薄层化碳布缝合碳/碳复合材料制备与性能

刘宇峰; 李同起; 冯志海; 王金明; 张莹; 王雅雷; 熊翔

doi:10.13801/j.cnki.fhclxb.20200713.005

薄层化碳布缝合碳/碳复合材料制备与性能

doi: 10.13801/j.cnki.fhclxb.20200713.005

刘宇峰^{1, 2, ,},
李同起^2,,
冯志海²,
王金明^2,,
张莹^2,,
王雅雷^1,,
熊翔^1,

1.
中南大学　粉末冶金研究院，长沙 410083
2.
航天材料及工艺研究所　先进功能复合材料技术重点实验室，北京 100076

基金项目: 装发共用技术预研项目(41422020106)；先进功能复合材料技术重点实验室基金(HTKJ2019KL703001)

详细信息

通讯作者:
刘宇峰，硕士，工程师，研究方向为新型碳纤维增强碳基、陶瓷基复合材料　E-mail：liuyufeng19890810@qq.com.

中图分类号: TB332；V254
计量
- 文章访问数: 1355
- HTML全文浏览量: 832
- PDF下载量: 155
- 被引次数: 0
出版历程
- 收稿日期: 2020-06-04
- 录用日期: 2020-07-07
- 网络出版日期: 2020-07-13
- 刊出日期: 2021-04-08

Preparation and properties of spreading carbon cloth stitched C/C composites

LIU Yufeng^{1, 2
, ,},
LI Tongqi^2
,,
FENG Zhihai²,
WANG Jinming^2
,,
ZHANG Ying^2
,,
WANG Yalei^1
,,
XIONG Xiang^1
,

1.
Powder Metallurgy Research Institute, Central South University, Changsha 410083, China
2.
Science and Technology of Advanced Functional Composites Laboratory, Aerospace Research Institute of Materials and Processing Technology, Beijing 100076, China

摘要

摘要: 为获得高性能、低成本碳/碳复合材料，以商用级T700大丝束薄层化碳纤维展宽平纹布和航空航天级T300小丝束碳纤维缎纹布为原材料制备缝合预制体，采用化学气相沉积工艺方法制备了一系列缝合碳/碳复合材料，对材料的气相致密化特征、微观结构特征和力学性能进行了测试与分析。研究结果表明，碳布规格和缝合间距对材料气相致密化效果和力学性能有较大影响。当选用T700-12 K、展宽16 mm大丝束纤维编织的面密度100 g/m²的平纹布为原材料且预制体缝合间距为5 mm×5 mm时，制备的密度为1.781 g/cm³薄层化碳布缝合碳/碳复合材料表现出良好的气相沉积工艺适应性和优异的力学性能，材料拉伸强度、压缩强度、弯曲强度和层间剪切强度高达342.9 MPa、285.5 MPa、328.4 MPa和15.2 MPa。通过商用级大丝束薄层化碳纤维的应用，大幅降低了高性能碳/碳复合材料的原材料成本，且制备的碳/碳复合材料性能达到了国际先进水平。
- 碳/碳复合材料 /
- 薄层化 /
- 缝合 /
- 化学气相沉积 /
- 力学性能
Abstract: In order to obtain high-performance and low-cost C/C composites, a series of preforms stitched with commercial grade large tow spreading carbon fiber cloth or aerospace grade small tow carbon fiber cloth were prepared. The carbon cloth stitched C/C composites were prepared by chemical vapor deposition (CVD), and the densification characteristics, microstructure features and mechanical properties of stitched C/C composites were characterized and discussed. The investigation results show that the types of carbon cloth and stitching density have obvious effects on the densification and mechanical properties of stitched C/C composites. When the type of preform selects key characteristics as spreading fiber cloth T700-12 K-100 g and stitching density 5 mm×5 mm, the values of tensile strength, compression strength, flexural strength and interlaminar shear strength for stitched C/C composites (1.781 g/cm³) reach 342.9 MPa、285.5 MPa、328.4 MPa and 15.2 MPa respectively, which are the international advanced level. The cost of high-performance C/C composites is greatly reduced by using spreading carbon cloth.
- C/C composites /
- spreading /
- stitch /
- chemical vapor deposition /
- mechanical properties

HTML全文

图 1 T700-12 K碳纤维薄层化效果^[13]

Figure 1. Effects of spread tow of T700-12 K carbon fibers^[13]

下载: 全尺寸图片幻灯片

图 2 薄层化碳布(T700-12 K-100 g)

Figure 2. Spreading carbon cloth (T700-12 K-100 g)

