CN113897707A - 一种航空级预浸料用碳纤维的制备方法 - Google Patents
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Abstract
本发明公开了一种航空级预浸料用碳纤维的制备方法。本发明的碳纤维采用干喷湿纺工艺制备,通过低损伤深度表面处理方法、耐高温型碳纤维上浆剂,获得了满足航空级预浸料应用要求的碳纤维。制备的碳纤维力学性能优异,其拉伸强度≥5900MPa,拉伸模量≥295GPa,断裂伸长率控制在1.95±0.20%范围内;碳纤维上浆剂含量控制在0.7±0.3%范围内;碳纤维丝束耐磨性好,起毛量≤4mg/30m;该碳纤维的航空级预浸料复合材料拉伸强度≥2800MPa,压缩强度≥1400MPa,冲击后压缩强度≥280MPa。本发明适合碳纤维在航空级预浸料领域的应用,能满足商用飞机等航空领域性能要求,可以用于制造商用飞机主承力结构件等。
Description
技术领域
本发明涉及一种航空级预浸料用碳纤维的制备方法,属于高性能碳纤维制备技术领域。
背景技术
高强中模级碳纤维是航空航天等高端领域主要使用的碳纤维种类。近年来日本T800S碳纤维、美国赫氏IM7碳纤维与第三代增韧树脂匹配的预浸料体系在B787、A350等大型民航客机上进行了大量使用。目前,国外碳纤维第三代技术已趋于成熟,航空级预浸料对碳纤维的强度、模量、工艺性以及复合材料性能都有严格的要求。由于国外高等级碳纤维领域对中国实行禁售禁运政策,导致国产商用飞机等航空航天领域的发展严重受制于人。此外,国产碳纤维在实际应用中也普遍存在与基体环氧树脂匹配性不佳的问题,导致碳纤维复合材料在诸如冲击后压缩强度等性能指标方面尚有一定欠缺。
发明内容
为了满足碳纤维在航空应用领域的预浸料工艺和复材性能要求,本发明提供一种航空级预浸料用碳纤维的制备方法。
实现本发明所述技术方案如下:
一种航空级预浸料用碳纤维的制备方法,该方法具体包括如下步骤:
a)制备碳纤维原丝,通过聚合原液经喷丝板牵伸纺丝,经过30~50℃水洗、60~80℃水牵、20~30℃上油、150~200℃烘干、0.3~0.6MPa的饱和蒸汽牵伸、120~190℃热辊干燥得到;
b)制备碳纤维,将碳纤维原丝在200~300℃进行预氧化,牵伸倍数为0.95~1.0倍;低温碳化温度为400~800℃,牵伸倍数为0.95~1.05倍;高温碳化温度为1100~1500℃,牵伸倍数为0.95~1.0倍的条件下得到碳纤维。
c)通过低损伤深度表面处理技术,表面处理电量控制在5~30C/g范围内,并采用强弱结合的氧化电解质提高纤维表面活性。
d)采用低环氧当量、耐高温的上浆剂,具有与纤维反应活性强、热分解温度高的特点,上浆剂含量控制在0.7±0.3%范围内。
优选地,碳纤维线密度控制在450±12g/km范围内。
优选地,碳纤维的体密度控制在1.79±0.02g/cm3范围内。
优选地,碳纤维丝束起毛量≤4mg/30m。
优选地,碳纤维上浆剂有效成分在氮气环境中加热,从20℃以10℃/min速率升温,失重率达到5%时的热分解温度≥230℃。
本发明相对于现有技术相比具有显著优点:
本发明通过低损伤深度表面处理技术,优化了电量分配和电解质类型,提高了纤维表面活性;开发了低环氧当量、耐高温的上浆剂,增强了纤维与树脂的结合能力,改善了复合材料的界面性能。碳纤维预浸料复合材料性能优异,拉伸强度≥2800MPa,压缩强度≥1400MPa,冲击后压缩强度≥280MPa。
附图说明
图1是本发明的环氧上浆剂在氮气环境中的热分解曲线。
具体实施方式
下面利用具体实施例进一步说明本发明的内容和技术方案,但不应理解为对本发明的限制。在不背离本发明思想情况下,对本发明方法、步骤或条件所作的简单修改或替换,均属于本发明的范围。
具体通过以下步骤实现:
步骤1:制备碳纤维原丝,通过聚合原液经喷丝板牵伸纺丝,经过30~50℃水洗、60~80℃水牵、20~30℃上油、150~200℃烘干、0.3~0.6MPa的饱和蒸汽牵伸、120~190℃热辊干燥得到。
