CN108349726B - 多层可适形复合材料 - Google Patents
多层可适形复合材料 Download PDFInfo
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- CN108349726B CN108349726B CN201680053434.5A CN201680053434A CN108349726B CN 108349726 B CN108349726 B CN 108349726B CN 201680053434 A CN201680053434 A CN 201680053434A CN 108349726 B CN108349726 B CN 108349726B
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- nanofiber
- sheet
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- polymer
- layer
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Abstract
本发明公开了一种包括可热适形聚合物和纳米纤维片材的复合材料。所述可热适形聚合物可以是热熔性粘合剂,并且所述组合可提供导电热熔性粘合剂复合材料。所述纳米纤维层是受保护的并且所述复合材料是可适形的和/或可以附着至多种表面。
Description
发明领域
本公开涉及包括纳米纤维片材和聚合物的层的多层复合材料,并且具体地涉及碳纳米管片材和可变形聚合物的复合材料。
背景
由碳纳米管(CNT)组成的片材可以是薄、结实且柔性的,并且具有独特的电特性。然而,这些片材难以成形和与另外的组分整合,所以在复合材料中使用CNT一直是受限的。
概述
在一方面,提供一种纳米纤维复合材料,所述纳米纤维复合材料包括纳米纤维片材,其包含纳米管;以及可热适形聚合物层,其附着至所述纳米纤维片材。所述纳米纤维复合材料的所述纳米管可包括碳纳米管。所述纳米管可以是单壁或多壁的。所述纳米纤维片材的厚度可以小于100nm。所述纳米纤维片材可从纳米纤维簇(nanofiber forest)拉延出并且可嵌入在所述聚合物层中。所述纳米纤维片材的电阻可以小于1000欧姆/平方。所述复合材料可在所述纳米纤维片材的表面上包括金属层。可以使用任何数目的纳米纤维片材,并且所述片材可以彼此电接触或可以彼此电隔离。所述可适形聚合物层可以分层于多个纳米纤维片材之间,并且在一些复合材料中,所述金属层的一部分是透过所述聚合物暴露的。所述聚合物可选自ABS、HDPE、LDPE、PP、PVB、PVA、HIPS、PETG、PC、丙烯酸类聚合物及其混合物和共聚物。所述可适形聚合物的Tg可小于200℃、小于150℃、小于100℃、小于75℃或小于50℃。所述可适形聚合物的Tg可大于200℃、大于150℃、大于100℃、大于50℃或大于25℃。所述纳米纤维复合材料可透射大于50%、大于75%、大于90%、大于95%、大于98%或大于99%的入射可见光。所述复合材料还可包含玻璃、陶瓷或透明聚合物。所述纳米纤维复合材料可包含聚乙烯醇缩丁醛(polyvinyl butural)或乙烯-乙酸乙烯酯并且可以是车辆挡风玻璃或窗户。挡风玻璃或窗户可以包括两个电接触部。
在另一方面,提供一种制备纳米纤维复合材料的方法,所述方法包括在高于可热适形聚合物的Tg的温度下将纳米纤维片材接合至所述可热适形聚合物以形成所述纳米纤维复合材料,以及将所述纳米纤维复合材料冷却至低于所述可热适形聚合物的Tg以形成所述纳米纤维复合材料。所述纳米纤维片材可包含碳纳米管,所述碳纳米管可以是单壁或多壁纳米管。所述纳米纤维片材的所述纳米纤维可以是金属化的。所述方法可包括将多个纳米纤维片材与一层或多层可热适形聚合物层接合。可使所述纳米纤维片材和所述可热适形聚合物通过一对相对的辊以使所述纳米纤维片材和所述聚合物嵌入在一起。多个纳米纤维片材可接合至所述可热适形层,并且多个可适形层可接合至一个或多个纳米纤维片材。
在另一方面,提供一种方法,所述方法包括向包括至少一种纳米纤维片材和至少一种可热适形聚合物的复合材料施加热、改变所述纳米纤维复合材料的形状以适形于下面的设备,以及使所述纳米纤维复合材料冷却以使所述纳米纤维复合材料变硬成将所述纳米纤维复合材料接合至所述设备的形状。所述复合材料的形状可通过重力或真空或通过按压所述纳米纤维复合材料的表面而改变以使所述纳米纤维复合材料适形于设备。所述设备可以是电子设备,并且所述纳米纤维复合材料可以减少到达所述设备的电磁辐射量。所述纳米纤维片材可以包含碳纳米管,并且所述片材中的所述纳米管可以是金属化的。可通过焦耳加热、感应加热、辐射加热、传导加热或对流加热施加所述热。所述纳米纤维复合材料可以通过加热所述纳米纤维层而加热,并且可通过焦耳加热或通过感应加热进行所述加热。
