CN112125672B - 一种三层包芯碳化硅纤维线材的制备方法及应用 - Google Patents

一种三层包芯碳化硅纤维线材的制备方法及应用 Download PDF

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CN112125672B
CN112125672B CN202010977047.9A CN202010977047A CN112125672B CN 112125672 B CN112125672 B CN 112125672B CN 202010977047 A CN202010977047 A CN 202010977047A CN 112125672 B CN112125672 B CN 112125672B
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邱海鹏
刘时剑
陈明伟
刘善华
谢巍杰
马新
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AVIC Beijing Aeronautical Manufacturing Technology Research Institute
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Abstract

本发明所述的三层包芯碳化硅纤维线材包括SiC纤维芯线，SiC纤维芯线外侧为聚四氟乙烯中间层，最外层为芳纶外包缠层，适用于二维SiC纤维预制体的缝合，从而制备二维SiC/SiC复合材料。本发明利用芳纶纱耐磨性等特点作为外包缠层，包缠具有聚四氟乙烯中间层的SiC纤维芯线，制备出外层密闭圆润且芯线不易断的三层包芯线，保证了SiC纤维作为缝合线在穿入穿出叠层SiC纤维布时，不与SiC纤维布直接接触，减少SiC纤维缝线所受的摩擦力和挤压应力，确保SiC纤维缝合线在缝合后的完整性和连续性，解决了用传统碳纤维作缝合线时易断线的问题。