步骤2:制备碳纤维,将碳纤维原丝在200~300℃进行预氧化,牵伸倍数为0.95~1.0倍;低温碳化温度为400~800℃,牵伸倍数为0.95~1.05倍;高温碳化温度为1100~1500℃,牵伸倍数为0.95~1.0倍的条件下得到碳纤维。
实施例1:经过步骤2所得碳纤维,先经过第一级表面处理,电解质硫酸,浓度5%,电量10C/g;再经过第二级表面处理,电解质碳酸氢铵,浓度2%,电量10C/g;然后经过低环氧当量和耐高温上浆剂,纤维含胶0.8%。碳纤维拉伸强度6037MPa,拉伸模量296GPa,断裂伸长率2.04%,碳纤维线密度450g/km,体密度1.793g/cm3,碳纤起毛量1.8mg;使用某一型号增韧型环氧树脂制备航空级碳纤维预浸料,环氧树脂的玻璃化转变温度Tg为204℃,纤维体积含量为59%,固化温度为180℃(下同)。碳纤维复合材料拉伸强度3100MPa,压缩强度1476MPa,冲击后压缩强度281MPa。
实施例2:经过步骤2所得碳纤维,先经过第一级表面处理,电解质硫酸,浓度2%,电量15C/g;再经过第二级表面处理,电解质碳酸氢铵,浓度5%,电量15C/g;然后经过低环氧当量和耐高温上浆剂,纤维含胶0.6%,碳纤维拉伸强度5993MPa,拉伸模量295GPa,断裂伸长率2.03%,碳纤维线密度448g/km,体密度1.791g/cm3,碳纤起毛量3.0mg;碳纤维复合材料拉伸强度3083MPa,压缩强度1435MPa,冲击后压缩强度282MPa。
实施例3:经过步骤2所得碳纤维,先经过第一级表面处理,电解质磷酸,浓度5%,电量25C/g;再经过第二级表面处理,电解质碳酸氢铵,浓度5%,电量25C/g;然后经过低环氧当量和耐高温上浆剂,纤维含胶0.6%,碳纤维拉伸强度5935MPa,拉伸模量296GPa,断裂伸长率2.01%,碳纤维线密度449g/km,体密度1.794g/cm3,碳纤起毛量3.1mg;碳纤维复合材料拉伸强度2929MPa,压缩强度1508MPa,冲击后压缩强度285MPa。
比较例1:经过步骤2所得碳纤维,经过一级表面处理,电解质碳酸氢铵2%,纤维表面处理电量10C/g;后经过常规环氧型上浆剂,纤维含胶0.3%,碳纤维拉伸强度6032MPa,拉伸模量295GPa,断裂伸长率2.04%,碳纤维线密度450g/km,体密度1.791g/cm3,碳纤起毛量4.7mg;碳纤维复合材料拉伸强度2987MPa,压缩强度1475MPa,冲击后压缩强度260MPa。
比较例2:经过步骤2所得碳纤维,经过一级表面处理,电解质碳酸氢铵2%,碳纤维表面处理电量10C/g,后经过常规环氧型上浆剂,纤维含胶1.2%,碳纤维拉伸强度6104MPa,拉伸模量296GPa,断裂伸长率2.06%,碳纤维线密度452g/km,体密度1.791g/cm3,碳纤起毛量0.8mg;碳纤维复合材料拉伸强度3024MPa,压缩强度1500MPa,冲击后压缩强度268MPa。
比较例3:经过步骤2所得碳纤维,经过一级表面处理,电解质碳酸氢铵2%,碳纤维表面处理电量0C/g,后经过常规环氧型上浆剂,碳纤维含胶0.7%,碳纤维拉伸强度5988MPa,拉伸模量296GPa,断裂伸长率2.02%,碳纤维线密度451g/km,体密度1.793g/cm3,碳纤起毛量2.2mg;碳纤维复合材料拉伸强度2915MPa,压缩强度1350MPa,冲击后压缩强度250MPa。
比较例4:经过步骤2所得碳纤维,经过一级表面处理,电解质碳酸氢铵2%,碳纤维表面处理电量35C/g,后经过常规环氧型上浆剂,碳纤维含胶0.7%,碳纤维拉伸强度5867MPa,拉伸模量295GPa,断裂伸长率1.99%,碳纤维线密度450g/km,体密度1.793g/cm3,碳纤起毛量2.3mg;碳纤维复合材料拉伸强度2776MPa,压缩强度1413MPa,冲击后压缩强度265MPa。
