CN113195216A - 生产复合材料的方法 - Google Patents
生产复合材料的方法 Download PDFInfo
- Publication number
- CN113195216A CN113195216A CN201980082179.0A CN201980082179A CN113195216A CN 113195216 A CN113195216 A CN 113195216A CN 201980082179 A CN201980082179 A CN 201980082179A CN 113195216 A CN113195216 A CN 113195216A
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- Prior art keywords
- carbon nanotube
- prepreg
- sheet
- curable
- curable system
- Prior art date
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Images
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Abstract
一种生产能够用于不同的工业,包括航天和汽车工业的复合材料的方法。具体地,本发明涉及使用一个或多个包含基本上非对齐的碳纳米管的自支撑式非织造碳纳米管片,来固化一个或多个预浸料坯和/或液体可固化组合物的方法。
Description
交叉参考的相关申请
本申请要求2018年12月12日提交的美国临时申请62/778,737的权益和优先权,其整体上通过参考引入本文。
关于联邦发起的研究或开发的声明
不适用。
技术领域
本发明总体上涉及一种生产能够用于例如航天和汽车工业的复合材料的方法。具体地,本发明涉及使用包含基本上非对齐的碳纳米管的一个或多个自支撑式非织造碳纳米管片,来固化预浸料坯和/或液体可固化组合物的方法。
背景技术
目前形成复合材料的方法依赖于使用外部施加的升高温度来加热可固化体系例如预浸料坯和液体树脂。但是,固化通常是放热反应,这产生另外的热,需要对其进行控制来防止可固化体系内过热。过热可固化体系会损害可固化体系和由其生产的复合材料,以及在固化过程中用于成形复合材料的任何模具。
可固化体系越厚(例如堆叠体或预制坯中的预浸料坯的数目越大),可固化体系过热的倾向越高。所以,需要特别控制用于较厚的可固化体系的固化方法,来减少在可固化体系中产生过高温度的风险和避免过热和失控的固化。过度加热(和随之而来的过热)通常归因于当使用外部施加的升高温度时不能有效控制施加到可固化体系的热量。避免过热的一种方式是确保固化周期足够长,以避免在可固化体系内产生过热。但是,这样的方法既耗费时间又耗费成本。
所以,有利的是提供与目前使用外部施加的升高温度的方法相比,以更有效和/或受控的方式固化可固化组合物来形成复合材料的方法。
附图说明
图1是非织造碳纳米管片的代表性图示。
图2显示了一种非织造碳纳米管片。
图3显示了一种具有连接体部分和结合机构的非织造碳纳米管片。
具体实施方式
在详细解释本发明的至少一个实施方案之前,要理解的是本发明的应用不限于在下面的说明书中阐述的结构细节和部件或步骤或方法的排列。本发明能够是其他的实施方案,或者以不同方式实践或进行。同样,还要理解的是本文所用的措词和术语用于说明目的,不应当认为是限制性的。
除非本文另有定义,否则就本发明所用的技术术语应当具有本领域技术人员通常所理解的含义。此外,除非上下文另有需要,否则单数术语应当包括复数,和复数术语应当包括单数。
说明书中提及的全部专利、公开的专利申请和非专利公开文献是本发明所属技术领域的技术人员水平的指示。本申请任何部分中提及的全部专利、公开的专利申请和非专利公开文献整体上明确地通过参考引入本文,如同每个单篇专利或公开文献具体地和单独地表明通过参考引入的程度,以及它们不与本发明相抵触的程度。
