CN100396367C - 分散体在制备电子元件中的应用 - Google Patents

分散体在制备电子元件中的应用 Download PDF

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CN100396367C
CN100396367C CNB2004800060223A CN200480006022A CN100396367C CN 100396367 C CN100396367 C CN 100396367C CN B2004800060223 A CNB2004800060223 A CN B2004800060223A CN 200480006022 A CN200480006022 A CN 200480006022A CN 100396367 C CN100396367 C CN 100396367C
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D·泰特福特
J·D·斯科菲尔德
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Abstract

用于制备电容器、印刷电路板等的分散体，其包括电子颗粒固体、载体和通式(1)的分散剂：R-(O-A-CO)x(O-B-CO)y-Z，其中R为氢或聚合终端基团；A为C8-20-亚烷基和/或C8-20-亚烯基；B为C1-6-亚烷基或其内酯；Z为羟基或碱性基团或含有碱性基团的部分；x为2-45；y为0-15；并且x∶y的比不小于3∶1，载体为沸点为150-350℃的高沸点有机液体，选自一元醇和二亚烷基二醇单烷基醚的酯。

Description

分散体在制备电子元件中的应用
技术领域
本申请公开了一种改进的分散剂，其用于分散用于制备电容器、印刷电路板和类似电子元件的介电材料和导体金属材料，其中由介电材料分隔的各种类型的导体通道是非常有用的。
背景技术
WO94/21368公开了与这里所述分散剂类似的各种分散剂。
发明内容
使用分散剂制备电子元件，其中所述分散体包含电子颗粒固体、载体和具有如下通式的分散剂：
R-(O-A-CO)x(O-B-CO)y-Z    1
其中：
R为氢或聚合终端集团；
A为C8-20-亚烷基和/或C8-20-亚烯基；
B为C1-6-亚烷基，例如可以由内酯衍生的(O-B-CO)；
Z为羟基或碱性基团或含有碱性基团的部分；
x为2-45；
y为0-15；
并且x∶y的比不小于3∶1。
由R-(O-A-CO)x(O-B-CO)y-表示的聚酯链可以是嵌段的或优选为无规的，并且由(O-A-CO)或(O-B-CO)表示的任一部分均可以与R直接相连。但优选的是基团(O-A-CO)与R相连。
具体实施方式
本发明涉及一定的含有分散体在载体中的电子颗粒固体的用途，以及应用这类分散体来制备电子元件如电容器和印刷电路板。
多层陶瓷电容器为本领域所周知，其通常通过如下方法来制备：向基质上施涂细小分散的介电材料，并向其上叠加一层以希望形式存在的细小分散的导体金属层如银以用作电容器电极或电容器板。多层陶瓷电容器由交替的介电材料层和导体材料层制成，两个最外层由介电材料组成。然后在介电材料的熔融或烧结温度下，烧制由交替的介电材料和导体材料组成的复合夹层物，操作通常在压力下进行，从而形成整块的电容器结构。在该熔融或烧结过程中，所应用的在不同层中均匀分配介电材料和导体材料的多种组分被″烧掉″了。介电层和导体层通常由介电材料和导体材料在载体中的分散体来制备，而所述载体通常为非极性有机液体。为了在载体中均匀地分配电子颗粒固体，优选应用分散剂，并且必须仔细地选择该分散剂，从而避免载体中电子颗粒固体的分离，并在随后的烧制过程中有效脱除。