从以上实施例及比较例可以看到,碳纤维的拉伸强度越高,往往其复合材料的拉伸性能也越好;同时,碳纤维表面处理电量以及上浆剂含量等对碳纤维的起毛量和复合材料性能具有重要影响。例如,随着碳纤维的上浆剂含量升高,纤维起毛量变小,当上浆剂含量过高时会带来复合材料界面性能下降。同样地,表面处理电量也需把控在合适的范围内,电量过高会对纤维表面造成损伤带来力学性能下降,电量过低则表面沟槽较少复合材料界面性能差。
多级氧化电解质处理有利于:通过第一级强电解质进行强氧化刻蚀,引入含氧官能团,增加O/C等活性基团比例,第二级表面处理选用弱电解质,进一步增加表面处理程度。通过先强后弱的表面处理组合,一方面避免了长时间深度表面处理对纤维的过度损伤,且更有利于在“大裂纹”的基础上形成更多“小裂纹”;同时第二级弱电解质也利于实现后续水洗段的低残留。
本发明多级氧化电解质处理比对表。
本发明中低损伤深度表面处理提高了纤维表面活性,耐高温适配的上浆剂增强了纤维与树脂的结合能力,两者协同改善了复合材料的界面性能。
综上,本发明公开的一种航空级预浸料用碳纤维的制备方法。本发明的碳纤维采用干喷湿纺工艺制备,通过低损伤深度表面处理技术,优化了电量分配、电解质类型,提高了纤维表面活性;开发了适合于耐高温树脂的环氧型上浆剂,增强了纤维与树脂的结合能力,改善了复合材料的界面性能,获得了满足航空级预浸料应用要求的碳纤维。
Claims (9)
1.一种航空级预浸料用碳纤维的制备方法,其特征在于,将碳纤维原丝依次进行预氧化、低温碳化、高温碳化;再进行低损伤深度表面处理后,用上浆剂进行上浆;
该碳纤维的拉伸强度≥5900MPa,拉伸模量≥295GPa,断裂伸长率控制在1.95±0.20%范围内。
2.根据权利要求1所述的航空级预浸料用碳纤维的制备方法,其特征在于,具体步骤如下:
a)制备碳纤维原丝,通过聚合原液经喷丝板牵伸纺丝,经过30~50℃水洗、60~80℃水牵、20~30℃上油、150~200℃烘干、0.3~0.6MPa的饱和蒸汽牵伸、120~190℃热辊干燥得到;
b)制备碳纤维,将碳纤维原丝在200~300℃下进行预氧化,牵伸倍数为0.95~1.0倍;低温碳化温度为400~800℃,牵伸倍数为0.95~1.05倍;高温碳化温度为1100~1500℃,牵伸倍数为0.95~1.0倍的条件下得到碳纤维;
c)通过低损伤深度表面处理方法,并采用强弱结合的氧化电解质提高纤维表面活性;
d)采用低环氧当量、耐高温的上浆剂进行上浆。
3.根据权利要求1或2所述的航空级预浸料用碳纤维的制备方法,其特征在于,所述的碳纤维的线密度控制在450±12g/km范围内,体密度控制在1.79±0.02g/cm3范围内。
4.根据权利要求1或2所述的航空级预浸料用碳纤维的制备方法,其特征在于,采用低损伤深度表面处理方法,表面处理电量控制在5~30C/g范围内,并采用强弱结合的多级氧化电解质提高纤维表面活性。
5.根据权利要求4所述的航空级预浸料用碳纤维的制备方法,其特征在于,多级氧化电解质分别为第一级为强电解质、第二级为弱电解质;强电解质为硫酸、磷酸或氢氧化钠;弱电解质为碳酸氢铵或碳酸铵。
6.根据权利要求2所述的航空级预浸料用碳纤维的制备方法,其特征在于,所述的碳纤维上浆剂含量控制在0.7±0.3%范围内。
7.根据权利要求6所述的航空级预浸料用碳纤维的制备方法,其特征在于,所述的碳纤维上浆剂有效成分在氮气环境中加热,从20℃以10℃/min速率升温,失重率达到5%时的热分解温度≥230℃。
8.根据权利要求1所述的航空级预浸料用碳纤维的制备方法,其特征在于,所述的碳纤维耐磨性好,起毛量≤4mg/30m。
9.根据权利要求1所述的航空级预浸料用碳纤维的制备方法,其特征在于,所述碳纤维制备的航空级预浸料复合材料拉伸强度≥2800MPa,压缩强度≥1400MPa,冲击后压缩强度≥280MPa。
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