热氧老化对纬编双轴向多层衬纱织物增强复合材料力学性能的影响

杨晨; 姜亚明; 项赫; 李佳楠

doi:10.13801/j.cnki.fhclxb.20220225.002

热氧老化对纬编双轴向多层衬纱织物增强复合材料力学性能的影响

doi: 10.13801/j.cnki.fhclxb.20220225.002

天津工业大学　纺织科学与工程学院，天津 300387

基金项目: 航空科学基金项目(201829Q2002)；天津自然科学基金(18JCZDJC10020)；中国国家留学基金项目(202008120134)

详细信息

通讯作者:
姜亚明，博士，教授，博士生导师，研究方向为先进纺织增强材料及其复合材料　E-mail: jiangyaming@tiangong.edu.cn

中图分类号: TB332
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出版历程
- 收稿日期: 2021-12-28
- 修回日期: 2022-02-05
- 录用日期: 2022-02-11
- 网络出版日期: 2022-02-28
- 刊出日期: 2023-01-15

Effect of thermo-oxidative aging on the mechanical properties of multi-layered biaxial weft knitted fabric reinforced composites

School of Textile Science and Engineering, Tiangong University, Tianjin 300387, China

Funds: Aeronautical Science Foundation of China (201829Q2002); Natural Science Foundation of Tianjin (18JCZDJC10020); China Scholarship Council (202008120134)

摘要

摘要: 通过改变预制体结构衬纱取向的方法制备了几种含不同剪切角的纬编双轴向多层衬纱(Multilayered biaxial weft knitted，MBWK)织物增强复合材料。基于Arrhenius模型和Ozawa法设计了热氧老化试验，采用力学性能测试、DSC、FTIR和DMA测试对老化前后的试样热-物理性能进行了表征。实验结果表明：预制体的纱线剪切角不同，其复合材料受热氧老化后力学性能的保留率也显著不同，由于乙烯基酯树脂在热氧老化环境中会发生后固化现象，因此复合材料的弯曲模量在老化过程中呈现先增加后下降的趋势，而拉伸性能则受到增强体结构的影响，纤维/基体界面的结合力退化使拉伸模量在老化过程中持续下降；随着老化时间的延长，树脂的固化度逐渐增加，玻璃化转变温度T_g逐渐升高，储能模量峰值在老化初期由于分子链交联上升，老化后期分子链断裂占据主导作用致使峰值逐渐下降。
- 纬编双轴向多层衬纱织物增强复合材料 /
- 芳纶纤维 /
- 热氧老化 /
- 力学性能 /
- 剪切角
Abstract: Several multilayered biaxial weft knitted (MBWK) fabric reinforced composites with different shear angles were prepared by changing the orientation of preform inserting yarns. The thermo-oxidative aging test was designed based on Arrhenius model and Ozawa method. The thermal and physical properties of the samples before and after aging were characterized by mechanical properties, DSC, FTIR and DMA tests. The experimental results show that: With the change of yarns’ shearing angle, the composite mechanical properties retention rate after thermo-oxidative aging is also significantly different, because the post curing will occur for the vinyl ester resin in the thermo-oxidative aging environment. Therefore, the bending modulus of the composite materials in the aging process presents downward trend after increased first, and the tensile properties are affected by the reinforcement structure. The degradation of adhesion strength at fiber/matrix interface makes the tensile modulus decrease continuously during the aging process. With the aging time prolongation, the curing degree of resin increases gradually, and the glass transition temperature T_g increases gradually. The peak value of energy storage modulus increases at the initial stage of aging due to molecular chain crosslinking, while decreasing of the peak value is caused by molecular chain fracture at the later stage of aging.
- multi-layered biaxial weft knitted fabric reinforced composite /
- aramid fiber /
- thermo-oxidative aging /
- mechanical properties /
- shear angle

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图 1 纬编双轴向多层衬纱(MBWK)织物

Figure 1. Multilayered biaxial weft knitted (MBWK) fabric

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图 2 复合成型工艺

Figure 2. Composite forming process

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图 3 预制体剪切角θ控制流程

Figure 3. Control flow of preform shear angle θ

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图 4 不同剪切角的MBWK复合材料试样

Figure 4. MBWK composite samples with different shear angles

Z-0°, Z-10°, Z-20°, Z-30°, Z-40°—Specimens with shear angles of 0°, 10°, 20°, 30°, 40° liner warp orientation in the same direction as the length of specimen; N-0°, N-10°, N-20°, N-30°, N-40°—Sample with shear angles of 0°, 10°, 20°, 30°, 40° liner warp orientation perpendicular to the sample length direction

