CN108368646A - 碳纤维开纤片材的制造方法 - Google Patents

碳纤维开纤片材的制造方法 Download PDF

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CN108368646A
CN108368646A CN201780004493.8A CN201780004493A CN108368646A CN 108368646 A CN108368646 A CN 108368646A CN 201780004493 A CN201780004493 A CN 201780004493A CN 108368646 A CN108368646 A CN 108368646A
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fibrillation
carbon fiber
sheet material
tow
manufacturing
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堀本歴
伊藤正道
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Kurashiki Spinning Co Ltd
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Abstract

本发明涉及一种碳纤维开纤片材(8)的制造方法，其包含对附着有上浆剂的碳纤维未开纤丝束进行表面活化处理的工序、和将所述碳纤维未开纤丝束(3a、3b)开纤、制成片材的工序。在开纤工序中，优选由用于使碳纤维未开纤丝束(3a、3b)弯曲并通过的按压轴(4a‑4d、5a‑5d)和沿丝束的宽度方向振动的开纤杆(6a‑6c)构成的至少一对开纤机构，按压轴(4a‑4d、5a‑5d)的端部与开纤杆(6a‑6c)的端部的高度之差△H优选为5～30mm。由此，即使使用附着有上浆剂的碳纤维未开纤丝束，也能够得到单纤维彼此之间易于分离、易于开纤、不易产生缺陷的碳纤维开纤片材。