下载: 全尺寸图片幻灯片

图 4 缝合预制体

Figure 4. Stitched preform

下载: 全尺寸图片幻灯片

图 5 缝合碳/碳复合材料

Figure 5. Stitched C/C composites

下载: 全尺寸图片幻灯片

图 3 缝合示意图

Figure 3. Diagram of stitching

下载: 全尺寸图片幻灯片

图 6 不同规格碳/碳复合材料的化学气相沉积(CVD)时间与密度关系曲线

Figure 6. Curves between density and chemical vapor deposition (CVD) time of different types C/C

下载: 全尺寸图片幻灯片

图 7 缝合间距对碳/碳复合材料增密效率的影响

Figure 7. Stitching density’s effects on the densification of C/C composites

下载: 全尺寸图片幻灯片

图 8 不同沉积时长T300-3 K碳/碳复合材料微观结构

Figure 8. Microstructures of C/C composites (T300-3 K) with different CVD reaction time

下载: 全尺寸图片幻灯片

图 9 热解碳封孔效应

Figure 9. Sealing effect of pyrocarbon

下载: 全尺寸图片幻灯片

图 10 500 h CVD后C/C复合材料截面形貌

Figure 10. Microstructures of C/C composites with 500 h CVD

下载: 全尺寸图片幻灯片

图 11 缝合线周边微观结构形貌

Figure 11. Microstructure around stitching fiber

下载: 全尺寸图片幻灯片

图 12 碳/碳复合材料薄层化效果

Figure 12. Spreading effects on C/C composites

下载: 全尺寸图片幻灯片

图 13 缝合碳/碳复合材料拉伸力学性能试样

Figure 13. Tensile specimens of stitched C/C compositess

下载: 全尺寸图片幻灯片

图 14 典型C/C复合材料拉伸断口形貌

Figure 14. Tensile fracture morphologies of C/C composites

下载: 全尺寸图片幻灯片

图 15 缝合线造成的预制体缺陷

Figure 15. Defects caused by stitching

下载: 全尺寸图片幻灯片

图 16 典型C/C复合材料弯曲破坏形貌

Figure 16. Flexural fracture morphologies of C/C composites

下载: 全尺寸图片幻灯片

表 1 不同预制体结构参数

Table 1. Parameters of stitched preform

No.	Types of preform	Types of fiber	Areal density of carbon cloth/(g·m⁻²)	Stitching density/ mm
1	T300-3 K-320 g-5	T300-3 K	320	5×5
2	T300-1 K-160 g-5	T300-1 K	160	5×5
3	T700-12 K-100 g-5	T700-12 K	100	5×5
4	T700-12 K-100 g-10	T700-12 K	100	10×10
5	T700-12 K-100 g-15	T700-12 K	100	15×15
6	T700-12 K-100 g-20	T700-12 K	100	20×20
7	T700-12 K-100 g-25	T700-12 K	100	25×25
8	T700-12 K-100 g-40	T700-12 K	100	40×40
9	T700-12 K-90 g-5	T700-12 K	90	5×5
10	T700-12 K-80 g-5	T700-12 K	80	5×5

下载: 导出CSV

表 2 不同种碳布实测参数

Table 2. Parameters of different carbon cloths

Type of fiber	T300-3 K	T300-1 K	T700-12 K
Fiber linear density/tex	198	66	797
Tensile strength of fiber/GPa	4.09	3.85	5.05
Tensile modulus of fiber/GPa	232.5	233.5	227.0
Fracture elongation of fiber/%	1.76	1.84	2.00
Spreading width of fiber/mm	−	−	16	18	20
Tensile strength of spreading fiber/GPa	−	−	5.01	4.96	4.89
Strength retention/%	−	−	99.2	98.2	96.3
Type of carbon cloth	Satin cloth		Plain cloth
Areal density of carbon cloth/(g·m⁻²)	320	160	100	90	80
Thickness of carbon cloth/mm	0.31	0.17	0.11	0.091	0.075
Tensile strength of carbon cloth(warp)/(N·50mm⁻¹)	5 604	3241	3639	3406	2706
Tensile strength of carbon cloth(weft)/(N·50mm⁻¹)	5 432	3335	3580	3354	2936

下载: 导出CSV

表 3 不同预制体结构参数及最终碳/碳复合材料密度

Table 3. Parameters of stitched preform and density of C/C composites

No.	Type of fiber	Areal density of carbon cloth/(g·m⁻²)	Stitching density/ mm	Layer density/ layer/cm	Theoretical fiber volume fraction/vol%	Experimental fiber volume fraction/vol%	Density of C/C composites/ (g·cm⁻³)
1	T300-3 K	320	5×5	24.9	45.3	46.9	1.637
2	T300-1 K	160	5×5	50.2	45.6	48.1	1.682
3	T700-12 K	100	5×5	81.8	46.0	45.7	1.781
4	T700-12 K	100	10×10	86.5	48.6	48.2	1.731
5	T700-12 K	100	15×15	90.0	50.6	50.0	1.675
6	T700-12 K	100	20×20	89.5	50.3	49.7	1.624
7	T700-12 K	100	25×25	90.5	50.8	50.3	1.571
8	T700-12 K	100	40×40	89.3	50.2	49.6	1.542
9	T700-12 K	90	5×5	95.7	48.4	47.8	1.754
10	T700-12 K	80	5×5	109.8	49.3	49.0	1.737