附图简述
图1是示出碳纳米管簇的一个实施方案的显微照片的副本;
图2是示出用于使碳纳米管簇生长的炉的一个实施方案的示意图;
图3示意性地示出纳米纤维片材的实施方案的尺寸;
图4是用于从碳纳米管簇拉延出碳纳米管片材的工艺的实施方案的侧视图的照片的副本;
图5提供在向下观看纳米纤维的轴线的情况下,纳米纤维复合材料的实施方案的示意性剖视图;
图6A-6D是透射电子显微镜(TEM)图像,其示出根据示例性实施方案的在其上已沉积钛缓冲层的碳纳米纤维;
图7A-7D是TEM图像,其示出根据示例性实施方案的在其上已沉积钛缓冲层和铜金属层的碳纳米纤维;
图8是TEM图像,其示出在其上已沉积铜适形层,但在碳纳米纤维与铜层之间无碳化物形成金属的缓冲层的碳纳米纤维;
图9A-9G示出纳米纤维复合材料的一个实施方案的构造;
图10是纳米纤维复合材料的另一个实施方案的剖视图;并且
图11A和11B是示出纳米纤维基底的另一实施方案的显微照片的副本。
所述附图仅出于说明性目的示出本公开的各种实施方案。多种变型、构型和其他实施方案将根据以下详细讨论而显而易见。
详述
碳纳米纤维和碳纳米纤维片材的特性
如本文所用,术语“纳米纤维”意指平均直径小于1μm的纤维。虽然本文的实施方案主要描述为由碳纳米管制造,但是应了解其他碳同素异形体(不论是石墨烯、微米级或纳米级石墨纤维和/或板)以及甚至其他组成的纳米级纤维诸如氮化硼可以用于使用下文所述的技术制造纳米纤维片材。出于本公开的目的,碳基材料(例如碳纳米管)和非碳基材料可以被认为是“纳米纤维”。
如本文所用,术语“纳米纤维”和“碳纳米管”涵盖碳原子连接在一起形成圆柱形结构的单壁碳纳米管和/或多壁碳纳米管。多壁纳米管具有两个或更多个壁。在一些实施方案中,如本文提及的碳纳米管具有在4个与10个之间的壁。如本文所用,“纳米纤维片材”或仅“片材”是指下述纳米纤维片材,所述纳米纤维片材通过拉延工艺(如PCT公开号WO 2007/015710中所述的并且所述专利以引用的方式整体并入)对齐,使得片材的纳米纤维的纵向轴线平行于片材的主表面,而非垂直于片材的主表面(即,呈片材的沉积态形式,通常称之为“簇”)。
碳纳米管的尺寸可以根据使用的产生方法而有很大变化。例如,具有一个、两个、三个、四个或更多个壁的碳纳米管的直径可以是0.4nm至100nm,并且在一些情况下可以在1nm与80nm之间、在10nm与70nm之间或在20nm与50nm之间。在一些实施方案中,碳纳米管的长度可以在10μm至大于55.5cm的范围内并且在一些实施方案中可以在20μm与50cm之间。碳纳米管还能够具有非常高的纵横比(长度与直径的比),其中一些高达132,000,000:1或更多。鉴于尺寸可能性的宽范围,碳纳米管的特性是高度可调节的或可调的。虽然已鉴定出碳纳米管的许多有趣特性,但是在实际应用中利用碳纳米管的特性需要使碳纳米管的特征被保持或增强的可规模化且可控的产生方法。
由于其独特结构,碳纳米管具有使其非常适于某些应用的特定的机械特性、电特性、化学特性、热特性和光学特性。具体地,碳纳米管表现出优异的电导率、高机械强度、良好热稳定性并且还是疏水性的。除了这些特性之外,碳纳米管还可表现出有用的光学特性。例如,碳纳米管可用于发光二极管(LED)和光检测器中来发射或检测在严密选定的波长下的光。碳纳米管也被证实可用于光子传输和/或声子传输。
虽然已鉴定出碳纳米管的许多有趣特性,但是在实际应用中利用碳纳米管的特性需要使碳纳米管的特征被保持或增强的可规模化且可控的产生方法。本文公开了提供呈各种构型的碳纳米管的可控组装的方法和设备。例如,公开了将对齐的碳纳米管组装在基底上或组装成独立形式的方法。除了其他特征之外,所公开的方法允许碳纳米管成功地转移而不破坏对齐、使碳纳米管构型密度受控并且提供光学调谐的机会。
纳米纤维簇
根据本公开的各种实施方案,纳米纤维(包括但不限于碳纳米管)可布置成各种构型,包括本文称之为“簇”的构型。如本文所用,纳米纤维或碳纳米管的“簇”是指具有大约等同尺寸的纳米纤维在基底上被布置成彼此大致上对齐的阵列。纳米纤维尤其是在其基部处大致上正交于基底。图1示出基底上的纳米纤维的示例性簇。基底可以是任何形状,但在一些实施方案中,基底具有在其上组装簇的平坦表面。如在图1中可看出的,簇中的纳米纤维的高度和/或直径可以大约相等。