Description

碳纤维开纤片材的制造方法
技术领域
本发明涉及易于开纤、缺陷少的碳纤维开纤片材的制造方法。
背景技术
碳纤维强化树脂(CFRP：Carbon Fiber Reinforced Plastics)、玻璃纤维强化树脂发挥高强度、轻量等特色，被广泛用于高尔夫球杆的杆身、钓竿等各种体育用品、航空器、汽车、压力容器等，或者期待今后的应用。作为纤维强化树脂通常的成形方法，例如使用手积法(hand lay-up method)、喷布法(spray-up method)等接触压成形法、纤维缠绕(FW)法、拉拔法、连续层叠法等连续成形法等而成形为目标成形物。基质树脂使用环氧树脂等热固性树脂或聚丙烯树脂等热塑性树脂。另外，为了提高与基质树脂的亲和性，使与基质树脂对应的上浆剂附着于强化用纤维表面。
作为现有技术，提出了对被赋予了上浆剂的碳纤维未开纤丝束进行加热而在使其柔软化的状态下进行开纤的方案(专利文献1)。另外，还提出了使用具有丙烯酸基和环氧基的碳纤维用上浆剂的方案(专利文献2)，还有对附着上浆剂之前的碳纤维表面进行臭氧氧化的方案(专利文献3)。
现有技术文献
专利文献
专利文献1：日本特开平11-172562号公报
专利文献2：日本特开2000-355884号公报
专利文献3：日本特开2009-79344号公报
发明内容
发明所要解决的课题
但是，附着有现有技术的上浆剂的碳纤维未开纤丝束存在单纤维彼此之间难以分离、难以开纤、易于产生缺陷的问题。
本发明为了解决上述以往的问题，提供一种即使使用附着有上浆剂的碳纤维未开纤丝束，也能够得到单纤维彼此之间易于分离、易于开纤、不易产生缺陷的碳纤维开纤片材的碳纤维开纤片材的制造方法。
用于解决课题的方法
本发明的碳纤维开纤片材的制造方法的特征在于，其包含对附着有上浆剂的碳纤维未开纤丝束进行表面活化处理的工序、和对所述碳纤维未开纤丝束进行开纤、制成片材的工序。
发明效果
本发明通过对附着有上浆剂的碳纤维未开纤丝束进行表面活化，能够得到单纤维彼此之间易于分离、易于开纤、不易产生缺陷的碳纤维开纤片材。即，通过对未开纤丝束进行表面活化，附着于各碳纤维表面的上浆剂通过氧化等活化，变得易于将单纤维彼此之间分离。由此，能够得到易于对未开纤丝束进行开纤、不易产生缺陷的开纤片材。另外，通过表面活化，能够使碳纤维与基质树脂的润湿性良好，进一步提高基质树脂的浸渗性。
附图说明
图1是本发明一个实施方式的丝束的开纤装置的示意剖视图。
图2是其示意立体图。
具体实施方式
通常的碳纤维未开纤丝束(以下也称为“未开纤丝束”)是为了提高与基质树脂的亲和性而以各碳纤维上附着有上浆剂的状态销售的。本发明对这种市售的附着有上浆剂的碳纤维未开纤丝束进行表面活化，使单纤维彼此之间易于分离。由此，易于对未开纤丝束进行开纤，得到不易产生缺陷的碳纤维开纤片材(以下也称为“开纤片材”)。另外，通过碳纤维的表面活化，能够使其与基质树脂的润湿性良好，进一步提高基质树脂的浸渗性。
本发明中，开纤是指将构成丝束的多根碳纤维沿宽度方向解开而形成薄的片状或带状。优选的厚度为0.02～0.4mm，进一步优选为0.02～0.3mm。本发明中所说的碳纤维未开纤丝束优选为3～60K，进一步优选为12～60K。在此，K为1000根，市售品的大号丝束例如为50K(50,000根)时，通常的宽度为12mm左右。
在所述进行开纤的工序中，优选利用由用于使碳纤维未开纤丝束弯曲并通过的按压轴、和在丝束的宽度方向上振动的开纤杆构成的至少一对开纤机构进行开纤。未开纤丝束以被按压轴按压的状态通过开纤杆在宽度方向上振动，因此未开纤丝束在宽度方向上扩开而开纤。开纤杆和按压轴优选截面为圆形、椭圆形、长圆形等，其中优选长圆形。从开纤杆能够使未开纤丝束与上表面和下表面接触的角度出发，特别优选截面为长圆形。由开纤杆和按压轴构成的开纤机构优选设置2～4对。这样，能够高效地进行开纤。
上述未开纤丝束优选在卷绕于绕线筒的状态下被多根供给，通过上述按压轴和开纤杆在宽度方向上振动而在宽度方向上扩开，同时被开纤，形成一张开纤片材。由此，能够从多根碳纤维未开纤丝束高效地制作宽幅的开纤片材。
在所述进行开纤的工序中，用于使碳纤维未开纤丝束弯曲并通过的按压轴的端部与开纤杆的端部的高度之差△H优选为5～30mm，更优选为10～20mm。为上述差的量时，碳纤维未开纤丝束弯曲而通过，变得易于与振动的开纤杆的表面接触而开纤。上述高度之差ΔH也可以最初较高、逐渐降低。开纤杆优选振幅为1～20mm，更优选为2～10mm，优选振动频率为10～100Hz，更优选为20～50Hz。由此，能够高效地对未开纤丝束进行开纤。
上述开纤片材的宽度优选每1000根构成纤维根数为0.5～5.0mm。具体而言，在上述开纤片材的宽度为50K或60K等大号丝束的情况下，每1000根构成纤维根数为0.5～1.5mm左右，在为12K或15K等常规丝束的情况下，每1000根构成纤维根数为1.5～5.0mm左右。每一根丝束的构成纤维根数越增加，纤维的扭曲变得越大，越难以开纤，因此开纤片材的宽度也变窄。由此，能够将碳纤维制造商所销售的未开纤丝束扩开，制成易于使用的开纤片材，供给到各种成形物。
上浆剂大多使用与基质树脂亲和性高的上浆剂，本发明中可以使用任意种类的上浆剂。优选的上浆剂是通用性高的环氧系树脂。上浆剂的优选附着量为0.1～5.0重量％，进一步优选为0.2～3.0重量％。
上述表面活化处理优选选自氧存在下的臭氧氧化、波长400nm以下的紫外线照射和等离子体处理中的至少一种处理。这是因为这些表面处理使上浆剂活化的效率高。其中，臭氧氧化可以在氧存在下进行，但也可以是其他方法。
作为臭氧的产生方法，有无声放电方式、沿面放电方式、紫外线照射方式、电解方式等。从效率方面出发，大容量的臭氧生成主要利用无声放电方式。目前，放电型臭氧发生器是最普遍使用的放电方式。在空气中一对平行电极的一方或双方上设置电介质(主要是玻璃或陶瓷)的层，当在两电极间施加交流高电压时产生无声放电。使臭氧浓度例如为40000ppm。处理时间优选为2～30分钟。碳纤维未开纤丝束在空气存在下放置而进行氧化处理。
