CN101629056B - 用于基材热可逆连接的多层粘合剂 - Google Patents
用于基材热可逆连接的多层粘合剂 Download PDFInfo
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Abstract
本发明涉及用于基材热可逆连接的多层粘合剂。本发明的一个具体实施方案包括能够可逆连接刚性基材的多层干燥粘合剂体系。
Description
本申请主张2007年5月23日提交的美国临时申请60/939,680的权利。
技术领域
本公开通常所涉及的领域包括多层粘合剂,含有它们的产品,以及多层粘合剂的制造及使用方法。
背景技术
上面具有纳米绒毛结构(nanohair structures)的壁虎的脚垫,是具有巧妙的干燥粘合剂(dry adhesives)的实例。壁虎抓着力的工作原理是那些纳米绒毛结构可以使脚垫与相对表面产生最大接触,而不管此表面的粗糙度和化学组成如何。这是由纳米绒毛实现的,这些纳米绒毛相对长并且从脚垫以一定角度突出,这样的话邻近的纳米绒毛就可以与相对表面接触而无论其表面形态(topography)怎样。所述最大接触进一步允许在壁虎脚垫和相对表面之间的以百万计的小范德华(van der Waals)(在微牛顿(microNewtons)范围之内)相互作用的积聚,导致约10N/cm2的总的粘附力(拉脱力)。然而,当以剥离模式使用剥离力时,完全分离是通过克服与很小面积对应的小粘合力逐步实现的。因此,该粘附是易于撤销的。总的来说,壁虎粘附的魅力就在于以下的组合:粘附强度(10N/cm2)、可逆性以及就表面粗糙度和组成来说能够适用于各种表面的能力。上述壁虎粘附的独特特征激发了科学研究的动力以生产合成巧妙干燥粘合剂,其采用与壁虎脚爪一样的原理来工作。到目前为止,两种最好的合成壁虎粘合剂显示出对玻璃的最大拉脱强度是3和10N/cm2。这两种粘合剂都受到仅仅在一或两个附着/分离周期后就发生严重的粘附损失的困扰,这是由于所述纳米结构的破坏或者侧面塌陷(lateral collapse)造成的,并且后者是指邻近的纳米绒毛的结合。此外,典型的合成壁虎粘合剂仅仅模仿壁虎脚垫的功能,其功能更像是粘合带。由壁虎的脚趾产生的脚垫的机械分离是在典型合成壁虎粘合剂中未曾发现的特点。如果双侧带状合成壁虎粘合剂被用来结合两个刚性基材,那么由于在两侧所述刚性背衬层的限制,此种结合是不具有可逆性的。
发明内容
本发明的一个具体实施方案包括能够可逆的连接刚性基材的热可逆多层干燥粘合剂体系(thermo-reversible multilayer dry adhesive system)。
本发明的其他典型的具体实施方案经过下面的详细说明将变得明确。应该理解的是,所述详细说明和具体实施例,虽然公开了本发明的典型的实施方案,但目的仅仅是为了进行例证说明,而不是对本发明范围的限制。
附图说明
本发明的典型的具体实施方案通过详细描述和附图将被更完全地理解,其中:
图1示出了依照本发明的一个实施方案,利用多层粘合剂将第一基材附着到第二基材上的方法。
图2示出了依照本发明的一个实施方案,利用多层粘合剂将第一基材附着到第二基材上的方法。
图3示出了依照本发明的一个实施方案,利用多层粘合剂将第一基材粘附到第二基材上的方法。
具体实施方式
下面对具体实施方案的描述仅仅是示例性的,决不是对本发明、其应用或用途的限制。