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图 5 VER温度-失重率曲线

Figure 5. Temperature-mass loss curves of VER

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图 6 100℃热氧环境下VER表面氧化层FTIR图谱

Figure 6. FTIR spectra of oxide layer on VER at 100℃

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图 7 不同老化时间VER的FTIR图谱局部图

Figure 7. Partial FTIR spectra of VER at different aging time

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图 8 VER浇铸体热氧老化后的玻璃化温度T_g和损耗因子tanδ峰值

Figure 8. Peak values of glass transition temperature T_g and loss factor tanδ before and after aging of the VER casting body

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图 9 VER浇铸体热氧老化后储存模量变化趋势

Figure 9. Changing trend of storage modulus of VER casting body after thermo-oxidative aging

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图 10 VER浇铸体老化前后的拉伸性能

Figure 10. Tensile properties before and after aging of the VER casting body

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图 11 Z组MBWK复合材料试样老化前后的拉伸性能

Figure 11. Tensile properties before and after aging of the Z series samples of MBWK composites

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图 12 N组MBWK复合材料试样老化前后的拉伸性能

Figure 12. Tensile properties before and after aging of the N series samples of MBWK composites

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图 13 VER浇铸体老化前后的弯曲性能

Figure 13. Flexural properties change before and after aging of the VER casting body

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图 14 Z组MBWK复合材料试样老化前后的弯曲性能

Figure 14. Flexural properties before and after aging of the Z series samples of MBWK composites

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图 15 N组MBWK复合材料试样老化前后的弯曲性能

Figure 15. Flexural properties before and after aging of the N series samples of MBWK composites

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表 1 MBWK织物参数

Table 1. MBWK fabric parameters

Type	Parameter
Weft inserting yarns	Kevlar-49	(474 g·km⁻¹(158×3))
Warp inserting yarns	Kevlar-49	(948 g·km⁻¹(158×6))
Stitching yarns	Polyester	(16.7 g·km⁻¹(8.33×2))
Layer structure	90°/0°/90°
Warp density/(tows·cm⁻¹)	30
Weft density(tows·cm⁻¹)	30
Thickness/mm	1.5

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表 2 RIPOXY R-806 乙烯基酯树脂(VER)成品性能指标

Table 2. RIPOXY R-806 vinyl ester resin (VER) finished product performance indicators

Parameter	Value
Tensile strength/MPa	69-89
Tensile modulus/GPa	2.9-3.3
Tensile elongation at break/%	3.2-4.0
Flexural strength/MPa	120-150
Flexural modulus/GPa	2.9-3.3
Distortion temperature/℃	108-118
Barcol hardness	40
Volume shrinkage/%	7.5-8.5

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表 3 VER浇铸体活化能计算数据

Table 3. Calculation data of activation energy of the VER casting body

Mass loss ratio	Slope	Activation energy/eV	Average value/eV	Deviation/%
0.90	−4315.24	0.8315	0.8029	3.56
0.85	−4238.74	0.7941		0.80
0.80	−4227.99	0.7832		1.97

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表 4 MBWK复合材料和VER浇铸体的热氧老化实验时间与自然老化时间对应关系

Table 4. Relationship between the thermo-oxidative aging experimental time and the natural aging time of the MBWK composite and VER casting body

Temperature/ ℃	Thermo-oxidative aging/h	Natural aging time/Month
100	0.5	1
	3.5	7
	6.5	13
	10	20
	13.5	27
	18	36

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表 5 VER液态体系DSC测试结果

Table 5. DSC test results of VER liquid system

Heating rate/(℃·min⁻¹)	Initial temperature/℃	Peak temperature/℃	Final temperature/℃	Total enthalpy of reaction/(J·g⁻¹)
2	83.6	88.9	93.0	266.1
5	89.3	98.6	113.6	235.1
10	125.1	138.4	155.5	279.5
12	149.9	164.1	173.9	249.9
15	155.5	172.8	185.3	256.6

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表 6 VER浇铸体热氧老化后DSC测试结果

Table 6. DSC test results of the VER casting body after thermo-oxidative aging

Aging time/h	Heating rate/ (℃·min⁻¹)	Initial temperature/℃	Peak temperature/℃	Final temperature/℃	Heat enthalpy/ (J·g⁻¹)	Degree of cure/%
0	5	61.4	80.5	132.6	73.270	71.54
0.5	5	76.5	93.9	131.3	37.770	85.33
3.5	5	128.9	135.3	148.7	11.460	95.55
6.5	5	129.7	137.1	150.8	11.400	95.57
10	5	111.4	120.3	134.9	11.310	95.60
13.5	5	119.4	137.6	146.4	4.078	98.42
18	5	123.1	136.1	150.3	3.635	98.60

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