CN110651336A - 导电性糊组合物、包含由该导电性糊组合物形成的电极的装置、及导电性糊组合物的制造方法 - Google Patents
导电性糊组合物、包含由该导电性糊组合物形成的电极的装置、及导电性糊组合物的制造方法 Download PDFInfo
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- CN110651336A CN110651336A CN201880033348.7A CN201880033348A CN110651336A CN 110651336 A CN110651336 A CN 110651336A CN 201880033348 A CN201880033348 A CN 201880033348A CN 110651336 A CN110651336 A CN 110651336A
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Classifications
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- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/22—Di-epoxy compounds
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- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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- C08K5/0025—Crosslinking or vulcanising agents; including accelerators
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- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
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Abstract
本发明提供一种低电阻、且在电极形成过程中不会引起过度的收缩、电极完成时内部应力得到抑制的导电性糊组合物等。该导电性糊组合物至少含有(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料,(A)粘合剂是以硅氧烷键为主骨架、且含有多个环氧乙烷环作为有机基团的反应性低聚物,(B)环氧单体含有环氧乙烷环,在将(A)~(D)合计设为100重量份的情况下,(A)(B)(C)(D)为特定范围的重量份。
Description
技术领域
本发明涉及导电性糊组合物、包含由该导电性糊组合物形成的电极的装置、及导电性糊组合物的制造方法。
背景技术
近来,在智能手机、平板电脑、薄型电视机、汽车导航***等平面面板显示器(FPD)中搭载的FPC(FlexiblePrinted Circuits)的配线、或太阳能电池的集电极中使用导电性糊组合物。
一般的导电性糊组合物在印刷于对象物(例如太阳能电池的硅基板)上后进行干燥、固化、烧成,但导电性糊组合物在固化时收缩,在烧成后也具有内部应力。这样的收缩或内部应力不仅会成为配线/电极本身的变形或破损等的原因,还会成为对象物的变形或破损等的原因。
为了抑制这些现象,例如,在专利文献1中,在导电性糊组合物中的粘合剂中采用橡胶。另外,在专利文献2中,在粘合剂中添加橡胶粒子。
现有技术文献
专利文献
专利文献1:日本特开2004-221006号公报
专利文献2:日本特开2015-111576号公报
发明内容
发明所要解决的问题
然而,两文献的导电性糊组合物中的橡胶成分为高分子,因此为高粘度,不能进行微细的印刷。在想要解决上述问题的情况下,考虑了将导电性糊组合物中的导电性填料的含量设为少量,但在该情况下,电极会高电阻化。
本发明为了解决上述问题而成,其目的在于,提供一种低电阻、且在电极形成过程中不会引起过度的收缩、电极完成时内部应力得到抑制的导电性糊组合物等。
解决问题的方法
本发明人们为了解决上述问题而反复进行了深入研究,结果完成了本发明。更具体而言,本发明提供以下的内容。
(1)一种导电性糊组合物,其至少含有(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料,
(A)粘合剂是以硅氧烷键为主骨架、且含有多个环氧乙烷环作为有机基团的反应性低聚物,
(B)环氧单体含有环氧乙烷环,
在将(A)~(D)合计设为100重量份的情况下,(A)粘合剂为1重量份以上且10重量份以下,(B)环氧单体为2重量份以上且20重量份以下,(C)交联剂为1重量份以上且20重量份以下,(D)导电性填料为70重量份以上且95重量份以下。
(2)根据(1)所述的导电性糊组合物,其中,
(B)环氧单体含有选自具有二醇结构的2官能单体及具有脂肪族结构的单官能单体中的至少1种。
(3)根据(1)或(2)所述的导电性糊组合物,其中,
(C)交联剂是具有潜热性的化合物。
(4)根据(1)~(3)中任一项所述的导电性糊组合物,其中,
(C)交联剂含有选自咪唑化合物、肼化合物、及酸酐中的至少1种。
(5)根据(1)~(4)中任一项所述的导电性糊组合物,其进一步含有(E)脱水剂。
(6)根据(5)所述的导电性糊组合物,其中,
(E)脱水剂为酸酐。
(7)一种装置,其包含由(1)~(6)中任一项所述的导电性糊组合物形成的电极。
(8)一种导电性糊组合物的制造方法,该导电性糊组合物至少含有(A)粘合剂、(B)环氧单体、(C)交联剂、(D)导电性填料、及(E)脱水剂,
(A)粘合剂是以硅氧烷键为主骨架、且含有多个环氧乙烷环作为有机基团的反应性低聚物,
(B)环氧单体含有环氧乙烷环,
在将(A)~(D)合计设为100重量份的情况下,(A)粘合剂为1重量份以上且10重量份以下,(B)环氧单体为2重量份以上且20重量份以下,(C)交联剂为1重量份以上且20重量份以下,(D)导电性填料为70重量份以上且95重量份以下,
在该制造方法中,
在对(A)粘合剂添加(B)~(D)中的任一者之前,对(A)粘合剂添加(E)脱水剂、或者
在对(D)导电性填料添加(E)脱水剂之后,进一步添加(A)~(C)。
发明的效果
本发明的导电性糊组合物为低电阻,且在电极形成过程中不会引起过度的收缩,电极完成时内部应力得到抑制。
具体实施方式
如下所述,对本发明的一实施方式进行说明,但本发明不限定于该实施方式。
[导电性糊组合物]
导电性糊组合物至少含有(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料。(A)粘合剂是以硅氧烷键为主骨架、且含有多个环氧乙烷环作为有机基团的反应性低聚物。(B)环氧单体含有环氧乙烷环。而且,在将(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料合计设为100重量份的情况下,(A)粘合剂为1重量份以上且10重量份以下,(B)环氧单体为2重量份以上且20重量份以下,(C)交联剂为1重量份以上且20重量份以下,(D)导电性填料为70重量份以上且95重量份以下。
这样的导电性糊组合物例如在FPD或太阳能电池这样的装置中作为配线材料或电极材料使用。需要说明的是,在本说明书中,为了方便,将配线或电极称为“电极”。
一般而言,为了保证作为电极材料的功能、即低电阻化,需要在导电性糊组合物中添加大量的导电性填料(在本发明中,需要如上所述地使导电性填料为70重量份以上)。在这样的条件下对导电性填料添加一般的粘合剂·交联剂而设计导电性糊组合物时,该导电性糊组合物变成高粘度,难以达到可进行微细的印刷的粘度。
在这样的情况下,为了调整粘度,考虑了添加稀释剂。然而,作为稀释剂,如果使用例如一般的高沸点溶剂,则在导电性糊组合物经过干燥/烧成而成为电极(电路)的情况下,该电极会因稀释剂的挥发引起的体积收缩而比期望的尺寸更细、翘曲。
为了防止该体积收缩,考虑了添加反应性稀释剂(单体)。然而,如果使用例如分子内具有多个官能团的反应性稀释剂或分子量小的反应性稀释剂,则因该反应性稀释剂本身导致的反应,会发生固化收缩,消除普通粘合剂(双酚A系环氧树脂等)的低收缩特性。