现在参考图1-2,本发明的一个实施方案包括含有热可逆多层粘合剂14的产品,该热可逆多层粘合剂14具有形状记忆聚合物(SMP)层18,第一干燥粘合剂层16,以及第二干燥粘合剂层20。该第一干燥粘合剂层16可以在该形状记忆聚合物层18之上,并且该第二干燥粘合剂20可以在该形状记忆聚合物层18下面。在本发明的一个具体实施方案中,第一干燥粘合剂层16和第二干燥粘合剂层20有着不同的轮廓(profiles)。在一个具体实施方案中,第一干燥粘合剂层16可以比第二干燥粘合剂层20薄。在一个具体实施方案中,该多层粘合剂14可以是三层粘合剂。
如图1所示,本发明的一个具体实施方案可以包括利用该多层粘合剂14将第一基材10粘附到第二基材12上的方法。在一个具体实施方案中,第一干燥粘合剂层16的厚度小于第二干燥粘合剂层20的厚度。
在一个具体实施方案中,该多层粘合剂14被设置于第一基材10与第二基材12之间。然后将该多层粘合剂14加热至高于所述形状记忆聚合物层18的玻璃化转变温度(Tg),并在载荷(load)下冷却,以使得该第一基材10被粘附到该第二基材12。此后,通过将多层粘合剂14加热至高于该形状记忆聚合物层18的玻璃化转变温度(Tg),可以将第一基材10与第二基材12彼此分离。因为干燥粘合剂层16与20的厚度可以是不同的,所以该不对称的多层粘合剂可以具有与弯曲的干燥粘合剂表面指向相同方向的弯曲,如图1所示。例如,第一干燥粘合剂层16和第二干燥粘合剂层20各自的外表面都具有通常凹陷的形状(concave shape)。当加热和在载荷下冷却时,该多层粘合剂变形并且能够获得最大拉脱强度。一旦将该形状记忆聚合物层18加热至其Tg之上,该形状记忆聚合物层18就具有返回其原始弯曲的倾向,这原则上会产生剥离力使得第二干燥粘合剂层20从第二基材12分离。实际上,干燥粘合剂20从基材12的这种剥离将会要求第一干燥粘合剂16从基材10上自发分离,考虑到图1中的特定几何形状,这是不被所述剥离分离模式允许的。这就意味着干燥粘合剂16从基材10的分离将必须对抗基材10与第一干燥粘合剂层16之间的强大拉脱强度。这样的分离机制是不利的,而且只有当该形状记忆聚合物层18的形状复原力大于该第一干燥粘合剂层16的拉脱强度时才是可能的。
现在参考图2,本发明的另一个具体实施方案包括具有几何形状的多层粘合剂14,其中第一和第二粘合剂层16,20的弯曲朝向相反的方向。例如第一干燥粘合剂层16和第二干燥粘合剂层20各自的外表面都具有通常凸起的形状(convex shape)。这样,形状记忆聚合物层18具有这样的构型,其中其中间部分最厚且向着该形状记忆聚合物层18的外边界变窄或逐渐减小。该多层粘合剂14被设置于第一基材10与第二基材12之间,并且被加热和然后在载荷下冷却以使第一基材10粘附到第二基材12。可以通过加热多层粘合剂14将第一基材10与第二基材12彼此分开。当加热时,多层粘合剂14的这种特定的几何设计,原则上将会允许在粘合剂两侧上的热活化的剥落分离模式,而这对于图1中的设计则是不可能的。第一和第二干燥粘合剂层16和20各自分别从基材10和12剥离,首先从靠近外边界22和24处,并且向中心26处发展。对于粘附分离,尽管图2中的设计确实允许在两侧剥离,但这种粘附结合将需要非常大的载荷以使多层粘合剂14变形,因为形状记忆聚合物层18在结合过程中的变形是压缩性的(compressive)。
在一个具体实施方案中,第一基材10和第二基材12可以是平坦的,并且该多层粘合剂14可以是弯曲的。在另一个具体实施方案中,第一基材10和第二基材12可以是弯曲的,且该多层粘合剂14可以是平坦的。