本文公开的全部的组合物和/或方法可以制造和执行,而无需根据本发明进行过度实验。虽然本发明的组合物和方法已经在实施方案或优选的实施方案中进行了描述,但是对本领域技术人员来说显然可以对本文所述的组合物和/或方法和方法的步骤或步骤顺序进行改变,而不脱离本发明的理念、主旨和范围。对本领域技术人员来说显然全部这样的类似替代和调整被认为处于本发明的主旨、范围和理念中。
本文中涉及碳纳米管的任何实施方案也可以在本发明的主旨和范围内调整,来替代其他管状纳米结构,包括例如无机或矿物纳米管。无机或矿物纳米管包括例如硅纳米管,硼纳米管,和在纳米管结构中具有杂原子取代的碳纳米管。
如根据本发明所使用,除非另有指示,否则下面的术语应当理解为具有下面的含义。
当与术语“包含”、“包括”、“具有”或“含有”(或这样的术语的变形)一起使用时,使用词语“一个”或“一种”可以表示“一个/种”,但是它也可以符合“一个/种或多个/种”,“至少一个/种”和“一个/种或多于一个/种”的含义。
术语“或”用于表示“和/或”,除非明确表示仅指的是替代选项并且仅当这些替代选项是互斥的时。
在本发明整体中,术语“约”用于表示值包括量化装置、机理或方法的误差的固有偏差,或者在要测量的对象中存在的固有偏差。例如但不限于,当使用术语“约”时,它表示的指定值可以在±10%,或9%,或8%,或7%,或6%,或5%,或4%,或3%,或2%,或1%,或其间的一个或多个分数中变化。
使用“至少一个/种”将被理解为包括一个/种以及多于一个/种的任何量,包括但不限于1,2,3,4,5,10,15,20,30,40,50,100等。术语“至少一个/种”可以扩展到100或1000或更大,这取决于它表示的术语。另外,100/1000的量不被认为是限制性的,因为更低或更高的端值也会产生令人满意的结果。
另外,短语“X,Y和Z的至少一种”将被理解为包括单独的X,单独的Y和单独的Z,以及X,Y和Z的任意组合。同样,短语“X和Y的至少一种”将被理解为包括单独的X,单独的Y,以及X和Y任意的组合。此外,要理解的是短语“至少一个/种”可以与任何数目的组成部分一起使用,并且具有与上述类似的含义。
使用序号术语(即“第一”,“第二”,“第三”,“第四”等)仅用于区分两个或更多个项目,除非另有指示,并不表示一个项目相对于另一项目的任何顺序或次序或重要性或者任何添加顺序。
如本文所使用,词语“包含”(和任何形式的包含,例如“含有”),“具有”(和任何形式的具有,例如“有”),“包括”(和任何形式的包括,例如“囊括”)或“含有”(和任何形式的含有,例如“包含”)是包容性的或开放式的,不排除另外的、未描述的元素或方法步骤。
如本文所使用,措词“或其组合”和“及其组合”指的是项目前面所列的项目的全部排列和组合。例如,“A,B,C或其组合”意在包括以下至少一种:A,B,C,AB,AC,BC,或ABC,如果在特定的上下文中顺序是重要的,则还包括BA,CA,CB,CBA,BCA,ACB,BAC,或CAB。继续这个例子,明确包括含有重复的一个或多个项目或术语的组合,例如BB,AAA,CC,AABB,AACC,ABCCCC,CBBAAA,CABBB等。本领域技术人员将理解,通常对于任意组合中的项目或术语的数目没有限制,除非上下文另有明确指示。同样地,术语“或其组合”和“及其组合”当与短语“选自”或“选自由以下组成的组”一起使用时,指的是该术语前面所列的项目的全部排列和组合。
短语“在一个实施方案中”,“在实施方案中”,“根据一个实施方案”等通常表示该短语之后的具体特征、结构或特性包括在本发明的至少一个实施方案中,并且可以包括在本发明的多于一个实施方案中。重要的是,这样的短语是非限定性的,不必指同一实施方案,而是当然可以指一个或多个在先和/或在后的实施方案。例如,在所附权利要求书中,任何要求保护的实施方案可以以任意组合来使用。
如本文所使用,术语“重量%”,“wt%”,“重量百分比”或“重量的百分比”可互换使用。
短语“基本上不含”在本文中应当用于表示存在量小于1重量%,或小于0.1重量%,或小于0.01重量%,或可选地小于0.001重量%基于所述及组合物的总重量计。
