CN107310240A - 碳纤维增强聚醚醚酮复合材料及其制备方法 - Google Patents

碳纤维增强聚醚醚酮复合材料及其制备方法 Download PDF

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CN107310240A
CN107310240A CN201710512623.0A CN201710512623A CN107310240A CN 107310240 A CN107310240 A CN 107310240A CN 201710512623 A CN201710512623 A CN 201710512623A CN 107310240 A CN107310240 A CN 107310240A
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carbon fiber
composite material
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张东兴
鲁春蕊
肖海英
贾近
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Harbin Institute of Technology
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/12—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by the relative arrangement of fibres or filaments of different layers, e.g. the fibres or filaments being parallel or perpendicular to each other
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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/20—All layers being fibrous or filamentary
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02—Synthetic macromolecular fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/106—Carbon fibres, e.g. graphite fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/14—Mixture of at least two fibres made of different materials
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/06—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyethers
    • D10B2331/061—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyethers polyetherketones, polyetheretherketones, e.g. PEEK

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Abstract

碳纤维增强聚醚醚酮复合材料及其制备方法，属于连续碳纤维增强复合材料的技术领域。本发明要解决现有APC‑2预浸料应用时制备复杂构件过程中存在的铺层困难的技术问题。碳纤维增强聚醚醚酮复合材料是将碳纤维与聚醚醚酮纤维用二维编织进行混编，再依次经剪切、层叠铺设、热压成型处理制成的；其中，经纱为碳纤维，纬纱为聚醚醚酮纤维，层叠铺设过程中任意相邻的两层的单向碳纤维呈夹角设置。本发明方法保留了纤维的柔韧性和垂悬性，铺层更加方便。