在一些实施方案中,簇的纳米纤维可各自以大约相同角度朝向基底取向。例如,簇的纳米纤维可相对于基底具有在45°与135°之间的平均角度。在具体实施方案中,簇的平均纳米纤维可以取向成偏离基底75°与105°之间,并且在选择的实施方案中,平均纳米纤维可以取向成偏离基底大约90°。
如本文公开的纳米纤维簇可以相对致密。具体地,所公开的纳米纤维簇(包括具有3、4、5或更多个壁的那些)在基底上的密度可以为至少109个纳米纤维/cm2。在一些具体实施方案中,如本文所述的纳米纤维簇的密度可以大于109个纳米纤维/cm2、大于1010个纳米纤维/cm2、大于2x1010个纳米纤维/cm2或大于3x1010个纳米纤维/cm2。在其他实施方案中,纳米纤维簇的密度(纳米纤维/cm2)可以在109与3x1010之间、在1010与3x1010之间、在1010与5x1010之间。簇可包括高密度或低密度区域并且特定区域可以不含纳米纤维。簇内的纳米纤维还可表现出纤维间连接性。例如,纳米纤维簇内的相邻纳米纤维可以通过靠近力(包括范德华力)彼此吸引。
用于产生纳米簇的示例性方法
各种方法可以用于产生根据本公开的纳米纤维簇。例如,在一些实施方案中,纳米纤维可以在高温炉中生长。在一些此类实施方案,催化剂可以沉积在基底上、放置于反应器中并且然后可以暴露于供应至反应器的燃料化合物。基底可以耐受大于800℃至1000℃的温度并且可以是惰性材料。基底可以包括设置在下面的硅(Si)晶片上的不锈钢(stainlessstreel)或铝,但是可以使用其他陶瓷基底替代Si晶片(例如,氧化铝、氧化锆、SiO2和玻璃陶瓷。在簇的纳米纤维是碳纳米管的实例中,碳基化合物,包括脂族烃诸如乙炔、甲烷和乙烷可以用作碳原子来源。在引入到反应器之后,燃料化合物然后可分解并且所得碳原子可聚集在催化剂上并且通过从基底向上生长开始组装纳米管以形成纳米纤维簇。
用于生长纳米纤维的示例性反应器的图示出于图2中。如在图2中可看出的,反应器可包括基底可定位其中的加热区以有利于纳米纤维簇生长。反应器还可包括可将燃料化合物和载气供应至反应器的气体入口和可使消耗的气体从反应器释放出的气体出口。载气的实例包括氮气、氢气、氩气和/或氦气。另外,待掺入纳米纤维中的掺杂剂可添加到气体流。示例性掺杂剂包括但不限于氮和硼。在沉积纳米纤维簇期间添加掺杂剂的示例性方法在美国专利号8,926,933的第287段处得到描述,所述专利以引用的方式整体并入本文。向簇掺杂或提供添加剂的其他示例性方法包括表面涂覆、掺杂剂注射或其他沉积和/或原位反应(例如,等离子体诱导的反应、气相反应、溅镀、化学气相沉积)。示例性添加剂包括聚合物(例如,聚(乙烯醇)、聚亚苯基四邻苯二酰胺(poly(phenylene tetrapthalamide))式树脂、聚(对亚苯基苯并双噁唑)、聚丙烯腈、聚(苯乙烯)、聚(醚醚酮)和聚(乙烯吡咯烷酮或其衍生物或组合)、元素或化合物(例如氟)的气体、金刚石、钯和钯合金等等。
可以改变纳米纤维生长期间的反应条件以调节所得纳米纤维簇的特性。例如,催化剂的粒径、催化剂图案、反应温度、气体流速和/或反应时间可按需调节以产生具有所需规格的纳米纤维簇。在一些实施方案中,对催化剂在基底上的位置进行控制以形成具有所需图案化的纳米纤维簇。例如,在一些实施方案中,催化剂以图案沉积在基底上并且根据图案化催化剂生长的所得簇被类似地图案化。示例性催化剂包括二氧化硅(SiO2)或铝氧化物(例如Al2O3)缓冲层上的铁。可使用任何合适方法将催化剂沉积在基底上,所述方法包括化学气相沉积(CVD)、激光辅助的CVD、等离子体增强的CVD、电子束(eBeam)沉积、溅镀、热蒸发、电化学方法或原子层沉积(ALD)。为了形成图案,在一些实施方案中,催化剂可沉积成图案的形式,并且在其他实施方案中,可在特定区域中将催化剂去除或使其中毒来产生纳米管纤维图案。缓冲层也可以图案施加至基底,并且可例如通过涂覆、压延、浸渍、喷墨印刷、移印或通过使用以上所述的物理或化学沉积方法施加。
在形成之后,纳米纤维簇可任选地进行改性。例如,在一些实施方案中,可使纳米纤维簇暴露于处理剂诸如氧化剂或还原剂。在一些实施方案中,簇的纳米纤维可任选地通过处理剂进行化学官能化。可通过任何合适方法将处理剂引入到纳米纤维簇,所述方法包括但不限于物理沉积、原子沉积、化学气相沉积(CVD)和液体或气体渗透。在一些实施方案中,纳米纤维簇可进行改性以形成图案化簇。簇的图案化可以例如通过从簇选择性地除去纳米纤维而达成。除去可以通过化学或物理手段诸如激光烧蚀来实现。