如本文所使用,术语“环境温度”指的是工作环境周围的温度(例如使用可固化组合物的区域、建筑物或房间的温度),不包括由于直接向可固化组合物施加热来促进固化而发生的任何温度变化。环境温度通常是约10℃至约30℃,更具体地是约15℃至约25℃。术语“环境温度”在本文中可与“室温”互换使用。
如本文所使用,术语“复合材料”指的是由具有不同的物理或化学性质的两种或更多种单个组分制成的材料,其当组合时产生特性不同于单个组分的材料。
术语“复合材料层合体”指的是由两层或更多层(可以相同或不同)的复合材料制成的制品。例如,复合材料层合体可以包含两层或更多层的预浸料坯。
术语“复合材料”,“复合材料层合体”和“层合体”在本文中可互换使用。
术语“预浸料坯”用于描述用可固化树脂浸渍的纤维材料,其处于未固化态或部分固化态,并且准备好固化。如本文所使用,术语“预浸料坯”指的是预浸料坯板层,其二者可互换使用。“多个预浸料坯”指的是多个预浸料坯板层。
碳纳米管
如就本发明所使用,碳纳米管可以使用多种方案来制作。目前,存在着多种用于生长纳米管的方法及其变体,包括:(1)化学气相沉积(CVD),其是一种常规方法,可以在接近环境压力或在高压,和在高于约400℃的温度进行,(2)电弧放电,其是一种高温方法,其可以产生具有高完备度的管,和(3)激光烧蚀。
在一些实施方案中,碳纳米管(包括单壁碳纳米管(SWNT),双壁碳纳米管(DWNT)和多壁碳纳米管(MWNT))可以通过在含碳反应气体(即在升高的温度的气态碳源)存在下暴露纳米尺寸的催化剂颗粒来生长。具体地,可以通过添加现有的颗粒或者通过由金属-有机前体,或甚至非金属催化剂原位合成颗粒,来将纳米尺寸的催化剂颗粒与含碳反应气体一起引入高热环境。
在一些实施方案中,碳纳米管(“CNT”)的长度可以大于约1微米,或约10微米,或约50微米,或约100微米。在其他实施方案中,CNT的长度可以大于约150微米,或大于约200微米,或大于约250微米,或大于约300微米,或大于约350微米,或大于约400微米,或大于约450微米,或大于约500微米。
就本发明所使用的单个纳米管的强度可以是约30GPa或更大。应当注意,强度通常对于缺陷是敏感的。但是,根据前述CVD方法制作的单个碳纳米管的弹性模量可以对缺陷不敏感,并且可以是约1TPa。此外,对于就本发明所使用的碳纳米管来说,破坏应变(strainto failure)(其通常可以是结构敏感性参数)可以是约10%至约25%。
此外,本发明的纳米管可以具有相对小的直径。在本发明的一些实施方案中,纳米管可以具有约1纳米至约几十纳米的直径。
这样的碳纳米管可以制成具有复杂性逐渐增加的分级形态的结构。通常的形成结构是但不限于CNT片,纱线和粉末(例如束,纤维或其他实体)。这样的纳米纤维宏观结构可以是可伸长的。
用于形成这样的碳纳米管及其结构(包括碳纳米管片)的***和方法更详细地描述在美国专利7,993,620中,其整体上通过参考引入本文。
碳纳米管片
如本文所使用,术语“碳纳米管片”通常涉及碳纳米管的非织造制品(包括本文前述的那些),其具有片材的一般外观和作为片材处理的足够的结构完整性。即,在一个实施方案中,碳纳米管片是基本上非对齐的碳纳米管的自支撑式非织造片。这样的片可以例如但不限于由压实的,基本上非对齐的,和互混的碳纳米管,碳纳米管束,或缠绕的碳纳米管的基质产生,具有作为片材处理的足够的结构完整性。
在一个具体实施方案中,碳纳米管片包含多个非织造碳纳米管的单个层,这些非织造碳纳米管相对于彼此取向,从而存在足够的接触,使得该单个层能够作为片材来处理。图1显示了碳纳米管片10的一个非限定性例子的图示。碳纳米管片可以经设计来使得电导率沿着它的长度,即在它的平面内。在一个实施方案中,碳纳米管片10可以是彼此叠置沉积的多个非织造碳纳米管12的单个层。图2显示了碳纳米管片14的另一非限定性实施方案,以及与之相关的x,y和z轴的透视。
在另一实施方案中,碳纳米管片包含非织造的基本上非对齐的碳纳米管的多个层,其中每层包含多个非织造碳纳米管,和其中碳纳米管和碳纳米管的层是经取向的,从而碳纳米管片在要作为片材处理的层之间具有足够的接触。
例如,在一个非限定性实施方案中,碳纳米管片包含碳纳米管的多个可辨别的层,其中非织造碳纳米管片的每层包含多个互混的碳纳米管,和其中每层的碳纳米管是压实的,从而非织造片中的层仍然彼此可区分,和其中在纳米管之间存在足够数目的接触位置,以提供具有形成可以如片材处理的连续结构所需的结合强度的非织造碳纳米管片。