因此,在本发明中,通过使用比较而言为低粘度/高反应、即使进行交联反应也为低收缩,且与一般的粘合剂不同组成的(A)粘合剂,则可使用双酚A系环氧树脂等中不能使用的反应性稀释剂[(B)环氧单体]。即,可使用相容性高的(A)粘合剂和(B)环氧单体。
此外,使用了即使在(A)粘合剂交联的情况下也可发挥缓和作为导电性糊组合物的内部应力的功能的(C)交联剂。
因此,以下,对构成导电性糊组合物的(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料、以及其它原材料(添加剂)进行说明。
<(A)粘合剂>
作为粘合剂,可举出例如以下的通式(I)表示的化合物均缩聚物、或通式(I)表示的化合物与通式(II)表示的化合物的缩合物,该均缩聚物或该缩合物是以硅氧烷键为主骨架、且含有多个环氧乙烷环作为有机基团的反应性低聚物。(A)粘合剂可以单独使用,也可以组合2种以上使用。
通式(I):
R1-(SiR2 a(OR3)3-a) (I)
需要说明的是,通式(I)中,R1是末端被含有环氧结构的基团取代的碳原子数1~10的烷基,R2分别独立地为氢原子或选自碳原子数1~10的烷基、碳原子数6~25的芳基及碳原子数7~12的芳烷基中的1价烃基,R3分别独立地为氢原子或碳原子数1~10的烷基。a为0~2的整数。由此,通式(I)表示的化合物为具有水解性甲硅烷基的硅烷化合物(I)。
通式(II):
R4-(SiR2 a(OR3)3-a) (II)
需要说明的是,通式(II)中,R4选自碳原子数1~10的取代或者非取代的烷基、烯基、以及取代芳基,且不具有含有环氧结构的基团。R2分别独立地为氢原子或选自碳原子数1~10的烷基、碳原子数6~25的芳基及碳原子数7~12的芳烷基中的1价烃基,R3分别独立地为氢原子或碳原子数1~10的烷基。a为0~2的整数。由此,通式(II)表示的化合物也是具有水解性甲硅烷基的硅烷化合物(II)。
作为成为粘合剂的一例的硅烷化合物(I)与硅烷化合物(II)的缩合物,可列举将硅烷化合物(II)相对于硅烷化合物(I)的摩尔比设为9以下、并在中性盐催化剂的存在下进行水解及缩合而得到的重均分子量30000以下的缩合物。另外,缩合物(A)所具有的与硅原子直接键合的OR3基的摩尔数Y相对于硅烷化合物(I)及硅烷化合物(II)所具有的与硅原子直接键合的OR3基的摩尔数X之比(Y/X)例如为0.2以下。
通式(I)及通式(II)的取代基如下所述。
作为通式(I)的R1中的末端被含有环氧结构的基团取代的碳原子数1~10的烷基的具体例,可列举例如:甲基、乙基、丙基、异丙基、丁基、异丁基、戊基、异戊基、己基、环己基、环己基甲基、庚基、异庚基、正辛基、异辛基、或2-乙基己基等,从固化时环氧基的反应性(mobility)的观点考虑,优选甲基、乙基、丙基、异丙基、丁基、或异丁基,更优选乙基或丙基。
作为通式(I)的R1中的含有环氧结构的基团,只要是含有环氧基的官能团即可,可列举例如:环氧基、缩水甘油醚基(即环氧丙氧基)、或环氧环己基等,从反应性等观点考虑,优选缩水甘油醚基或环氧环己基。
需要说明的是,“末端”在上述烷基为直链的情况下是指离Si最远端的甲基。在为具有支链的烷基的情况下,是指离主链所具有的Si最远端的甲基、和/或离1或者多个支链所具有的Si最远端的甲基。
通式(I)及通式(II)的R2为氢原子或选自碳原子数1~10的烷基、碳原子数6~25的芳基、及碳原子数7~12的芳烷基中的1价烃基。作为这样的烃基,可列举例如:甲基、乙基、丙基、丁基、戊基、己基、辛基、壬基、癸基、苯基、甲苯基、二甲苯基、萘基、苄基、或苯乙基等。从反应性等观点考虑,R2优选为氢原子、甲基、乙基、或丙基,更优选为甲基或乙基。
通式(I)及通式(II)的R3是氢原子或碳原子数1~10的烷基。作为烷基,可列举例如:甲基、乙基、丙基、丁基、戊基、己基、辛基、壬基、或癸基等。从容易使具有水解性甲硅烷基的硅烷化合物水解/缩合的观点考虑,R3的烷基的碳原子数优选为1~3,最优选为1。
通式(II)的R4选自碳原子数1~10的取代或者非取代的烷基、烯基、以及取代芳基,且不具有环氧基。
作为烷基,可列举例如:甲基、乙基、丙基、异丙基、丁基、异丁基、戊基、戊基、异戊基、己基、环己基、环己基甲基、环己基乙基、庚基、异庚基、正辛基、异辛基、2-乙基己基、壬基、或癸基等。
作为烷基的取代基,可列举例如:硫醇基、氨基、异氰酸酯基、(甲基)丙烯酰基、苯基、或氯基等。
作为烯基,可列举例如:乙烯基、芳基、1-甲基乙烯基、2-甲基乙烯基、2-丙烯基、1-甲基-3-丙烯基、3-丁烯基、4-戊烯基、5-己烯基、环己烯基、双环己烯基、6-庚烯基、7-辛烯基、癸烯基、十五碳烯基、二十碳烯基、或二十三碳烯基等。
作为取代芳基,可列举例如:苯乙烯基等。
这些中,从储存稳定性良好、活性能量射线照射时的固化速度快、进而可抑制得到的涂膜产生裂纹的方面考虑,在R4为非取代的烷基的情况下,优选碳原子数为3以上且10以下,更优选碳原子数为3以上且6以下。
从同样的观点考虑,在R4为取代烷基的情况下,除取代基以外的部分的碳原子数优选为3以上且10以下,更优选为3以上且6以下,取代基优选为苯基、环己基、或(甲基)丙烯酰基等。
从同样的观点考虑,在R4为烯基的情况下,优选为例如乙烯基或芳基等。
在R4为非取代烷基且碳原子数为3以上的情况、R4为取代烷基且除取代基以外的部分的碳原子数为3以上的情况、或R4为取代烷基且取代基为苯基、环己基、或(甲基)丙烯酰基的情况下,交联时不易成为致密的交联结构,不易凝胶化。
另外,在R4为非取代烷基且碳原子数为10以下的情况、R4为取代烷基且除取代基以外的部分的碳原子数为10以下的情况、或R4为取代烷基且取代基为苯基、环己基、或(甲基)丙烯酰基的情况下,疏水性不会变得过高,水解速度不易极端地降低,活性能量射线照射时的固化速度不易降低。
通式(I)及通式(II)的a为0~2的整数,根据固化性组合物所要求的物性适宜选择。
作为硅烷化合物(I)的具体例,可列举例如:1-缩水甘油氧基甲基三甲氧基硅烷、1-缩水甘油氧基甲基甲基二甲氧基硅烷、1-缩水甘油氧基甲基三乙氧基硅烷、1-缩水甘油氧基甲基甲基二乙氧基硅烷、2-缩水甘油氧基乙基三甲氧基硅烷、2-缩水甘油氧基乙基甲基二甲氧基硅烷、2-缩水甘油氧基乙基三乙氧基硅烷、2-缩水甘油氧基乙基甲基二乙氧基硅烷、3-缩水甘油氧基丙基三甲氧基硅烷、3-缩水甘油氧基丙基甲基二甲氧基硅烷、3-缩水甘油氧基丙基三乙氧基硅烷、3-缩水甘油氧基丙基甲基二乙氧基硅烷、4-缩水甘油氧基丁基三甲氧基硅烷、4-缩水甘油氧基丁基甲基二甲氧基硅烷、4-缩水甘油氧基丁基三乙氧基硅烷、4-缩水甘油氧基丁基甲基二乙氧基硅烷、6-缩水甘油氧基己基三甲氧基硅烷、6-缩水甘油氧基己基甲基二甲氧基硅烷、6-缩水甘油氧基己基三乙氧基硅烷、6-缩水甘油氧基己基甲基二乙氧基硅烷、8-缩水甘油氧基辛基三甲氧基硅烷、8-缩水甘油氧基辛基甲基二甲氧基硅烷、8-缩水甘油氧基辛基三乙氧基硅烷、8-缩水甘油氧基辛基甲基二乙氧基硅烷等含缩水甘油基硅烷;1-(3,4-环氧环己基)甲基三甲氧基硅烷、1-(3,4-环氧环己基)甲基甲基二甲氧基硅烷、1-(3,4-环氧环己基)甲基三乙氧基硅烷、1-(3,4-环氧环己基)甲基甲基二乙氧基硅烷、2-(3,4-环氧环己基)乙基三甲氧基硅烷、2-(3,4-环氧环己基)乙基甲基二甲氧基硅烷、2-(3,4-环氧环己基)乙基三乙氧基硅烷、2-(3,4-环氧环己基)乙基甲基二乙氧基硅烷、3-(3,4-环氧环己基)丙基三甲氧基硅烷、3-(3,4-环氧环己基)丙基甲基二甲氧基硅烷、3-(3,4-环氧环己基)丙基三乙氧基硅烷、3-(3,4-环氧环己基)丙基甲基二乙氧基硅烷、4-(3,4-环氧环己基)丁基三甲氧基硅烷、4-(3,4-环氧环己基)丁基甲基二甲氧基硅烷、4-(3,4-环氧环己基)丁基三乙氧基硅烷、4-(3,4-环氧环己基)丁基甲基二乙氧基硅烷、6-(3,4-环氧环己基)己基三甲氧基硅烷、6-(3,4-环氧环己基)己基甲基二甲氧基硅烷、6-(3,4-环氧环己基)己基三乙氧基硅烷、6-(3,4-环氧环己基)己基甲基二乙氧基硅烷、8-(3,4-环氧环己基)辛基三甲氧基硅烷、8-(3,4-环氧环己基)辛基甲基二甲氧基硅烷、8-(3,4-环氧环己基)辛基三乙氧基硅烷、8-(3,4-环氧环己基)辛基甲基二乙氧基硅烷等含脂环环氧基硅烷;环氧三甲氧基硅烷、环氧甲基二甲氧基硅烷、环氧三乙氧基硅烷、环氧甲基二乙氧基硅烷、1-环氧甲基三甲氧基硅烷、1-环氧甲基甲基二甲氧基硅烷、1-环氧甲基三乙氧基硅烷、1-环氧甲基甲基二乙氧基硅烷、2-环氧乙基三甲氧基硅烷、2-环氧乙基甲基二甲氧基硅烷、2-环氧乙基三乙氧基硅烷、2-环氧乙基甲基二乙氧基硅烷、3-环氧丙基三甲氧基硅烷、3-环氧丙基甲基二甲氧基硅烷、3-环氧丙基三乙氧基硅烷、3-环氧丙基甲基二乙氧基硅烷、4-环氧丁基三甲氧基硅烷、4-环氧丁基甲基二甲氧基硅烷、4-环氧丁基三乙氧基硅烷、4-环氧丁基甲基二乙氧基硅烷、6-环氧己基三甲氧基硅烷、6-环氧己基甲基二甲氧基硅烷、6-环氧己基三乙氧基硅烷、6-环氧己基甲基二乙氧基硅烷、8-环氧辛基三甲氧基硅烷、8-环氧辛基甲基二甲氧基硅烷、8-环氧辛基三乙氧基硅烷、8-环氧辛基甲基二乙氧基硅烷等含环氧基硅烷等。