现在已经发现在制备电子电容器所应用的非极性有机液体载体中分散电子颗粒固体时应用由蓖麻油酸和聚乙烯亚胺衍生的聚酯胺分散剂是特别有效的，并且这种分散剂随后可以在烧制过程中被脱除而对最终的电容器不产生任何有害影响。
按照本发明，提供分散体在生产电子元件中的应用，其中所述分散体包含电子颗粒固体、载体和具有如下通式1的分散剂：
R-(O-A-CO)x(O-B-CO)y-Z    1
其中：
R为氢或聚合终端集团；
A为C8-20-亚烷基和/或C8-20-亚烯基；
B为C1-6-亚烷基，例如可以由内酯衍生的(O-B-CO)；
Z为羟基或碱性基团或含有碱性基团的部分；
x为2-45；
y为0-15；
并且x∶y的比不小于3∶1。
由R-(O-A-CO)x(O-B-CO)y-表示的聚酯链可以是嵌段的或优选为无规的，并且由(O-A-CO)或(O-B-CO)表示的任一部分均可以与R直接相连。但优选的是基团(O-A-CO)与R相连。
x∶y的比优选不小于5∶1，更优选不小于8∶1，并且特别为不小于10∶1。特别优选y为零。
当R为聚合物终端基团时，其优选为羧酸R1-COOH的残基，其中R1可以为芳基、杂芳基、环烷基或优选为烷基，并且其可以被卤素、C1-6-烷氧基、氨基或醚基所取代。R1优选未被取代。当R1为烷基时，其可以为直链或支链的饱和或不饱和的，但优选为饱和的。
R中的碳原子总数可以高达50，但优选的是R中的碳原子不小于8个，更优选为不小于12个，特别为不小于14个。另外优选的是R的碳原子数不大于30个，更优选为不大于24个，并且特别为不大于20个。
具有通式R1-COOH的羧酸的例子有乙酸、甲氧基乙酸、己酸、油酸、月桂酸、癸酸、十二烷酸、硬脂酸和棕榈酸。支链烷基羧酸的例子有2-乙基丁酸、2-乙基己酸、2-丁基辛酸、2-己基癸酸、2-辛基十二烷酸和2-癸基十四烷酸。支链脂族酸也可以以商标名Isocarb(得自Sasol)获得，并且具体的例子有Isocarb 12、16、20、28、32、34T和36。也可以应用羧酸的混合物。由基团(CO-A-O)表示的不饱和羟基羧酸可以含有烷基或烯基羧酸，并且这些可以用作聚合终端基团。当羟基羧酸衍生自天然产品时，这一点特别正确。
A优选含有不小于12个碳原子，并且特别为不小于14个碳原子。可以衍生得到基团(CO-A-O)的羟基羧酸的例子有蓖麻油酸、12-羟基硬脂酸、12-羟基十二烷酸、5-羟基十二烷酸、5-羟基癸酸和4-羟基癸酸。特别优选的是(CO-A-O)为蓖麻油酸的残基。
由B表示的亚烷基残基可以是直链的或支链的。(CO-B-O)由其衍生得到的羟基羧酸的例子有羟基乙酸、6-羟基己酸和5-羟基戊酸。
内酯的例子有β-丙醇酸内酯和任选烷基取代的ε-己内酯和任选烷基取代的δ-戊内酯。烷基取代基优选为C1-6-烷基，特别为C1-4-烷基，其可以是直链的或支链的。烷基取代的ε-己内酯可以按WO98/19784中所描述的通过烷基取代的环己酮的氧化得到。其例子包括7-甲基-、3-甲基-、5-甲基-、6-甲基-、4-甲基-、5-叔丁基-、4，6，6-三甲基-和4，4，6-三甲基ε-己内酯。烷基取代的戊内酯的例子为β-甲基-δ-戊内酯。优选的内酯为ε-己内酯和δ-戊内酯。
可以应用羟基羧酸和内酯的混合物。
y优选不大于6，更优选不大于4，甚至更优选不大于2，特别为零。
聚酯链R-(O-A-CO)x(O-B-CO)-与Z的重量比优选不小于5，并且特别为不小于8。还优选的是聚酯链与Z的重量比不大于30，更优选为不大于20，并且特别为不大于15。特别有用的分散剂为那些聚酯链R-(O-A-CO)x(O-B-CO)y-与Z的重量比为8-15的分散剂。
Z优选为聚胺或聚亚胺的残基，如聚烯丙基胺、聚乙烯基胺，更优选为聚(C2-4-亚烷基亚胺)(下文称为PAI)，更特别为聚(亚乙基亚胺)(下文称为PEI)。