如本文所使用,“基本上非对齐”表示碳纳米管的对齐程度可以小于30%,或小于20%,或小于15%,或小于10%,或小于5%,或小于1%对齐,基于碳纳米管的总数计。在任何情况中,“基本上非对齐”确定地表示碳纳米管不是基本上竖直对齐的。
在一个可选的实施方案中,碳纳米管片的碳纳米管可以仅在“y”方向上拉伸,以使得碳纳米管在“y”方向上的对齐程度小于20%,或小于15%,或小于10%,或小于5%,基于碳纳米管的总数计。
本文所述的非织造碳纳米管片的密度可以是约0.1mg/cm2至(或超过)约5mg/cm2。
本文所述的非织造碳纳米管片还可以具有约10,000至约20,000psi的标称强度和/或约30Mpa至约300MPa的拉伸强度。
在一个实施方案中,碳纳米管片已经过改性来在片的每个相对端处具有连接体部分(例如电气总线),其能够具有附接的电极,以使得电流可以经过碳纳米管片。
连接体部分可以是直接沉积例如电镀到导电元件的每个端部上的涂层。将连接体部分沉积或电镀到碳纳米管片上可以使用本领域公知的方法进行。电镀的连接体部分的例子包括金,银,镍,铝,铜,铋,锡,锌,镉,锡-镍合金,铜合金,锡-锌合金,铋-铜合金,铜-镍合金,镉-镍合金,其他导电金属和它们的合金,或其组合。在一个实施方案中,一个或多个连接体部分可以位于碳纳米管片上的任何位置。在一个实施方案中,连接体部分可以是一片导电材料,其机械地或化学地连接到碳纳米管片的每个对端,以使得电流可以经过碳纳米管片。
在一个实施方案中,连接体部分可以基本上均匀地沉积或电镀到碳纳米管片的相对端上,以允许在跨过连接体部分上的接触表面积导电中纳米管均匀地接触。同样,连接体部分可以使碳纳米管片内的导电纳米结构的数目基本上最大化,这可以主动包括在电导率中来提高电和热的传输效率和减小接触电阻。为此目的,来自于电源且通过碳纳米管片运载的相对高的电流可以被导向外部电路,而没有明显的降低。
在一个实施方案中,当结合到碳纳米管片时,连接体部分允许来自于电源的相对高的电流(其可以通过碳纳米管片运载)导向外部电路,而没有明显降低。为此,碳纳米管片可以进一步包含结合机构来增加碳纳米管片的端部与连接体部分之间的接触。在一个实施方案中,结合机构可以由玻璃状碳材料制成,其能够提供显著低的电阻耦合。玻璃状碳通常可以为与碳纳米管有关的碳的形式,并且可以含有大量的石墨烯如包含无定形碳的基质的带。这些带包括sp2键合的带,其可以基本上类似于sp2键合的纳米管。作为结果,它们可以具有相对好的热导率和电导率。可以制造玻璃状碳的前体材料的例子包括糠醇,RESOL树脂(即催化的烷基-苯基甲醛),聚乙烯醇(“PVA”),或液体树脂,或者在热处理时形成玻璃状碳的任何已知材料。当然,可以使用其他商购的玻璃状碳材料或前体材料。
另外,结合机构还可以为碳纳米管片提供跨过连接体部分上的接触表面积与连接体部分基本上均匀的接触。为此,结合机构可以使碳纳米管片内的导电纳米结构的数目基本上最大化,这可以主动包括在电导率中来提高电和热的传输效率。例如,来自于电源且通过碳纳米管片运载的相对高的电流可以被导向外部电路,而没有明显的降低。因此,可以使用本发明的碳纳米管片以能够有效传导到标准连接体,来用于传统的热回路和/或电路***。
在一个实施方案中,碳纳米管片的连接体部分可以用环氧,聚合物树脂或另一类结合剂浸渍,来增加结构完整性。
本文所述的连接体部分和结合机构的另外的例子可以参见美国专利9,198,232,其整体上通过参考引入本文。
图3显示了碳纳米管片20的一个非限定性实施方案,其具有连接体部分21和结合机构22。
可固化体系
根据一个方面,本发明涉及一种可固化体系,其包含预浸料坯和位于预浸料坯的顶部和/或底部的一个或多个碳纳米管片。
在另一方面中,本发明涉及一种可固化体系,其包含(i)两个或更多个预浸料坯的堆叠体,和(ii)一个或多个碳纳米管片,其中碳纳米管片中的至少一个位于两个或更多个预浸料坯之间。