如上所述,从容易使具有水解性甲硅烷基的硅烷化合物水解及缩合的观点考虑,通式(I)中的R3的烷基的碳原子数优选为1~3,最优选为1。另外,从固化时的环氧基的反应性(mobility)的观点考虑,将环氧基和硅原子键合的亚烷基的碳原子数是重要的,该碳原子数优选为1~4,进一步优选为2或3。如果综合这些观点,则作为硅烷化合物(I),其中,优选R1为2-(3,4-环氧环己基)乙基、或3-缩水甘油氧基丙基的化合物。
具体而言,优选2-(3,4-环氧环己基)乙基三甲氧基硅烷、2-(3,4-环氧环己基)乙基甲基二甲氧基硅烷、3-(3,4-环氧环己基)丙基三甲氧基硅烷、3-(3,4-环氧环己基)丙基甲基二甲氧基硅烷、2-缩水甘油氧基乙基三甲氧基硅烷、2-缩水甘油氧基乙基甲基二甲氧基硅烷、3-缩水甘油氧基丙基三甲氧基硅烷、或3-缩水甘油氧基丙基甲基二甲氧基硅烷。
作为硅烷化合物(II)、通式(II)中的R4为非取代的烷基的化合物,可列举例如:甲基三甲氧基硅烷、二甲基二甲氧基硅烷、甲基三乙氧基硅烷、二甲基二乙氧基硅烷、乙基三甲氧基硅烷、乙基甲基二甲氧基硅烷、乙基三乙氧基硅烷、乙基甲基二乙氧基硅烷、丙基三甲氧基硅烷、丙基甲基二甲氧基硅烷、丙基三乙氧基硅烷、丙基甲基二乙氧基硅烷、丁基三甲氧基硅烷、丁基甲基二甲氧基硅烷、丁基三乙氧基硅烷、丁基甲基二乙氧基硅烷、己基三甲氧基硅烷、己基甲基二甲氧基硅烷、己基三乙氧基硅烷、己基甲基二乙氧基硅烷、辛基三甲氧基硅烷、辛基甲基二甲氧基硅烷、辛基三乙氧基硅烷、或辛基甲基二乙氧基硅烷等。
另外,作为通式(II)中的R4为取代烷基的化合物,可列举下述的化合物。此处,作为取代基,没有特别限制,从获取容易性的观点考虑,优选硫醇基、异氰酸酯基、(甲基)丙烯酰基、苯基、环己基、或氯基等。
然而,这些取代基中,由于硫醇基(巯基)有可能在水解性甲硅烷基进行水解及缩合反应的过程中与环氧基发生反应,因此,作为硅烷化合物(I),可选择具有不易受到亲核攻击的环氧环己基的环氧硅烷化合物。
另一方面,由于具有氨基或酸酐基作为取代基的硅烷化合物在水解性甲硅烷基进行水解及缩合反应的过程中与环氧基反应的可能性比巯基更高,因此,不优选在本申请中使用。
作为R4为硫醇基取代烷基的化合物,可列举例如:1-巯基甲基三甲氧基硅烷、1-巯基甲基甲基二甲氧基硅烷、1-巯基甲基三乙氧基硅烷、1-巯基甲基甲基二乙氧基硅烷、2-巯基乙基三甲氧基硅烷、2-巯基乙基甲基二甲氧基硅烷、2-巯基乙基三乙氧基硅烷、2-巯基乙基甲基二乙氧基硅烷、3-巯基丙基三甲氧基硅烷、3-巯基丙基甲基二甲氧基硅烷、3-巯基丙基三乙氧基硅烷、3-巯基丙基甲基二乙氧基硅烷、4-巯基丁基三甲氧基硅烷、4-巯基丁基甲基二甲氧基硅烷、4-巯基丁基三乙氧基硅烷、4-巯基丁基甲基二乙氧基硅烷、6-巯基己基三甲氧基硅烷、6-巯基己基甲基二甲氧基硅烷、6-巯基己基三乙氧基硅烷、6-巯基己基甲基二乙氧基硅烷、8-巯基辛基三甲氧基硅烷、8-巯基辛基甲基二甲氧基硅烷、8-巯基辛基三乙氧基硅烷、8-巯基辛基甲基二乙氧基硅烷等。
作为R4为异氰酸酯基取代烷基的化合物,可列举例如:1-异氰酸酯甲基三甲氧基硅烷、1-异氰酸酯甲基甲基二甲氧基硅烷、1-异氰酸酯甲基三乙氧基硅烷、1-异氰酸酯甲基甲基二乙氧基硅烷、2-异氰酸酯乙基三甲氧基硅烷、2-异氰酸酯乙基甲基二甲氧基硅烷、2-异氰酸酯乙基三乙氧基硅烷、2-异氰酸酯乙基甲基二乙氧基硅烷、3-异氰酸酯丙基三甲氧基硅烷、3-异氰酸酯丙基甲基二甲氧基硅烷、3-异氰酸酯丙基三乙氧基硅烷、3-异氰酸酯丙基甲基二乙氧基硅烷、4-异氰酸酯丁基三甲氧基硅烷、4-异氰酸酯丁基甲基二甲氧基硅烷、4-异氰酸酯丁基三乙氧基硅烷、4-异氰酸酯丁基甲基二乙氧基硅烷、6-异氰酸酯己基三甲氧基硅烷、6-异氰酸酯己基甲基二甲氧基硅烷、6-异氰酸酯己基三乙氧基硅烷、6-异氰酸酯己基甲基二乙氧基硅烷、8-异氰酸酯辛基三甲氧基硅烷、8-异氰酸酯辛基甲基二甲氧基硅烷、8-异氰酸酯辛基三乙氧基硅烷、8-异氰酸酯辛基甲基二乙氧基硅烷等。
作为R4为(甲基)丙烯酰基取代烷基的化合物,可列举例如:1-(甲基)丙烯酰氧基甲基三甲氧基硅烷、1-(甲基)丙烯酰氧基甲基甲基二甲氧基硅烷、1-(甲基)丙烯酰氧基甲基三乙氧基硅烷、1-(甲基)丙烯酰氧基甲基甲基二乙氧基硅烷、2-(甲基)丙烯酰氧基乙基三甲氧基硅烷、2-(甲基)丙烯酰氧基乙基甲基二甲氧基硅烷、2-(甲基)丙烯酰氧基乙基三乙氧基硅烷、2-(甲基)丙烯酰氧基乙基甲基二乙氧基硅烷、3-(甲基)丙烯酰氧基丙基三甲氧基硅烷、3-(甲基)丙烯酰氧基丙基甲基二甲氧基硅烷、3-(甲基)丙烯酰氧基丙基三乙氧基硅烷、3-(甲基)丙烯酰氧基丙基甲基二乙氧基硅烷、4-(甲基)丙烯酰氧基丁基三甲氧基硅烷、4-(甲基)丙烯酰氧基丁基甲基二甲氧基硅烷、4-(甲基)丙烯酰氧基丁基三乙氧基硅烷、4-(甲基)丙烯酰氧基丁基甲基二乙氧基硅烷、6-(甲基)丙烯酰氧基己基三甲氧基硅烷、6-(甲基)丙烯酰氧基己基甲基二甲氧基硅烷、6-(甲基)丙烯酰氧基己基三乙氧基硅烷、6-(甲基)丙烯酰氧基己基甲基二乙氧基硅烷、8-(甲基)丙烯酰氧基辛基三甲氧基硅烷、8-(甲基)丙烯酰氧基辛基甲基二甲氧基硅烷、8-(甲基)丙烯酰氧基辛基三乙氧基硅烷、8-(甲基)丙烯酰氧基辛基甲基二乙氧基硅烷等。
作为R4为苯基取代烷基的化合物,可列举例如:苄基三甲氧基硅烷、苄基三乙氧基硅烷、2-苯基乙基三甲氧基硅烷、2-苯基乙基三乙氧基硅烷、3-苯基丙基三甲氧基硅烷、3-苯基丙基三乙氧基硅烷、4-苯基丁基三甲氧基硅烷、4-苯基丁基三乙氧基硅烷、5-苯基戊基三甲氧基硅烷、5-苯基戊基三乙氧基硅烷、6-苯基己基三甲氧基硅烷、6-苯基己基三乙氧基硅烷等。
作为R4为环己基取代烷基的化合物,可列举例如:环己基甲基三甲氧基硅烷、环己基甲基三乙氧基硅烷、2-环己基乙基三甲氧基硅烷、2-环己基乙基三乙氧基硅烷、3-环己基丙基三甲氧基硅烷、3-环己基丙基三乙氧基硅烷、4-环己基丁基三甲氧基硅烷、4-环己基丁基三乙氧基硅烷、5-环己基戊基三甲氧基硅烷、5-环己基戊基三乙氧基硅烷、6-环己基己基三甲氧基硅烷、6-环己基己基三乙氧基硅烷等。
作为R4为氯基取代烷基的化合物,可列举例如:氯甲基三甲氧基硅烷、氯甲基三乙氧基硅烷、2-氯乙基三甲氧基硅烷、2-氯乙基三乙氧基硅烷、3-氯丙基三甲氧基硅烷、3-氯丙基三乙氧基硅烷、4-氯丁基三甲氧基硅烷、4-氯丁基三乙氧基硅烷、5-氯戊基三甲氧基硅烷、5-氯戊基三乙氧基硅烷、6-氯己基三甲氧基硅烷、6-氯己基三乙氧基硅烷等。
作为R4为烯基的化合物,可列举例如:乙烯基三甲氧基硅烷、乙烯基甲基二甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基甲基二乙氧基硅烷、芳基三甲氧基硅烷、芳基甲基二甲氧基硅烷、芳基三乙氧基硅烷、芳基甲基二乙氧基硅烷、1-氧杂环丁烷氧基甲基三甲氧基硅烷、1-氧杂环丁烷氧基甲基甲基二甲氧基硅烷、1-氧杂环丁烷氧基甲基三乙氧基硅烷、1-氧杂环丁烷氧基甲基甲基二乙氧基硅烷、2-氧杂环丁烷氧基乙基三甲氧基硅烷、2-氧杂环丁烷氧基乙基甲基二甲氧基硅烷、2-氧杂环丁烷氧基乙基三乙氧基硅烷、2-氧杂环丁烷氧基乙基甲基二乙氧基硅烷、3-氧杂环丁烷氧基丙基三甲氧基硅烷、3-氧杂环丁烷氧基丙基甲基二甲氧基硅烷、3-氧杂环丁烷氧基丙基三乙氧基硅烷、3-氧杂环丁烷氧基丙基甲基二乙氧基硅烷、4-氧杂环丁烷氧基丁基三甲氧基硅烷、4-氧杂环丁烷氧基丁基甲基二甲氧基硅烷、4-氧杂环丁烷氧基丁基三乙氧基硅烷、4-氧杂环丁烷氧基丁基甲基二乙氧基硅烷、6-氧杂环丁烷氧基己基三甲氧基硅烷、6-氧杂环丁烷氧基己基甲基二甲氧基硅烷、6-氧杂环丁烷氧基己基三乙氧基硅烷、6-氧杂环丁烷氧基己基甲基二乙氧基硅烷、8-氧杂环丁烷氧基辛基三甲氧基硅烷、8-氧杂环丁烷氧基辛基甲基二甲氧基硅烷、8-氧杂环丁烷氧基辛基三乙氧基硅烷、8-氧杂环丁烷氧基辛基甲基二乙氧基硅烷等。
