CN101522843A - 特别用于电子元件和导线通道的结合的可热活化胶带 - Google Patents
特别用于电子元件和导线通道的结合的可热活化胶带 Download PDFInfo
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Abstract
可热活化胶带,其特别用于生产和进一步加工电子组件和导线通道,具有至少由以下组分构成的粘合剂:a)具有末端氨基和/或酸基团的聚酰胺,b)环氧树脂,c)具有含至少6个碳原子的长的非极性链和至少一个能够与环氧树脂反应的反应性端基的化合物,d)任选的增塑剂,所述聚酰胺与环氧树脂在至少150℃的温度反应,以及a)和b)的重量分数之比为50∶50至99∶1。
Description
本发明涉及特别用于结合柔性印刷导线通道(conductor tracks)(柔性印刷电路板,FPCB)的在高温具有低流动性的可热活化粘合剂。
当今,柔性印刷电路板用于大量诸如手机、收音机、计算机、打印机等等电子设备。柔性印刷电路板由同铜和高耐熔的热塑性材料(大多数为聚酰亚胺,较少的为聚酯)的层构成。这些FPCB往往使用要求特别严格的胶带制备。一方面,为了制备FPCB,将铜箔与聚酰亚胺片结合在一起;另一方面,还将单个的FPCB彼此相结合,此时将聚酰亚胺和聚酰亚胺结合。除了这些应用之外,FPCB还与其他基底结合。
对于用于这些结合任务的胶带有非常严格的要求。因为,必须获得非常高的结合性能,所用的胶带通常为在高温下处理的可热活化胶带。这些胶带在结合FPCB期间的高温载荷中(常常在约200℃的温度进行)必须不释放出挥发性组分。为了获得高水平的内聚力,胶带必须在此温度荷载期间交联。结合操作期间的高压使得在高温下胶带的流动性必须很低。这通过未交联胶带的高粘度或非常快速的交联来实现。而且,胶带还必须耐焊料浴(solder bath resistance),换言之,必须短时间耐受288℃的温度荷载。
为此使用纯的热塑性材料不合理,虽然它们熔融得非常快,确保结合基底有效润湿并在几秒内产生非常快速的结合。但是,在高温下,它们如此柔软使得它们往往在结合过程的压力下胀出粘合层外。因此,也不耐焊料浴。
对于可交联的胶带,通常使用环氧树脂或酚醛树脂,这些树脂与特定的硬化剂反应形成聚合物网络。在此特定情形中,不能使用酚醛树脂,因为在交联过程中它们产生消除反应产物(elimination product),该产物释放出来,在固化过程或者最迟在焊料浴中引起起泡。
在结构粘结中主要使用环氧树脂,并且在用合适的交联剂固化之后产生非常脆的粘合剂,这确实获得了高的结合强度,但实际不具有柔韧性。
增加柔韧性对于在FPCB中使用至关重要。一方面,使用理想地卷绕成卷筒的胶带进行结合;另一方面,所研究的导线通道是柔性的且必须还可以弯曲,例如在膝上型电脑的导线通道中方便看到的,其中可折叠的显示屏经由FPCB与其他电路连接。
可以两种方式使这些环氧树脂粘合剂柔韧化。首先,存在用弹性体链柔韧化的环氧树脂,但它们产生的柔韧性是有限的,因为弹性体链非常短。另一种可行方式是通过添加弹性体(将其加入粘合剂)获得柔韧性。该方案的缺点是弹性体不能化学交联,意味着可以使用的弹性体仅仅是那些在高温下仍保持高粘度的弹性体。