Description

一种三层包芯碳化硅纤维线材的制备方法及应用
技术领域
本发明属于纺织纤维制备技术领域，涉及一种三层包芯碳化硅纤维线材的制备方法及应用。
背景技术
碳化硅增强碳化硅陶瓷基复合材料(SiC/SiC)因其密度低、强度高、模量高、耐高温、抗氧化等特点，已成为航空航天领域中最有潜力的热结构材料，具有广阔的应用前景。陶瓷基复合材料是由高强度的陶瓷纤维和陶瓷基体复合而成，一般包括增强纤维、界面相、基体以及涂层四大结构单元。增强纤维相当于复合材料的骨架，是主要承载结构单元。当其应用于复合材料构件设计，需要编织成各种预制体。其中，平面二维(2D)SiC纤维预制体具有编织成本低和周期短等特点，成为了SiC纤维常用的预制体形式。2D纤维预制体结构是按照一定铺设角度堆积的各单层或二维织物。目前应用的较多的是采用碳纤维作为缝合线，将铺层的纤维布在厚度方向叠层缝合起来，构成准二维立体织物。
碳纤维具有耐摩擦、耐高温、柔软等特点，具有能连续缝合模量较高的SiC纤维面料，能耐受SiC/SiC复合材料工艺过程中的高温处理，不引入杂质元素等特点。但由于碳纤维与SiC/SiC复合材料的组元存在热膨胀系数失配的问题，在致密化工艺的升温-降温反复循环中，基体极易因为热应力而出现裂纹等缺陷，从而影响复合材料最终的力学性能。此外，碳纤维在高温下容易氧化，对于一些高温含氧的实际应用环境下，层间的碳纤维容易氧化失效，使得复合材料层间结合力下降，影响二维SiC/SiC复合材料的应用范围。对于二维缝合的SiC/SiC复合材料，采用SiC纤维作为缝合线为最理想的选择，不仅耐高温，抗氧化，而且与复合材料组元热匹配，但由于SiC纤维自身模量较高，在缝合过程中容易因为与布料之间的摩擦阻力以及挤压应力导致缝线断开，使得缝合质量下降，不利于层间的结合，从而降低复合材料的整体性能。目前未见用SiC纤维缝合制备2D SiC/SiC复合材料的相关报道或专利。
发明内容
基于上述现有技术存在的问题，本发明提出了一种三层包芯碳化硅纤维线材的制备方法，采用高耐磨性的芳纶对SiC纤维芯线进行缠绕包覆，包缠工艺在经过改造的编织机上完成，从而保护内层SiC纤维芯线，使其在穿入穿出叠层SiC纤维布过程时不断线，保持线材的完整性和连续性，取代传统碳纤维缝线，避免出现碳纤维与SiC/SiC复合材料组元热不匹配等问题。
一种三层包芯碳化硅纤维线材的制备方法，所述三层包芯碳化硅纤维线材包括SiC纤维芯线，SiC纤维芯线外侧为聚四氟乙烯中间层，最外层为芳纶外包缠层；
所述三层包芯碳化硅纤维线材采用以下方法制成：
(1)确定SiC纤维芯线：根据SiC纤维织物的缝合线规格及强度要求，确定SiC纤维芯线丝束中单丝数；
(2)制备聚四氟乙烯中间层：通过拉挤工艺，将SiC纤维芯线经浸渍聚四氟乙烯树脂混合液，固化成型，即得到SiC纤维芯线外的聚四氟乙烯中间层；
(3)制备芳纶外包缠层：利用编织机以八字形编织方式在聚四氟乙烯中间层外侧包缠芳纶纱，即得到三层包芯碳化硅纤维线材。
具体地，SiC纤维芯线丝束中单丝数为0.5k-1k。
具体地，所述步骤(2)中，拉挤工艺时的牵引速度为0.2m/min-1.0m/min，固化成型时，成型模具三个加热区分别设为一区115-125℃，二区155-165℃，三区175-185℃。
具体地，上述步骤(2)中，聚四氟乙烯树脂混合液由以下重量份的组分制成：聚四氟乙烯树脂分散液65-75份、丙烯酸酯类粘合剂15-25份、水性环氧树脂8-12份。
具体地，上述步骤(3)中，芳纶纱由芳纶纤维材料通过赛络纺工艺纺成，其中芳纶纱规格为200D-1000D，编织角为10°-60°，编织结构为两向编织结构。
具体地，所述步骤(3)中，编织机编织的速度为50m/h-200m/h，编织目数为20-50。
具体地，所述聚四氟乙烯中间层的厚度为0.01mm-0.15mm。
具体地，所述SiC纤维芯线、聚四氟乙烯中间层、芳纶外包缠层厚度比为(60-75):(10-15):(10-30)。
本发明还提供了三层包芯碳化硅纤维线材的应用，所述三层包芯碳化硅纤维线材用于缝制航空发动机构件、航空航天热结构部件及核聚变反应堆炉第一壁材料所用的SiC/SiC复合材料。
由以上的技术方案可知，本发明的有益效果是：
1)本发明提供的三层包芯碳化硅纤维线材中，内部SiC纤维芯线、聚四氟乙烯中间层和外部芳纶纤维包缠层之间为紧密包覆，不存在脱出情况，外部的芳纶纱保护内层SiC纤维，避免内层SiC纤维与SiC纤维布料直接接触，起到缓冲作用，降低SiC纤维线材所受到的摩擦力以及挤压应力，保证SiC纤维线材在缝合后留在SiC纤维布料中的完整性、连续性。聚四氟乙烯中间层使得芳纶外包缠层与SiC纤维芯线包缠的更加紧密，有效填充了SiC纤维芯线和芳纶外包缠层间空隙，增强整体的结构强度；此外，聚四氟乙烯中间层可以提供SiC纤维芯线全面的保护，进一步增强其耐磨性。
2)本发明提供的三层包芯碳化硅纤维线材采用八字形包覆缠绕的方式，用芳纶纱保护SiC纤维芯线，强度高，耐磨性好，适用性强，避免缝合过程中SiC缝合线损坏断裂，符合预期效果，可取代常用的碳纤维，用于2D SiC纤维预制体的缝合。在2D SiC/SiC复合材料的z向上成功引入SiC纤维，提高了复合材料的层间结合力和层间损伤容限；同时避免了常用的碳纤维与SiC/SiC复合材料组元间的热膨胀系数失配以及高温抗氧化性较差等问题，具有广阔的工程化应用前景；
3)本发明提供的三层包芯碳化硅纤维线材，可推广并应用于其他连续陶瓷纤维三层包芯线材的制备，从而提高其他连续陶瓷纤维增强陶瓷基复合材料的二维缝合预制体的缝合质量，有利于推动其他连续纤维增强陶瓷基复合材料的工程化应用。
附图说明
图1是三层包芯碳化硅纤维线材的结构示意图。
图2是三层包芯碳化硅纤维线材的局部剖面示意图。
