CN1420904A - 粉末填充物和聚合物粘合剂的复合材料及其制备方法 - Google Patents

粉末填充物和聚合物粘合剂的复合材料及其制备方法 Download PDF

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CN1420904A
CN1420904A CN00811914A CN00811914A CN1420904A CN 1420904 A CN1420904 A CN 1420904A CN 00811914 A CN00811914 A CN 00811914A CN 00811914 A CN00811914 A CN 00811914A CN 1420904 A CN1420904 A CN 1420904A
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filler
preparation
matrix material
polymer
mixture
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CN1175033C (zh
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理查德·A·霍尔
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Holl Technologies Co
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Holl Technologies Co
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    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/227—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by organic binder assisted extrusion
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Abstract

一种复合材料，其中包含体积含量至少为60％、最好为70％的制成细粉末的填充物，将该填料粉末均匀掺杂在聚乙烯(亚芳基醚)聚合物粘合剂中，形成混合物并制成特定形状，然后给该混合物施加足够高的温度令聚合物材料熔化，同时施加足够大的压力，令熔化的聚合物均匀分散在填料微粒缝隙之间。一个意外收获是：要想所述聚合物真正成为有效的粘合剂，所加入的固体填料的含量必须达到上述特定比例，低于该含量则所制成的成品易于脆裂；这一发现与现有技术刚好相反，过去认为随着所加入的固体填料的含量的增加，复合材料的强度将逐步降低，因此必须限制该固体填料的含量。为了将混合物中各种成分混合到足够的均匀程度，所述混合物各原料分别在各自的液态离散媒介中进行混合，其中聚合物内还包括有必要的添加剂，为了获得要求的微粒尺寸，可以分别对每种混合原料进行研磨，然后将它们混合，并再次进行搅拌研磨，令其实现完全均匀分布，继而将混合物与液态离散剂分离，由粘糊状混合材料制成坯料，再对该坯料进行热压处理。为达到最后的制成品所要求的化学和物理组合特性，填料可以是由多种成分混和而成，该制成品可以用来制造电子电路基底产品。

Description

粉末填充物和聚合物粘合剂的复合材料及其制备方法
技术领域
本发明涉及一种将制成细粉末的填充物与聚合物粘合剂粘合而成的复合材料的制备方法及根据此类方法所制成的复合材料。
背景技术
电子产业是最为广泛地应用此类复合材料的领域之一，该复合材料被制成具备严格的原材料、物理和电学特性的薄板，用于制造印刷电路板及在电子电路中作为支撑和绝缘的基底材料。电子产业的发展历史表明：以玻璃纤维进行强化的聚合物，如环氧树脂、氰化酶、聚四氟乙烯(PTFE)以及聚酰亚胺等材料，一直被用于制造镀铜电路板，其高频特性日渐增长，目前已达800兆赫(MHz)。目前常用来作为此类薄板材料的聚合物是FR-4，是由环氧树脂在织物玻璃纤维中沉积而得，它具备容易制造和成本低廉的特性。这类材料的典型介电常数为4.3-4.6，其耗散因数为0.016-0..22，在工作频段500MHz以内的计算机行业用的最多。而现在移动电话的常用工作频段为1-40GHz，在某些计算机上也已达到了0.5GHz，预计将来所用频段还会更高，因而在计算机行业，为了提高信号传输速度，那些具有最低介电常数的材料将最受青睐。象FR-4这类材料的工作频率则比较高，为0.8GHz左右，虽然它的造价较低，但由于其存在着难以忍受的高介电损耗和发热率，又没有良好的一致性，此外，其糟糕的各向异性、在电介质材料和金属镀层之间所存在的热膨胀不匹配性，以及在基底材料工作温度上下波动时所产生的热膨胀各向异性等问题，决定了这种材料在今后不会有太大的用途。造成这些与热膨胀有关的问题的原因是：用来制造基底的聚合物有着较大的热膨胀系数，与具有一定长度和厚度直径的增强纤维的热膨胀系数不一致，而超过800MHz的基底电介质材料，在信号传输过程中其电容性将被激活，所以现在常常选用适宜颗粒的无机物粉末烧结而成的陶瓷材料，例如熔融石英、氧化铝、氮化铝、氮化硼、钛酸钡、钛酸钡复合物如Ba(Mg1/3Ti2/3)O2，Ba(Zr，Sn)TiO4，以及掺杂了Sc2O3的BaTiO3，稀土元素氧化物，由醇盐衍生出的SrZrO3以及具有烧绿石结构的Ba(Zr，Nb)氧化物。此外，基底材料还可以选用半导体材料，该半导体材料内含有金属粉末并掺入玻璃纤维和聚合物粘合剂—特别是PTFE一类的原料聚合物。
