CN1121468C - 微级粘合用可热固化的单组分lva(低粘度粘合剂)粘合体系 - Google Patents

微级粘合用可热固化的单组分lva(低粘度粘合剂)粘合体系 Download PDF

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CN1121468C
CN1121468C CN97197995A CN97197995A CN1121468C CN 1121468 C CN1121468 C CN 1121468C CN 97197995 A CN97197995 A CN 97197995A CN 97197995 A CN97197995 A CN 97197995A CN 1121468 C CN1121468 C CN 1121468C
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K·赫恩
H·拜尔
M·洪斯贝格-里德尔
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Abstract

本发明涉及单组分的粘合剂体系，它至少是由浇铸树脂，特别是环氧树脂和多元醇组成。低粘度的粘合剂体系是可微计量的，贮存稳定的，可完全固化的并适合于尺寸公差在微米和小于微米级的应用。

Description

微级粘合用可热固化的单组分 LVA(低粘度粘合剂)粘合体系
说明
本发明涉及一种浇铸树脂体系，该体系适用于尺寸公差在微米和小于微米级形成粘合。
已知有粘合剂体系用于微粘合，它通常是由树脂组分和固化剂组分组成的。这两种组分的粘合剂体系用于微级粘合所需少的用量还存在问题。特别是在使用前准确的计量，混合和各组分的均化有均问题。还有一缺点是，它的粘度一般太高，所以在较高的温度(约70℃)下才变成稀薄的液体，这样可进行微计量的粘合剂涂敷-所谓的LVA(低粘度粘合剂)-粘合剂的涂敷。此外，已知的两组分体系还有缺点是，由于在薄层中或在小液滴中的非均匀性，使它本身在惰性气体-或氮气中不能完全固化。所有这些因素造成了至今不可能实现按所要求的，有重现性质量的，在复合强度和在微米和小于微米级的尺寸公差(＜1μm)方面工业生产可利用的复合物。
因此，需要一种粘合剂体系，该体系有可能使合理的，自动化的、安全的和价格适宜的粘合技术成为电子和光电技术的低-价-体系。特别是需要用于微米-级和小于微米级粘合的粘合体系，它能在极薄层或小的液滴进行可靠的计量和固化。在固化后能保持上述尺寸。
本发明的任务是，将一种粘合剂体系供给使用，该体系在用量少的情况下也不会表现出非均匀性并且适用于微计量。本发明的另一任务是，将一种粘合剂体系供给使用，它在薄层中能完全固化。因此，提高了复合物粘合的可靠性和强度并能降低制成的粘合复合物不希望的排气。最后，本发明的粘合剂体系与其它已知体系相比显示较低的粘度和有均匀的流动性。最后，粘合剂体系的使用期可允许各个结构元件的接缝公差在微级和在其以下。
这些任务通过本发明的粘合剂体系加于解决。本发明的内容是包括以下成分的可热固化的单组分浇铸树脂体系：
60-98％(重量)的浇铸树脂，
2-30％(重量)的醇或糖，
0.2-2.0％(重量)的热引发剂
0.2-2.0％(重量)的增粘剂和/或
0-3.0％(重量)的助流动剂
0-4％(重量)的触变剂和/或流动改性剂。
优选的粘合剂体系是可固化的单组分的粘合剂体系，该体系包含：
60-98％(重量)的浇铸环氧树脂己二酸双(3，4-环氧基环己基甲基)酯；
2-30％(重量)的多元醇或糖，所述多元醇为3(4)，8(9)双(羟甲基)-三环[5，2，1，02，6]-癸烷；
0.2-2.0％(重量)的选自鎓盐和(S-苄基锍杂戊环六氟锑酸盐的热引发剂；
0.2-2.0％(重量)的增粘剂；
0-3.0％(重量)的助流剂；
0-4.0％(重量)的触变剂；和
0-4.0％(重量)的流动改性剂。
更优选的粘合剂体系是可固化的单组分的粘合剂体系，该体系包括以下组成：
85-93％(重量)的浇铸环氧树脂己二酸双(3，4-环氧基环己基甲基)酯；
4.5-12％(重量)的多元醇，所述多元醇为3(4)，8(9)双(羟甲基)-三环[5，2，1，02，6]-癸烷；
0.7-1.0％(重量)的选自鎓盐和(S-苄基锍杂戊环六氟锑酸盐的热引发剂；
03-0.6％(重量)的增粘剂；
0-1.5％(重量)的助流动剂；
0-2.0％(重量)的触变剂，和
0-2.0％(重量)的流动改性剂。
此外，本发明的主题是，这种浇铸树脂用于形成尺寸公差在微米级和小于微米级的粘合。其它优点形成从说明中以及从实例和下属权利要求中得出。从本发明的意义来讲，“浇铸树脂”可理解为可热固化的树脂体系和反应树脂，它具有如此低粘度，以致使它可在相应的模子中浇铸，然后，即通过对现有合适的添加剂(引发剂、促进剂，其它组分)升温可使其固化。本发明优选的浇铸树脂是环氧树脂。在本发明的配方中，浇铸树脂含量为60-98％(重量)，更好的为75-95％(重量)，优选为80-95％(重量)和特别优选的为85-93％(重量)范围。