作为R4为取代芳基的化合物,可列举例如:对苯乙烯基三甲氧基硅烷、对苯乙烯基三乙氧基硅烷等。
其中,从储存稳定性、固化速度、抑制裂纹产生等观点考虑,作为硅烷化合物(II),可列举例如:甲基三甲氧基硅烷、1-(甲基)丙烯酰氧基甲基三甲氧基硅烷、苄基三甲氧基硅烷、环己基甲基三甲氧基硅烷、乙烯基三甲氧基硅烷、对苯乙烯基三甲氧基硅烷等。
在成为粘合剂的缩合物中,分别含有硅烷化合物(I)及硅烷化合物(II)1种以上即可。例如,可分别含有硅烷化合物(I)、硅烷化合物(II)各1种,也可以分别含有硅烷化合物(I)、硅烷化合物(II)各2种以上。另外,也可以含有硅烷化合物(I)及硅烷化合物(II)中的一者1种、并含有另一者2种以上。在含有2种以上化合物的情况下,各个化合物的使用比率是任意的。
另外,在对导电性糊组合物要求耐摩耗性或耐化学药品性的情况下,优选在硅烷化合物(II)相对于硅烷化合物(I)的摩尔比(硅烷化合物(II)的摩尔数/硅烷化合物(I)的摩尔数)成为0以上且9以下的条件下进行水解及缩合而获得粘合剂。
除含有环氧结构的基团以外的官能团、例如具有(甲基)丙烯酰基的硅烷化合物相对于硅烷化合物(I)的摩尔比大于9时,可得到耐摩耗性或耐化学药品性高的固化物,但与环氧基的交联相比,固化收缩变大,因此,存在因热或湿度带来的负荷的情况下,存在产生裂纹的忧虑。与此相对,利用含有环氧结构的基团的固化伴随着开环反应,因此,也可以得到固化物,而收缩少,几乎不发生固化收缩。
另外,如果粘合剂中的含有环氧结构的基团的含量降低,则分子间交联变得不充分,存在硬度或耐擦伤性降低的忧虑。因此,如果考虑到硬涂性(即硬度、耐擦伤性),则硅烷化合物(II)相对于硅烷化合物(I)的摩尔比更优选为0以上且5以下,进一步优选为0以上且3以下,特别优选为0以上且1以下。
另外,作为导电性糊组合物中的粘合剂,优选硅烷化合物进行水解及缩合而形成硅氧烷键的2~200聚体。
粘合剂的重均分子量为500以上,更优选为1000以上,进一步优选为2000以上。另外,粘合剂的重均分子量优选为30000以下,更优选为28000以下,进一步优选为25000以下。
粘合剂的重均分子量为500以上时,粘合剂不易具有挥发性,因此,在通过对粘合剂进行紫外线照射而使其固化前,将稀释溶剂通过加热除去时,可以有效地抑制粘合剂的一部分或全部挥发。另外,重均分子量不会过低,因此,容易充分地确保耐冲击性。
另一方面,粘合剂的重均分子量为30000以下时,与其它配合物的相容性不易降低,容易抑制形成涂膜时的白浊。此处,重均分子量是通过GPC测定的重均分子量。
需要说明的是,在为重均分子量小于500的粘合剂的情况下,为低分子量、低粘度,因此,优选制备成含有粘合剂的涂敷液,而不使用稀释溶剂。在该情况下,在照射紫外线前,不需要为了除去稀释溶剂而对粘合剂进行加热。
需要说明的是,作为缩合物的硅氧烷树脂(粘合剂)的重均分子量可通过适当选择用于反应的水的量、催化剂的种类及量来控制。例如,通过增加最初加入的水的量,可提高重均分子量。
粘合剂所具有的与硅原子直接键合的OR3基的摩尔数Y相对于作为粘合剂的原料的硅烷化合物(I)及硅烷化合物(II)所具有的与硅原子直接键合的OR3基的摩尔数X之比Y/X优选为0.2以下,更优选为0.1以下,进一步优选为0.05以下,最优选实质上为0。
Y/X为0.2以下时,照射活性能量射线后,涂膜不易经时收缩,容易抑制裂纹的产生。此处,Y/X可通过用1H-NMR及29Si-NMR进行测定而求出。需要说明的是,Y/X可通过适当选择用于反应的水的量、催化剂的种类及量而设为0.2以下。例如,水的量越多,越促进水解,Y/X成为越低的值。
从涂膜收缩及抑制裂纹产生等观点考虑,粘合剂中残存的OR3基的个数优选粘合剂1分子中为2个以下,更优选为1个以下,进一步优选为0.5个以下,特别优选为0.1个以下,最优选实质上不残存。
从提高交联点密度、提高固化物的硬度、耐擦伤性的观点考虑,优选粘合剂中的含有环氧结构的基团的摩尔数相对于粘合剂中的含有环氧结构的基团的残存率、即作为原料的硅烷化合物(I)所具有的含有环氧结构的基团的摩尔数的比例高的情况。
在硅烷化合物(I)与硅烷化合物(II)形成的缩合物(粘合剂)中,含有环氧结构的基团的含量降低时,分子间交联变得不充分,存在硬度或固化性降低的忧虑。因此,硅烷化合物(II)相对于硅烷化合物(I)的摩尔比优选为0以上且5以下,进一步优选为0以上且3以下,特别优选为0以上且1以下。
需要说明的是,以上,举例硅烷化合物(I)与硅烷化合物(II)的缩合物的粘合剂作为一例,但并不限定于此,例如硅烷化合物(I)的均缩聚物也作为粘合剂发挥功能。
另外,在将(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料合计设为100重量份的情况下,(A)粘合剂为1重量份以上且10重量份以下,优选为1.5重量份以上且8重量份以下,更优选为2重量份以上且7重量份以下。
粘合剂小于1重量份时,导电性糊组合物的固化性降低。另一方面,粘合剂大于10重量份时,导电性糊的电阻难以降低。
<(B)环氧单体>
如上所述,作为反应性稀释剂的(B)环氧单体对(A)粘合剂具有高相容性。另外,作为该环氧单体的分子结构,为聚醚结构。推测由于将醚结构设为直线状结构,因此,分子彼此之间的缠结少,对于拉伸、压缩等外部应力,分子彼此之间容易解开,由此,可缓和导电性糊组合物的内部应力。另外,根据与上述同样的考虑,推测也可缓和导电性糊组合物固化时的收缩,可实现低翘曲。(B)环氧单体可以单独使用,也可以组合2种以上使用。
需要说明的是,关于醚结构,没有特别限定,优选为直链状,另外,从内部应力缓和方面考虑,与单独具有1个相比,优选具有多个。另外,具有醚结构的单体中所含的环氧官能团数也没有特别限定,但出于内部应力缓和与固化性的平衡,优选为2个。
另一方面,作为关于环氧官能团的限定,必须在单体两端中的至少一个分子末端具有1个环氧官能团。作为官能数对翘曲带来的效果,通过具有1个官能团,导电性糊固化时,单体本身不参与交联,因此,作为粘合剂的扩链剂发挥功能。
此外,由于官能团位置为末端,因此,环氧单体的官能团以外的分子部分以梳状配置于粘合剂彼此之间。该梳状链发挥增塑剂的功能。由此推测,可抑制由导电性糊组合物的固化收缩导致的翘曲。
需要说明的是,官能团以外的分子结构没有特别限定,可以是直链状、芳香族结构、脂环式结构的任一种。
鉴于上述内容,优选(B)环氧单体含有选自具有二醇结构的2官能单体及具有脂肪族结构的单官能单体中的至少1种。
作为二醇结构,可列举例如:乙二醇、二乙二醇、聚乙二醇、丙二醇、或聚丙二醇等。
需要说明的是,出于配合物的粘度问题,聚乙二醇、或聚丙二醇的聚合度n为30以下,优选为20以下,进一步优选为10以下。
作为具有脂肪族结构的单官能单体,为例如烷基单缩水甘油醚、烷基单3,4-环氧环己烷、3,4-环氧环己醇与羧酸形成的酯、烷基单氧杂环丁烷。作为其具体例,可列举新戊基单缩水甘油醚、丁基缩水甘油醚、十二烷基缩水甘油醚、十六烷基缩水甘油醚、1-乙烯基-3,4-环氧环己烷、1-羟甲基-3,4-环氧环己烷、2-乙基己基-3,4-环氧环己烷羧酸酯、3-乙基-3-羟基甲基氧杂环丁烷、或2-乙基己基氧杂环丁烷等。
另外,例如,在将双酚A系环氧树脂作为粘合剂、将脂环式环氧树脂作为环氧单体的导电性糊组合物制电极的情况下,成为比较高的电阻,但含有(A)粘合剂和(B)环氧单体的导电性糊组合物的电极可抑制电阻。
需要说明的是,从反应性、柔软性赋予、或电阻抑制效果的平衡的方面考虑,优选十二烷基缩水甘油醚、十六烷基缩水甘油醚、或2-乙基己基-3,4-环氧环己烷羧酸酯。
另外,在将(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料合计设为100重量份的情况下,(B)环氧单体为2重量份以上且20重量份以下,优选为2重量份以上且15重量份以下,更优选为3重量份以上且10重量份以下。
环氧单体小于2重量份时,导电性糊组合物的粘度变高,而且翘曲改善的效果降低。另一方面,环氧单体大于10重量份时,导电性糊组合物的粘度降低,而且固化性降低。
<(C)交联剂>
交联剂在粘合剂交联的情况下,发挥缓和作为导电性糊组合物的内部应力的功能。另外,为了防止导电性糊组合物对粘贴的对象物的损害,交联剂可以在200℃以下的比较低温下的加热干燥、烧成,且使用防止电阻上升的材料。(C)交联剂可以单独使用,也可以组合2种以上使用。