下载: 导出CSV

表 4 碳/碳复合材料力学性能

Table 4. Mechanical properties of C/C composites

No.	Tensile			In-plane compression		Flexural		Interlaminar shear strength/MPa
No.	Strength/ MPa	Discrete values	Modulus/ GPa	Strength/ MPa	Modulus/ GPa	Strength/ MPa	Modulus/ GPa	Interlaminar shear strength/MPa
1	141.3	13.1%	52.8	121.2	65.0	132.3	50.5	7.2
2	237.4	14.6%	61.4	176.2	63.8	196.3	52.9	19.7
3	342.9	5.30%	67.6	285.5	63.8	328.4	53.8	15.2
4	366.6	5.90%	73.9	256.8	60.1	216.4	56.9	11.7
5	298.3	10.7%	63.9	177.2	57.4	186.9	52.5	7.9
6	196.1	21.2%	52.3	99.1	45.9	112.1	30.8	5.0
7	150.1	18.6%	53.1	56.8	42.9	33.1	18.1	4.5
8	139.2	16.9%	43.6	54.8	48.7	27.9	11.2	3.5
9	351.3	7.10%	70.9	259.1	62.6	307.7	54.1	14.7
10	324.1	6.50%	62.8	241.6	59.1	227.0	52.9	12.9

下载: 导出CSV

参考文献(20)