其中，1-SiC纤维芯线，2-聚四氟乙烯中间层，3-芳纶外包缠层。
具体实施方式
下面将结合实施例对本发明的实施方案进行详细描述，但是本领域技术人员将会理解，下列实施例仅用于说明本发明，而不应视为限制本发明的范围。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1
如图1所示，三层包芯碳化硅纤维线材包括SiC纤维芯线1，SiC纤维芯线1外侧为聚四氟乙烯中间层2，最外层为芳纶外包缠层3，其中聚四氟乙烯中间层2的厚度为0.01mm-0.15mm，SiC纤维芯线、聚四氟乙烯中间层、芳纶外包缠层厚度比为(60-75):(10-15):(10-30)；
所述三层包芯碳化硅纤维线材采用以下方法制成：
(1)确定SiC纤维芯线：根据SiC纤维织物的缝合线规格及强度要求，确定SiC纤维芯线丝束中单丝数为0.5k，选用国产二代SiC纤维；
(2)制备聚四氟乙烯中间层：通过拉挤工艺，将SiC纤维芯线经浸渍聚四氟乙烯树脂混合液，固化成型，即得到SiC纤维芯线外的聚四氟乙烯中间层，其中拉挤工艺时的牵引速度为0.2m/min-1.0m/min，固化成型时，成型模具三个加热区分别设为一区115-125℃，二区155-165℃，三区175-185℃，所述聚四氟乙烯树脂混合液由以下重量份的组分制成：聚四氟乙烯树脂分散液65-75份、丙烯酸酯类粘合剂15-25份、水性环氧树脂8-12份，在本实施例中，聚四氟乙烯树脂分散液的含固量为65％，购于浙江传化股份有限公司，丙烯酸酯类粘合剂的含固量为40％，购于浙江传化股份有限公司，水性环氧树脂的含固量为35％，购于上海绿嘉水性涂料有限公司；
(3)制备芳纶外包缠层：利用编织机以八字形编织方式在聚四氟乙烯中间层外侧包缠芳纶纱，即得到三层包芯碳化硅纤维线材，其中芳纶纱由芳纶纤维材料通过赛络纺工艺纺成，纱管容量为63cm，纱锭数为16，工作锭数8，芳纶纱规格为200D-1000D，编织角为10°-60°，编织结构为两向编织结构其中，编织机编织的速度为50m/h-200m/h，编织目数为34。
本实施例制得的三层包芯碳化硅纤维线材主要用于缝制航空发动机构件、航空航天热结构部件及核聚变反应堆炉第一壁材料所用的SiC/SiC复合材料。
参照标准GB/T14344-2003，通过比较断裂强度来比较三层包芯碳化硅纤维线材的可缝性，具体过程如下：先将样品放在标准大气条件下进行调湿处理，再使用YG061FQ电子单纱强力仪测试其断裂强力和断裂伸长率。
测试结果如下表1所示，经测试，SiC纤维芯线的断裂强度为2.63cN/dtex，采用本实施例制备的三层包芯碳化硅纤维线材断裂强度为41.59cN/dtex，有效提高了SiC纤维芯线的力学性能和可缝性。本实施例采用的包缠工艺与传统包芯或包覆工艺有所不同，创新性的使用编织机(GB-16A02)对碳化硅纤维进行包缠，包缠效果好，而且用三层包芯碳化硅纤维线材替代现有的碳纤维对SiC/SiC复合材料进行缝合，有效的解决了碳纤维缝合SiC/SiC复合材料时出现的缝合质量下降、不利于层间的结合，从而降低复合材料的整体性能的问题。
对比例1
将SiC纤维芯的芳纶外包覆层改用锦纶包缠，锦纶纱是由锦纶6纺成，规格为1.67dtex×39mm，其余的操作步骤与实施例1完全相同，制得三层包芯碳化硅纤维线材。如表1所示，对比例2制得的三层包芯碳化硅纤维线材最终断裂强度为12.94cN/dtex，与实施例1相比效果要差的多。锦纶具有优异的耐磨性，较好的弹性，但与SiC纤维芯的包覆性差，且其不耐高温，利用本对比例1所制得的三层包芯碳化硅纤维线材，对缝合后的复合材料使用范围会有一定的限制。
对比例2
SiC纤维芯、聚四氟乙烯中间层和最外层芳纶纤维包缠层厚度分别为三层包芯SiC纤维线材的厚度比为80、5、15，其余操作步骤与实施例1完全相同，制得三层包芯碳化硅纤维线材，测试其拉伸性能。
表1实施例1和对比例1、2中三层包芯碳化硅纤维线材拉伸性能测试
Figure BDA0002686064420000051
对比例3
参照实施例1，将步骤三中芳纶外包缠层编织工艺的编织目数分别改为24，26，46、48，其他条件不变，制得三层包芯碳化硅纤维线材，测试其拉伸性能，具体结果见表2。
表2对比例3中三层包芯碳化硅纤维线材的拉伸性能.
编织目数 24 26 46 48 实施例1
断裂强度(cN/dtex) 28.34 30.75 26.41 21.96 41.59
由表2可知，实施例1选用的编织目数为34后，可有效的提升三层包芯碳化硅纤维线材的力学性能。
对比例4
参照实施例1，将步骤二中聚四氟乙烯层的拉挤工艺中的牵引速度分别改0.1m/min，1.2m/min，其他条件不变，制得三层包芯碳化硅纤维线材。测试其拉伸性能，具体结果见表3。
表3对比例4中三层包芯碳化硅纤维线材的拉伸性能
拉挤速度(m/min) 0.1 1.2 实施例1
断裂强度(cN/dtex) 18.92 20.89 41.59
由表3可知，实施例1选用的0.6m/min的牵引速率，能有效的提升三层包芯碳化硅纤维线材的力学性能。
对比例5
参照实施例1，所述步骤三中，芳纶纱的编织角改为5°、65°，其他条件不变，制得三层包芯碳化硅纤维线材。测试其拉伸性能，具体结果见表4。
表4对比例5中三层包芯碳化硅纤维线材的拉伸性能
角度(°) 5 65 实施例1
断裂强度(cN/dtex) 23.08 30.45 41.59
由表4可知，实施例1选用的45°编织角，能有效的提升三层包芯碳化硅纤维线材的力学性能。
以上所描述的实施例是本发明一部分实施例，而不是全部的实施例。本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。