纳米纤维片材的详细解释
除了布置成簇构型之外,本申请的纳米纤维还可布置成片材构型。如本文所用,术语“纳米纤维片材”、“纳米管片材”或仅“片材”是指其中纳米纤维在平面中端至端对齐的纳米纤维的布置,所述平面的长度和/或宽度比片材的厚度大超过100倍。纳米纤维片材可具有例如大约5nm与20μm之间的厚度和适于预期应用的任何长度和宽度。在一些实施方案中,纳米纤维片材可具有大于100m的长度和大于1m的宽度。示例性纳米纤维片材示出在图3中,其中示出了相对尺寸。如在图3中可看出的,纳米纤维端至端对齐的方向称之为纳米纤维对齐的方向。在一些实施方案中,纳米纤维对齐的方向可以在整个纳米纤维片材上是连续的。
纳米纤维片材可以堆叠在彼此的顶部上以形成多层片材。纳米纤维片材可以堆叠成具有相同的纳米纤维对齐方向或具有不同的纳米纤维对齐方向。任何数目的纳米纤维片材可以堆叠在彼此的顶部上以形成多层纳米纤维片材。例如,在一些实施方案中,纳米纤维片材可包括2、3、4、5、10或更多个单独的纳米纤维片材。邻接片材上的纳米纤维对齐方向可相差小于1°、小于5°或小于10°。在其他实施方案中,邻接片材上的纳米纤维对齐方向可相差超过40°、超过45°、超过60°、超过80°或超过85°。在具体实施方案中,邻接片材上的纳米纤维对齐方向可以是90°。
可使用任何类型的能够产生片材的合适方法组装纳米纤维片材。在一些示例性实施方案中,可从纳米纤维簇拉延出纳米纤维片材。从纳米纤维簇拉延出的纳米纤维片材的实例示出在图5中。如在图4中可看出的,纳米纤维可从簇侧向地拉延出,并且然后端至端地对齐以形成纳米纤维片材。在纳米纤维片材从纳米纤维簇拉延出的实施方案中,可以对簇的尺寸进行控制以形成具有特定尺寸的纳米纤维片材。例如,纳米纤维片材的宽度可以大约等于片材从其中拉延出的纳米纤维簇的宽度。另外,片材的长度可以例如通过在实现所需片材长度时结束拉延过程来进行控制。
在形成之后,可以使纳米纤维片材经受一个或多个后处理过程。例如,在一些实施方案中,纳米纤维片材可任选地致密化。任何适当的致密化方法可以用于致密化纳米纤维片材,包括但不限于使纳米纤维片材暴露于液体并且随后除去液体(例如,通过蒸发)。液体可以多种方式引入到纳米纤维片材,包括例如吸收液体、将片材暴露于液体的气溶胶、蒸汽冷凝或其组合。液体可以是水性或非水性的并且可以是质子或非质子溶剂。具体液体包括但不限于甲苯、苯乙烯、乙醇、乙二醇、丙酮、甲醇、异丙醇、氯仿、氯苯以及正甲基吡咯烷酮。还可以使用两种、三种或更多种液体的混合物。致密化可以影响片材的厚度。在一些具体实例中,纳米纤维片材致密化之前的拉延态密度可以在10与20μm之间,并且致密化之后的密度可以在10至50nm之间。在致密化之前,纳米纤维片材的体积密度可以在0.001至0.005g/cm3、0.001至0.003g/cm3或约0.0015g/cm3的范围内。使用致密化技术,碳纳米管片材的各种实施方案的体积密度可以增加大于10X、20X、50X、100X、500X或1000X倍。应注意,虽然体积密度可以大大增加,但是伴随的面密度增加可以是零或接近于零。这意味着致密化片材可具有与致密化片材由其致密化的原生片材基本上相同的长度和宽度。在各种实施方案中,致密化可使得面积收缩小于10%、小于5%或小于1%。
纳米纤维片材具有可用于各种应用的许多特性。例如,纳米纤维片材可具有可调不透明度、高机械强度和柔韧性、导热性和导电性,并且还可表现出疏水性。鉴于片材内的纳米纤维高度对齐,纳米纤维片材可以是极其薄的,使得其几乎是二维的。在一些实例中,纳米纤维片材在10nm与200nm厚之间(如在正常测量公差内测量的)。这些厚度可以对于390nm至750nm的波长范围内的可见光是完全透明的。片材还可以对于许多其他波长的电磁辐射是透明的。如本文所用,如果产品透射一定波长或波长范围的入射辐射的95%以上,则所述产品对于所述波长或波长范围是透明的。纳米纤维片材的包括可以仅向部件或表面添加极少的附加区域和/或体积。如本文公开的纳米纤维片材还可具有高纯度,其中在一些情况下,超过90%、超过95%或超过99%的重量百分比的纳米纤维片材归属于纳米纤维。类似地,纳米纤维片材可包含超过90重量%、超过95重量%、超过99重量%或超过重量99.9%的碳。纳米纤维和片材可以不含脂族碳并且可以仅是形成单壁管和多壁管(包括具有两个、三个、四个、五个或更多个壁的那些)的芳族结构。在各种实施方案中,纳米管可包括或限于扶手椅型、Z字型和手性结构。