Description

碳纤维增强聚醚醚酮复合材料及其制备方法
技术领域
本发明属于连续碳纤维增强复合材料的技术领域；具体碳纤维增强聚醚醚酮复合材料及其制备方法。
背景技术
连续碳纤维增强聚醚醚酮复合材料具有优异的性能，且应用领域十分广泛。上世纪80年代英国ICI公司首先通过拉挤熔融浸渍的方法制备出单向碳纤维增强聚醚醚酮预浸料，并相继研制了一系列牌号为APC(aromatic polymer composites的缩写)的预浸料，其中APC-2是目前应用最多的连续碳纤维增强聚醚醚酮复合材料预浸料，这种预浸料本身就已经是一种复合材料，具有一定的力学强度，在制备复杂构件时存在着很大的局限性。
近年来伴随着对于连续碳纤维增强聚醚醚酮复合材料需求的不断扩大，一系列新的成型技术不断出现，有效克服了聚醚醚酮浸渍困难的问题。利用包缠纱的方式得到聚醚醚酮纤维与碳纤维混杂纤维束，用这种纤维束再与聚醚醚酮纤维混编，得到织物，最后对织物进行层叠热压。尽管这种方法可以一定程度上提高树脂与纤维的浸渍效果，但是制备包缠纱过程比较复杂，对试验条件要求比较高。因此，对碳纤维增强聚醚醚酮复合材料的制备进行成型工艺的优化显得十分必要。
发明内容
本发明要解决现有APC-2预浸料应用时制备复杂构件过程中存在的铺层困难的技术问题；而提供了碳纤维增强聚醚醚酮复合材料及其制备方法。
本发明碳纤维增强聚醚醚酮复合材料，其特征在于碳纤维增强聚醚醚酮复合材料是将碳纤维与聚醚醚酮纤维用二维编织进行混编，再依次经剪切、层叠铺设、热压成型处理制成的；其中，经纱为碳纤维，纬纱为聚醚醚酮纤维，层叠铺设过程中任意相邻的两层的单向碳纤维呈夹角设置。
本发明中碳纤维增强聚醚醚酮复合材料的制备方法是按下述步骤进行的：
步骤一、采用二维编织法对碳纤维与聚醚醚酮纤维进行混编后剪切，经纱为碳纤维，纬纱为聚醚醚酮纤维，得到混编柔性预混料；
步骤二、将步骤一获得的混编柔性预混料层叠铺设，其中任意相邻的两层的单向碳纤维呈夹角设置；
步骤三、然后热压成型，得到碳纤维增强聚醚醚酮复合材料。
进一步限定：步骤一所述的二维编织法为平纹编织。
步骤二中层叠铺设至少3层。
步骤二中任意相邻的两层的单向碳纤维呈30°～90°夹角设置。
步骤三中热压成型过程分三段阶梯升温，压力均控制在0.5～1.0Mpa，三个阶段的温度分别为180～200℃，290～320℃以及360～380℃，三阶段保压时间分别为20～30min，30～40min，30～40min。
步骤一所述的碳纤维为碳纤维T300，所述的聚醚醚酮纤维为型号为200D36F的聚醚醚酮纤维，编织用的聚醚醚酮纤维的股数为6股～18股，优选为12股。
本发明碳纤维聚醚醚酮混编柔性预混料的制备也采用的是混杂纤维法，采用碳纤维和聚醚醚酮纤维进行二维编织，得到的混编预混料保留了纤维的柔韧性和垂悬性，铺层更加方便。
碳纤维聚醚醚酮混编柔性预混料的制备方法更加简单且加工过程绿色环保，成型方法简单，可以任意调整铺层角度和层数，而且可以在一定范围内调整聚醚醚酮和碳纤维的比例。
本发明碳纤维增强聚醚醚酮复合材料的制备方法，填补了连续碳纤维增强聚醚醚酮复合材料的制备上的空白，为碳纤维增强聚醚醚酮复合材料制备的市场提供了更广阔的思路；
本发明采用编织的方法将树脂纤维与增强纤维制备成柔性预混料，与现有的预浸料相比，具有应用范围广容易加工的优点，在制备复杂构件时更加容易弯折铺层，保证增强纤维的连续性以及构件在材料上的均匀性。
附图说明
图1是不同股数的CF/PEEK织物表面形貌，其中a)、b)——6股，c)、d)——12股，e)、f)——18股；
图2是不同树脂含量的CF/PEEK复合材料的拉伸断面形貌，a)树脂含量51.05％，b)树脂含量57.3％，c)树脂含量62.68％，d)树脂含量62.68％；
图3是热压之后的不同树脂含量的CF/PEEK复合材料的板材形貌；
图4是PEEK纤维为12股时的织物热压前后的超景深图像；
图5是不同树脂含量复合材料的红外光谱，1——树脂含量51.05％，2——树脂含量57.3％，3——树脂含量62.68％；
图6是不同热压成型方式获得的CF/PEEK织物表面形貌，a)——室温升温至370℃,b)——三段式升温(180℃,300℃,360℃),c)——三段式升温方法(180℃,300℃,370℃)。
具体实施方式
具体实施方式一：本实施方式中使用的碳纤维为哈尔滨玻璃钢研究院提供的T300型碳纤维；聚醚醚酮细丝从常州创赢新材料科技有限公司购买，型号为200D36F；采用小型手工编织机进行平纹编织。
本实施方式中碳纤维增强聚醚醚酮复合材料的制备方法具体是按下述步骤进行的：
步骤一、采用平纹编织对碳纤维与聚醚醚酮纤维进行混编后剪切，经纱为碳纤维，纬纱为聚醚醚酮纤维，聚醚醚酮纤维的股数分别是6股、12股或18股，得到混编柔性预混料；
步骤二、将步骤一获得的混编柔性预混料层叠铺设，一共铺设8层，其中任意相邻的两层的单向碳纤维呈90°夹角设置，铺层方式为[0°/90°/0°/90°/90°/0°/90°/0°]，见图1；
步骤三、然后热压成型，其中热压成型过程分三段阶梯升温，压力均控制在0.5Mpa，三个阶段的温度分别为180℃，300℃以及370℃，三阶段保压时间分别为20min，30min，30min，得到碳纤维增强聚醚醚酮复合材料。
编织用6股、12股或18股聚醚醚酮纤维经热压成型分别得到三种树脂含量的复合材料(树脂含量分别为51.05％，57.30％，62.68％)，经力学性能测试以及拉伸断面微观形貌分析见附图2，得到聚醚醚酮的最优含量为12股57.30％。
热压之后的板材形貌见附图3，从图3中可以看出，采用6股纤维得到的板材表面存在细微缺陷，而18股纤维得到的板材由于树脂含量太多，加工过程中树脂将编织的纤维冲散，板材不均匀。
采用12股纤维织物进行热压前后的超景深图像，见附图4，观察发现热压之后不能明显看出树脂纤维与碳纤维，已经形成一个整体，扫描电镜观察发现表面均匀，树脂可以完全包覆纤维。
经测定树脂含量分别为51.05％，57.30％以及62.68％，红外光谱发现聚醚醚酮与纤维之间并未发生化学反应，红外光谱结果见附图5，对三种含量的试样进行拉伸断面表面形貌分析，附图2，发现树脂含量为51％时，树脂并不能全部包覆碳纤维，而树脂含量为62％时，材料表面由很多孔隙。
进行力学测试发现，树脂含量为57％的试样测试均匀性比较好，测得的性能也最好，而树脂含量最高时，由于孔隙的影响，材料的力学性能也受到影响。
不同热压成型方式制备的CF/PEEK织物表面形貌，热压成型方式如表1所示；采用的聚醚醚酮碳纤维织物中聚醚醚酮纤维为12股,按具体实施方式一方法制备CF/PEEK织物，其它步骤和参数与具体实施方式一相同，热压成型方式及结果如表1和图6所示：
表1
由表1，发现采用三段式阶梯升温的方式具体实施方式一的热压成型方式得到的板材最均匀稳定。