Claims (7)

1.一种三层包芯碳化硅纤维线材的制备方法，其特征在于，所述三层包芯碳化硅纤维线材包括SiC纤维芯线，SiC纤维芯线外侧为聚四氟乙烯中间层，最外层为芳纶外包缠层；所述SiC纤维芯线、聚四氟乙烯中间层、芳纶外包缠层厚度比为(60-75):(10-15):(10-30)；所述三层包芯碳化硅纤维线材采用以下方法制成：
(1)确定SiC纤维芯线：根据SiC纤维织物的缝合线规格及强度要求，确定SiC纤维芯线丝束中单丝数；
(2)制备聚四氟乙烯中间层：通过拉挤工艺，将SiC纤维芯线经浸渍聚四氟乙烯树脂混合液，固化成型，即得到SiC纤维芯线外的聚四氟乙烯中间层；所述聚四氟乙烯中间层的厚度为0.01mm-0.15mm；
(3)制备芳纶外包缠层：利用编织机以八字形编织方式在聚四氟乙烯中间层外侧包缠芳纶纱，即得到三层包芯碳化硅纤维线材。
2.根据权利要求1所述一种三层包芯碳化硅纤维线材的制备方法，其特征在于，SiC纤维芯线丝束中单丝数为0.5k-1k。
3.根据权利要求1所述一种三层包芯碳化硅纤维线材的制备方法，其特征在于，步骤(2)中，拉挤工艺时的牵引速度为0.2m/min-1.0m/min，固化成型时，成型模具三个加热区分别设为一区115-125℃，二区155-165℃，三区175-185℃。
4.根据权利要求1所述一种三层包芯碳化硅纤维线材的制备方法，其特征在于，步骤(2)中，聚四氟乙烯树脂混合液由以下重量份的组分制成：聚四氟乙烯树脂分散液65-75份、丙烯酸酯类粘合剂15-25份、水性环氧树脂8-12份。
5.根据权利要求1所述一种三层包芯碳化硅纤维线材的制备方法，其特征在于，步骤(3)中，芳纶纱由芳纶纤维材料通过赛络纺工艺纺成，其中芳纶纱规格为200D-1000D，编织角为10°-60°，编织结构为两向编织结构。
6.根据权利要求1所述一种三层包芯碳化硅纤维线材的制备方法，其特征在于，步骤(3)中，编织机编织的速度为50m/h-200m/h，编织目数为20-50。
7.一种如权利要求1所述方法制得的三层包芯碳化硅纤维线材的应用，其特征在于，所述三层包芯碳化硅纤维线材用于缝制航空发动机构件、航空航天热结构部件及核聚变反应堆炉第一壁材料所用的SiC/SiC复合材料。
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