一个或多个碳纳米管片无需位于堆叠体的每个预浸料坯之间。但是,在一个实施方案中,可以想到碳纳米管片可以置于每个预浸料坯之间,和任选地置于预浸料坯堆叠体的顶部和/或底部。在另一实施方案中,碳纳米管片可以置于整个预浸料坯堆叠体的不同位置。
在一个具体实施方案中,一个或多个碳纳米管片置于预浸料坯堆叠体的中间处或基本上附近,以使得一个或多个碳纳米管片两侧上的预浸料坯的厚度基本上相同。
本发明的每个预浸料坯包含纤维增强物和可固化树脂的混合物。当然,纤维增强物包含纤维。在一个实施方案中,纤维增强物为例如纤维的束或层的形式。纤维增强物可以由单向纤维,织造纤维,短切纤维,非织造纤维,或长的不连续纤维构成。
在一个实施方案中,纤维选自导电纤维,非导电纤维,及其组合。
具体地,纤维可以选自玻璃,例如S玻璃,S2玻璃,E玻璃,R玻璃,A玻璃,AR玻璃,C玻璃,D玻璃,ECR玻璃,玻璃长丝,短玻璃纤维,T玻璃和锆玻璃,碳聚丙烯腈,碳纤维,丙烯酸纤维,聚对亚苯基对苯二甲酰胺,二氧化硅,芳酰胺,硼,聚亚烷,石英,聚苯并咪唑,聚醚酮,聚苯硫醚,聚对苯撑苯并二噁唑,碳化硅,酚醛树脂,邻苯二甲酸酯,环烷酸酯,及其组合。
在一个实施方案中,纤维增强物基本上不含碳纳米管。
在另一实施方案中,当纤维增强物含有导电纤维时,可固化体系进一步需要(i)非导电分隔体,置于碳纳米管片与预浸料坯之间,或者(ii)用可固化树脂至少部分地浸渍碳纳米管片。碳纳米管片中的可固化树脂可以与预浸料坯中的可固化树脂相同或不同。
不意在受限于理论,据认为如果使电流经过碳纳米管片(如本文将更详细描述的那样)来固化预浸料坯,则使碳纳米管片与含有导电纤维的预浸料坯直接接触会引起短路。
在又一实施方案中,一个或多个碳纳米管片基本上不含可固化树脂,并且在可固化体系中基本上保持游离,这是因为预浸料坯和一个或多个碳纳米管片之间放置了非导电分隔体。
可固化树脂可以选自例如但不限于聚酰亚胺,聚偏二氟乙烯,聚醚酰亚胺,聚酰胺,聚丙烯腈丁二烯苯乙烯,聚苯硫醚,聚苯乙烯,聚碳酸酯,聚乳酸,聚醚醚酮,聚醚酮酮,氟化乙烯丙烯,聚乙烯醇,及其组合。
可固化树脂的另外的非限定性例子包括但不限于环氧树脂,氰酸酯树脂,马来酰亚胺树脂,双马来酰亚胺-三嗪树脂,酚树脂,间苯二酚树脂,不饱和聚酯树脂,邻苯二甲酸二烯丙酯树脂,脲树脂,三聚氰胺树脂,苯并噁嗪树脂(例如多官能的N-苯基苯并噁嗪树脂,如酚酞系,硫代二苯基系,双酚A系,双酚F系,二环戊二烯系苯并噁嗪树脂),聚氨酯,以及它们的混合物。合适的混合物的例子可以是环氧树脂和苯并噁嗪树脂的混合物。
环氧树脂可以是二官能或更高官能的环氧树脂。这样的环氧树脂由前体如胺(例如四缩水甘油基二氨基二苯基甲烷,三缩水甘油基对氨基酚,三缩水甘油基间氨基酚,和三缩水甘油基氨基甲酚,和它们的异构体),酚(例如双酚A环氧树脂,双酚F环氧树脂,双酚S环氧树脂,酚-酚醛清漆环氧树脂,甲酚-酚醛清漆环氧树脂和间苯二酚环氧树脂),和具有碳-碳双键的化合物(例如脂环族环氧树脂)制备。应当注意的是,环氧树脂不限于上面的例子。还可以使用通过卤化这些环氧树脂而制备的卤化环氧树脂。此外,可以将这些环氧树脂的两种或更多种的混合物,以及单环氧化合物用于可固化树脂中。
在一个实施方案中,可固化树脂可以与一种或多种添加剂相组合,添加剂包括例如但不限于催化剂或固化剂,抗氧化剂,增韧剂,UV稳定剂,和阻燃剂。
在一个实施方案中,碳纳米管片在片的每个相对端处具有连接体部分(如前所述),其能够具有附接的电极,以使得电流可以经过碳纳米管片。
在可固化体系如本文所述组装之前或之后,连接体部分可以附接于碳纳米管片的每个端部。
预浸料坯或预浸料坯的堆叠体的厚度可以是约0.1mm至约160mm,或约1mm至约160mm,或约5mm至约155mm,或约10mm至约140mm,或约20mm至约130mm,或约50mm至约100mm,或约50mm至约80mm。
在另一方面中,本发明涉及一种生产可固化体系的方法,其包括(i)提供本文所述的两个或更多个预浸料坯和一个或多个碳纳米管片,(ii)任选地将可固化树脂注入碳纳米管片中以形成预浸的碳纳米管片,和(iii)将碳纳米管片中的一个或多个置于至少两个预浸料坯之间。
在一个实施方案中,一个或多个碳纳米管片已经注有一种或多种可固化树脂,以形成预浸的碳纳米管片。
