5	950	0.5	1	0
6	950	1	3	0
7	950	1	0.5	0
8	900	3	1	0
9	900	1	0.5	0
10	900	1	3	0
11	900	1	1	0
12	850	1	0.5	0
13	850	1	1	0
14	850	1	3	0
15	950	3	3	1.5
16	950	3	3	3
17	950	1	3	0.5
18	950	1	3	1
19	900	3	1	1.5
20	900	3	1	3

图2 三个典型代表样品的TEM表征结果

Fig. 2 TEM charaterizations of three typical samples (a) SEM image of interphase, (b) HRTEM image of interphase and (c) Fourier transform of HT (Group 2); (d) SEM image of interphase, (e) HRTEM image of interphase and (f) Fourier transform of MT (Group 4); (g) SEM image of interphase, (h) HRTEM image of interphase and (i) Fourier transform of LT (Group 8)

表2 PyC界面相XRD半峰全宽、拉曼光谱R(R=ID/IG)汇总及织构分类

Table 2 Summary of XRD FWHM and R (R=ID/IG) for Raman spectra of PyC interphases, and texture classifications

	1	2	3	4	5	6	7	8	9	10
XRD FWHM/(°)	5.522	5.495	5.217	5.664	5.809	5.579	5.469	5.805	5.883	5.942
I_D/I_G	0.995	0.979	0.991	0.988	0.998	1.021	0.991	0.994	1.001	1.050
Texture	HT			MT				LT
	11	12	13	14	15	16	17	18	19	20
XRD FWHM/(°)	5.926	6.056	5.873	5.940	5.518	5.597	5.623	5.961	5.773	5.914
I_D/I_G	1.028	1.031	1.037	1.033	0.978	0.974	1.011	0.992	1.012	1.003
Texture	LT				HT		MT	LT

图3 不同工艺制备的碳纤维表面PyC界面相的(a)XRD图谱和(b)Raman图谱

Fig. 3 (a) XRD patterns and (b) Raman spectra of PyC interphase on carbon fiber prepared by different fabrication processes

图4 (a)低织构, (b)中织构和(c)高织构的沉积机理及边界条件

Fig. 4 Deposition mechanism and boundary conditions for (a) LT, (b) MT and (c) HT

图5 (a)夹具摆放示意图, (b)夹具主视图和(c)纤维织物取样位置

Fig. 5 (a) Fixture layout diagram, (b) fixture main view and (c) sampling position of fiber fabric

图6 不同温度下PyC界面相的沉积速率, 均匀性及其典型横截面SEM照片

Fig. 6 Deposition rate, uniformity and typical SEM images of cross-section of PyC interphases at various temperatures

图7 不同丙烯分压下PyC界面相的沉积速率, 均匀性及其典型横截面的SEM照片

Fig. 7 Deposition rate, uniformity and typical SEM images of cross-section of PyC interphases at various pC3H6

图8 不同滞留时间下PyC界面相的沉积速率, 均匀性及其典型横截面SEM照片

Fig. 8 Deposition rate, uniformity and typical SEM images of cross-section of PyC interphases at various residence time

图9 不同丙烯分压和氢气分压比例下PyC界面相的沉积速率, 均匀性及其典型横截面SEM照片

Fig. 9 Deposition rate, uniformity and typical SEM images of cross-section of PyC interphases at various pC3H6 : pH2

图10 界面相沉积速率, 沉积均匀性与PyC界面相织构之间的关系

Fig 10 Relationship between interphase deposition rate, deposition uniformity and texture of PyC interphase

图11 界面相均匀性的影响因素及其与工艺参数之间的关系

Fig. 11 Influence factors of interphase uniformity and their relations with process parameters