人们不断探索更好的电子基底材料和电子仪器组件应用复合材料的制作方法，期望能够绕开烧结和高温处理工序，以避免与之相伴的制造和研磨难度大、造价过高等问题。
目前那些可用的聚合物粘合剂，因为其自身固有的低强度和过高热膨胀系数的缘故，必须需要在基底内部掺入强化材料，例如织物玻璃纤维进行强化并修正其过高的热膨胀系数，但是，这类强化材料又反过来造成了在结构上的极度不均一性，例如，该强化材料的存在使得在基底内均匀添加粉末填料变得很困难，另一个问题是通常所用的聚合物粘合剂与常用填料之间的粘合性很差。一直以来，在此领域的研究和探索也作过不少，希望能发现它们和已知的基底用聚合物如PTFE之间合适的偶联剂，从而在聚合物和粉末材料间提供足够的附着力，同时在合成后的基底材料内还要具备另人满意的机械强度。
电介质材料常用来作为电路中的绝缘层以及多层复合电路中的隔层，过去最常用的是硅，其介电常数因不同的处理工艺而处在3.0-5.0之间，一般为4.0-4.5。显然，介电常数越低越好，而有机聚合物，因为其自身特性决定了它们的介电常数较低，为1.9-3.5，所以研究探索适合应用于此类场合的聚合物的工作就大行其道，其中聚酰亚胺(通常加于氟化)、PTFE、氟化聚乙烯(亚芳基醚)均属其中的研究成果，它们中有些材料的介电常数与空气一样低，即等于1.00，目前常用的聚合物处理工艺是通过对之进行氟化来降低介电常数、提高光学透明度，同时弱化其亲水性和在有机溶剂中的可溶性。但是氟化处理又通常会带来聚合物在某种程度上的极化问题，从而也妨碍其获得理想的绝缘性能。
公开于1997年8月19日的美国专利Nos.5,658,994，以及公开于1999年1月23日的美国专利Nos.5,874,516均为宾夕法尼亚州Allentown航空产品及化学制品公司所申请，正如上面所述，它们公开了一组可应用于微电子装置上的聚乙烯(亚芳基醚)材料结构，以取代硅作为基底材料，在该聚乙烯(亚芳基醚)内没有包含非芳香性炭分子(除了多苯基化炭perphenylated之外)，同时还公开了其氟化取代基或者其可显著极化官能团。这些材料很容易合成，而且具有非常适宜的组合特性，诸如热稳定性、低介电常数、低吸水性和低除气性。
美国专利No.5,658,994公开了其合成的一种绝缘材料及其微电子合成制造装置，该绝缘材料由该微电子装置提供，它包含一个聚乙烯(亚芳基醚)聚合物，其基本的非官能团重复单元结构为：
        -{-O-Ar1-O-Ar2-}m-{-O-Ar3-O-Ar4-}n-
其中：m＝0到1.0；n＝1.0-m；Ar1、Ar2、Ar3、Ar4分别为包含下述不同分子式的双价键亚芳基自由基，它们是亚苯基、联苯双自由基、对三联苯双自由基、偏三联苯双自由基、邻位三联苯双自由基、萘双自由基、蒽双自由基、菲双自由基、特殊形态的9.9-联二苯芴双自由基、以及4，4’-氧芴双自由基及其混合物。但在Ar1、Ar2、Ar3、Ar4中，除了9.9-联二苯芴双自由基以外，其它均非同质异构的等价体。
美国专利Nos.5,874,516所公开的聚乙烯(亚芳基醚)聚合物，其基本的非官能团重复单元结构为：
        -{-O-Arx-O-Ar1-}m-{-O-Ar2-O-Ar3-}n-
其中：m＝0.2到1.0；n＝1.0-m；Ar1、Ar2、Ar3分别为包含上述分子时的双价键自由基；或者是具备下类基本非官能团的重复单元结构：
        -{-O-Arx-O-Ar1-}m-{-O-Arx-O-Ar3-}n-
其中：m＝0到1.0；n＝1.0-m；Arx为特殊的双自由基9，9-双(4-氧化苯基)芴，而Ar1和Ar3分别为包含前一段中所述分子时的双价键自由基。
Ar1、Ar2、Ar3、Ar4的数值可以改变，而材料的一系列特性会随之而改变：如其可结晶性、模量、张力强度、玻璃传导温度等均可因此得以降低或消除。这些聚合物据说是具备了基本的化学惰性，较低的极性、没有额外的官能团或反应团，在400°-450℃之间的惰性环境下具有热稳定性等等，此外，还可以对具有上述基本结构的聚合物进行交联，既可以在350°-450℃的温度下进行自身的交联，也可以加入硫化剂或是利用封端剂对该聚合物进行封端，如苯乙烯、苯并环丁烯、乙炔基和腈。在渐次升高温度的情形下进行交联，其分子量和密度会随之增加，使得材料更为适用于微电子领域，因为它们更容易在溶剂中溶解，并通过加热生成耐溶涂层。
此类特定的聚合物具有非官能性，即它们具有化学惰性，在微电子合成装置内进行复合时，没有携带任何有害官能团，它们中不含半价羰基(carbonyl moietites)，如酰胺、酰亚胺和甲酮，这些物质会都增加吸水性，它们中没有携带卤素，如氟、氯、溴和碘，这些物质会在金属电镀过程中与金属元素发生反应。除了9，9-fluorenylidene基桥联炭分子以外，它们均由基本的芳香族炭分子组成，因为其类似于芳香族的结构特征而且具有大部分芳香族炭分子的性能，所以该发明中的该类炭分子可被称做多苯基化炭(perphenylated carbon)。