现在参考图3,本发明的另一个实施方案包括具有形状记忆聚合物层18、第一干燥粘合剂层16以及第二干燥粘合剂层20的多层粘合剂14。该多层粘合剂具有这样的几何形状,其中第一和第二粘合剂层16,20的弯曲指向相反的方向。例如第一干燥粘合剂层16和第二干燥粘合剂层20各自的外表面都具有通常凸起的形状。第一和第二粘合剂层16,20在外边界22和24处彼此相接。该形状记忆聚合物层18包括邻近第一粘合剂层16的第一部分15和邻近第二粘合剂层20的第二部分17,以及在第一部分15与第二部分17之间形成空腔19。在一个具体实施方案中,该形状记忆聚合物层18具有在形状记忆聚合物的中央部分最厚并且朝其外边界逐渐减小的几何形状。空腔19的厚度也可以是在中心部分最大且朝其外边界逐渐减小。
在一个具体实施方案中,该多层粘合剂14被设置在第一基材10与第二基材12之间并且加热至高于形状记忆聚合物层18的Tg,然后在载荷下冷却,以使第一基材10粘附到第二基材12。当在载荷下冷却时,该空腔19可以变得非常小或者可以完全消失。可以通过将该多层粘合剂14加热至高于形状记忆聚合物18的Tg而将第一基材10与第二基材12彼此分离。一旦加热,第一和第二干燥粘合剂层16和20各自分别从基材10和12剥离,首先从靠近外边界22和24处,并向中心26处发展。在加热时,空腔19在形状记忆聚合物层18的第一部分15与第二部分17之间形成。图3中示出的设计允许多层粘合剂14两侧上的剥离,并且所述结合不需要很大的载荷,因为在结合过程中该形状记忆聚合物18的变形实际上是弯曲。
本发明的另一个具体实施方案包括一种方法,其包括加热多层热可逆干燥粘合剂14,该多层热可逆干燥粘合剂14包括形状记忆聚合物层18、第一干燥粘合剂层16以及第二干燥粘合剂层20,且其中该多层粘合剂14在室温下具有弯曲的结构,和向该粘合剂施加载荷以使该粘合剂粘附到下面的基材上,从而该粘附的粘合剂具有大于10N/cm2的拉脱力,和此后使该粘合剂分离,其包括加热该粘合剂至高于形状记忆聚合物18的Tg的温度,以使得该粘合剂恢复回弯曲的结构。
干燥粘合剂层16和20可以提供连续的接触表面,或者所述干燥粘合剂层可以包括许多的间隔隔开的(spaced apart)指状物,每个指状物都提供相对较小的接触表面,这样的话所述粘合层的总接触表面是不连续的。
一个具体实施方案包括能可逆的连接刚性基材的多层干燥粘合剂体系,具有显著高于用于去连接或分离或去偶联的剥离力的用于连接的拉脱粘附力(pull-off adhesion force)。
在本发明的不同的实施方案中可以使用多种形状记忆聚合物。例如,从Tg为约90℃的典型的芳香族二环氧化物/二胺体系开始,该芳香族环氧组分系统地被脂肪族二环氧组分替代,得到Tg范围为从3℃至90℃的一系列的环氧形状记忆聚合物。这样,如操作于特定温度范围之中的特定应用所需要的那样,可以特制用于干燥粘合剂的形状记忆聚合物。这样,所述干燥粘合剂层可以具有从-90℃至200℃的Tg,并且所述形状记忆聚合物可以具有从25℃至200℃的Tg。
一些实施方案涉及到多层环氧干燥粘合剂。应该理解的是可以采用多于两层。例如,可以有两或更多层的形状记忆聚合物层,其可以是并排关系或者是叠加关系。同样地,可以有两或更多个处于并排关系或者叠加关系的干燥粘合剂层。这样,可以制造具有定制的或者特制的性能的设备。