由于胶带通常由溶液制备,往往难以找到如下弹性体,其具有足够长的链特性,从而不在高温下流动,同时还具有可以溶于溶液的足够的短链特性。
可以经由热熔体操作进行制备,但在交联体系中非常困难,因为必须防止在制备操作过程中过早交联。
通过使用与环氧树脂交联的可溶性聚酰胺可以获得具有特定内聚力和高结合强度的组合物。缺点是聚酰胺往往吸收水,如果吸收的水再次蒸发并在结合处形成气泡,这一方面对结合会具有不利影响。另一方面,吸水性改变了粘合剂的电性质:强的绝缘效果减弱。
描述了基于聚酰胺或其衍生物的可交联的粘合剂。
讨论的聚酰胺是优选含有聚碳酸酯基团或聚亚烷基二醇基团的改性聚酰胺,如US 5,885,723 A或JP 10 183 074 A或JP 10 183 073 A中描述的。将这些聚酰胺反应,使得它们含有环氧端基,并因此可以通过硬化剂与这些环氧基团交联。
另外,例如在US 6,121,553 A中公开了含有组成非常具体的聚酰胺酰亚胺的粘合剂。
因此,本发明的目的是提供一种胶带,其是可热活化的,在热状态下交联,在热状态下具有低粘度,显示与聚酰亚胺的有效粘合,其未交联态在有机溶剂中是可溶的,并仅具有低的吸水性。
令人惊讶的是,通过具有如第一独立权利要求详细描述的特征的胶带实现了该目的。从属权利要求提供了本发明主题的有利方案,还有该胶带应用的可能性。
可热活化粘合剂,其特别用于生产和进一步加工电子组件和导线通道,具有至少由以下组分构成的粘合剂:
a)具有末端氨基和/或酸基团的聚酰胺,
b)环氧树脂,
c)化合物,其具有含至少6个碳原子的长的非极性链和至少一个能够与环氧树脂反应的反应性端基,
所述聚酰胺与环氧树脂在至少150℃的温度反应,a)和b)的重量分数之比为50:50至99:1。
用于本发明目的的通用表述“胶带”包括所有片状结构,如二维延展的片材或片段,具有延伸长度和有限宽度的带状物,带段,冲切片等。
a)和b)的重量分数之比优选为70:30至95:5。
在本发明的粘合剂中使用的聚酰胺应没有太高的分子量(优选重均分子量Mw小于40000)并且应已经进行柔韧化和/或仅仅部分结晶或根本没有结晶。一方面,这对于所述粘合剂的柔韧性是必须的,另一方面,优选由溶液处理原料,而完全结晶的聚酰胺难溶,仅可以在不方便使用的溶剂如三氟乙酸或硫酸中溶解。
因此,根据本发明的一种有利方案,使用共聚物而非均聚物,例如PA6,6。为了使PA 6,6柔韧化,可以与PA 6共聚。同样可以使用其他共聚物,例如PA 6,6/6,12或PA 6,6/6,11。降低分子量增加了聚酰胺的溶解度。分子量不应低至损失掉良好机械性能的程度。
重均分子量Mw应该大于500g/mol。
另外,为了降低结晶度,还可以使用三元共聚物。不仅可以使用纯的脂族聚酰胺,而且可以使用脂族-芳族聚酰胺。优选具有长脂族链的那些,或者理想地,由于共聚具有长度不同的脂族链的那些。本文中溶解度的提高还可以通过使用具有间位和/或邻位取代的芳族化合物而实现。使用间苯二甲酸代替对苯二甲酸显著地降低了结晶度。为了降低脂族-芳族聚酰胺的结晶度,还可以使用下式的单体:
在这些式子中,X可以为氧、氮或硫,但也可以是具有至少一个碳原子的亚烷基。亚异丙基也是可行的。
同样可行的是通过芳族化合物的取代扩展这些结构,或者通过其他芳族基团延长该结构。
在US 6,121,553 A中给出了本发明可以使用的胺的其他实例。