作为“浇铸环氧树脂”可采用脂肪族的环氧树脂例如Ciba Geigy的CY 177树脂己二酸双(3，4-环氧基环己基甲基)酯或同样是CibaGeigy的CY 179树脂(3，4-环氧基-环己基甲基-3′，4＇-环氧基-环己烷羧酸酯)。此外，直链脂肪族环氧树脂例如环氧化的聚丁二烯或环氧化的大豆油也适用。其它阳离子固化的树脂如乙烯醚或乙烯基芳香族化合物也同样适用。此外，缩水甘油醚型的环氧树脂也适用。以下化合物可作缩水甘油醚的基础，双酚，例如双酚A，二或多羟基芳族化合物，例如间苯二酚，带有酚的OH-基的聚芳烷基化合物，酚醛清漆，聚烷撑乙二醇或多元醇，例如甘油，或季戊四醇。此外适用的化合物是缩水甘油-酯-型，例如对-羟基苯甲酸-缩水甘油醚酯；带有脂肪族或芳香核的多元羧酸的纯缩水甘油酯，例如六氢化邻苯二甲酸或邻苯二甲酸。
作为“醇或糖”采用按本发明带有1-15个羟基的醇或糖。优选采用带有1至5个羟基的醇。醇或糖的基本构架在此可随意改变，可以是脂肪族，环状或双环状的，可只由单键或也可由多键组成的并且也可是芳族体系。优选采用Hoechst公司制造的TCD-醇DM，它是3(4)，8(9)双(羟甲基)-三环[5，2，1，02，6]-癸烷。优选的多元醇在粘合剂配方中所含的质量份额为2-30％(重量)。它优选的质量份额在2.5和20％(重量)之间，特别优选份额在4.5和12％(重量)之间。
作为热引发剂，可采用所有可行的，按阳离子机理固化的引发剂，例如鎓盐。这里优选应用Aldrich公司制造的(S-苄基锍杂戊环六氟锑酸盐)。
作为增粘剂可应用Huls公司生产的A 187，即缩水甘油氧化丙基-三-甲氧基硅烷。
作为助流动剂，可应用Modaflow(孟山都公司制造)和作为流动改性剂或触变剂，例如可应用商业上拥有的Aerosil-型(Degussa公司制造)。
除了已列举的组分之外，在本发明的粘合剂体系中还包含有其它的，已熟知的添加剂。对此，粘合剂体系也可得到附加的性能，如特殊的颜色或透明度，以及难燃性或耐温性。所以，在此意义上，例如添加剂可以是染料、颜料，流动改性剂、普通的稳定剂、阻燃剂或矿物质的或其它填充剂。在此，几乎总是可能通过添加剂达到规定的性能，例如通过添加一种着色剂达到自然吸收和透明度。
粘合剂体系的制备如同可比较的体系一样。配方组成，如环氧树脂，多元醇，热引发剂，增粘剂和必要时助流动剂，必要时也可在升温和重新除去溶剂的情况下，相互进行均匀地混合。对于粘合剂体系的制备，也可依靠当前技术水平采用可靠的方法。
以下借助于实例进一步解释本发明。表1表明一种有代表性的粘合剂体系的配方组分。
                   表1：代表性配方的组分和化学名称
组成(来源)化学名称    份额〔质量份〕
树脂：CY 177(Ciba Geigy)己二酸双(3，4-环氧基环己基甲基)酯 100
多元醇：TCD-醇DM(Hoechst)，3(4)，8(9)-双(羟甲基)-三环[5，2，1，02，6]癸烷 10
热引发剂：S-苄基锍杂戊环六氟锑酸盐(Aldrich) 1
增粘剂：A 187(Hüls)3-缩水甘油氧基丙基三甲氧基硅烷 0.5
表2概括了选择的在实例中列举的配方材料的特性。
   表2：加工和选出的交联粘合剂的材料特性参数
固化    1h 120℃(完全固化)
树脂性能：粘度η[mPas]室温60℃80℃反应性2η(80℃)[min]DSC(10K/min)：T(开始反应)[℃]T(min)[℃]热效应ΔHR[-J/g] 880120805596130415
成形材料性能：玻璃化转变温度[℃](DSC，10k/min)动态力学分析(拉伸模量，3K/min)弹性模数(20℃)[N/mm2]α-(-60 bis 40℃)[ppm/K]α-转变〔℃〕β-转变〔℃〕肖氏硬度热稳定性：TG/DTA(10K/min)，N2)5％质量损失〔℃〕DTG(max)〔℃〕降解速率〔％/min〕 682.4009663-64D81350.4413.422.7
表3表示配方可贮存性的试验研究。确定2个月作为观察周期并同时在冰箱贮存中(5-8℃)不致出现不相容性和分解，例如，如同热引发剂结晶一样。表3：在不同贮存温度的粘度变化η(t)
贮存时间                室温                 7℃
  [d]              η(60℃)[mPas]       η(60℃)[mPas]
   0                    120                  120
   60                   2.200                120
采用本发明的粘合剂体系有可能使电子和光电元件在微米-和小于微米级内进行自动化的和可靠的微粘合。按本发明的单组分浇铸环氧树脂不会立即固化，以致允许单个构件的接缝直至最终固定为止。环氧树脂组分和整个的粘合剂体系的粘度是够低的，以使能应用在微粘合中。最后可用醇和糖，特别是用多元醇调节粘合剂体系的液滴-、湿润-和流动性能以及粘合复合物的机械性能。
粘合剂体系应毫无问题的进行微量计量并可使液滴-，湿润-和流动性能还通过添加助流动剂进行优化。通过输入热量，亦即通过待粘合部件的局部加热或加热粘合剂体系迅速交联成一种均匀的粘合复合物。
已知用于微粘合技术的双组分粘合剂配方开始时提到的缺点由此得到克服。尤其是可计量性和计量准确性得到改进，以及避免了不充分混合和混合误差，并降低了粘度。
本发明涉及单组分的粘合剂体系，该体系至少由浇铸树脂，特别是浇铸环氧树脂和多元醇组成的。低粘度的粘合剂体系是可微计量的，贮存稳定的，可完全固化的和适合于尺寸公差在微米级和小于微米级的应用。