公开的纳米纤维复合材料可具有各种特征和特性。例如,在一些实施方案中,粘合剂纳米纤维复合材料可具有低电阻。具体地,在一些实施方案中,示例性粘合剂纳米纤维复合材料的电阻可小于1000Ω/平方、小于100Ω/平方、小于10Ω/平方、小于1Ω/平方并且在一些情况下可小于0.9Ω/平方、小于0.8Ω/平方、小于0.7Ω/平方、小于0.6Ω/平方、小于0.5Ω/平方、或小于0.1Ω/平方。所公开的纳米纤维复合材料可具有任何所需厚度。例如,在一些实施方案中,公开的纳米纤维复合材料的厚度:小于1mm、小于100、小于10μm、小于1μm、小于0.5μm、小于0.2μm、小于0.1μm、小于50nm、小于40nm或小于30nm。纳米纤维片材与粘合剂比可以按体积计小于1:5、小于1:10、小于1:100或小于1:1000。纳米纤维片材与粘合剂比可以按质量计小于1:5、小于1:10、小于1:100、小于1:1,000或小于1:10,000。
可适形复合材料
在不同实施方案中,纳米管片材可接合到聚合物片材的外表面、可嵌入在聚合物片材中或可部分地嵌入在聚合物片材中。在其他实施方案中,可使用夹层结构,其中一个或多个纳米管片材夹置于两个或更多个聚合物片材之间。在夹层结构中,两个或更多个纳米管片材可彼此直接接触。两个或更多个聚合物片材之间的一个或多个纳米管片材的这种交替结构可重复任何次数,诸如2、3、4或5个堆叠在一起的结构。不同类型的纳米管片材和不同类型的聚合物片材可用于相同结构内。例如,纳米管片材可夹置于熔融可适形聚合物与传导性聚合物之间或熔融可适形聚合物与热固性聚合物之间。
纳米纤维复合材料可包括为可热适形聚合物的一种或多种聚合物。热熔性聚合物是在加热时发生软化并且变得适形的一类可热适形聚合物。当冷却时,它们可变硬并且保持其形状。在一些情况下,将聚合物加热至高于它们的Tg,使得其变得柔韧。可热适形聚合物可以是提供冷却或交联后的两个表面之间的粘附的粘合剂。对于本文所述的大多数复合材料,纳米纤维层在宽泛的温度范围内是柔性的,所以任何刚性将通过一种或多种聚合物组分提供。虽然各种实施方案可使用热塑性塑料、热固性材料或两者的组合,但是如本文所用术语“热熔性聚合物”是指热塑性塑料和可以可逆地硬化的其他聚合物。热塑性塑料包括聚烯烃诸如聚乙烯和聚丙烯、热塑性聚氨酯(TPU)、丙烯酸类树脂、丙烯腈-丁二烯-苯乙烯(ABS)、聚碳酸酯、聚氯乙烯(PVC)、聚酯、聚砜、聚偏二氟乙烯(PVDF)、聚苯醚(PPO)和乙烯-乙酸乙烯酯(EVA)。热熔性聚合物的Tg可大于50℃、大于75℃、大于100℃、大于150℃、大于200℃、大于250℃或大于300℃。在这些和其他实施方案中,聚合物的Tg可小于500℃、小于300℃、小于200℃、小于100℃或小于75℃。不同聚合物的共聚物、混合物和组合可用于达到定制的软化点。
在一些实施方案中,热熔性聚合物可以是热熔性粘合剂(HMA)。热熔性粘合剂是提供通过HMA接合的两种材料之间的粘附的聚合物。热熔性粘合剂在其是热的时通常是可流动的并且在已固化时提供粘合。在一些情况下,热熔性粘合剂可以可逆地使用并且附着的部件可以在重新加热材料之后去除。在其他实施方案中,热熔性粘合剂可以是不可逆的,诸如具有热固性,并且材料可以是永久性粘结在一起的,而与暴露于高温无关。可起热熔性粘合剂作用的聚合物包括乙烯-乙酸乙烯酯(EVA)、乙烯丙烯酸酯、聚烯烃、聚酰胺、聚酯、聚氨酯、苯乙烯嵌段共聚物、聚己内酯、聚碳酸酯、含氟聚合物、硅氧烷和聚吡咯。聚烯烃可以是结晶的或非晶形的并且包括聚乙烯诸如低密度聚乙烯(LDPE)和高密度聚乙烯(HDPE)、聚丙烯、无定形聚丙烯和聚丁烯。聚氨酯包括热塑性聚氨酯(TPU)和反应性聚氨酯。
复合材料可包括与一个或多个平坦的聚合物片材组合的纳米管片材。在这些情况下,聚合物通常覆盖大于90%、大于95%或大于99%的纳米管片材表面积。在其他情况下,聚合物可以不连续图案与纳米管片材组合。例如,聚合物可以条纹、点、圆形或其他规则或不规则图案施加至纳米管片材。在一些情况下,可向纳米管片材的一个侧面施加图案,而向相反侧面施加完整的材料层。聚合物图案可覆盖小于100%、小于80%、小于50%、小于25%或小于10%的纳米管片材表面积。聚合物可施加至纳米管片材的需要粘附或电绝缘的部分,而纳米管片材的其他部分可不含聚合物,使得可与基底、接触材料或其他导电材料形成电接触。金属层还可以不覆盖整个片材的图案形式施加至纳米管片材。在其他情况下,金属可施加至纳米管片材的不含聚合物的区域。例如,聚合物图案可留下不含聚合物的两个接触点,并且金属可沉积在这些点上以提供与例如两个电极的电接触。