此类聚合物在微电子仪器中可以用于电镀、隔层、密封、界定区间或区分层面，或用作基底材料，所述微电子仪器中应包含而不局限于多层芯片模式、集成电路、集成电路传导层、集成电路电路图中的导电体，电路板以及类似的需要绝缘体或绝缘区域的电子器件，它们还可以作为基底材料用在电路板或印刷电路中，在上述电路板的表面蚀刻不同的电路图式，还可以在里面添加强化剂，如玻璃纤维等非导电织物纤维，这些电路可以是单面、双面或者是多层结构。
为了获取特殊的性能，还可以添加一些在传统的复合工艺中众所周知的稳定剂、阻燃剂、染色剂、可塑剂、表面活性剂或类似物质，此外还可以添加粘度促进剂以增加聚合物与适宜的基底材料的附着力，这些促进剂具有类似于六甲基二硅烷胺的结构形式，它可以用来与可能存在于某些元素表面如硅表面的羟基官能团进行反应。
发明内容
本发明的目的在于提供一种将制成细粉末的填充物与聚合物粘合剂进行复合的新的制备方法、以及根据此类方法所制成的复合材料和采用此复合材料制成的产品。
本发明的另一个目的是所提供的复合材料和产品中，填料至少应占总体积含量60％以上，剩余含量是聚合物粘合剂和必要的添加剂。
因此，本发明所提供的将制成细粉末的填充物与聚合物粘合剂进行复合的制备方法包括如下步骤：
将体积为60％至97％的填料细粉末与对等含量的包含非活性聚乙烯(亚芳基醚)的聚合物粘合剂进行混合；
设定足够高的温度和压力，令聚合物材料熔化并均匀分散在填料微粒缝隙间。
同理，本发明所提供的由制成细粉末的填充物与聚合物粘合剂进行复合的材料包含：
体积含量为60％至97％的研碎填料与对等含量的包含非活性聚乙烯(亚芳基醚)的聚合物粘合剂组成的混合物；
该混合物被设定到足够高的温度和压力，令聚合物材料熔化并均匀分散在填料微粒缝隙间。
所述聚合物材料的微粒最大线度或等价球径的最佳值为50μm。
附图说明
图1是本发明的复合材料复合方法和装置的流程图的第一部分，特别是电路基底材料与矩形铜箔条的压制和贴覆过程；
图2是混料/溶剂脱水搅拌器的侧视图；
图3是图2所示搅拌器的A-A断面结构示意图；
图4是图1所示流程图的后继部分；
图5是图4所示流程图的后继部分；
图6和图7是局部放大的本发明材料的截面微粒显微结构示意图，图6中金属层正在贴近复合材料表面，图7中金属层已经贴覆完毕。
具体实施方式
下面将结合附图和举例详细描述本发明中新复合材料的制备方法及其装置，并给出采用此种方法和装置所复合的材料自身的最佳实施例。
本发明人无意中发现在已知的一类聚合物族中有一个特殊的分类，叫做聚乙烯(亚芳基醚)，它跟作为电子电路基底材料之一的填料细微粒之间具有极高的粘合力，这种聚合物即为组成该基底的另一种材料。同样是无意之中，该基底材料的复合特性与过去的材料复合工序完全相反，在现有技术中，进行材料复合和应用该材料制造基底成品时通常会遇到这样一个主要问题：即随着所加入的固体填料粉末的含量的增加，最后复合出来的材料的机械强度将会逐步降低，迄今为止，只要加入含量超过40％的填料，复合后的材料会变的非常易碎，对其进行测试时，将拉力加载到实际商业应用所要求的强度，它就会分崩离析而变成一堆散砂，而且，过去也无法真正将固体填料加到超过40％的含量，因为此时的混合物已经变得过于粘滞，根本不可能进行均匀搅拌。因此，只能限制添加填料的含量以保证基底材料所需要的强度，而不得不接受因此而导致的较差的电学性能。本人的发现是，采用本发明中的方法，要令复合材料获得更理想的性能，所加入的固体填料的含量必须远远超过现有技术中传统复合方法中的界限，其新的最低下限值达到60％，此时复合的材料才具备所要求的最低强度，随着加入固体填料粉末含量的逐渐增加，直至达到95-97％这个最高极限，其最后所获得的复合材料的机械强度将会逐步增高而不是降低，如果超过这一比例，则聚合物的含量将不足于均匀分布到填料微粒间并维持必要的粘着力。这一现象虽然可能存在着其它的解释，但本发明人认为对此意外结果的合理解释是—当然本发明不能也不应该受此局限：这种特定的聚合物跟某些氧化物如硅、氧化铝、金属粉末、氮化硼等之间具有超乎寻常的粘合力，它们的机械强度均不甚高，在这一全新而特定的应用实例中，只有采用本发明中的方法，同时固体填料的含量又达到足够高时，在填料微粒间嵌入非常薄的粘合层的处理方式才会有效。我们很难精确规定所嵌入微粒间的粘合层的最大厚度，不过已能确知的是，当厚度为1-3微米时，是可以获得非常理想的粘着力和足够的强度的，其可能的厚度上限值是40微米(0.001英寸)。
本发明中的混合材料可以按重量或体积比例进行掺杂，所有那些被选定的没有极化、也没有官能团的聚合物材料的微粒线度或其等价球径的数值要足够小，介于0.1到50微米之间，与之对应含量的被选定的填料的微粒线度或其等价球径的数值同样也要足够小，介于0.1到50微米之间，将该混合物加热到足以导致聚合物材料熔化的温度，即280°-400℃之间，同时加压到3.5-1,380MPa(500到200,000psi)，最佳压力值为70-1,380MPa(10,000到200,000psi)，令熔化的聚合物微粒均匀渗透到填料微粒之间。其中，等价球径的含义是具有该特定球径值的理想的球形微粒的体积与所选的实际微粒的体积相等。在后面还要详细描述的备选复合过程中，聚合物可以溶液形式添加，一旦填料和聚合物混合均匀，就采取步骤将溶剂全部除去，聚合物材料最好选用包含聚亚芳基醚-2、聚亚芳基醚-3和聚亚芳基醚-4的一类材料，这些材料下面还会详细述及，而填料则可以选用那些无机材料颗粒、电磁材料颗粒、或者颗粒的核心是无机材料并在外面包覆一层氧化金属物的材料、金属颗粒、磁性材料颗粒、以及具有低介电常数和高熔点温度的聚合物颗粒，所有的这些颗粒还可以是中空的。