需要说明的是,关于防止电阻上升,其机理尚未详细明确,但优选在不影响导电性糊的固化性的范围内降低交联密度。另外,作为交联剂,优选在单组分化配合中、在25℃左右的常温下稳定,因此,优选具有潜热性的化合物、或UV(紫外光)反应性的化合物。可列举例如:酸酐、肼化合物、三氟化硼络合物、二氰基二酰胺化合物、氨基氰化合物、咪唑化合物、光致产酸剂、或光致产碱剂等。这些中,从对导电性糊组合物的配合、单组分化时的储存稳定性、固化活性、或对导电性填料的耐腐蚀性的方面考虑,优选酸酐、肼化合物、咪唑化合物、或光致产碱剂。
作为酸酐,可列举例如:丙酸酐、丁酸酐、辛酸酐、2-乙基己酸酐、马来酸酐、富马酸酐、乙酸酐、邻苯二甲酸酐、1,2,3,6-四氢邻苯二甲酸酐、3,4,5,6-四氢邻苯二甲酸酐、六氢邻苯二甲酸酐、琥珀酸酐、4-甲基六氢邻苯二甲酸酐、甲基双环[2.2.1]庚烷-2,3-二羧酸酐、乙二醇双脱水偏苯三甲酸酯、乙二醇双脱水偏苯三甲酸酯、乙二醇双脱水偏苯三甲酸酯、乙二醇双脱水偏苯三甲酸酯、甘油双脱水偏苯三甲酸酯单乙酸酯、琥珀酸酐、四丙烯琥珀酸酐(3-十二烷基琥珀酸酐)、或2-辛烯基琥珀酸酐等。优选酸酐具有C6以上的烃基。通过使酸酐具有C6以上的长碳链,容易提高(A)粘合剂与酸酐的混和性。另外,优选酸酐在碳链中具有至少1个双键。酸酐在碳链中具有至少1个双键时,熔点有效地降低,因此,制备导电性糊组合物时的混和性容易变得良好。从这些观点考虑,酸酐优选为2-辛烯基琥珀酸酐。
作为肼化合物,可列举例如:单盐酸肼、二盐酸肼、单氢溴酸肼、碳酸肼、己二酸二酰肼、癸二酸二酰肼、十二烷二酰肼、间苯二甲酸二酰肼、丙酸酰肼、水杨酸酰肼、羟基-2-萘酸酰肼、二苯甲酮腙、3-羟基-2-萘酸酰肼、二苯甲酮腙、或聚丙烯酸酰胺型水***联剂等。
作为三氟化硼络合物,可列举例如:三氟化硼乙基醚络合物、三氟化硼甲醚络合物、三氟化硼乙基甲醚络合物、三氟化硼丁醚络合物、三氟化硼苯酚络合物、三氟化硼烷基胺络合物、三氟化硼氨络合物、三氟化硼哌啶络合物、三氟化硼三乙醇胺络合物、三氟化硼醇络合物、三氟化硼酮络合物、三氟化硼醛络合物、三氟化硼酯络合物、三氟化硼酸酐络合物、或三氟化硼酸络合物等。
作为二氰基二酰胺化合物,可列举例如:二氰基二酰胺、邻甲苯基缩二胍、二苯基缩二胍等。
作为氨基氰化合物,可列举例如:单甲基氨基氰、单乙基氨基氰、单丙基氨基氰、单丁基氨基氰、二甲基氨基氰、二乙基氨基氰、二丙基氨基氰、二丁基氨基氰、六亚甲基二氨基氰、七亚甲基二氨基氰、八亚甲基二氨基氰、九亚甲基二氨基氰、或十亚甲基二氨基氰等。
作为咪唑化合物,可列举例如:咪唑、1-甲基咪唑、2-甲基咪唑、3-甲基咪唑、4-甲基咪唑、5-甲基咪唑、1-乙基咪唑、2-乙基咪唑、3-乙基咪唑、4-乙基咪唑、5-乙基咪唑、1-正丙基咪唑、2-正丙基咪唑、1-异丙基咪唑、2-异丙基咪唑、1-正丁基咪唑、2-正丁基咪唑、1-异丁基咪唑、2-异丁基咪唑、2-十一烷基-1H-咪唑、2-十七烷基-1H-咪唑、1,2-二甲基咪唑、1,3-二甲基咪唑、2,4-二甲基咪唑、2-乙基-4-甲基咪唑、1-苯基咪唑、2-苯基-1H-咪唑、4-甲基-2-苯基-1H-咪唑、2-苯基-4-甲基咪唑、1-苄基-2-甲基咪唑、1-苄基-2-苯基咪唑、1-氰乙基-2-甲基咪唑、1-氰乙基-2-乙基-4-甲基咪唑、1-氰乙基-2-十一烷基咪唑、1-氰乙基-2-苯基咪唑、2-苯基-4,5-二羟基甲基咪唑、2-苯基-4-甲基-5-羟基甲基咪唑、或1-氰乙基-2-苯基-4,5-二(2-氰乙氧基)甲基咪唑等。
作为光致产酸剂,可列举例如:[4-(4-乙酰基)苯基硫基]苯基二苯基锍三(五氟乙基)三氟磷酸酯、[4-(4-乙酰基)苯基硫基]苯基二苯基锍四(五氟苯基)硼酸酯、[4-(4-乙酰基)苯基硫基]苯基二苯基锍三(三氟甲磺酰基)甲基化物、[4-(4-乙酰基)苯基硫基]苯基二苯基锍六氟锑酸盐、[4-(4-乙酰基)苯基硫基]苯基二苯基锍六氟磷酸酯、[4-(4-乙酰基)苯基硫基]苯基二苯基锍三氟甲磺酸酯、[4-(4-乙酰基)苯基硫基]苯基二苯基锍九氟丁磺酸酯、[4-(4-乙酰基)苯基硫基]苯基二苯基锍甲磺酸酯、[4-(4-乙酰基)苯基硫基]苯基二苯基锍丁磺酸酯、[4-(4-乙酰基)苯基硫基]苯基二苯基锍樟脑磺酸酯、[4-(4-乙酰基)苯基硫基]苯基二苯基锍对甲苯磺酸酯及[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍三(五氟乙基)三氟磷酸酯、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍四(五氟苯基)硼酸酯、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍三(三氟甲磺酰基)甲基化物、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍六氟锑酸盐、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍六氟磷酸酯、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍三氟甲磺酸酯、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍九氟丁磺酸酯、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍甲磺酸酯、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍丁磺酸酯、[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍樟脑磺酸酯、或[4-(4-苯甲酰基)苯基硫基]苯基二苯基锍对甲苯磺酸酯等。
作为光致产碱剂,不仅可列举例如:α-氨基苯乙酮化合物、肟酯化合物、或酰氧基亚胺基,N-甲酰化芳香族氨基、N-酰化芳香族氨基、硝基苄基氨基甲酸酯基、或者烷氧基苄基氨基甲酸酯基等具有取代基的化合物叔胺,还可列举脒/胍的羧酸盐、硼酸酯、氨基甲酸酯、或酰胺系化合物等。
作为具体的化合物,优选2-甲基-1-(甲基硫基苯基)-2-吗啉代丙烷-1-酮、2-苄基-2-二甲基氨基-1-(4-吗啉代苯基)-丁酮、2,2-(二甲基氨基)-2-[(4-甲基苯基)甲基]-1-[4-(4-吗啉基)苯基]-1-丁酮、1,2-辛二酮,1-[4-(苯基硫基)苯基]-,2-(邻苯甲酰基肟)(BASF公司制Irgacure OXE01,1,2-octanedione,1-[4-(phenylthio)phenyl]-,2-(o-benzoyloxime))、乙酮,1-[9-乙基-6-(2-甲基苯甲酰基)-9H-咔唑3-基]-,1-(邻乙酰基肟)(BASF公司制Irgacure OXE02,Ethanone,1-[9-ethyl-6-(2-methylbenzoyl)-9H-carbazol-3-yl]-,1-(O-acetyloxime)、(2E)-2-(苯甲酰基肟基)-1-[4-(苯基硫基)苯基]辛烷-1-酮、二-N-(对甲酰基氨基)二苯基己烷、二-N(对乙酰基氨基)二苯基甲烷、二-N-(对苯甲酰胺)二苯基甲烷、4-甲酰基氨基芪、4-乙酰基氨基芪、2,4-二甲酰基氨基芪、1-甲酰基氨基萘、1-乙酰基氨基萘、1,5-二甲酰基氨基萘、1-甲酰基氨基蒽、1,4-二甲酰基氨基蒽、1-乙酰基氨基蒽、1,4-二甲酰基氨基蒽醌、1,5-二甲酰基氨基蒽醌、3,3’-二甲基-4,4’-二甲酰基氨基联苯、4,4’-二甲酰基氨基二苯甲酮、双{{(2-硝基苄基)氧基}羰基}二氨基二苯基己烷、2,4-二{{(2-硝基苄基)氧基}芪、双{{(2-硝基苄基氧基)羰基}己烷-1,6-二胺、间二甲基苯胺{{(2-硝基-4-氯苄基)氧基}酰胺}、)9-二蒽醌甲基N,N-二甲基氨基甲酸酯、(E)-1-哌啶基-3-(2-羟基苯基)-2-丙烷-1-酮、1-(蒽醌-2-基)乙基咪唑羧酸酯、(2-硝基苯基)甲基4-[(2-甲基丙烯酰氧基]哌啶-1-羧酸酯、1,2-二异丙基-3-[双(二甲基氨基)亚甲基]胍2-(3-苯甲酰基苯基)丙酸酯、或1,2二环己基-4,4,5,5-四甲基双胍正丁基三苯基硼酸酯。
这些中,从与导电性糊组合物的配合、单组分化时的储存稳定性、固化活性、或对导电性填料的耐腐蚀性的方面考虑,特别优选2-辛烯基琥珀酸酐、癸二酸二酰肼、1-甲基咪唑。