还可以使用聚酯酰胺,条件是它们可以溶于适合施用至背衬的溶剂。
为了合成聚酰胺,使用过量的氨基组分或酸组分是重要的,由此,一方面分子量不会变得太高,另一方面存在可以与环氧树脂反应的端部反应性基团。
由于聚酰胺是交联的,因此还可以使用相当低分子量的低聚物(特别是重均分子量Mw为500-2000g/mol的那些),以获得足够的强度。
环氧树脂通常理解为每分子含有多于一个环氧基团的单体化合物和低聚化合物。它们可以是缩水甘油基酯或表氯醇与双酚A或双酚F或两者的混合物的反应产物。同样适合使用的是线型酚醛环氧树脂,得自酚类和甲醛的反应产物与表氯醇的反应。也可以使用含有两个或更多个环氧端基的单体化合物,其充当环氧树脂的稀释剂。同样适合使用的是弹性改性的环氧树脂。
环氧树脂的实例为得自Ciba Geigy的AralditeTM 6010,CY-281TM,ECNTM 1273,ECNTM 1280,MY 720,RD-2;得自Dow Chemicals的DERTM 331,732,736,DENTM 432;得自Shell Chemicals的EponTM 812,825,826,828,830等;同样得自Shell Chemicals的HPTTM 1071,1079;以及得自Bakelite AG的BakeliteTM EPR 161,166,172,191,194等。
市售的脂族环氧树脂例如为乙烯基环己烷二氧化物,如得自UnionCarbide Corp.的ERL-4206,4221,4201,4289或0400。
经弹性处理的弹性体可得自Noveon,商品名为Hycar。
环氧稀释剂,即含有两个或更多个环氧基团的单体化合物例如为得自Bakelite AG的BakeliteTM EPD KR,EPD Z8,EPD HD,EPD WF等,或者得自UCCP的PolypoxTM R9,R12,R15,R19,R20等。
在本发明的一种优选实施方式中,同时使用多于一种的环氧树脂。
聚酰胺的高强度和环氧树脂与这些聚酰胺硬化剂的额外交联意味着在粘合剂膜内获得非常高的强度。然而,与聚酰亚胺的结合强度也是极高的。
理想的是,环氧树脂和聚酰胺的使用比例使得环氧基团和氨基和/或酸基团的摩尔分数刚好相等。然而,硬化剂基团和环氧基团之间的比例可以在宽范围内变化,但对于充分交联,两个基团的任何一个存在的摩尔当量都不应该过量超过10倍。
对于额外交联,还可以加入与环氧树脂反应的化学交联剂。交联剂对于该反应不是必须的,但为了除去过量的环氧树脂而可以特别添加。
主要使用的交联剂或硬化剂如下所述或者如US 3,970,608 A中更详细描述的:
—多官能脂族胺,如三亚乙基四胺
—多官能芳族胺,如异氟尔酮二胺
—胍,如氰基胍
—多元酚
—多元醇
—多官能硫醇
—多元羧酸
—具有一个或多个酐基的酸酐
尽管基于聚酰胺和环氧树脂的胶带(含有或不含硬化剂)可以获得非常高的保持力(holding power),但这些粘合剂的软化点相当高,在一些情况下限制了加工。由于在压制到欲结合的制品之前将胶带进行层合,因此需要高于160℃的非常高的温度。为了降低该温度,在本发明的一种更优选的实施方式中,将增塑剂加入粘合剂。试验显示,混有增塑剂的聚酰胺类粘合剂比那些没有添加增塑剂的粘合剂在存储后的稳定性高得多。除了降低层合温度之外,还可以添加增塑剂降低交联温度,同时增加存储稳定性。