纳米管片材可任选地在形成聚合物复合材料之前或之后处理。例如,金属层可以图案形式沉积在纳米管片材的一部分上,或沉积在整个纳米管片材上。纳米管片材可在形成聚合物复合材料之前或之后致密化。纳米管片材的表面特征还可通过例如改变纳米管和纳米管片材的表面能来改变。例如,可通过氧化片材的暴露表面的至少一些,诸如通过臭氧化使得片材更具聚合物相容性,以产生具有较高表面能和较大粘附能力的纳米管片材。在其他实施方案中,电接插件可在形成复合材料之前或之后附接至纳米管片材的一个或多个部分。电接插件可通过金属层和/或缓冲层连接至纳米管片材。
在一组实施方案中,纳米管片材可嵌入在聚合物片材诸如可热适形聚合物片材中。纳米管片材可以是拉延态的或可以是致密化的。纳米管片材可以放置于基底上并且基底可以是低表面能基底诸如PTFE或硅氧烷。一个或多个聚合物片材可放置于纳米管片材上,并且聚合物可通过例如将聚合物加热至其Tg或更高来软化。软化的聚合物可渗透进纳米管片材的纳米管之间的空隙。如果一些纳米管涂覆有金属,则聚合物可优选接触未涂覆的纳米管,而避免金属涂覆的纳米管。为了增大聚合物和纳米管的渗透,可向纳米管/聚合物叠层施加压力,或可使用真空。例如,可将叠层置于按压机中或使所述叠层通过一对辊。
在另一组实施方案中,复合材料包括纳米纤维片材和可热适形聚合物。可热适形聚合物在加热时可软化并且可改变形状并且可以是粘合性或非粘合性的。可热适形聚合物在加热时可变得更有延展性和柔韧性并且在冷却时可变硬并且有更小延展性。一些可热适形聚合物在加热时将液化并且可流动。聚合物可例如是热塑性或热固性聚合物。聚合物和纳米纤维片材例如碳纳米管片材可以设置在不同的层中或者可以彼此嵌入。复合材料中可以包括另外的材料诸如导电层、颜料、染料、绝缘体、增粘剂、流变改性剂、电接触部和防粘片。导电材料可包括可沉积在纳米纤维片材上、聚合物上或复合材料上的金属。金属层可通过本领域的技术人员已知的方法沉积,所述方法诸如化学气相沉积(CVD)、压力辅助化学气相沉积(PCVD)、电子束沉积(eBeam)、溅镀、原子层沉积(ALD)和/或电镀。纳米纤维片材可单独地金属化,或在一些实施方案中在呈一个以上的纳米纤维片材的堆叠布置的时候金属化。金属沉积将增大纤维的直径并且在一些情况下可使纤维的直径增大超过2X、5X、10X、15X或20X。在一些金属化纳米纤维片材的堆叠布置的此类实施方案中,金属可不仅沉积在最上面片材的纳米纤维上,而且还沉积在一个或多个下面的纳米纤维片材上。在一些实施方案中,一个以上的金属层可沉积在纳米纤维片材上。在金属化粘合剂纳米纤维复合材料的实施方案中,缓冲层可在沉积金属之前沉积在纳米纤维片材上。在一些此类实施方案中,缓冲层可使用用于金属化纳米纤维片材的任何技术沉积,所述技术包括CVD、PCVD、电子束沉积、溅镀、ALD和/或电镀。在各种实施方案中,缓冲层可改善粘附性、佩戴性、导电性或反射性。本文关于缓冲层110所述的任何材料可以用于形成缓冲层。电接触部可以电连接到导电层。金属层可自身提供传导性层或可充当至纳米纤维片材的电接插件。例如,CNT片材可嵌入聚合物中,同时一体的金属层提供CNT片材与外部电接触部之间的低电阻电接触。在不存在金属层的情况下,聚合物层可阻挡接入并且防止与CNT片材的有效电接触。虽然CNT片材可表现出允许聚合物隔离它的表面特征,但是金属层可能与聚合物不太相容并且因此可在施加时流出聚合物并且向CNT片材提供无聚合物的电接口。
纳米纤维片材诸如CNT片材可表现出优异特性诸如拉伸强度和柔韧性,但是在许多情况下这些片材可易于通过与相邻材料的摩擦而磨损。包括聚合物和纳米纤维片材的复合材料可保持纳米纤维片材的强度特性,同时保护其免受磨损。聚合物可层合在纳米纤维片材的一个或两个侧面上,或者在一些实施方案中,聚合物可嵌入纳米纤维片材中,或者纳米纤维片材可嵌入聚合物中。在其他实施方案中,聚合物层可挤出到纳米纤维片材上。在另外的实施方案中,当聚合物在类似于共挤出的过程中挤出时,聚合物层和纳米纤维片材可接合在一起。例如,纳米纤维片材可在与聚合物挤出机并行运行的过程中使用本文所述的方法形成。在产生纳米纤维片材和聚合物片材时,它们可层合在一起形成复合材料。因为聚合物片材在离开模具时通常是可流动的或低于其玻璃化转变温度(Tg),所以在两组分通过一对辊时所述聚合物片材可嵌入纳米纤维片材中。可调节速度、压力和温度以确定例如复合材料的厚度和聚合物在纳米纤维片材中的嵌入量。可添加纳米纤维片材或聚合物的另外的层,使得在一些实施方案中,纳米管片材是由两个聚合物层环绕的中间层。纳米纤维片材可在形成复合材料之前或之后致密化。在一些情况下,聚合物还可向纳米管片材提供致密化。