经过热压处理的混合物材料可以被制成平板、薄膜或窄条，将铜箔置于其上的某个平面，通过喷射或在真空中加热加压的直接粘合方式进行铜箔贴覆，或者，也可以将高温高压处理之前的坯料制成平板或窄条，然后将其密封并进行热塑压处理，再将铜箔置于其某个平面上，通过喷射或在真空中加热加压的直接粘合方式进行贴覆，其制成品可以被用来制作电路基底或电路及仪器附件。本发明中后面将要提及的方法可以是与制造这些扁平薄板产品有关的方法，但是，它很显然也可以用于制造其它任何既定的模具成型产品形状，也就是那些要求能直接获得上佳表面质量、非常均匀的微观结构以及成品微粒间具备高度一致性的产品。
由于微电子仪器目前的高频特性，它要求基底材料必须具备极高的物理和化学结构一致性和良好的物理化学特性，而上面所说的简单的混合处理工序通常并不能实现足够的一致性，还需要采用下面的方法和装置。
请参阅附图1，在本实施例中，所选用的填料为某些材料的组合，选用这种方式是因为它可以为基底材料制成品带来更好的机械和电学综合特性。所选聚合物采用适宜的溶剂如环己酮溶液做为载体(浓度通常为10％)，这种溶剂正好还能被用来作为填料的液态离散和悬浮媒介，将所选定的填料—通常是无机材料的细微粉末，同该聚合物溶液预先混合，在另外的实施例中当然也可以使用其它媒介，填料或填料混合物可以分别从适宜的母体溶液中通过沉淀或共沉淀而获得，但要求所得材料必须具备足够的纯度、介电常数、损耗因数以及微粒粒度。在本实施例中，至少有4种原材料可以分别通过进料和计量装置中的多个进料口10、12、14和16加入，同时聚合物的环己酮溶液可以自其进料口18加入，在需要适宜的表面活化添加剂如表面活性剂、可塑剂和润滑剂等的场合，它们可以由单独的进料口20加入，每种粉末状材料可以直接由进料口10、12、14、16添加，或通过各自的沉淀或共沉淀系统22、24、26(进料口16的原料沉淀或共沉淀系统未绘出)获得，如果聚合物呈粉末状，它可以从进料口18加入，而液态离散剂将由另外的进料口添加，或和其它添加剂一起从进料口20加入，自进料口倾入的填料粉末流量由各自的计量仪28进行持续而精确的检测，聚合物溶液流量由计量仪32检测，表面活性添加剂则由计量仪34检测，而上述填料、聚合物和添加剂混合后的分别由计量仪36检测，所以这些预先混合的聚合物溶液、填料和添加剂分别被装入鼓形混料/研磨搅拌机38内，该搅拌机下面还要详细介绍。
本发明与现有技术中的一个显著区别是它选用造价低廉、颗粒粒度取值范围更大的材料来获得最佳的组合微粒，其间混合极薄的聚合物中间层，现有技术则与之相反，特别是由陶瓷烧结而成的基底材料中，为了得到充分的结构一致性，就需要(颗粒)尺寸特别均一，也就是说造价更为高昂的粉末。在混合物形成以前，每种粉末通常会包含大小不一的颗粒，以及由许多微小颗粒组成的、其尺寸范围更为宽广的团块，这种情形必须要加以矫正，特别是那些大团块，需要将之研碎和分散成微粒状态，所以，要由每个混料/研磨器38均将原料进行混合并将粉末材料在液体媒介中充分离散，同时作为研磨器，还要将各种粉末颗粒和团块研磨到所要求的统一尺寸并将之搅拌到所要求的均匀程度，然而该离散过程也会导致孔径的压缩。
由各进料口加入的填料、聚合物溶液和添加剂的预先混料中，固体材料所占的体积含量比例为40-95％，离散剂和添加剂的含量应尽可能少，但至少可以维持混合物呈黏糊状或泥浆状，以便于在相对狭小的研磨器38和后面的装置内流动自如，其较为适宜的粘度为100-10,000厘泊。本发明中预先混料的研磨、团块打散和离散在各自的研磨器38内同时进行，这种特殊的研磨器在本人授权于1994年1月18日的美国专利Nos.5,279,463和授权于1996年7月23日的美国专利Nos.5,538,191中已经给以公开，此处可以参考。
这种特殊研磨器可以有两种主要结构形式，第一种由两个同轴圆盘组成，圆盘之间形成一定的操作空隙，旋转轴与水平线垂直，但第二种研磨器更为常用，它在一个中空的固定好的外圆筒组件内嵌套了一个可以绕水平转轴旋转的内圆筒组件，两个圆筒组件的转轴略微偏置，这两个管壁之间，在与转轴平行且相邻管壁的纵向间距最为接近的位置上，环绕整个圆周所形成的间隙叫搅拌室或叫微量室，而在它的对面，垂直于径向的另外的那个纵向间距要大的多，它所形成的同样与转轴平行的间隙，称做补位室或宏量室。流经搅拌室的混合浆料在宏量室内和其附近形成的涡流叫上位-Kolmorgoroff，在微量室或搅拌室内产生的涡流叫下位-Kolmorgoroff。该固定组件上还安装有超声波谐振器，由它向操作间内施加纵向振动力并进一步强化下位-Kolmorgoroff涡流，采用这种装置，可以在数分钟内处理好相对而言较为粘稠的微米级微粒浆料，而在传统技术中使用高剪切搅拌器和球磨机或者砂磨机则往往需要几天的时间。
然后，这些分散盛装的预先混料被合并到一个混料/研磨器40内，搅拌成均匀一致的浆料或黏糊状混合体，在该混料/研磨器40内，还要对所述混料进行团块研碎和均匀搅拌处理，该混料/研磨器40仍属于上述本人专利Nos.5,279,463和专利Nos.5,538,191内公开的特制研磨器之一，它同样是在一个中空并固定的外圆筒组件内嵌套了一个可以旋转的内圆筒组件。虽然本实施例中只用上了一个单独的混料/研磨器40，但在某些实施例中，同时采用两个或者更多的此类研磨器进行组配也是可以的，所选用研磨器的数量可以根据混料的数量和要求的研磨、打碎和搅拌程度而定。