在不同的具体实施方案中,所述干燥粘合剂层可以是环氧弹性体干燥粘合剂(epoxy elastomeric dry adhesive)。在不同的具体实施方案中,所述形状记忆聚合物可以是环氧树脂。在本发明的不同具体实施方案中,可以采用形状记忆聚合物和干燥粘合剂的任何组合。下述形状记忆聚合物和干燥粘合剂的实例仅仅是为了说明目的。
在不同的实施方案中,所述干燥粘合剂的组分或者所述形状记忆聚合物的组分可以包括刚性环氧树脂(rigid epoxy)和柔性环氧树脂(flexible epoxy)。可以被用来得到干燥粘合剂或者形状记忆聚合物的可能的交联化学的范围可以包括α(alpha),ω(omega)-二氨基烷烃,有机多元羧酸,酸酐,或者催化(例如咪唑类型)交联反应。存在着许多种不同的方式来实现分子性能之间的恰当的关联。例如,所述干燥粘合剂或者形状记忆聚合物可以包括刚性的环氧树脂,环氧填充剂(epoxy extender)以及交联剂;或者刚性的环氧树脂,柔性的交联剂,以及柔性的环氧树脂;或者刚性的环氧树脂,刚性的交联剂,以及柔性的环氧树脂;或者刚性的环氧树脂,柔性的环氧树脂,以及催化固化剂;或者刚性的环氧树脂,交联剂,以及稀释剂;或者柔性的环氧树脂,交联剂,以及稀释剂;或者刚性的环氧树脂和柔性的交联剂;或者柔性的环氧树脂和催化固化剂;或者柔性的环氧树脂和交联剂;和其中所述刚性环氧树脂是具有至少两个环氧基团的芳香族环氧树脂,所述柔性环氧树脂是具有至少两个环氧基团的脂肪族环氧树脂,所述环氧填充剂具有一个环氧基团,以及所述交联剂是多胺、有机多元羧酸或者酸酐中的一种,并且所述稀释剂是一元胺或者单羧酸。在不同的具体实施方案中,所述催化固化剂(或者催化固化)促进环氧与环氧或者环氧与羟基的反应。所述催化固化剂可以包括,但不限于,叔胺,胺盐,三氟化硼络合物,或者胺硼酸盐类。在一个具体实施方案中,所述干燥粘合剂的组分可以以这样的量存在,其中当该组合物固化时,所述量足以提供玻璃化转变温度为-90℃至200℃并且从基材上的拉脱强度为1-200N/cm2的干燥粘合剂。在一个实施方案中,所述形状记忆聚合物组合物的组分可以以这样的数量存在,其中当该组合物固化时,所述量足以提供在其玻璃化转变前后其储能模量具有2到3个数量级的变化的环氧形状记忆聚合物。
本发明的一个实施方案包括制造多层热可逆干燥粘合剂的方法,其包括将3.6g的EPON 826(双酚A基环氧树脂)加热至约75℃,并将其与2.16g新戊二醇二缩水甘油醚(NGDE)以及2.3g二胺例如Jeffamine D-230混合。JeffamineD-230是聚醚胺,其是平均分子量为约230的双官能伯胺。所述伯胺基团处在脂肪族聚醚链末端的仲碳原子上。Jeffamine可以从Huntsman获得。
然后该混合物可以在特别设计的模具中进行固化以生产出具有图3所示的几何形状的环氧形状记忆聚合物层。固化条件为在100℃下1.5小时。然后把2.16gNGDE与1.15g胺例如Jeffamine D-230的混合物在该形状记忆聚合物层的外表面上在100℃下固化1.5小时。在第三步中,烘箱的温度可以升至130℃,以进行后固化约一小时。在后固化结束时,将该固化的多层环氧树脂脱模。总的来说,通过模制得到图3中所示的有利弯曲结构。正如在下文将中变得显而易见的那样,这种弯曲结构对于提供粘附的可逆性是有利的。
在本发明的不同的实施方案中可以使用多种形状记忆聚合物。例如,从Tg为约90℃的典型的芳香族二环氧化物/二胺体系开始,该芳香族环氧组分系统地被脂肪族二环氧组分替代,得到Tg范围为从3℃至90℃的一系列的环氧形状记忆聚合物。这样,如操作于特定温度范围之中的特定应用所需要的那样,可以特制用于干燥粘合剂的形状记忆聚合物。