作为臭氧氧化处理的另一例，有准分子灯照射。准分子灯是利用产生大量介质阻挡放电的短时间放电的特征，放射来自由稀有气体原子、或稀有气体原子和卤素原子形成的准分子的光的放电灯。准分子灯的代表性的放射波长有：Ar2*(126nm)、Kr2*(146nm)、Xe2*(172nm)、KrCl*(222nm)、XeCl*(308nm)等。灯是石英玻璃的双重结构，在内管的内侧实施金属电极、在外管的外侧实施金属网电极，在石英玻璃管内填充有放电气体。当对电极施加交流的高电压时，在两个电介质之间产生大量细丝状的放电等离子体(介质阻挡放电)。该放电等离子体包含高能量的电子，并且具有瞬时消失的特征。通过该放电等离子体，放电气体的原子被激发，瞬间成为准分子状态。在从该准分子状态返回到原来的状态(基态)时，发出该准分子特有的光谱(准分子发光)。发光光谱可以通过所填充的放电气体来设定。优选的照射条件根据波长的不同而不同。在波长172nm的情况下，光强度例如为5～6mW/cm2时，照射时间优选为0.5～30分钟左右。波长为222nm时，光强度例如为40～60mW/cm2时，照射时间优选为2～30分钟左右。如果在灯与被处理物之间存在空气层(间隙)，则在波长172nm的情况下，空气中的氧吸收光能而产生臭氧，因此也发生由臭氧进行的氧化作用。
作为其他的表面活性处理方法，还有低压汞灯法、等离子体照射处理法。低压汞灯(低压UV灯)利用点亮中的汞压力为100Pa以下的汞蒸气中的电弧放电的发光。发光管中封入有氩气等稀有气体和汞或其汞合金。有波长185nm、254nm等紫外放射的灯。使光强度例如为40～60mW/cm2。照射时间优选为2～30分钟左右。
等离子体通常是构成气体的分子部分或完全电离，分为阳离子和电子而***的状态。关于使用等离子体处理装置对碳纤维进行等离子体照射的条件，当用功率密度(W·分/m2)表示照射量时，优选为1000～50000W·分/m2。另外，在氮气或氮气+氧气气氛中处理速度(被处理物移动速度)优选为0.05～1m/min。
上述处理可以单独或任意组合。通过这些处理，使纤维表面的上浆剂活化，易于开纤，能够进一步使与基质树脂的润湿性良好，进一步提高浸渗性。更具体而言，推测或者切断上浆剂的分子，或者形成羟基、羰基、羧基、铵基或它们的过渡状态的中间体或类似基团而活化。
基质树脂可以使用热塑性树脂也可使用热固性树脂。作为热塑性树脂，可以使用聚乙烯、聚丙烯等聚烯烃树脂、尼龙树脂、聚酯树脂、聚碳酸酯树脂、聚醚醚酮树脂等，但并不限定于这些。作为热固性树脂，可以使用环氧树脂、不饱和聚酯树脂、酚醛树脂、三聚氰胺树脂等，但并不限定于这些。
上述碳纤维开纤片材上优选进一步一体化有用于维持宽度方向的连续性的增强材料。作为增强材料，例如也可以将玻璃纤维制棉麻织物(scrim)、聚乙烯、聚丙烯等聚烯烃制棉麻织物、网等熔融一体化而贴合，或撒上环氧树脂等树脂粉末进行加热。由此，碳纤维开纤片材在宽度方向连续，构成碳纤维不会散开，作为片材的操作性变得良好。增强材料优选选择与基质树脂具有亲和性的树脂。
接着，使用附图进行说明。在以下的图中，同一符号表示同一部件。图1是本发明一个实施方式的丝束的开纤装置的示意剖视图，图2是其示意立体图。该开纤装置1的主要部分由沿丝束的宽度方向振动的开纤杆6a、6b、6c和按压丝束的按压轴4a-4d、5a-5d构成。碳纤维未开纤丝束3a从多根供给绕线筒2a供给，在按压轴4a-4d与开纤杆6a、6b、6c之间弯曲而通过，未开纤丝束3a在被按压轴4a-4d按压的状态下通过开纤杆6a、6b、6c在宽度方向上振动，因此在宽度方向上扩开而开纤，成为开纤片材。多根未开纤丝束3b也同样地从供给绕线筒2b供给，在按压轴5a-5d与开纤杆6a、6b、6c之间弯曲而通过，未开纤丝束3b在被按压轴5a-5d按压的状态下通过开纤杆6a、6b、6c在宽度方向上振动，因此在宽度方向上扩开而开纤，成为开纤片材。该开纤片材在导向辊7a上排列成一列，形成片状，在通过导向辊7b后，从棉麻织物供给辊10供给棉麻织物9，在加热装置11内被一体化。一体化有棉麻织物的碳纤维开纤片材8被卷绕到卷绕绕线筒12上。所得到的碳纤维开纤片材8的构成碳纤维不会散开而能够作为一体化的片材进行处理。图2的箭头13a-13c表示开纤杆6a、6b、6c的振动方向。
在前文中，棉麻织物9为玻璃纤维制的厚度为0.25mm、每单位面积的质量为15g/m2的片材，加热装置11内的温度为180℃、滞留时间为1.55分钟。玻璃纤维上附着有热塑性树脂。作为热塑性树脂，有乙烯-乙酸乙烯酯共聚物等。除了棉麻织物以外，例如也可以撒上环氧树脂粉末，或贴合树脂制网状物。由此，碳纤维开纤片材在宽度方向连续，构成碳纤维不会散开而能够作为片材进行处理。
实施例
以下使用实施例对本发明进行具体说明。需要说明的是，本发明并不限于下述实施例。
(实施例1))
(1)碳纤维未开纤丝束
碳纤维未开纤丝束使用三菱人造丝公司制造、型号：PYROFILE TRH5060M、形状：大号丝束长丝50K(50,000根、宽度为12mm左右)、单纤维直径为6μm。在该碳纤维未开纤丝束中，碳纤维上附着有环氧系化合物作为上浆剂。
(2)碳纤维未开纤丝束的表面处理
碳纤维未开纤丝束的臭氧氧化处理如下进行：在密闭空间中加入碳纤维未开纤丝束，暴露于臭氧气氛中。具体而言，在可密闭的容器中加入碳纤维未开纤丝束，在室温25℃下进行30分钟的臭氧氧化处理。从氧气瓶向可密闭的容器供给氧气，用下述的臭氧气体发生器产生臭氧。关于臭氧产生能力，使用3台1个单元为2.16g/h(电压为100V、氧气浓度为90％、流量为1L/min)的设备时，为约6g/h。臭氧发生器使用制造商：REGALJOINT公司制、型号：ORZ-3.2、产生方法：无声放电、臭氧浓度：40000ppm。
(3)未开纤丝束的开纤机构
使用图1所示的开纤装置进行开纤。从6个供给绕线筒分别供给所述(1)的碳纤维未开纤丝束，开纤杆的端部与按压轴的端部的高度之差△H为10mm，开纤杆以6mm的振幅、30Hz的振动频率振动。开纤片材的卷绕速度为20m/分钟。如此将开纤宽度为35mm/50K、厚度为0.2mm的开纤片材卷绕。6个供给绕线筒的各绕线筒为50K，所制造的开纤片材的宽度为从50K的未开纤丝束得到的宽度的大致6倍。
(4)开纤片材的评价
得到的开纤片材通过目视观察起毛，根据下述的评价基准进行评价。
A：几乎没有起毛。
B：起毛多。
将以上结果汇总示于表1。
(比较例1～2))
比较例1～2是使用没有表面处理的碳纤维未开纤丝束进行开纤的结果。
[表1]
由表1可知，实施例1的起毛少，损伤缺陷少，得到了良好的碳纤维开纤片材。
产业上的可利用性
本发明的碳纤维开纤片材能够广泛应用于风力发电中使用的叶片、高尔夫球杆的杆身、钓竿等各种体育用品、航空器、汽车、压力容器等。
符号说明
1 开纤装置
2a、2b 供给绕线筒
3a、3b 碳纤维未开纤丝束
4a-4d、5a-5d 按压轴
6a、6b、6c 开纤杆
7a、7b 导向辊
8 碳纤维开纤片材
9 棉麻织物
10 棉麻织物供给辊
11 加热装置
12 卷绕绕线筒