研磨好的浆料从研磨器40中倒出，进入混料/溶剂挥发研磨器42中，该研磨器42同样具有一个内部圆筒组件44，嵌套在一个中空并固定的外圆筒组件46内，所述黏浆被置于组件44的外表面并形成一层薄膜47，在此研磨器内，大部分环己酮溶剂在剧烈的搅拌过程中已被排除，自挥发器加料口48的螺旋状通道进入的黏浆在抵达出料口50前，随着越来越多的溶剂由溶剂挥发口52逸出而变的越来越粘稠，所述溶剂自挥发口52进入冷凝器(未绘出)进行回收处理以备再次使用。在该研磨器的底部还安装有一排筒状加热器54，用以促进溶剂挥发，其热能可以使圆筒内材料温度达到150℃。当该研磨器的出料口50附近的黏料已经变的足够坚硬时，可以通过常规黏料挤压机58挤压成型并送到与之相连的薄板输送带56上。因为此时输送带上的材料仍含有少量溶剂和添加剂，必须在长条烘箱内进一步加热处理，在输送带的另一端连接有环状链条60，该输送带由该链条带动穿过烘箱62，所述溶剂和大部分添加剂都在此处被除掉，输送带上只剩下均匀混合的填料(或组合填料)微粒及聚合物(或组合聚合物)。烘箱的温度可以定在150°-250℃之间，加热升温过程必须缓慢进行，以尽量避免由于离散媒介以及添加剂逸出或添加剂分解时所产生的气泡形成孔隙。烘干后的材料经由输送带送至切割机64，切割成小块的基底用粗加工坯料，它通常是呈矩形，其尺寸将根据该材料所应用的电路板基底的具体要求而定。该粗加工坯料随后经由人工或自动方式放入压模中、由上下两块热压板68、70所形成的空腔，该空腔位于下热压板70内，用来承受加载处理。一旦粗加工坯料放入空腔，上热压板68下降将模具空腔闭合，上热压板68的突出部位就会伸进该空腔，将坯料压制成预定的尺寸和密度，模具内的温度设定到足够将坯料中的聚合物熔化并令其在所施加压力下自由流动，均匀填充和覆盖填料微粒之间的缝隙，该温度的最高值是聚合物将产生降解反应从而为不能再被正常使用，最小压力值的设定是与温度值相关联的，其效用则如上所述是令聚合物熔化在所施压力下可以实现自由流动，闭合的模具腔体内的压力和加压时间要足够令坯料获得最大的压强和密度。在热压工序中，熔化的聚合物将进行相对自由的流动，该温度和压力值需要维持一段足够长的时间，令该聚合物充分填充填料微粒之间的微小缝隙，形成一层薄薄的聚合物膜。温度的取值范围为280°-400℃，压力值为70MPa至1,380MPa(10,150至200,000psi)，虽然最佳压力值为345MPa(50,000psi)，但某些时候将该压力值降低到3.5MPa(500psi)也是可行的。与坯料接触的热压板面须进行抛光或更为精细的处理，以实现电子基底材料的电磁波频率所要求的光滑表面特性。
本发明的另一个意外收获是非官能性聚乙烯(亚芳基醚)，由于它在350°-450℃的有氧环境下可以进行交联，将制好的基底材料进行循环加热，其中的聚合物将会再次熔化并在基体内充分扩散开来，当达到交联温度点后，聚合物就开始变稠。或者，也可以在混合物中添加交联剂和/或封端剂，这样在较低的温度下即可以实现聚合物的稠度增加。正如上面所述，这种升温状态下的交联和/或封端效应使得该基底材料在微电子行业中具有极好的应用价值，它可以被直接用做低粘性材料，甚至溶解在上面所述的溶剂中，通过加热还可以生成一层高密度的抗侵蚀物质。
自压模取出的基底材料66又被送入一个多轴平磨滚筒研磨器72内，该基底材料在此被精确碾压到预定厚度并被磨平，这些滚筒的表面仍然需进行抛光或更精细的处理，以获得所要求的光滑表面特性。此时坯料已经被压制成厚度不超过60mil(千分之一英寸)的薄膜或薄片，该厚度还可以薄到30mil、10mil、4mil甚至1mil以下。在电子电路中应用的基底材料通常的厚度为0.125mm至1.5mm(5-60mil)之间，通常的厚膜所用材料要达到0.75-0.9微米(22-40微英寸)的范围，而薄膜所用材料则必须要达到0.5微米(2微英寸)以下。再将所述坯料送入热压机74中，在这里，该坯料的单面或双面上将压覆上与之相同尺寸的铜料薄板74，在后面的工序中还要进行电路蚀刻。此处的铜料薄板是由绕在滚筒(未绘出)上的铜带78经由铜箔切割和表面抛光仪80切割成小块而成，其表面处理装置包括一对热压板组件，切割好的铜板在这对热压板之间压制成形，该热压板须进行抛光或更为精细的处理，以赋予铜材光滑的表面特性。基底材料和铜板材料的这种表面抛光特性在特高频应用中尤为重要，因为，正如前面提到的，只有在这样光滑的表面上电流才能流经导电层并令蚀刻导电层保持良好的一致性。
在本发明的方法中，填料成分可以占据60％或更高比例，其最小含量是内部聚合物层过厚从而无法获得所需要的机械强度的界限值，其基底材料成品也因此无法达到机械强度要求，其最大含量要求所选定的聚合物的含量至少可以维持该填料足够的粘性，也就是说，在混合材料中固体填料的含量可以轻易达到60％-97％的体积比例，其最佳值为70％-97％，聚合物所占体积含量的比例则只要能够维持足够的粘性、在施压后能将无机填料微粒间的微小缝隙均匀填充直至完全覆盖并具备足够高的强度即可。在混合材料中聚合物材料的相对含量较小，必须保证它能绝对均匀地散布在填料微粒间，这一点通过上述的处理方法可以轻易实现，而与填料微粒的大小无关。