合适的增塑剂首先包括常规用于PVC的增塑剂。
例如,可以选择以下的这些:
—邻苯二甲酸酯,如DEHP(二乙基己基邻苯二甲酸酯),DBP(邻苯二甲酸二丁酯),BBzP(丁基苄基邻苯二甲酸酯),DnOP(邻苯二甲酸二正辛酯),DiNP(邻苯二甲酸二异壬酯)和DiDP(邻苯二甲酸二异癸酯)
—偏苯三酸酯,如TOTM(偏苯三酸三辛酯),TINTM(偏苯三酸三异壬酯)
—脂族二羧酸酯,如DOM(马来酸二辛酯),DOA(己二酸二辛酯)和DINA(己二酸二异壬酯)
—磷酸酯,如TCEP(三(2-氯乙基)磷酸酯)
—天然油类,如蓖麻油或樟脑
此外,还可以使用以下增塑剂:
—低分子量聚环氧烷烃,如聚环氧乙烷、聚环氧丙烷和聚THF
—低熔点的松香类增粘树脂,如Eastman的Abalyn或Foralyn 5040
本文优选最后面的两种,因为它们具有更好的环境相容性,并且从粘合剂组件扩散出去的趋势下降。也可以使用各增塑剂的混合物。
根据本发明的优选实施方式,增塑剂的含量为5wt%~45wt%,基于粘合剂的总重量。
为了降低吸水性,使用一方面能够与环氧树脂或与聚酰亚胺本身在高温反应,另一方面含有完全非极性基团的化合物。所有这些化合物必须在与用于聚酰亚胺的相同的溶剂中可溶。
该非极性基团优选是可以完全饱和的烃基,但分子中的双键也是允许的。为了实现吸水性下降,该非极性链必须含有至少6个碳原子。
能够与环氧树脂或聚酰胺反应的可交联基团例如为:酸基团、酸酐基团、氨基、醇基团、巯基、腈基团、卤素或环氧基团。在分子中还可以存在两个官能团。该非极性基团可以位于这两个基团之间。
还适合使用的是,仅在高温通过化学反应产生官能团的分子。
除了非极性链和反应性基团之外,在分子中还可以存在其他官能团和非官能团。
这类能够降低吸水性且含有能够与环氧化物反应的官能团的化合物的实例是硬脂酸、油酸、棕榈酸、月桂酸、十二胺、辛胺和十二烷基硫醇。
例如,癸二酸、氨基十一烷酸和二氨基辛烷携带两个官能团。
根据本发明的优选实施方式,含有反应性基团的化合物的含量为1wt%~10wt%,基于粘合剂的总重量,
除了聚酰胺、环氧树脂和降低吸水性的化合物之外,在粘合剂中还可以存在其他成分。
为了加快交联反应的反应速率,可以使用那些称为促进剂的化合物。可行的促进剂的实例包括以下:
—叔胺,如苄基二甲胺、二甲基氨基甲基苯酚和三(二甲基氨基甲基)苯酚
—三卤化硼-胺络合物
—取代的咪唑
—三苯基膦
可以使用的其他添加剂通常包括:
—主抗氧化剂,如位阻酚
—辅助抗氧化剂,如亚磷酸酯或硫酯
—过程稳定剂(in-process stabilizer),如C-自由基清除剂
—光稳定剂,如UV吸收剂或位阻胺
—加工助剂
—填料,如二氧化硅、玻璃(粉状或珠的形式)、氧化铝、氧化锌、碳酸钙、二氧化钛、炭黑、金属粉,等等
—有色颜料和染料,以及光学增亮剂
为了制备该胶带,将粘合剂的各组分溶于合适的溶剂,例如热乙醇、热甲醇、N-甲基吡咯烷酮、二甲基甲酰胺、二甲基乙酰胺、二甲基亚砜、γ-丁内酯或卤代烃或这些溶剂的混合物,然后将溶液涂布在配置有防粘层如防粘纸或防粘膜的柔性基底上,干燥涂层,使得组合物可以容易地再次从基底上除去。在适当转变之后,可以在室温制得冲切片、卷筒或其他形状。然后将相应的形状优选在高温下粘附到欲结合的基底,如聚酰亚胺上。