Claims (10)

1.碳纤维增强聚醚醚酮复合材料，其特征在于碳纤维增强聚醚醚酮复合材料是将碳纤维与聚醚醚酮纤维用二维编织进行混编，再依次经剪切、层叠铺设、热压成型处理制成的；其中，经纱为碳纤维，纬纱为聚醚醚酮纤维，层叠铺设过程中任意相邻的两层的单向碳纤维呈夹角设置。
2.碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于该制备方法是按下述步骤进行的：
步骤一、采用二维编织法对碳纤维与聚醚醚酮纤维进行混编后剪切，经纱为碳纤维，纬纱为聚醚醚酮纤维，得到混编柔性预混料；
步骤二、将步骤一获得的混编柔性预混料层叠铺设，其中任意相邻的两层的单向碳纤维呈夹角设置；
步骤三、然后热压成型，得到碳纤维增强聚醚醚酮复合材料。
3.根据权利要求2所述碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于步骤一所述的二维编织法为平纹编织。
4.根据权利要求2所述碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于步骤二中层叠铺设至少3层。
5.根据权利要求2所述碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于步骤二中任意相邻的两层的单向碳纤维呈30°～90°夹角设置。
6.根据权利要求2所述碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于步骤三中热压成型过程分三段阶梯升温，压力均控制在0.5～1.0Mpa，三个阶段的温度分别为180～200℃，290～320℃以及360～380℃，三阶段保压时间分别为20～30min，30～40min，30～40min。
7.根据权利要求2所述碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于步骤三中热压成型过程分三段阶梯升温，压力均控制在0.5Mpa，三个阶段的温度分别为180℃，300℃以及370℃，三阶段保压时间分别为20min，30min，30min。
8.根据权利要求2-7任意一项所述碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于步骤一所述的碳纤维为碳纤维T300，所述的聚醚醚酮纤维为型号为200D36F的聚醚醚酮纤维。
9.根据权利要求8所述碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于编织用的聚醚醚酮纤维的股数为6股～18股。
10.根据权利要求8所述碳纤维增强聚醚醚酮复合材料的制备方法，其特征在于编织用的聚醚醚酮纤维的股数为12股。
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