如上所述的方法和装置特别适用于所述混合材料的大批量生产过程，但对该方法进行某种简化和较少装置的使用，应该仍属于本发明范畴之内。例如，上面所述的被逐一分开的填料和聚合物、悬浮剂及其所必需的添加剂，完全可以在某一个或一组混料/研磨器38及/或40内混合起来，在制成所需要的均匀混料的同时，又获得所需要的微粒尺寸，然后再进入前面所述处理过程中的烘箱46等装置进行加工。
在许多应用领域，要想真正满足基底材料制成品的一致性要求，哪怕是上述最严格的处理工序也难以做到，此时就需要一系列的附加工序，用来将基底材料重新打碎研磨，再恢复到最初的微粒状态，此时的填料微粒于上面所述的填料微粒的不同之处在于：该微粒内还含有复合其上的聚合物微粒和薄膜，将这些均匀搅拌的材料同样置于合适的溶剂中，经由一个或一组研磨器—例如上述研磨器38和40进行研磨，直至达到最佳的均匀一致性，然后去除其中的悬浮剂，将所生成的材料经过再次热压处理，制成所要求的基底成品，此时只要温度适宜，该聚合物将具备足够的热塑性。
图6和图7为本发明材料的典型截面显微结构示意图，分别表示抛光后的铜板76与抛光后的基底材料贴覆前后的状况，该基底材料中含有紧密排列的填料微粒82，其形状尺寸均为不规则排列，聚合物84不再是离散的微粒，而是形成薄膜状填充并粘接在填料微粒之间，为了给出微粒尺寸的直观概念，图6中所示正方形每一边所代表的实际长度约为5微米，本发明中仅由聚合物的粘性即可提供足够的粘合力，不再需要增强纤维或纤维织物。
目前最常用的一类聚乙烯(亚芳基醚)聚合物，其重复单元为联苯双自由基链接9，9-二苯基芴的4，4’-双自由基，属于特定的PAE-2结构，而另一组常用聚合物重复单元为对-三联苯双自由基链接9，9-二苯基芴的4，4’-双自由基，属于特定的PAE-3结构，第三组常用聚合物重复单元为PAE-2与PAE-3的组合，它属于特定的PAE-4结构。这些聚合物的制造方法在前述美国专利Nos.5,658,994和5,874,516中已经公开，以此为参考，可以得到所述聚合物样品的特性如下：
                      PAE-2         PAE-3        PAE-4重均分子量Mw              65,300         45,400        75,800数均分子量Mn              20,700         11,400        25,700Mw/Mn                     2.58           3.98          2.95玻璃化转变温度Tg via DSC  257℃          271℃         273℃拉伸系数(dynes/cm2)      1.45×1010    1.45×1010   39×1010400℃-6小时后重量损失     0.36           0.57          0.65450℃-6小时后重量损失     0.91           1.65          1.2685°F/85RH的重量比Wt％    0.279          0.301         0.274
在上面所述美国专利中还指出，该类材料与传统的氟化聚乙烯(亚芳基醚)材料PAE-1相比其特性均有所改善，对照样品的性能参数如下：PAE-1
重均分子量Mw                          20,000
数均分子量Mn                          7,700
Mw/Mn                                 2.58
玻璃化转变温度Tg via DSC              166℃
拉伸系数(dynes/cm2)                  1.23×1010
400℃-6小时后重量损失                 0.72
450℃-6小时后重量损失                 3.16
其中的PAE-2已获得十分成功的应用，这种材料在空气中不会氧化，不需要耦合剂而且粘性极佳，在所需频率范围(1-10GHz)内的损耗因数小于0.0008，而目前一般用于电子电路中的其它热固性聚合物材料的损耗因数则为0.02-0.005。该聚合物具有热塑性，可以在280-300℃之间进行处理，而在300-400℃范围还可以进行交联，交联后，其热塑性被强化，损耗因数会降到0.0008以下，如果一种聚合物的重均分子量低于30,000，就认为它低于本发明的方法所提要求，甚至就连上述PAE-2/3/4材料也不具备足够的结构强度，无法形成薄膜、薄片或其它任何三维空间形状，它们在这些相对厚重的结构下会很容易碎裂成小片，但本人意外发现即使是具有较低分子量的材料在厚度为微米量级以下的1-3微米薄膜状时，却能够保持完整和足够的粘度，我们完全可以利用这一特性，当然分子量高的材料会更为适用。
填料和聚合物材料的相对含量比例在某种程度上取决于基底材料所要应用的场合，如果用在非常高的高频电路上，最好将作为绝缘材料的填料含量加到最大，而将聚合物含量降至最小。正如前面所述，聚合物的最低含量应能在微粒间隙压至最小时满足其充分填充的要求，此外该微粒涂层还要令复合后材料的机械强度满足要求。为了这个缘故，在混合物中，聚合物的体积含量通常需要达到其最低比例3％，剩余的97％则应包括绝缘填料、残留的表面活化剂和耦合剂、有机或无机强化材料、强度增强纤维和鬃毛等固体材料。