下面是本发明的另一个具体实施方案,其提供了形状记忆聚合物的制造方法。将EPON 826称重置入玻璃瓶中,然后放入到预置温度为70℃的烘箱中进行熔融。熔融需要约1小时。在将含有EPON 826的瓶从烘箱中取出后,立即将称量过的Jeffamine D-230和NGDE加入到瓶中。用手剧烈摇晃瓶约10秒钟以使组分混合。按照该方法制备的五种环氧SMP样品的详细配方总结于表格1中。表1环氧树脂样品1-5的配方
接下来,所述混合物被倒入模具中。环氧树脂样品在100℃下热固化1.5小时并且在130℃下后固化1小时。在固化结束时,将环氧树脂样品脱模。所得到的形状记忆聚合物层的几何形状由采用的模具决定。
在另一个具体实施方案中,体系由EPON826,作为交联剂的JeffamineD-230以及作为一元胺的癸胺组成。如表2所示,从样品6到11,交联剂的分数系统地减少,而环氧官能度和胺上活性氢的官能度的总数保持相等。在这些样品中,样品11被用来作为参比样品,因为它不含交联剂并被认为不具有形状记忆特性。依照表2中配方的形状记忆环氧聚合物具有从25℃至90℃的Tg。表2环氧树脂样品6-11的配方
上述对本发明具体实施方案的描述仅仅是示例性的,因此,它们的各种变形不能被认为是偏离了本发明的精髓和范围。
Claims (19)
1.包括能可逆的连接刚性基材的多层干燥粘合剂体系的产品,具有显著高于用于去连接的剥离力的用于连接的拉脱粘附力,
其中所述多层干燥粘合剂体系包括第一外层和第二外层,以及中间层,其中所述第一和第二外层各自都包含干燥粘合剂,并且所述中间层包含形状记忆聚合物。
2.如权利要求1所述的产品,其中所述第一和第二外层具有相反的弯曲。
3.如权利要求1所述的产品,其中所述形状记忆聚合物具有在该形状记忆聚合物的中间部分最厚并且朝其外边界逐渐减小的几何形状。
4.如权利要求1所述的产品,其中所述干燥粘合剂包括:
刚性环氧树脂或者柔性环氧树脂的至少一种;和
交联剂或者催化固化剂的至少一种;
其中该刚性环氧树脂是具有至少两个环氧基团的芳香族环氧树脂,该柔性环氧树脂是具有至少两个环氧基团的脂肪族环氧树脂,并且该交联剂是多胺、有机多元羧酸或者酸酐中的一种。
5.如权利要求1所述的产品,其中所述形状记忆聚合物包括:
刚性环氧树脂或者柔性环氧树脂的至少一种;和
交联剂或者催化固化剂的至少一种;
其中该刚性环氧树脂是具有至少两个环氧基团的芳香族环氧树脂,该柔性环氧树脂是具有至少两个环氧基团的脂肪族环氧树脂,并且该交联剂是多胺、有机多元羧酸或者酸酐中的一种。
6.包括能可逆的连接刚性基材的多层干燥粘合剂体系的产品,具有显著高于用于去连接的剥离力的用于连接的拉脱粘附力,其中所述多层干燥粘合剂体系包括第一干燥粘合剂层,第二干燥粘合剂层,以及形状记忆聚合物层,该形状记忆聚合物层包括其间具有空腔的第一部分和第二部分。
7.如权利要求6所述的产品,其中所述第一干燥粘合剂层在所述形状记忆聚合物层上面,并且第二干燥粘合剂层在所述形状记忆聚合物层下面。
8.如权利要求7所述的产品,其中所述第一干燥粘合剂层具有弯曲方向不同于所述第二干燥粘合剂层外表面的外表面。
9.如权利要求6所述的产品,其中所述形状记忆聚合物层具有在该形状记忆聚合物层的中间部分最厚并且朝其外边界逐渐减小的几何形状。
10.如权利要求6所述的产品,其中当该形状记忆聚合物低于其玻璃化转变温度时,第一干燥粘合剂层和第二干燥粘合剂层各自都具有凸起形状的外表面。
11.如权利要求6所述的产品,其中所述形状记忆聚合物层包括:
刚性环氧树脂或者柔性环氧树脂的至少一种;和
交联剂或者催化固化剂的至少一种;
其中该刚性环氧树脂是具有至少两个环氧基团的芳香族环氧树脂,该柔性环氧树脂是具有至少两个环氧基团的脂肪族环氧树脂,并且该交联剂是多胺、有机多元羧酸或者酸酐中的一种。
12.如权利要求6所述的产品,其中所述第一和第二干燥粘合剂层包括:
刚性环氧树脂或者柔性环氧树脂的至少一种;和
交联剂或者催化固化剂的至少一种;
其中该刚性环氧树脂是具有至少两个环氧基团的芳香族环氧树脂,该柔性环氧树脂是具有至少两个环氧基团的脂肪族环氧树脂,并且该交联剂是多胺、有机多元羧酸或者酸酐中的一种。
13.连接刚性基材的方法,包括加热和冷却包括形状记忆聚合物和粘合剂层的多层干燥粘合剂体系,以改变该多层粘合剂体系的表面轮廓以产生粘附结合。
14.连接基材的方法,包括:
在第一基材与第二基材之间放置多层粘合剂体系,该多层粘合剂体系包括第一干燥粘合剂层、第二干燥粘合剂层以及在这两者之间的形状记忆聚合物层;
加热该多层粘合剂体系;
将基材与位于基材之间的被加热的多层粘合剂体系挤压在一起,并且在载荷下冷却该多层粘合剂体系以使该第一基材连接到该第二基材;和
然后,加热该多层粘合剂体系以使该多层粘合剂体系改变形状并且从该多层干燥粘合剂体系的外边界处开始从所述基材剥离。
15.如权利要求14所述的方法,其中所述第一干燥粘合剂层具有与所述第二干燥粘合剂层相反的弯曲轮廓。
16.如权利要求14所述的方法,其中所述多层粘合剂体系的形状记忆聚合物包括第一部分和第二部分以及它们之间的空腔。
17.如权利要求14所述的方法,其中所述形状记忆聚合物层具有在该形状记忆聚合物层的中间部分最厚并且朝其外边界逐渐减小的几何形状。
18.如权利要求14所述的方法,其中该形状记忆聚合物层包括:
刚性环氧树脂或者柔性环氧树脂的至少一种;和
交联剂或者催化固化剂的至少一种;
其中该刚性环氧树脂是具有至少两个环氧基团的芳香族环氧树脂,该柔性环氧树脂是具有至少两个环氧基团的脂肪族环氧树脂,并且该交联剂是多胺、有机多元羧酸或者酸酐中的一种。
19.如权利要求14所述的方法,其中所述第一粘合剂层和第二粘合剂层包括:
刚性环氧树脂或者柔性环氧树脂的至少一种;和
交联剂或者催化固化剂的至少一种;
其中该刚性环氧树脂是具有至少两个环氧基团的芳香族环氧树脂,该柔性环氧树脂是具有至少两个环氧基团的脂肪族环氧树脂,并且该交联剂是多胺、有机多元羧酸或者酸酐中的一种。
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US11/867,558 US8012292B2 (en) | 2007-05-23 | 2007-10-04 | Multilayer adhesive for thermal reversible joining of substrates |
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US20110311783A1 (en) | 2011-12-22 |
US8354167B2 (en) | 2013-01-15 |
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US8012292B2 (en) | 2011-09-06 |
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