另外,在将(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料合计设为100重量份的情况下,(C)交联剂为1重量份以上且20重量份以下,优选为1.5重量份以上且8重量份以下,更优选为2重量份以上且7重量份以下。
交联剂小于1重量份时,固化性变得不充分。另一方面,交联剂大于20重量份时,会导致翘曲的发生或储存稳定性的降低。
<(D)导电性填料>
作为导电性填料中所含的导电性粒子,可列举例如:银粉末、氧化银粉末、碳酸银粉末、乙酸银粉末、银涂层粉末、含银合金粉末、镍粉末、铜粉末、或铝粉末等。另外,可以将它们单独使用或混合2种以上使用。需要说明的是,在银粉末的情况下,优选由含量70质量%以上的银形成导电性粒子。
作为导电性填料的烧成温度,考虑到对电气/电子电路用的膜基材的应用,优选为200℃以下,更优选为150℃以下。需要说明的是,在导电性粒子为银的情况下,即使不设为还原性气氛,也不会因表面氧化而导致导电性降低。
另外,导电性粒子的平均粒径对烧结特性造成影响。粒径大的导电性粒子与粒径小的导电性粒子相比,以更缓慢的速度烧结。因此,平均粒径优选为0.1μm以上且15μm以下。这是因为平均粒径小于0.1μm时,烧结速度过快,物理粘接强度不足,另一方面,平均粒径大于15μm时,烧结速度变得稍微缓慢,但导电性糊组合物中的分散性及印刷性变差,微细的印刷变得困难。
另外,导电性粒子的比表面积优选为0.05m2/g以上且5m2/g以下。这是因为导电性粒子的比表面积小于0.05m2/g时,粒径大,不能描绘细线,另一方面,导电性粒子的比表面积大于5m2/g时,粘度调整需要大量溶剂等,操作性变差。
需要说明的是,导电性粒子的形状可以为鳞片状、球形、片状、无规状或将它们混合而成的形状。
另外,在将(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料合计设为100重量份的情况下,(D)导电性填料为70重量份以上且95重量份以下,优选为80重量份以上且93重量份以下,更优选为85重量份以上且91重量份以下。
导电性填料小于70重量份时,配合量过少,烧成而得到的电极的固有电阻上升。另一方面,导电性填料大于95重量份时,导电性糊组合物的印刷性变差,对粘贴对象物的粘接强度不足。
<(E)脱水剂>
可以在导电性糊组合物中添加脱水剂。在导电性糊组合物的制作中,在对(A)粘合剂添加(B)环氧单体、(C)交联剂、及(D)导电性填料中的任一种之前,对(A)粘合剂添加脱水剂。或者对(D)导电性填料添加(E)脱水剂之后,进一步添加(A)粘合剂、(B)环氧单体、及(C)交联剂。如此地添加脱水剂时,水分通过化学反应变化成其它化合物,因此,以单组分型制备的导电性糊组合物的储存稳定性。(E)脱水剂可以单独使用,也可以组合2种以上使用。
脱水剂可以是非反应性,也可以是反应性。另外,作为脱水剂,可使用作为交联剂例示出的酸酐。然而,与作为交联剂使用的酸酐相比,优选作为脱水剂使用的酸酐为低分子量。另外,在不是酸酐的交联剂的情况下,也优选作为脱水剂的酸酐为低分子量。
通过本发明的导电性糊组合物形成电极时,对基材表现出低内部应力特性的成分是以硅氧烷键为主骨架、且含有多个环氧乙烷环作为有机基团的反应性低聚物、即(A)成分。需要说明的是,是否含有(A)成分、其含量可通过以下的方法分析。
通过在导电性糊组合物100重量份中,以权利要求1所述的一定范围添加(A)成分,容易发挥低内部应力性能。(A)成分的结构、导电性糊组合物中的配合量的分析可通过下述方法进行:将(D)成分通过离心分离法等从导电性糊组合物中分离后,将液态残渣供于气相色谱质谱法、热分解气相色谱质谱法、或液相色谱质谱法等色谱分析,由此对(A)成分进行分析而进行,且可进行定性分析、定量分析。
另外,也可以根据以电极的形式印刷、烧成后的电路分析是否含有(A)成分。具体而言,使用X射线光电子分光方法。更详细而言,使用XPS法(X-ray PhotoelectronSpectroscopy)或ESCA法(Electron Spectroscopy for Chemical Analysis)。作为分析顺序,对电极表面照射X射线,检测反射来的X射线,对官能团的结构进行定性分析。通常,用于导电性糊的一般的环氧树脂不具有硅氧烷骨架,可容易地区分。然而,在烧成后的固化物的情况下,像烧成前的液态导电性糊组合物那样的定量分析方法变得困难。
<流平剂>
为了调整固化时的表面凹凸,可以在导电性糊组合物中添加流平剂。流平剂可以单独使用,也可以组合2种以上使用。
在将导电性糊组合物粘着于对象物的情况下,为了确保导电性糊组合物的涂膜的平滑性、防止折损而添加流平剂。需要说明的是,作为流平剂,有氟系、有机硅系、丙烯酸系、醚系、或酯系,没有特别限定。
<稀释剂>
可在导电性糊组合物中进一步添加与(B)环氧单体不同的稀释剂。另外,该稀释剂可以为非反应性,也可以为反应性。稀释剂可以单独使用,也可以组合2种以上使用。
关于非反应性的稀释剂,没有特别限定,优选可在200℃以下干燥的稀释剂。作为这样的非反应性稀释剂,可列举例如:2-苯氧基乙醇、乙基溶纤剂、丁基溶纤剂、乙酸溶纤剂、丙二醇单甲醚乙酸酯、丁基卡必醇、二乙二醇单丁醚、γ-丁内酯、吡咯烷酮、乙烯基吡咯烷酮、N-甲基-2-吡咯烷酮、二甲基甲酰胺、或二甲基甲酰胺等。
关于反应性的稀释剂,只要是反应性的低分子量化合物,就没有特别限定。作为这样的反应性稀释剂,可列举例如:硅烷偶联剂、(甲基)丙烯酸单体、异氰酸酯化合物、硫醇化合物、乙烯基醚、或氧杂环丁烷化合物等。
需要说明的是,从固化、烧成时的反应性的方面考虑,进一步优选氧杂环丁烷化合物。
作为氧杂环丁烷化合物,可列举例如:双(3-乙基-3-氧杂环丁烷基甲基)醚、双{[1-乙基(3-氧杂环丁烷基)]甲基}醚、1,4-双[〔(3-乙基-3-氧杂环丁烷基)甲氧基〕甲基]苯、1,4-双〔(1-乙基-3-氧杂环丁烷基)甲氧基〕苯、1,3-双〔(1-乙基-3-氧杂环丁烷基)甲氧基〕苯、4,4’-双〔(3-乙基-3-氧杂环丁烷基)甲氧基〕联苯、新戊基二醇双(3-乙基-3-氧杂环丁烷基甲基)醚、聚乙二醇双(3-乙基-3-氧杂环丁烷基甲基)醚、或聚丙二醇双(3-乙基-3-氧杂环丁烷基甲基)醚等2官能氧杂环丁烷化合物等。
<增粘剂>
为了提高对基材的粘接性,可以在导电性糊组合物中添加增粘剂。增粘剂可以单独使用,也可以组合2种以上使用。
从提高对基材的粘接性的观点考虑,作为增粘剂,优选含交联性甲硅烷基化合物、具有极性基团的乙烯基系单体,进一步优选硅烷偶联剂、含有酸性基团的乙烯基系单体。
作为硅烷偶联剂,可使用例如分子中同时具有环氧基、异氰酸酯基、异氰脲酸酯基、氨基甲酸酯基、氨基、巯基、羧基、卤代基、(甲基)丙烯酰基等具有除碳原子及氢原子以外的原子的有机基团和交联性甲硅烷基的硅烷偶联剂。
<填充剂>
为了保证一定的强度,可以在导电性糊组合物中添加除(D)导电性填料以外的填充剂。填充剂可以单独使用,也可以组合2种以上使用。
作为填充剂,只要是除(D)导电性填料以外的填充剂,就没有特别限定,优选结晶性二氧化硅、熔融二氧化硅、白云石、炭黑、碳酸钙、氧化钛、或滑石等。特别是在想要通过这些填充剂得到强度高的固化物的情况下,优选选自结晶性二氧化硅、熔融二氧化硅、硅酸酐、含水硅酸、炭黑、表面处理微细碳酸钙、烧成粘土、粘土、及活性锌白等中的至少1种填充剂。
<触变性赋予剂>
为了防止垂流、提高操作性,可以在导电性糊组合物中添加触变性赋予剂(防垂流剂)。
作为触变性赋予剂,没有特别限定,可列举例如:聚酰胺蜡类;氢化蓖麻油衍生物类;硬脂酸钙、硬脂酸铝、硬脂酸钡等金属皂类等。
需要说明的是,触变性赋予剂可以单独使用,也可以组合2种以上使用。另外,在将(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料合计设为100重量份的情况下,触变性赋予剂优选为0.1重量份以上且20重量份以下。触变性赋予剂的量为上述范围内时,可保持本发明的效果,同时容易确保充分的触变性,且容易根据上述量来调整触变性。
<增塑剂>
为了调整粘度、流动性、或固化情况下的硬度、拉伸强度、或者伸长等机械特性,可以在导电性糊组合物中添加增塑剂。增塑剂可以单独使用,也可以组合2种以上使用。
作为增塑剂,可列举例如:
邻苯二甲酸二丁酯、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二庚酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二异癸酯(DIDP)、邻苯二甲酸丁基苄酯等邻苯二甲酸酯化合物;
1,4-苯二羧酸双(2-乙基己基)酯等对苯二甲酸酯化合物(EASTMAN168(EASTMANCHEMICAL制造));
1,2-环己烷二羧酸二异壬酯等非邻苯二甲酸酯化合物(HexamollDINCH(BASF制造));
己二酸二辛酯、癸二酸二辛酯、癸二酸二丁酯、琥珀酸二异癸酯、乙酰基柠檬酸三丁酯等脂肪族多元羧酸酯化合物;
油酸丁酯、乙酰蓖麻油酸甲酯等不饱和脂肪酸酯化合物;
烷基磺酸苯酯(Mesamoll(LANXESS制造));
磷酸三甲苯酚酯、磷酸三丁酯等磷酸酯化合物;
偏苯三酸酯化合物;
氯化石蜡;
烷基联苯、部分氢化三联苯等烃类油;
加工油;
环氧化大豆油、环氧硬脂酸苄酯等环氧增塑剂;等等。
[导电性糊组合物的制造方法]
导电性糊组合物通过在含有(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料作为原材料、并且根据需要含有其它原材料的状态下进行混炼分散而制造。作为混炼分散方法,没有特别限定,可列举使用例如混炼辊、球磨机、混合器、或行星式搅拌脱泡机的方法等。
需要说明的是,在进行混炼的情况下,需要注意不要使反应性的粘合剂因混炼时的发热而进行交联反应。从稳定性与利用混炼进行的导电性填料分散的平衡的观点考虑,混炼时的温度优选为0℃以上且80℃以下,进一步优选为5℃以上且60℃以下,更进一步优选为10℃以上且50℃以下。
[导电性糊组合物的特性]
如上所述,以上这样的导电性糊组合物例如成为FPD或太阳能电池这样的装置的电极材料。因此,如果是FPD,则导电性糊组合物作为ITO(Indium Tin Oxide)膜上的线状电极使用,作为聚酰亚胺制的FPC(Flexible Printed Circuits)的电路使用。另外,如果是太阳能电池,导电性糊组合物作为硅基板上的集电极使用。特别是在背面电极型太阳能电池中,电极仅形成于硅基板的一个主面上。
在对这样的装置应用时,粘着了导电性糊组合物的对象物(ITO膜、硅基板等)显著受到由该导电性糊组合物的烧成等导致的收缩、以电极的形式完成后起因于该电极的内部应力的影响。然而,以上的导电性糊组合物为低电阻,且在烧成时为低收缩,并且以电极的形式完成后也为低内部应力(参照后述的实施例/比较例)。因此,以上的导电性糊组合物可合适地用作例如经曲面设计的FPD或背面电极型太阳能电池这样的装置的电极材料。
[包含由导电性糊组合物形成的电极的装置]
本发明的装置包含由本发明的导电性糊组合物形成的电极。根据本说明书中的上述记载,作为上述装置,可列举例如:FPD、太阳能电池等。作为上述装置,还可举出例如具备FPD的装置,具体而言,可列举智能手机、平板电脑、薄型电视机、汽车导航***等。
本发明不限定于上述的实施方式,可在权利要求中示出的范围内进行各种变更。即,将在权利要求中示出的范围内进行适宜变更而成的技术方案组合而得到的实施方式也包括在本发明的技术范围内。
实施例
以下,通过实施例具体地进行说明,但本发明不限定于这些实施例。
<粘合剂>
将以下的材料加入具备搅拌机/温度计/回流冷凝器的反应器中,在反应温度105℃下回流8小时,进行反应,得到了缩合物(粘合剂)。
·作为脂环式环氧化合物的2-(3,4-环氧环己基)乙基三甲氧基硅烷(Silquest-A186;Momentive Performance Materials Japan LLC制造):100重量份
·氯化镁(MgCl2;和光纯药(株)制造):0.05重量份
·蒸馏水:11.0重量份
·甲醇(三菱瓦斯化学(株)制造):11.0重量份
使用蒸发器,对得到的缩合物进行减压脱挥及浓缩,使用PGME(1-甲氧基-2-丙醇;(株)大赛璐制造)制备了70重量%溶液。
得到的缩合物利用GPC测定的重均分子量为3200,残存环氧率超过0.9,Y/X比为0.2以下,粘度为500mPa·s(参照下式)。需要说明的是,以上的重均分子量、残存环氧率、Y/X比、粘度通过以下的方法测定。
[化学式1]
(重均分子量)
重均分子量通过GPC测定。即,使用东曹(株)制HLC-8220GPC作为送液***,使用东曹(株)制TSK-GEL H类型作为柱,使用THF作为溶剂,通过聚苯乙烯换算而算出。
(环氧基的残存性评价(残存环氧率))
使用日本电子制JNM-LA400,将重丙酮作为溶剂,对得到的缩合物(粘合剂)进行了1H-NMR测定。将结果作为“残存环氧率”。
(与硅直接键合的OR基的定量(Y/X比))
测定反应前后与硅烷化合物的硅直接键合的OR基,计算出Y/X比。使用日本电子制JNM-LA400,将氘代丙酮作为溶剂,通过1H-NMR及29Si-NMR进行测定,测定了OR的浓度。
(粘度)
粘度使用JISZ8803中记载的B型粘度计来测定。特别地,由于导电性糊组合物为高粘度,因此通过HB型(英弘精机制造)进行测定。
<导电性糊组合物(参照表1)>
[实施例1]
在混合专用容器(内容量470cc、聚丙烯制)中添加以下的原材料,用药匙轻轻地混合后,使用真空式搅拌脱泡机(ARV-310LED;(株)Thinky制造),在2000rpm、真空度30Pa条件下进行1分钟的搅拌脱泡,得到了导电性糊配合物。
·<粘合剂>…上述粘合剂:2.70g
·<环氧单体>…二乙二醇二缩水甘油醚(Epolite 100E;共荣社化学(株)制造、参照下式):7.80g
[化学式2]
·<交联剂>…2-辛烯基琥珀酸酐(东京化成工业(株)制造、参照下述左式):3.80g、及1-甲基咪唑(东京化成工业(株)制造、参照下述右式):0.02g
[化学式3]
·<导电性填料>…银粉(:AY-6080;田中贵金属工业(株)制造):136.50g
[实施例2]
将二乙二醇二缩水甘油醚替换为聚乙二醇二缩水甘油醚(Epolite 200E;共荣社化学(株)制造、参照下式),除此以外,与实施例1同样地制造了导电性糊组合物。
[化学式4]
[实施例3]
将二乙二醇二缩水甘油醚变更为C12、13混合高级醇缩水甘油醚(M-1230;共荣社化学(株)制造、参照下式),重新制成流平剂,并添加氟系分散剂(LE607;共荣社化学(株)制造)0.75g,除此以外,与实施例1同样地制造了导电性糊组合物。
[化学式5]
[实施例4]
将银粉变更为镀银铜粉(TFM-CO2P(球状填料、平均粒径2μm);东洋铝业(株)制造),除此以外,与实施例3同样地制造了导电性糊组合物。
[实施例5]
在实施例5中,除了使用实施例1中使用的原材料以外,使用乙酸酐(东京化成工业(株)制造、化学式:CH3-CO-O-CO-CH3)0.1g作为脱水剂,制造了导电性糊组合物。具体而言,在实施例1中的上述混合专用容器中添加粘合剂和脱水剂,用药匙轻轻地混合后,使用实施例1中的上述真空式搅拌脱泡机,在2000rpm、真空度30Pa条件下进行1分钟的搅拌脱泡,使粘合剂充分脱水。然后,在上述容器中进一步添加环氧单体、交联剂以及导电性填料,用药匙轻轻地混合后,使用上述搅拌脱泡机,在2000rpm、真空度30Pa条件下进行1分钟的搅拌脱泡,得到了导电性糊配合物。
[实施例6]
作为交联剂,使用癸二酸二酰肼(参照下式)代替1-甲基咪唑,并且不使用流平剂,除此以外,与实施例3同样地制造了导电性糊组合物。
[化学式6]
[实施例7]
在上述容器中添加导电性填料和脱水剂,以代替在上述容器中添加粘合剂和脱水剂,使导电性填料充分脱水,以代替使粘合剂充分脱水,在上述容器中进一步添加粘合剂、环氧单体以及交联剂,以代替进一步添加环氧单体、交联剂以及导电性填料,除此以外,与实施例5同样地制造了导电性糊组合物。
[比较例1]
在与实施例相同的混合专用容器中添加以下的原材料,用药匙轻轻地混合后,使用真空式搅拌脱泡机(ARV-310LED;(株)Thinky制造),在2000rpm、真空度30Pa条件下进行1分钟的搅拌脱泡,制造了导电性糊组合物。
·<粘合剂>…双酚A系的树脂(EPICOTE 828;三菱化学(株)制造、参照下式):5.00g
[化学式7]
·<环氧单体>…二氧化柠檬烯(LDO;巴工业(株)制造、参照下式):3.00g
[化学式8]
·<交联剂>…1-甲基咪唑(东京化成工业(株)制造):1.00g
·<导电性填料>…银粉(AY-6080;田中贵金属工业(株)制造):136.50g、
[比较例2]