Claims (4)

1.可热固化的单组分的粘合剂体系，该体系包含：
60-98％(重量)的浇铸环氧树脂己二酸双(3，4-环氧基环己基甲基)酯；
2-30％(重量)的多元醇或糖，所述多元醇为3(4)，8(9)双(羟甲基)-三环[5，2，1，02，6]-癸烷；
0.2-2.0％(重量)的选自鎓盐和(S-苄基锍杂戊环六氟锑酸盐的热引发剂；
0.2-2.0％(重量)的增粘剂；
0-3.0％(重量)的助流剂；
0-4.0％(重量)的触变剂；和
0-4.0％(重量)的流动改性剂。
2.权利要求1的粘合剂体系，还包含选自染料、颜料、流动改性剂、普通的稳定剂、阻燃剂和矿物质或其它填充剂的添加剂。
3.可热固化的单组分的粘合剂体系，该体系包括以下组成：
85-93％(重量)的浇铸环氧树脂己二酸双(3，4-环氧基环己基甲基)酯；
4.5-12％(重量)的多元醇，所述多元醇为3(4)，8(9)双(羟甲基)-三环[5，2，1，02，6]-癸烷；
0.7-1.0％(重量)的选自鎓盐和(S-苄基锍杂戊环六氟锑酸盐的热引发剂；
0.3-0.6％(重量)的增粘剂；
0-1.5％(重量)的助流动剂；
0-2.0％(重量)的触变剂，和
0-2.0％(重量)的流动改性剂。
4.按权利要求1、2或3的可热固化的单组分的粘合剂体系在尺寸公差在微米和小于微米级的粘合方面的应用。
CN97197995A 1996-07-18 1997-07-17 微级粘合用可热固化的单组分lva(低粘度粘合剂)粘合体系 Expired - Fee Related CN1121468C (zh)

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