还可以将粘合剂直接涂布到聚酰亚胺背衬上。然后可以将这种类型的粘合剂片用于遮蔽FPCB的铜导线通道。
不需要该结合操作是一步过程,而是可以首先通过进行热层合将胶带粘附在两个基底之一。然后在与第二基底(第二聚酰亚胺片或铜箔)的实际热结合操作过程中,将环氧基团全部或部分固化,粘合层获得高结合强度。
混合的环氧树脂和聚酰胺应优选在层合温度下还没有参与任何化学反应,而应仅在热结合时彼此相互反应。
与许多结合FPCB的常规粘合剂相比,制备的粘合剂具有如下优势:在结合之后具备非常高的温度稳定性,因此产生的组件即使在高于150℃的温度仍保持高强度。
本发明的粘合剂的优点在于,在实际中弹性体与树脂化学交联;无需为环氧树脂添加硬化剂,因为弹性体本身充当硬化剂。
该交联既可以通过端部酸基团又可以通过端部氨基进行。通过两种机理同时进行交联也是可行的。为了存在足够多的端基,聚酰胺的分子量必须不能太高,因为否则交联度会变得太低。高于40000的分子量仅仅得到少量交联的产物。
实施例
下面通过多个实施例更详细地描述本发明,而不以任何方式限制本发明。
实施例1
将90份(根据ISO 307,在96%浓度的硫酸中的粘数为122ml/g)共聚酰胺6/66/136(得自BASF的Ultramid 1C)边搅拌边溶于沸腾的乙醇(20%浓度的溶液)中,然后将冷却后的溶液与12份环氧树脂EPR 161(Bakelite,环氧值为172),20份平均分子量为2000的聚乙二醇,和3份月桂酸混合。
在组分完全溶解之后,将溶液涂布到硅化的背衬上,使得干燥后得到25μm厚的粘合剂膜。
对比实施例2
如实施例1,将聚酰胺与环氧树脂和增塑剂溶解,但这次略去月桂酸。再次,如上所述后进行涂布得到厚度为25μm的粘合剂膜。
用制备的胶带结合FPCB
在每种情况使用实施例1和2制得的胶带之一结合两个FPCB。为此,将胶带在140℃和170℃层合到聚酰亚胺/铜箔FPCB层合体的聚酰亚胺片上。随后,将另一FPCB的第二聚酰亚胺片和胶带结合,在可加热的Bürkle压机中在200℃和1.3Mpa的压力下将整个组件压制1小时。
测试方法
通过以下测试方法考察上述实施例制备的粘合剂片的性质。
和FPCB的T-剥离测试
使用Zwick的拉伸测试机、将根据上述方法制备的FPCB/胶带/FPCB组件以180°的角度和50mm/min的速率彼此剥离开,测量需要的力,以N/cm计。在20℃和50%相对湿度下进行测量。每个测量值测定三次。
耐焊料浴
将根据上述方法结合的FPCB组件在288℃的焊料浴上搁置10秒。如果没有形成导致FPCB的聚酰亚胺片膨胀的气泡,则该结合定级为耐焊料浴。如果形成了甚至是微小的气泡,则该测试定级为失效。
吸水性
在110℃的烘箱中干燥尺寸为5×5cm的纯的粘合剂,然后在含有干燥剂的干燥器中冷却至室温,并称重。接着将样品在23℃水中存放24小时。从水浴中取出之后,将样品用纤维素拭干并再次称重。两次测量结果的差值和干燥后的测量结果之间的比值表示可以吸收的水量。
结果
对于上述实施例的粘合剂组件,进行T-剥离测试。
在表1示出了结果。
表1
T-剥离测试[N/cm]
实施例1 在约15N/cm铜/聚酰亚胺组件部分分层。否则,
数值为15-16N/cm.