使用以下的原材料,与比较例1同样地制造了导电性糊组合物。
·<粘合剂>…实施例中使用的粘合剂:8.4g
·<交联剂>…3,4,5,6-四氢邻苯二甲酸酐(东京化成工业(株)制造、参照下式):5.1g、及1-甲基咪唑(东京化成工业(株)制造):0.02g
[化学式9]
·<导电性填料>…银粉136.50g(AY-6080;田中贵金属工业(株)制造)136.5g、
·稀释剂…2-苯氧基乙醇(东京化成工业(株)制造、参照下式):12.00g
[化学式10]
对选择后的实施例及比较例进行以下的测定及评价。需要说明的是,结果记载于下述的表1中。
(电阻值测定)
将导电性糊组合物在玻璃板(尺寸10mm×30mm×2mm厚)上印刷成线宽1mm、厚度55μm的细线后,在130℃下干燥30分钟,进一步在180℃下烧成60分钟。然后,测定对该细线的2mm部分的电阻。需要说明的是,测定使用日置电机株式会社制造的万用表(tester),在23℃条件下以将端子置于细线上的状态实施。
(对铝制基材进行涂敷、干燥、烧成后的该基材翘曲的测定)
将导电性糊组合物均匀地印刷在厚0.1mm、宽25mm、长150mm的铝制基材上,从而达到厚55μm、宽20mm、长145mm,在130℃下干燥30分钟,进一步以180℃烧成60分钟。然后,以水平为基准测定了烧成后的铝制基材端部的翘曲状态。
(对硅基板进行印刷、干燥、烧成后的该基板有无缺损的评价)
使用线宽40μm、厚度15μm的印刷板,将导电性糊组合物在纵横6英寸、180μm厚的硅基板上印刷成条纹(line and space)的集电极图案(线宽55μm×长度153mm、细线间距离2.04mm、厚度12μm)后,在130℃下干燥30分钟,进一步以180℃烧成60分钟。然后评价烧成后的硅基板中有无缺损。
(在ITO膜上进行印刷、干燥、烧成后的该膜的翘曲的测定)
将导电性糊组合物以厚度20μm、Line/Space=100μm/300μm印刷于纵横50mm的ITO膜(下层:PET(厚度50μm)、上层:ITO(20nm))上后,在150℃下进行60分钟的干燥/烧成。然后,以水平为基准测定了烧成后的ITO膜端部的翘曲状态。
(储存稳定性评价)
将导电性糊组合物放入100cc塑料制遮光瓶,在50℃下保存,通过肉眼确认了糊的流动性。
[综合评价]
实施例1~7含有具有多个环氧乙烷环作为有机基团的反应性低聚物作为粘合剂,由此,与含有和该反应性低聚物不同的粘合剂的比较例1相比,在电阻值及铝制基材的翘曲的方面示出优异的结果。另外,实施例1~7与不含环氧单体的比较例2相比,也至少在铝制基材的翘曲的方面示出优异的结果。
另外,将铝制基材翘曲的比较例1、2与未翘曲的实施例1进行比较时,可知导电性糊组合物制的电极发生使铝制基材翘曲程度的收缩,由此使硅基板造成缺损。
另外,还可知在比铝制基材柔软的ITO膜上形成导电性糊组合物制的电极时(参照实施例3/比较例1),由该导电性糊组合物的收缩引起的翘曲容易明显表现。
另外,实施例1、5含有具有多个环氧乙烷环作为有机基团的反应性低聚物作为粘合剂,由此,与含有和该反应性低聚物不同的粘合剂的比较例1相比,在储存稳定性的方面示出优异的结果。另外,在制作导电性糊组合物时,在添加交联剂之前,将体系中(更具体而言将粘合剂)通过低分子量的酸酐事先脱水的实施例5与实施例1相比,储存稳定性示出更优异的结果。
在添加脱水剂的情况下,将脱水剂直接添加于银粉、并事先脱水而制造导电性糊组合物的实施例7与在粘合剂中添加脱水剂并事先脱水的实施例5相比,细线的电阻值更低。由此认为,通过导电性填料的事先脱水,交联剂体系中的反应效率提高,成为更低的电阻值。
另外可知,在将双酚A系环氧树脂作为粘合剂、将脂环式环氧树脂作为环氧单体的比较例1的情况下,成为比较高的电阻,但实施例的含有粘合剂和环氧单体的导电性糊组合物可抑制电阻。
Claims (8)
1.一种导电性糊组合物,其至少含有(A)粘合剂、(B)环氧单体、(C)交联剂、及(D)导电性填料,其中,
(A)粘合剂是以硅氧烷键为主骨架、且含有多个环氧乙烷环作为有机基团的反应性低聚物,
(B)环氧单体含有环氧乙烷环,
在将(A)~(D)合计设为100重量份的情况下,(A)粘合剂为1重量份以上且10重量份以下,(B)环氧单体为2重量份以上且20重量份以下,(C)交联剂为1重量份以上且20重量份以下,(D)导电性填料为70重量份以上且95重量份以下。
2.根据权利要求1所述的导电性糊组合物,其中,
(B)环氧单体含有选自具有二醇结构的2官能单体及具有脂肪族结构的单官能单体中的至少1种。
3.根据权利要求1或2所述的导电性糊组合物,其中,
(C)交联剂为具有潜热性的化合物。
4.根据权利要求1~3中任一项所述的导电性糊组合物,其中,
(C)交联剂含有选自咪唑化合物、肼化合物、及酸酐中的至少1种。
5.根据权利要求1~4中任一项所述的导电性糊组合物,其进一步含有(E)脱水剂。
6.根据权利要求5所述的导电性糊组合物,其中,
(E)脱水剂为酸酐。
7.一种装置,其包含由权利要求1~6的中任一项所述的导电性糊组合物形成的电极。
8.一种导电性糊组合物的制造方法,该导电性糊组合物至少含有(A)粘合剂、(B)环氧单体、(C)交联剂、(D)导电性填料、及(E)脱水剂,
(A)粘合剂是以硅氧烷键为主骨架、且含有多个环氧乙烷环作为有机基团的反应性低聚物,
(B)环氧单体含有环氧乙烷环,
在将(A)~(D)合计设为100重量份的情况下,(A)粘合剂为1重量份以上且10重量份以下,(B)环氧单体为2重量份以上且20重量份以下,(C)交联剂为1重量份以上且20重量份以下,(D)导电性填料为70重量份以上且95重量份以下,
在该制造方法中,
在对(A)粘合剂添加(B)~(D)中的任一者之前,对(A)粘合剂添加(E)脱水剂;或者
在对(D)导电性填料添加了(E)脱水剂之后,进一步添加(A)~(C)。
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JPH07161740A (ja) * | 1993-12-02 | 1995-06-23 | Sumitomo Bakelite Co Ltd | 半導体用導電性樹脂ペースト |
JPH08176409A (ja) * | 1994-12-26 | 1996-07-09 | Sumitomo Bakelite Co Ltd | 導電性樹脂ペースト |
JPH09176607A (ja) * | 1995-12-22 | 1997-07-08 | Sumitomo Bakelite Co Ltd | 半導体用導電性樹脂ペースト |
JPH11286630A (ja) * | 1998-04-03 | 1999-10-19 | Asahi Chem Ind Co Ltd | ビア充填用導電性ペースト組成物 |
CN101111580A (zh) * | 2004-12-28 | 2008-01-23 | 琳得科株式会社 | 涂层用组合物、硬涂膜及光记录介质 |
CN101248525A (zh) * | 2005-06-07 | 2008-08-20 | 莫门蒂夫功能性材料公司 | 可b阶化的膜、电子装置和相关方法 |
CN101506321A (zh) * | 2006-08-22 | 2009-08-12 | 日立化成工业株式会社 | 电路连接材料、电路部件的连接结构及电路部件的连接结构的制造方法 |
JP2014088466A (ja) * | 2012-10-29 | 2014-05-15 | Yokohama Rubber Co Ltd:The | 導電性組成物および太陽電池セル |
CN104736641A (zh) * | 2012-10-29 | 2015-06-24 | 横滨橡胶株式会社 | 导电性组合物及太阳能电池单元 |
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WO2018216814A1 (ja) | 2018-11-29 |
JP6734476B2 (ja) | 2020-08-05 |
JPWO2018216814A1 (ja) | 2020-01-16 |
US11066509B2 (en) | 2021-07-20 |
CN110651336B (zh) | 2022-05-17 |
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