图S1 组1 SEM照片

Fig. S1 Group 1 SEM images

图S2 组2 SEM照片

Fig. S2 Group 2 SEM images

图S3 组3 SEM

Fig. S3 Group 3 SEM images

图S4 组4 SEM照片

Fig. S4 Group 4 SEM images

图S5 组5 SEM照片

Fig. S5 Group 5 SEM images

图S6 组6 SEM照片

Fig. S6 Group 6 SEM images

图S7 组7 SEM照片

Fig. S7 Group 7 SEM images

图S8 组8 SEM照片

Fig. S8 Group 8 SEM images

图S9 组9 SEM照片

Fig. S9 Group 9 SEM images

图S10 组10 SEM照片

Fig. S10 Group 10 SEM images

图S11 组11 SEM照片

Fig. S11 Group 11 SEM images

图S12 组12 SEM照片

Fig. S12 Group 12 SEM images

图S13 组13 SEM照片

Fig. S13 Group 13 SEM images

图S14 组14 SEM照片

Fig. S14 Group 14 SEM images

图S15 组15 SEM照片

Fig. S15 Group 15 SEM images

图S16 组16 SEM照片

Fig. S16 Group 16 SEM images

图S17 组17 SEM照片

Fig. S17 Group 17 SEM images

图S18 组18 SEM照片

Fig. S18 Group 18 SEM images

图S19 组19 SEM照片

Fig. S19 Group 19 SEM images

图S20 组20 SEM照片

Fig. S20 Group 20 SEM images

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碳纤维布表面PyC界面相微观结构及均匀性的工艺调控

Process Control of PyC Interphases Microstructure and Uniformity in Carbon Fiber Cloth

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Group	T/℃	p_C3H6/kPa	τ/s	p_H2/kPa
1	950	5	3	0
2	950	3	3	0
3	950	3	1	0
4	950	1	1	0
5	950	0.5	1	0
6	950	1	3	0
7	950	1	0.5	0
8	900	3	1	0
9	900	1	0.5	0
10	900	1	3	0
11	900	1	1	0
12	850	1	0.5	0
13	850	1	1	0
14	850	1	3	0
15	950	3	3	1.5
16	950	3	3	3
17	950	1	3	0.5
18	950	1	3	1
19	900	3	1	1.5
20	900	3	1	3

Group	T/℃	p_C3H6/kPa	τ/s	p_H2/kPa
1	950	5	3	0
2	950	3	3	0
3	950	3	1	0
4	950	1	1	0
5	950	0.5	1	0
6	950	1	3	0
7	950	1	0.5	0
8	900	3	1	0
9	900	1	0.5	0
10	900	1	3	0
11	900	1	1	0
12	850	1	0.5	0
13	850	1	1	0
14	850	1	3	0
15	950	3	3	1.5
16	950	3	3	3
17	950	1	3	0.5
18	950	1	3	1
19	900	3	1	1.5
20	900	3	1	3

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Group	T/℃	p_C3H6/kPa	τ/s	p_H2/kPa
1	950	5	3	0
2	950	3	3	0
3	950	3	1	0
4	950	1	1	0
5	950	0.5	1	0
6	950	1	3	0
7	950	1	0.5	0
8	900	3	1	0
9	900	1	0.5	0
10	900	1	3	0
11	900	1	1	0
12	850	1	0.5	0
13	850	1	1	0
14	850	1	3	0
15	950	3	3	1.5
16	950	3	3	3
17	950	1	3	0.5
18	950	1	3	1
19	900	3	1	1.5
20	900	3	1	3

Group	T/℃	p_C3H6/kPa	τ/s	p_H2/kPa
1	950	5	3	0
2	950	3	3	0
3	950	3	1	0
4	950	1	1	0
5	950	0.5	1	0
6	950	1	3	0
7	950	1	0.5	0
8	900	3	1	0
9	900	1	0.5	0
10	900	1	3	0
11	900	1	1	0
12	850	1	0.5	0
13	850	1	1	0
14	850	1	3	0
15	950	3	3	1.5
16	950	3	3	3
17	950	1	3	0.5
18	950	1	3	1
19	900	3	1	1.5
20	900	3	1	3

Group	T/℃	p_C3H6/kPa	τ/s	p_H2/kPa
1	950	5	3	0
2	950	3	3	0
3	950	3	1	0
4	950	1	1	0
5	950	0.5	1	0
6	950	1	3	0
7	950	1	0.5	0
8	900	3	1	0
9	900	1	0.5	0
10	900	1	3	0
11	900	1	1	0
12	850	1	0.5	0
13	850	1	1	0
14	850	1	3	0
15	950	3	3	1.5
16	950	3	3	3
17	950	1	3	0.5
18	950	1	3	1
19	900	3	1	1.5
20	900	3	1	3

Group	T/℃	p_C3H6/kPa	τ/s	p_H2/kPa
1	950	5	3	0
2	950	3	3	0
3	950	3	1	0
4	950	1	1	0
5	950	0.5	1	0
6	950	1	3	0
7	950	1	0.5	0
8	900	3	1	0
9	900	1	0.5	0
10	900	1	3	0
11	900	1	1	0
12	850	1	0.5	0
13	850	1	1	0
14	850	1	3	0
15	950	3	3	1.5
16	950	3	3	3
17	950	1	3	0.5
18	950	1	3	1
19	900	3	1	1.5
20	900	3	1	3