在另一组实施方案中,纳米纤维片材可浸泡在液体聚合物或预聚合物中以便用聚合物饱浸和浸透纳米纤维片材。所述过程可以是连续带式过程,其中纳米纤维片材通过液体或分散的聚合物或预聚合物。然后可使饱浸的片材例如通过有隙刮墨刀或一对相对的辊,以去除过量聚合物并且限定复合材料的厚度。然后可硬化、聚合或固化聚合物组分使得可处理和储存复合材料。
在许多实施方案中,纳米纤维复合材料可适形成为多种形状。复合材料可提供可热模塑的导电片材,其可快速地模塑成规则或不规则表面。可通过在导电纳米纤维片材上施加电流来焦耳加热复合材料。在其他应用中,可使用例如热空气或红外线辐射外部加热复合材料。在又另一实施方案中,可通过向复合材料施加磁场来感应加热复合材料。复合材料的传导性纳米纤维片材组分允许复合材料用于电子部件或敏感于电磁辐射的其他设备周围的EMI屏蔽。纳米纤维复合材料还可用作天线。复合材料的柔韧性允许其模塑在原本可能难以包封在导电片材中的不规则形状的物体周围。
如图9A至9G的实施方案中所示,纳米纤维片材可与弯曲的可适形聚合物片材组合以提供可拉伸且可在一个或多个方向上拉伸以能够与多种形状适形的复合材料。在图9A中,弹性层900沿一个或多个方向处于受张力状态,这取决于最终产品的所需能力。弹性材料的实例包括橡胶材料,诸如硅橡胶、聚氨酯橡胶、氟橡胶、丁基橡胶、丁二烯橡胶、异戊二烯橡胶、氯丁二烯橡胶、丙烯酸类橡胶、丁腈橡胶、表氯醇橡胶、胶乳、丁苯橡胶、乙丙橡胶和天然橡胶。弹性材料的另外的实例包括树脂材料(例如热塑性弹性体),诸如硅树脂、氟碳树脂、聚氨酯树脂、聚苯乙烯树脂、聚烯烃树脂和聚酰胺树脂。
在图9B中,可为热熔性粘合剂的可热适形聚合物层910在弹性层900处于受张力状态时施加至弹性层900,以形成复合材料950。图9B示意性地示出在已释放系统中的张力之后图9B的复合材料950看起来的样子。在图9D中,已从复合材料去除弹性层900,留下了可热适形聚合物9D的弯曲层。在图9E中,已将纳米纤维层950放置在弯曲的可热适形聚合物910上以形成复合材料960。在这个阶段,纳米纤维层950可任选地例如通过化学或机械致密化进行致密化。两个层可例如通过施加热附着在一起。在一些情况下,另外的可热适形聚合物层可放置在纳米纤维层950上,使得纳米纤维层950不暴露。图9F和9G提供了复合材料960可如何拉长以在多种应用中使用复合材料的实例。在一些情况下,可加热复合材料960以软化可热适形聚合物层910,但是在许多实施方案中,复合材料960不是弹性的,但是由于可热适形层910的预弯曲而可被拉伸。应注意弯曲是在微观尺度上,并且在许多情况下不能通过人眼观察到。对于弯曲纳米纤维片材看起来的样子的显微照片参见图11A和11B。纳米纤维片材可以任何取向放置在弯曲片材上。例如,纳米纤维可被对齐使得其轴线是沿着可热适形层的拉伸轴线(在图9E中从左至右)或使得其与拉伸轴线成90度(进入页面中观看图9E)。也可使用0°与90°之间的任何构型。多个纳米纤维片材可以堆叠成相对于可热适形层处于相同或不同的取向。在一些实施方案中,可在纳米纤维片材与可热适形层之间使用粘结剂。
在另一个实施方案(诸如图10中示出的)中,复合材料1000包括夹置于两个玻璃片材1010a和1010b之间的纳米纤维片材1030。纳米纤维片材可以是碳纳米管片材。也可包括另外的层诸如粘合剂片材1020a和1020b以及一种或多种金属。粘合剂可使部件夹置在一起,而金属层可添加功能性诸如导电性、IR吸收性或IR反射性。纳米纤维片材可以是传导性的,但具体地对于可见光而言还是半透明或透明的。因此,可见光可穿过玻璃/聚合物粘合剂/纳米纤维片材/聚合物粘合剂/玻璃中的三个、四个、五个或更多个层的复合材料(呈任何次序)。在其他实施方案中,可以使用一个粘合剂片材或粘合剂可嵌入在纳米纤维片材中,从而提供了包含两种组分的单层。纳米纤维片材的导电性可提供抵抗电子窃听的防护并且可有助于防止透射电磁辐射,同时保持良好的光学透明性。此外,纳米纤维层可提供改善的强度和击碎防护,使得产生防爆型窗户。应用包括例如用于可能经受以电子方式和物理方式袭击的政府和私人建筑物的窗户。在其他实施方案中,复合材料可用作挡风玻璃或窗户,并且施加至纳米纤维层的电流可加热挡风玻璃以提供即时的除霜或除冰。另外的层可包括例如粘合剂、颜料或染料。粘合剂包括聚合物诸如由聚乙烯醇(包括聚乙烯醇缩丁醛(PVB)和聚乙烯醇缩甲醛(PVF))制成的那些。这些和其他粘合剂可以片材形式提供。这些聚合物可层合在相对的玻璃片材之间并且可通过施加热、压力或两者来粘结。可将粘合剂层1020a和1020b熔融或软化以使得它们发粘。在冷却后,粘合剂可永久性地或暂时地将层粘结在一起。加热过程可改善粘合剂的清晰度,使得其可用于挡风玻璃或窗户用途。在一些实施方案中,粘合剂可例如是热固化、辐射固化或蒸发固化聚合物体系。玻璃片材中的一个或多个可通过其他透明材料诸如透明陶瓷如蓝宝石或透明聚合物诸如聚碳酸酯替代。因此,纳米纤维片材可保持在牢固接合在一起的两个相对的透明材料片之间。复合材料1000还可包括一个、两个或更多个电接触部以提供电流至纳米纤维片材或提供电接地。