在另一实施方案中,生产可固化体系的方法进一步包括将连接体部分附接于一个或多个碳纳米管片的每个相对端上,其能够具有附接的电极,以使得电流可以经过碳纳米管片。
在一个可选的实施方案中,在将一个或多个碳纳米管片置于至少两个预浸料坯之间之前,在一个或多个碳纳米管片的每个相对端上已经附接有连接体部分。
在又一实施方案中,生产可固化体系的方法还包括将非导电分隔体置于每个碳纳米管片与预浸料坯之间的步骤。
固化单个预浸料坯或预浸料坯的堆叠体
本发明的一个具体方面涉及一种用碳纳米管片固化单个预浸料坯来形成复合材料层合体的方法。该方法包括(i)提供包含预浸料坯和一个或多个碳纳米管片的可固化体系,其中碳纳米管片中的至少一个置于预浸料坯的顶部和/或底部;和(ii)通过以下任一项来至少部分地固化可固化体系:(a)使电流经过一个或多个碳纳米管片,以使预浸料坯的至少一部分固化,(b)使可固化体系经历交变电磁场(EMF),以使预浸料坯的至少一部分固化,或者(c)使电流经过一个或多个碳纳米管片,并且使可固化体系经历交变电磁场,以使预浸料坯的至少一部分固化。
在另一方面中,本发明涉及一种用一个或多个碳纳米管片固化预浸料坯的堆叠体来形成复合材料层合体的方法。该方法包括(i)提供包含两个或更多个预浸料坯的堆叠体和一个或多个碳纳米管片的可固化体系,其中碳纳米管片中的至少一个置于两个或更多个预浸料坯之间;和(ii)通过以下任一项来至少部分地固化可固化体系:(a)使电流经过一个或多个碳纳米管片,以使预浸料坯的至少一部分固化,(b)使可固化体系经历交变电磁场(EMF),或者(c)使电流经过一个或多个碳纳米管片,并且使可固化体系经历交变电磁场,以使预浸料坯的至少一部分固化。
在一个实施方案中,碳纳米管片是包含基本上非对齐的碳纳米管的自支撑式非织造片。不意在受限于任何一种特定的理论,据信当使电流经过碳纳米管片和/或使可固化体系经历交变电磁场时,包含基本上非对齐的碳纳米管的碳纳米管片具有改进的热的随机化,这有助于将热在碳纳米管片的全部方向上更均匀地辐射/分布,由此使得预浸料坯的固化更均匀。
在另一实施方案中,通过使电流经过碳纳米管片和/或使可固化体系经历交变电磁场,可固化体系不是仅部分固化,而是基本上或完全固化。
可选地,可固化体系可以通过前述方法与通常的固化技术(其包括例如将可固化体系暴露于外部施加的升高温度)组合使用来固化。外部施加的升高温度可以是例如但不限于70℃至110℃,和任选的升高压力。即使使用这样的外部施加的升高温度,据信所需能量将显著减少,这是因为来自于一个或多个碳纳米管片的受控的、均匀分布的热的内部分布所带来的受控的、有效的热分布。
使电流经过一个或多个碳纳米管片的步骤包括将电极连接到碳纳米管片的两侧(例如两个相对端)来形成电路,和供给约0.5W/in2至50W/in2的量的电功率以通过碳纳米管片产生电阻式红外加热。可以经过一个或多个碳纳米管片的电流的电压可以是约1至10V。在一个实施方案中,将电极连接到附接于一个或多个碳纳米管片的连接体。
如本领域技术人员会理解的,可以根据供给到一个或多个碳纳米管片的电功率的量来控制碳纳米管片产生的红外加热的量。同样,可以主动控制单个预浸料坯或预浸料坯的堆叠体的固化条件来避免过度加热和失控固化,并且同样地避免引起保持预浸料坯的堆叠体或预浸料坯本身的模具的损坏。这样的主动控制预浸料坯或预浸料坯的堆叠体的固化条件的能力使得形成的复合材料基本上均匀地固化。
在用一个或多个碳纳米管片固化预浸料坯的堆叠体的情况中,提供到每个碳纳米管片的电功率可以对于每个碳纳米管片相同或不同,以产生可固化体系受控的加热和固化。例如,具有锥状厚度的预浸料坯堆叠体可以具有引入其中的多个碳纳米管片,其接收不同的电功率输入,从而预浸料坯堆叠体最厚的段将以与最薄的段相同或相似的速率均匀固化,由此形成基本上均匀固化的复合材料。
使可固化体系经历交变电磁场的步骤可以包括使用辐射源来发射电磁场,从而在碳纳米管片内产生涡电流,和产生感应加热。
固化液体可固化树脂