Claims (9)

1.一种碳纤维开纤片材的制造方法，其特征在于，其包含：
对附着有上浆剂的碳纤维未开纤丝束进行表面活化处理的工序；和
对所述碳纤维未开纤丝束进行开纤、制成片材的工序。
2.根据权利要求1所述的碳纤维开纤片材的制造方法，其中，
在所述进行开纤的工序中，利用由用于使碳纤维未开纤丝束弯曲而通过的按压轴、和在所述碳纤维未开纤丝束的宽度方向上振动的开纤杆构成的至少一对开纤机构对碳纤维未开纤丝束进行开纤。
3.根据权利要求1或2所述的碳纤维开纤片材的制造方法，其中，
所述未开纤丝束在卷绕于绕线筒的状态下被多根供给，通过所述按压轴和开纤杆在宽度方向上振动而在宽度方向上扩开，同时被开纤，形成一张开纤片材。
4.根据权利要求1～3中任一项所述的碳纤维开纤片材的制造方法，其中，
在所述进行开纤的工序中，用于使碳纤维未开纤丝束弯曲而通过的按压轴的端部与开纤杆的端部的高度之差△H为5～30mm。
5.根据权利要求1～4中任一项所述的碳纤维开纤片材的制造方法，其中，
关于所述碳纤维开纤片材的宽度，每1000根构成纤维根数为0.5～5.0mm。
6.根据权利要求1～5中任一项所述的碳纤维开纤片材的制造方法，其中，所述上浆剂为环氧系树脂。
7.根据权利要求1～6中任一项所述的碳纤维开纤片材的制造方法，其中，
所述表面活化处理是选自臭氧氧化处理、波长400nm以下的紫外线照射和等离子体处理中的至少一种处理。
8.根据权利要求1～7中任一项所述的碳纤维开纤片材的制造方法，其还包含：
在所述碳纤维开纤片材上进一步贴合用于维持宽度方向的连续性的增强材料并加热而进行一体化的工序。
9.根据权利要求1～8中任一项所述的碳纤维开纤片材的制造方法，其中，
所述增强材料为棉麻织物。
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