这些材料最好呈微小颗粒状，特别是作为填充料的原材料，如果选用的是固态聚合物或聚合物组，也应该将其制成颗粒，填充料的原材料微粒粒径最好介于0.01到50微米之间，聚合物颗粒粒径则为0.1到50微米，如上所述，最佳方案是同时选用具备不同粒径的一组系列填充材料，因为这样反而能够减小微粒间的缝隙空间，提高材料强度，从而赋予产品本发明所特有的超薄而粘性极强的粘合层特性，此外还减少了用于填充和粘连微粒缝隙的聚合物的含量；这一点可以从理论上求证：当堆积的球类物品的尺寸一致性达到45％时，其缝隙空间将达到最大值，而将粒径范围更宽的不同材料搭配，这个数值可以大大下降，直到最理想的3％。
如上所述，在选择填料及聚合物材料时，必须考虑基底材料的一系列重要特性，包括拉伸强度、撕裂强度、焊接牢固度、柔顺度即低量模数、过孔电镀可靠性、介电常数、化学稳定性、结构稳固性及Q因数等。其中必须达到的最低指标有吸水性能，色度亮度干扰v曲线间距，以及损耗因数或耗散因数(Q因数的倒数)。
本发明的方法特别适用于复合材料的生产领域，其中的填料粉末可以是任何一种或数种在目前陶瓷烧结法制造电子电路基底的工业中的“优选性能”原料，最常见的有氮化铝、钛酸钡、钛酸钡-钕、钨酸钡铜、钛酸铅、铌酸铅镁、铌酸铅锌、铌酸铅铁、钨酸铅铁、钛酸锶、钨酸锆、以及这些材料的化学和/或物理等价物、氧化铝、熔凝石英、氮化硼、金属粉末及半导体材料。在过去的生产中，还有另外一组包含有铁酸盐类的感应材料与聚合物粘合剂的混合物也十分重要，它主要应用在中性电磁产品如变压器、感应器和铁酸盐芯仪器上，但传统的生产方法中，聚合物中粉末填料和固体材料的体积含量一般限定在50％以下，采用本发明的方法则可以将固体材料的体积含量提到很高，达到比如说80％以上。
目前仅有的具备温度恒定特性的陶瓷材料的介电常数，其数值在2.6到12、37到39、以及80到90之间，在飞速扩展的无线通讯领域，其电磁波的传输频率范围自800MHz直至超过30GHz，其应用材料的小型化、轻量化就变成了越来越重要的特性，如果是设定最适宜的电路结构并依此为根据来选择原材料，其最佳介电常数的数值需要跨越从8直到2000的范围，但是，目前的情形是电路结构总要受原材料实际上非常窄的介电常数范围的约束，电磁波或GHz频率信号的传输更多地依赖于电路的波导特性，所以只有那些具备高介电常数的材料上允许使用更窄更短的的导线，才可以进行大幅度的小型化。例如，如今正用在世界各地超过2千5百万部移动电话上的同轴电介质共振器，如果基底材料的介电常数可以自目前氧化铝的9升高到400以上，而其介电损耗(损耗因数)仍继续保持在0.0005以下的话，其体积和重量可以减小到一半以上，其造价则可以降低2/3或更多。
如果能够选配出适宜的两种或多种粉末填料进行混和，应用本发明中的方法来构造这样的复合材料是可行的。在实际应用特别是在特高频应用场合，对基底材料的特性要求是非常严格的，需要考虑大量的物理性能包括填料含量、容积密度(范围)、表面抛光度、微粒尺寸(平均)、吸水性(％)、弯曲强度、弹性模量、线性热膨胀系数、热传导率、电介质强度、介电常数、耗散因数、以及体积电阻率等。只有多种填料的混和才可以获得基底材料在特定应用场合所要求的组合特性，而在陶瓷烧结工艺中则无法实现，因为这样会违反一般的烧结规律，烧制出来的材料也会碎裂。我们之所以希望能够依照任意比例混合填料，其中一个重要理由是为了获得理想的介电常数，该介电常数可以在一定的温度范围如-50℃到200℃之间保持恒定，同时还可以获得非常高的Q因数(相当于非常低的损耗因数)，该Q因数要求达到500以上甚至可以高达5,000。

Claims (26)

1、一种将制成细粉末的填充物与聚合物粘合剂进行充分混合的复合材料制备方法，其特征在于：
所形成的混合物中包含占总体积含量60-97％的填料微粒和含量与之对应的非极性聚合物粘合剂，该聚合物粘合剂由非官能团的聚乙烯(亚芳基醚)组成；
给所述混合物施加足够高的温度令聚合物材料熔化，同时施加足够大的压力，令熔化的聚合物均匀分散在填料微粒缝隙之间。
2、根据权利要求1所述的制备方法，其特征在于：所述的聚合物材料选自包含聚亚芳基醚-2、聚亚芳基醚-3和聚亚芳基醚-4的一类材料。
3、根据权利要求2所述的制备方法，其特征在于：所述聚合物被加热至350-450℃以实现交联。
4、根据权利要求2或3所述的制备方法，其特征在于：所述复合材料的混合物包含有交联剂和/或封端剂。
5、根据权利要求1至4中任意一个所述的制备方法，其特征在于：所述填料选自包含有无机材料颗粒、电磁材料颗粒、或者颗粒的核心是无机材料并在外面包覆一层氧化金属物的材料、金属材料颗粒、以及具有低介电常数和高熔点温度的聚合物颗粒等一类的材料，所有的这些颗粒可以是中空的。
6、根据权利要求1至5中任意一个所述的制备方法，其特征在于：将所述混合物加热到280°-400℃，同时加压到3.5-1,380MPa(500到200,000psi)，其最佳压力值为70-1,380MPa(10,000到200,000psi)。
7、根据权利要求1至6中任意一个所述的制备方法，其特征在于：所述方法还包括以下步骤：
将填料细粉末、聚合物、以及一种液态离散媒介混合成为一种可流动的混合材料，然后；搅拌该可流动混合材料直至其细粉末均匀地分散到所述液态离散媒介中；