本文所讨论的实施方案主要以包括单个纳米纤维片材和单个聚合物层的复合构型讨论。然而,可以使用包括多层纳米管片材、多层聚合物层或两者的复合材料。例如,单个纳米纤维片材可夹置于可以相同或不同的两个聚合物层之间。可产生纳米纤维片材和聚合物层的交替层,所述交替层可包括每个的一个、两个、三个、四个或更多个层。在多层复合材料中,最外面的相对层可以是两个聚合物层、两个纳米纤维层或聚合物层和纳米纤维层的组合。在其他实施方案中,复合材料的一个或两个外层可以是第三材料诸如金属、玻璃、玻璃纤维或陶瓷。
本公开的实施方案的前述描述已经出于说明的目的来呈现;其并非旨在为详尽的或者使本公开限于权利要求书的精确形式。相关领域的技术人员可了解到根据以上公开内容,许多修改和变化是可能的。
说明书中使用的语言原则上是出于可读性和指导目的而选择的,并且其可并未被选择来界定或者限制发明主题。因此旨在使本公开的范围不受限于此详细说明,而是受限于基于在此申请所提出的任何权利要求。因此,实施方案的公开内容旨在说明而非限制权利要求书中阐明的本发明的范围。
Claims (19)
1.一种纳米纤维复合材料,其包括:
纳米纤维片材,其包含在纳米纤维片材的平面中端至端对齐的碳纳米管,
在纳米纤维片材上的使纳米纤维片材金属化的缓冲层,
在缓冲层上的金属层,
其中所述纳米纤维片材的电阻小于1000欧姆/平方;以及
可热适形聚合物层,其附着至所述纳米纤维片材。
2.如权利要求1所述的纳米纤维复合材料,其中所述纳米纤维片材的平均厚度小于100nm。
3.如权利要求1所述的纳米纤维复合材料,其中所述纳米纤维片材嵌入在所述聚合物层中。
4.如权利要求1所述的纳米纤维复合材料,其在所述纳米纤维片材的表面上还包括金属层。
5.如权利要求4所述的纳米纤维复合材料,其中所述金属层的至少一部分是透过所述聚合物层暴露的。
6.如权利要求1所述的纳米纤维复合材料,其还包括多个纳米纤维片材。
7.如权利要求6所述的纳米纤维复合材料,其中所述多个纳米纤维片材彼此电接触。
8.如权利要求6所述的纳米纤维复合材料,其中所述多个纳米纤维片材彼此电隔离。
9.如权利要求6所述的纳米纤维复合材料,其中至少一个可适形聚合物层分层于所述多个纳米纤维片材之间。
10.如权利要求1所述的纳米纤维复合材料,其中所述复合材料透射大于50%、大于75%、大于90%、大于95%、大于98%或大于99%的与所述纳米纤维复合材料的表面成90°的可见光。
11.如权利要求1所述的纳米纤维复合材料,其还包括玻璃或陶瓷或透明聚合物。
12.如权利要求1所述的纳米纤维复合材料,其中所述可热适形聚合物层包括聚乙烯醇缩丁醛或乙烯-乙酸乙烯酯。
13.如前述权利要求中任一项所述的纳米纤维复合材料,其中所述复合材料组成车辆挡风玻璃或窗户。
14.一种使用纳米纤维复合材料的方法,所述方法包括:
向包括至少一种碳纳米纤维片材和至少一种可热适形聚合物的复合材料施加热;其中所述碳纳米纤维片材包含在纳米纤维片材的平面内且端至端对齐的碳纳米管,且其中所述热适形聚合物包含热熔性聚合物;
改变所述纳米纤维复合材料的形状以适形于下面的设备;以及
使所述纳米纤维复合材料冷却以使所述纳米纤维复合材料变硬成将所述纳米纤维复合材料接合至所述设备的形状;
其中所述纳米纤维片材是金属化的。
15.如权利要求14所述的方法,其中改变所述纳米纤维复合材料的所述形状包括使用真空。
16.如权利要求14所述的方法,其还包括按压所述纳米纤维复合材料的表面以使所述纳米纤维复合材料适形于所述设备。
17.如权利要求14所述的方法,其中通过焦耳加热、感应加热、辐射加热、传导加热或对流加热施加所述热。
18.如权利要求14所述的方法,其中通过加热所述纳米纤维复合材料中的纳米纤维层施加所述热。
19.如权利要求14-18中任一项所述的方法,其中所述纳米纤维复合材料减少到达所述设备的电磁辐射量。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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