本发明的另一方面涉及一种固化液体可固化组合物的方法。该方法包括(i)使碳纳米管片与可固化组合物接触,其中与碳纳米管片接触的可固化组合物的量足以在该碳纳米管片上形成厚度约1mm至160mm,或约5mm至约155mm,或约10mm至约140mm,或约20mm至约130mm,或约50mm至约100mm,或约50mm至约80mm的层;和(ii)通过以下任一项来至少部分地固化液体可固化组合物(即将液体可固化组合物固化到该液体可固化组合物至少部分固化的程度):(a)使电流经过一个或多个碳纳米管片,以使液体可固化组合物的至少一部分固化,(b)使可固化体系经历交变电磁场(EMF),以使液体可固化组合物的至少一部分固化,或者(c)使电流经过一个或多个碳纳米管片,并且使可固化体系经历交变电磁场,以使液体可固化组合物的至少一部分固化。
在一个实施方案中,碳纳米管片是基本上非对齐的碳纳米管的自支撑式非织造片。
在一个具体实施方案中,一个或多个碳纳米管片在具有特定形状的模具中。
在另一实施方案中,碳纳米管片至少部分地覆盖在硅酮基底和/或聚烯烃,尼龙,氟化聚合物,乙烯-乙酸乙烯酯或其组合的层合体中。氟化聚合物的非限定性例子包括氟化乙烯,偏二氟乙烯(即1,1-二氟乙烯)和四氟乙烯。
仅通过使电流经过碳纳米管片和/或使可固化体系经历交变电磁场,液体可固化组合物可以部分地,大部分或完全地固化。可选地,液体可固化组合物可以通过这样的方法与常规的固化技术(其包括例如将可固化体系暴露于外部施加的升高温度)组合使用来固化。外部施加的升高温度可以是例如但不限于70℃至110℃,和任选地使用升高压力。
液体可固化组合物包含本文所述的一种或多种可固化树脂和任选的一种或多种添加剂,其包括但不限于催化剂或固化剂,抗氧化剂,增韧剂,UV稳定剂和阻燃剂。
如前所述,使电流经过一个或多个碳纳米管片的步骤包括将电极连接到碳纳米管片的两侧(例如两个相对端)来形成电路,和供给0.5W/in2至50W/in2的量的电功率以通过碳纳米管片产生电阻式红外加热。可以经过一个或多个碳纳米管片的电流的电压可以是约1至10V。在一个实施方案中,将电极连接到附接于一个或多个碳纳米管片的连接体。
同样,如本领域技术人员会理解的,可以根据供给到一个或多个碳纳米管片的电功率的量来控制碳纳米管产生的红外加热的量。同样,可以主动控制液体可固化组合物的固化条件来避免液体可固化组合物过度加热和失控固化,并且同样地避免引起保持液体可固化组合物的模具的损坏。这样的主动控制可固化组合物的固化条件的能力使得形成的复合材料基本上均匀地固化。
在一个实施方案中,液体可固化组合物可以进一步包含增强元件,其包括单向纤维,织造纤维,短切纤维,非织造纤维或长的不连续纤维。这样的纤维可以选自导电纤维,非导电纤维,及其组合。
具体地,纤维可以选自导电纤维,非导电纤维,及其组合。具体地,纤维可以选自玻璃,例如S玻璃,S2玻璃,E玻璃,R玻璃,A玻璃,AR玻璃,C玻璃,D玻璃,ECR玻璃,玻璃长丝,短玻璃纤维,T玻璃和锆玻璃,碳聚丙烯腈,碳纤维,丙烯酸纤维,聚对亚苯基对苯二甲酰胺,二氧化硅,芳酰胺,硼,聚亚烷,石英,聚苯并咪唑,聚醚酮,聚苯硫醚,聚对苯撑苯并二噁唑,碳化硅,酚醛树脂,邻苯二甲酸酯,环烷酸酯,及其组合。
在一个实施方案中,增强元件基本上不含碳纳米管。
在另一实施方案中,当纤维增强物含有导电纤维时,则(i)必须存在非导电分隔体,置于碳纳米管片与液体可固化组合物之间,或者(ii)必须用可固化树脂来至少部分地浸渍碳纳米管片。至少部分地浸渍碳纳米管片的可固化树脂可以与预浸料坯中的可固化树脂相同或不同。
本文所述的复合材料(及其制造方法)可以用于生产多种材料,和可以特别用于制造和组装用于航天和汽车应用的复合部件。此外,本文公开的复合材料及其制造方法可以用于生产风轮机叶片,其通常具有非常厚的区段和非常薄的区段,这就必需对固化进行高水平控制以避免会导致过度加热和/或失控固化的高放热。
Claims (19)
1.生产复合材料层合体的方法,其包括:
(i)提供可固化体系,其包含:
-两个或更多个预浸料坯的堆叠体,和
-一个或多个碳纳米管片,其中该碳纳米管片中的至少一个置于该两个或更多个预浸料坯之间,和其中该碳纳米管片是基本上非对齐的碳纳米管的自支撑式非织造片;和