从该可流动混合材料中去除掉所述液态离散媒介，所生成的粘稠混料制成粘稠混合坯料；
对该坯料施加特定的温度和压力。
8、根据权利要求7所述的制备方法，其特征在于：所述聚合物材料和填料分别在各自的液态离散媒介中进行混合，并利用各自的鼓形混料/研磨搅拌机进行搅拌，以均匀分布其内的各种成分，该鼓形混料/研磨搅拌机的结构在美国专利Nos.5,279,463和Nos.5,538,191中已经公开。
9、根据权利要求7所述的制备方法，其特征在于：所述的混合材料应至少通过一个在美国专利Nos.5,279,463和Nos.5,538,191中已经公开的鼓形混料/研磨搅拌机进行搅拌，以均匀分布其内的各种成分。
10、根据权利要求1至9中任意一个所述的制备方法，其特征在于：所述填料的微粒尺寸介于0.1到50微米之间，所聚合物材料在粉末状态时的微粒尺寸介于0.01到50微米之间，其中填料可以由一组具有不同化学成分的填料混合物组成。
11、根据权利要求1至10中任意一个所述的制备方法，其特征在于：所述制备方法还包括如下步骤：将所述经过热压处理的复合材料制成平板、薄膜或窄条状坯料。
12、根据权利要求11所述的制备方法，其特征在于：所述制备方法还包括如下步骤：将铜箔置于所述坯料的某个平面上，通过选择喷射或在真空中加热加压的直接粘合方式进行铜箔的贴覆。
13、根据权利要求11或12所述的制备方法，其特征在于：所述平板、薄膜或窄条状坯料的厚度应小于60mil，或是小于30mil，或是小于10mil，或是小于4mil，或是小于1mil。
14、根据权利要求1至13中任意一个所述的制备方法，其特征在于：所述制备方法还包括如下步骤：将铜箔置于所述经过热压处理的混合物材料表面，通过喷射或直接粘合方式进行铜箔的贴覆。
15、根据权利要求1至14中任意一个所述的制备方法，其特征在于：所述制备方法还包括如下步骤：将经过热压处理的基底材料重新打碎研磨，恢复到最初的细粉末状态，此时的填料微粒内还包含有裹覆其内的聚合物材料，将搅拌均匀的材料再次经过热压处理，制成复合材料的固态坯料。
16、根据权利要求1至15中任意一个所述的制备方法，其特征在于：所述制备方法还包括如下步骤：将所述经过热压处理的复合材料加工成电子电路基底。
17、根据权利要求1至15中任意一个所述的制备方法，其特征在于：所述制备方法还包括如下步骤：在所述经过热压处理的复合材料上贴覆电子电路或电子器件。
18、一种由制成细粉末的填充物均匀掺杂在聚合物粘合剂中所合成的复合材料，其特征在于：所述复合材料包含：
体积含量为60％至97％的填料与对等含量的包含有非活性聚乙烯(亚芳基醚)的聚合物粘合剂所组成的混合物；
给该混合物施加足够高的温度令聚合物材料熔化，同时施加足够大的压力，令熔化的聚合物均匀分散在填料微粒缝隙之间。
19、根据权利要求18所述的复合材料，其特征在于：所述的聚合物材料选自包含聚亚芳基醚-2、聚亚芳基醚-3和聚亚芳基醚-4的一类材料。
20、根据权利要求18或19所述的复合材料，其特征在于：所述填料选自包含有无机材料颗粒、电磁材料颗粒、或者颗粒的核心是无机材料并在外面包覆一层氧化金属物的材料、金属材料颗粒、以及具有低介电常数和高熔点温度的聚合物颗粒等一类的材料，所有的这些颗粒可以是中空的。
21、根据权利要求18至20中任意一个所述的复合材料，其特征在于：所述填料的微粒尺寸介于0.1到50微米之间，该填料微粒可以由一组具有不同化学成分的填料混合组成。
22、根据权利要求18至21中任意一个所述的复合材料，其特征在于：所述复合材料具有平板、薄膜或窄条形状，其厚度应小于60mil，或是小于30mil，或是小于10mil，或是小于4mil，或是小于1mil。
23、根据权利要求22所述的复合材料，其特征在于：所述复合材料上还贴覆有一层铜箔，将该铜箔置于所述平板、薄膜或窄条的某个平面上，通过喷射或在真空中加热加压的直接粘合方式进行铜箔的贴覆。
24、根据权利要求18至21中任意一个所述的复合材料，其特征在于：所述复合材料上还贴覆有一层铜箔，将该铜箔置于其某个表面上，通过喷射或直接粘合方式进行贴覆。
25、根据权利要求18至24中任意一个所述的复合材料，其特征在于：所述复合材料经热压处理的混合材料可以用于制造电子电路基底。
26、根据权利要求18至24中任意一个所述的复合材料，其特征在于：所述复合材上贴覆有电子电路或电子器件。
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WO2001002468A1 (en) 2001-01-11
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CN1175033C (zh) 2004-11-10
DE60016228D1 (de) 2004-12-30
KR20020085865A (ko) 2002-11-16
US6391082B1 (en) 2002-05-21
ATE283305T1 (de) 2004-12-15
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US20020038582A1 (en) 2002-04-04

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