[1]	杜善义. 先进复合材料与航空航天[J]. 复合材料学报, 2007, 24(1):1-12. doi: 10.3321/j.issn:1000-3851.2007.01.001 DU Shanyi. Advanced composite materials and aerospace engineering[J]. Acta Materiae Compositae Sinica,2007,24(1):1-12(in Chinese). doi: 10.3321/j.issn:1000-3851.2007.01.001
[2]	冯志海. 关于我国高性能碳纤维需求和发展的几点想法[J]. 新材料产业, 2010(9):19-24. doi: 10.3969/j.issn.1008-892X.2010.09.005 FENG Zhihai. Ideas on the demand and development of high performance carbon fiber in China[J]. Advanced Materials Industry,2010(9):19-24(in Chinese). doi: 10.3969/j.issn.1008-892X.2010.09.005
[3]	李贺军. 炭/炭复合材料[J]. 新型炭材料, 2001, 16(2):79-80. doi: 10.3321/j.issn:1007-8827.2001.02.017 LI Hejun. Carbon/carbon composites[J]. New carbon materials,2001,16(2):79-80(in Chinese). doi: 10.3321/j.issn:1007-8827.2001.02.017
[4]	SHARMA R, RAVIKUMAR N L, DASGUPTA K, et al. Advanced carbon-carbon composites: Processing properties and applications[J]. Composite Materials,2016(4):315-367.
[5]	徐林, 杨文彬, 陈铮, 等. 高性能二维碳/碳复合材料的制备与性能[J]. 复合材料学报, 2016, 33(12):2877-2883. XU Lin, YANG Wenbin, CHEN Zheng, et al. Preparation and properties of high performance two-dimensional carbon/carbon composites[J]. Acta Materiae Compositae Sinica,2016,33(12):2877-2883(in Chinese).
[6]	嵇阿琳, 李贺军, 崔红, 等. 不同预制体结构C/C复合材料轴向热力学性能分析[J]. 无机材料学报, 2010, 25(9):994-998. doi: 10.3724/SP.J.1077.2010.00994 JI Alin, LI Hejun, CUI Hong, et al. Axial thermodynamic performance analysis of the different preform C/C compo-sites[J]. Journal of Inorganic Materials,2010,25(9):994-998(in Chinese). doi: 10.3724/SP.J.1077.2010.00994
[7]	刘宇峰, 俸翔, 王金明, 等. 高性能针刺碳/碳复合材料的制备与性能[J], 无机材料学报, 2020, 35(10): 1105-1111. LIU Yufeng, FENG Xiang, WANG Jinming, et al. Preparation and properties of high-performance needled C/C composites[J]. Journal of Inorganic Materials, 2020, 35(10): 1105-1111(in Chinese).
[8]	罗云烽, 孙永春, 段跃新, 等. 大丝束碳纤维薄层化技术[J]. 复合材料学报, 2010, 27(1):123-128. LUO Yunfeng, SUN Yongchun, DUAN Yuexin, et al. A technology used in spreading large tow carbon fibers[J]. Acta Materiae Compositae Sinica,2010,27(1):123-128(in Chinese).
[9]	LIFKE J L, BUSSELLE L D, FINLEY D J, et al. Method and apparatus for spreading fiber: United States, 6049956[P]. 2000-04-18.
[10]	SIHNA S, KIMA R Y, TSAI S W, et al. Experimental studies of thin ply laminated composites[J]. Composites Science and Technology,2007,67:996-1008. doi: 10.1016/j.compscitech.2006.06.008
[11]	杨薇薇, 于亮, 郭志强. 薄层碳纤维织物预浸料的制备与性能[J]. 纤维复合材料, 2017, 9(3):8-11. doi: 10.3969/j.issn.1003-6423.2017.03.002 YANG Weiwei, YU Liang, GUO Zhiqiang. Preparation and properties of thin ply carbon fiber fabric prepreg[J]. Fiber Composites,2017,9(3):8-11(in Chinese). doi: 10.3969/j.issn.1003-6423.2017.03.002
[12]	罗云烽, 孙永春, 段跃新, 等. 薄层化大丝束碳纤维复合材料性能研究[J]. 航空制造技术, 2010, 20:75-78. doi: 10.3969/j.issn.1671-833X.2010.02.014 LUO Yunfeng, SUN Yongchun, DUAN Yuexin, et al. Study on property of spreaded large tow carbon fiber compo-sites[J]. Aeronautical Manufacturing Technology,2010,20:75-78(in Chinese). doi: 10.3969/j.issn.1671-833X.2010.02.014
[13]	刘军, 朱星名, 胡伯仁, 等. 基于超声引导法的薄层化碳纤维性能研究[J]. 热加工工艺, 2014, 43(8):108-119. LIU Jun, ZHU Xingming, HU Boren, et al. Research on property of spread carbon fiber based on supersonic and traction method[J]. Hot Working Technology,2014,43(8):108-119(in Chinese).
[14]	孙乐, 王成, 李晓飞, 等. C/C复合材料预制体的研究进展[J]. 航空材料学报, 2018, 38(2):86-95. doi: 10.11868/j.issn.1005-5053.2017.000010 SUN L, WANG C, LI X F, et al. Research progress on preforms of C/C composites[J]. Journal of Aeronautical Materials,2018,38(2):86-95(in Chinese). doi: 10.11868/j.issn.1005-5053.2017.000010
[15]	吴宁宁, 张中伟, 梅敏, 等. 缝合结构碳/碳复合材料层间性能测试方法研究[C]. 第六届无机材料结构、性能及测试表征技术研讨会, 2015. WU Ningning, ZHANG Zhongwei, MEI Min, et al. Study on interlaminar properties testing method of stitched C/C composites[C]. TEIM 2015(in Chinese).
[16]	房金铭, 许正辉, 张中伟, 等. 碳布缝合预制体孔隙与热解碳沉积时变相依的多尺度研究[J]. 宇航材料工艺, 2015, 45(5):36-39. doi: 10.3969/j.issn.1007-2330.2015.05.007 FANG Jinming, XU Zhenghui, ZHANG Zhongwei, et al. Multi-scale relationship of pores in carbon cloth stitched preform and deposition of pyrocarbon[J]. Aerospace Materials and Technology,2015,45(5):36-39(in Chinese). doi: 10.3969/j.issn.1007-2330.2015.05.007
[17]	航天材料及工艺研究所. 细编穿刺碳/碳复合材料拉伸试验方法: DqES415—2005[S]. 北京: 航天材料及工艺研究所, 2005. Aerospace Research Institute of Materials and Processing Technology. Test method for tensile properties of fine weave pierced carbon/carbon composites: DqES415—2005[S]. Beijing: Aerospace Research Institute of Materials and Processing Technology, 2005(in Chinese).
[18]	国防科学技术工业委员会. 连续纤维增强陶瓷基复合材料常温压缩性能试验方法: GJB 6476—2008[S]. 北京: 国防科学技术工业委员会, 2008. State Administration of Science Technology and Industry for National Defense. Test method for compressive properties of continuous fiber-reinforced ceramic composites at ambient temperature: GJB 6476—2008[S]. Beijing: State Administration of Science Technology and Industry for National Defense, 2008(in Chinese).
[19]	American Society for Testing and Materials International. Standard method for flexural properties of continuous fiber-reinforced advanced ceramic composites: ASTM C1341—00[S]. West Conshohocken: ASTM International, 2000.
[20]	中华人民共和国工业和信息化部. 纤维增强塑料短梁法测定层间剪切强度: JC/T 773—2010[S]. 北京: 中国建材工业出版社, 2010. Ministry of Industry and Information Technology of the People’s Republic of China. Fiber-reinforced plastics composites-Determination of apparent interlaminar shear strength by short-beam method: JC/T 773—2010[S]. Beijing: China Building Materials Press, 2010(in Chinese).