(ii)通过以下任一种来至少部分地固化该可固化体系:(a)使电流经过该一个或多个碳纳米管片,以使该预浸料坯的至少一部分固化,(b)使该可固化体系经历交变电磁场,以使该预浸料坯的至少一部分固化,或者(c)使电流经过该一个或多个碳纳米管片,并且使该可固化体系经历交变电磁场,以使该预浸料坯的至少一部分固化。
2.根据权利要求1所述的方法,其中每个预浸料坯包含纤维增强物和可固化树脂的混合物。
3.根据权利要求2所述的方法,其中该纤维增强物包含选自导电纤维、非导电纤维,及其组合的纤维。
4.根据权利要求3所述的方法,其中该纤维增强物包含导电纤维。
5.根据权利要求4所述的方法,其中将非导电片置于该一个或多个碳纳米管片的每个与该预浸料坯之间。
6.根据权利要求1所述的方法,其中该碳纳米管片进一步包含引入其中的可固化树脂。
7.根据权利要求1所述的方法,其中该两个或更多个预浸料坯的堆叠体的厚度是0.1mm至160mm。
8.根据权利要求1所述的方法,其中该两个或更多个预浸料坯的堆叠体的厚度是50mm至约80mm。
9.根据权利要求1所述的方法,其中该碳纳米管片可以分别置于预浸料坯之间的不同位置。
10.根据权利要求1所述的方法,其中一个或多个碳纳米管片置于该两个或更多个预浸料坯的堆叠体的中间,以使得在该一个或多个碳纳米管片的两侧上的该预浸料坯的厚度基本上相同。
11.根据权利要求1所述的方法,其中至少部分地固化该可固化体系的步骤包括使电流经过该一个或多个碳纳米管片,以使该预浸料坯的至少一部分固化。
12.根据权利要求1所述的方法,其中至少部分地固化该可固化体系的步骤包括使该可固化体系经历交变电磁场,以使该预浸料坯的至少一部分固化。
13.根据权利要求11或12所述的方法,其中该可固化体系基本上均匀固化。
14.固化液体可固化组合物的方法,其包括:
-使碳纳米管片与液体可固化组合物接触,其中(i)与该碳纳米管片接触的可固化组合物的量足以在该碳纳米管片上形成厚度1mm至160mm的层,和(ii)该碳纳米管片是基本上非对齐的碳纳米管的自支撑式非织造片;和
-通过以下任一项来至少部分地固化该可固化体系:(a)使电流经过该一个或多个碳纳米管片,以使该预浸料坯的至少一部分固化,(b)使该可固化体系经历交变电磁场,以使该预浸料坯的至少一部分固化,或者(c)使电流经过该一个或多个碳纳米管片,并且使该可固化体系经历交变电磁场,以使该预浸料坯的至少一部分固化。
15.根据权利要求14所述的方法,其中首先将该碳纳米管片置于模具中。
16.根据权利要求14所述的方法,其中该碳纳米管片进一步包含至少部分地引入其中的可固化树脂。
17.根据权利要求14所述的方法,其中该碳纳米管片至少部分地覆盖在硅酮基底和/或聚烯烃、尼龙、氟化聚合物、乙烯-乙酸乙烯酯或其组合的层合体中。
18.生产复合材料层合体的方法,其包括:
(i)提供可固化体系,其包含:
-预浸料坯,和
-一个或多个碳纳米管片,其中该碳纳米管片中的至少一个置于该预浸料坯的顶部和/或底部,和其中该碳纳米管片是基本上非对齐的碳纳米管的自支撑式片;和
(ii)通过以下任一项来至少部分地固化该可固化体系:(a)使电流经过该一个或多个碳纳米管片,以使该预浸料坯的至少一部分固化,(b)使该可固化体系经历交变电磁场(EMF),或者(c)使电流经过该一个或多个碳纳米管片,并且使该可固化体系经历交变电磁场,以使该预浸料坯的至少一部分固化。
19.通过根据权利要求1、14或18中任一项所述的方法获得的复合材料。
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JP2022518347A (ja) | 2022-03-15 |
EP3894211A4 (en) | 2022-08-31 |
US12017421B2 (en) | 2024-06-25 |
US20220080681A1 (en) | 2022-03-17 |
EP3894211A1 (en) | 2021-10-20 |
WO2020123326A1 (en) | 2020-06-18 |
KR20210110612A (ko) | 2021-09-08 |
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