对比实施例2 在约15N/cm铜/聚酰亚胺组件分层。用本发明胶
带结合没有失效。
实施例和对比实施例均得到具有非常高结合强度的粘合剂。降吸水剂的添加实际上不影响结合强度。
两个实施例全部通过了焊料浴测试。这表明月桂酸已经结合到网络中并实际上已经与环氧树脂发生了反应。
两个实施例在吸水方面的差异是明显的。虽然对比实施例吸收了3.6wt%的水,但实施例1中相应的吸水量仅为2.1%。这说明可以显著降低吸水性。
Claims (11)
1.可热活化胶带,其特别用于生产和进一步加工电子组件和导线通道,具有至少由以下组分构成的粘合剂
a)具有末端氨基和/或酸基团的聚酰胺,
b)环氧树脂,
c)化合物,其具有含至少6个碳原子的长的非极性链和至少一个能够与环氧树脂反应的反应性端基,
d)任选的增塑剂,
所述聚酰胺与环氧树脂在至少150℃的温度反应,以及a)和b)的重量分数之比为50:50至99:1。
2.权利要求1的可热活化胶带,其特征在于,所述聚酰胺为非晶共聚酰胺,如PA6,6/6,12或PA6,6/6,11。
3.权利要求1或2的可热活化胶带,其特征在于,所述聚酰胺的粘数根据ISO 307在96%浓度的硫酸中测量时为100-130ml/g。
4.权利要求1-3至少一项的可热活化胶带,其特征在于,化合物c)含有至少一个酸基团、酸酐基团、氨基、醇基、巯基、腈基团、卤素或环氧基团。
5.前述权利要求至少一项的可热活化胶带,其特征在于,所述含有反应性基团的化合物的含量为1wt.%~10wt.%,基于粘合剂的总重量。
6.前述权利要求至少一项的可热活化胶带,其特征在于,所述增塑剂选自选自邻苯二甲酸酯、偏苯三酸酯、磷酸酯、天然油类、聚环氧烷烃、松香和/或聚乙二醇。
7.前述权利要求至少一项的可热活化胶带,其特征在于,所述增塑剂的有效量为粘合剂总重量的5-45wt.%。
8.前述权利要求至少一项的可热活化胶带,其特征在于,所述胶带包括促进剂、染料、炭黑和/或金属粉。
9.前述权利要求至少一项的可热活化胶带用于结合塑料部件的用途。
10.前述权利要求至少一项的可热活化胶带用于电子元件和/或柔性印刷电路(FPCB)的结合的用途。
11.前述权利要求至少一项的可热活化胶带用于结合聚酰亚胺的用途。
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US8871874B2 (en) | 2012-06-13 | 2014-10-28 | E I Du Pont De Nemours And Company | Thermoplastic melt-mixed composition with epoxy-amino acid compound heat stabilizer and processes for their preparation |
JP6416756B2 (ja) | 2012-06-13 | 2018-10-31 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニーE.I.Du Pont De Nemours And Company | アミノ酸熱安定剤を含む熱可塑性溶融混合組成物 |
CN104662091A (zh) | 2012-06-13 | 2015-05-27 | 纳幕尔杜邦公司 | 具有聚醚醇热稳定剂的热塑性熔融混合组合物 |
US20130338274A1 (en) * | 2012-06-13 | 2013-12-19 | E I Du Pont De Nemours And Company | Thermoplastic melt-mixed compositions with epoxy-amine heat stabilizer |
CN111040678B (zh) * | 2019-12-28 | 2021-10-19 | 广东生益科技股份有限公司 | 一种无卤树脂组合物、包含其的挠性印制电路用补强板及其应用 |
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- 2007-09-24 JP JP2009530840A patent/JP2010505976A/ja not_active Withdrawn
- 2007-09-24 CN CNA2007800373289A patent/CN101522843A/zh active Pending
- 2007-09-24 WO PCT/EP2007/060084 patent/WO2008043658A1/de active Application Filing
- 2007-09-24 KR KR1020097009341A patent/KR20090080064A/ko not_active Application Discontinuation
- 2007-09-24 US US12/439,629 patent/US20090260761A1/en not_active Abandoned
- 2007-09-24 EP EP07820491A patent/EP2079814A1/de not_active Withdrawn
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106520056A (zh) * | 2016-10-09 | 2017-03-22 | 浙江大学 | 一种pet覆膜铝板及其制备方法 |
CN106520056B (zh) * | 2016-10-09 | 2019-08-06 | 浙江大学 | 一种pet覆膜铝板及其制备方法 |
WO2023124668A1 (zh) * | 2021-12-28 | 2023-07-06 | 金发科技股份有限公司 | 一种聚酰胺复合材料及其制备方法和应用 |
Also Published As
Publication number | Publication date |
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EP2079814A1 (de) | 2009-07-22 |
KR20090080064A (ko) | 2009-07-23 |
DE102006047735A1 (de) | 2008-04-10 |
TW200829674A (en) | 2008-07-16 |
US20090260761A1 (en) | 2009-10-22 |
JP2010505976A (ja) | 2010-02-25 |
WO2008043658A1 (de) | 2008-04-17 |
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