直链聚亚乙基亚胺可以按Takeo Saegusa等在Macromolecular，1972，第5卷，第4470页中所述通过聚(N-酰基)亚烷基亚胺的水解而制备。分子量不同的支链聚亚乙基亚胺可以由BASF和Nihon Shokubai得到。分子量不同的聚烯丙基胺和聚(N-烷基)烯丙基胺可以由NittoBonseki得到。聚乙烯基胺可以由Mitsubishi Kasei得到。聚(亚丙基亚胺)枝状聚合物(dendrimer)可以由DSM Fine Chemicals得到，而聚(氨基胺)枝状聚合物可作为″Starburst″枝状聚合物由AldrichChemical Company得到。
聚胺或聚亚胺优选具有500-600,000的重均分子量，更优选为1,000-200,000，甚至更优选为1,000-100,000，特别是1,000-70,000。
由R-(O-A-CO)x(O-B-CO)y-表示的聚酯部分的数均分子量优选为600-4,000，并且特别为800-2,000。
由R-(O-A-CO)x(O-B-CO)y-表示的聚酯链部分可以与聚胺或聚亚胺组分Z通过在聚酯链的终端羰基和聚胺或聚亚胺中的伯或仲胺基的氮原子之间形成的共价酰胺基团-CON＝相连，或者通过在聚酯链的终端羧酸基团和聚胺或聚亚胺中的铵基之间形成的盐连接-COO-HN+≡相连。
分散剂优选含有多个与聚胺或聚亚胺相连的聚酯链，并因而依据反应器条件的苛刻程度可以含有酰胺和盐连接的混合物。
分散剂也可以适宜地由通式2表示：
其中：
X-x-x-X代表聚胺或聚亚胺；
Y代表聚酯链部分R-(O-A-CO)x(O-B-CO)y-；并且
q为4-2,000。
q优选为不小于10。另外优选的是q不大于1,000，并且特别为不大于500。
分散剂可以通过本领域已知的任意方法制备，并且更典型按WO94/21368所述方法制备。
分散体中的电子颗粒固体可以是任何的介电固体或导电固体，包括它们的混合物，这些固体在电子或电器元件的制备中应用。
导电固体优选为金属，其可以为粉末状也可以为薄片状，但优选为微粉化的粉末。金属的粒度优选不大于3μ，并且特别为不大于1μ。导电金属的例子有铜、银、金、钯、铂、钌、铑、锇、铱和镍，以及它们的混合物和合金。
镍和银是优选的金属。
介电固体可以是任何不导电的固体，并且优选为金属氧化物或含氧的无机金属衍生物。合适的介电固体的例子有玻璃、钛酸钡、锆酸铅、锡酸铋、二氧化钛、铌酸铅镁、氧化铅、碳酸钾、碳酸镁、碳酸锂、硝酸锶、钛酸钡锶、三氧化二铋和氧化铝，以及它们的混合物。通常，可以应用能够熔融或烧结以提供连续介电层的任何不导电的固体。介电固体的粒度在天然态时可能相当粗，但是当与导电金属一起加入分散体中时，粒度优选为不大于5μ，更优选为不大于3μ，特别为不大于1μ。
分散体中的载体为有机液体，或优选为不含水的有机液体的混合物。有机液体可以具有极性，或优选为非极性的，并且特别为沸点为150-350℃的高沸点有机液体。沸点优选不小于180℃并且特别为不小于200℃。还优选的是沸点不大于300℃，并且特别为不大于280℃。
优选的高沸点有机液体有一元醇如辛醇、癸醇、十二烷醇、十四烷醇、松油醇(包括其立体异构体)和二亚烷基二醇单烷基醚如二乙基二醇单烷基醚，特别是C1-6-单烷基醚如二亚乙基二醇单丁基醚。其它优选的高沸点有机液体有二亚烷基二醇单烷基醚的酯，如丁基卡必醇乙酸酯(2-(2-丁氧基乙氧基)乙基乙酸酯)。
松油醇是优选的高沸点有机液体。
为了处理方便，分散剂优选制成载体中的溶液。因此，按照本发明的另一个方面，提供一种组合物，该组合物包括沸点为150-350℃的高沸点有机液体和通式1的分散剂。
高沸点有机液体优选为芳烃如萘(naptha)，或优选为一元醇，并且特别为松油醇，包括其异构混合物。
组合物可进一步包括电子颗粒固体，所述电子颗粒固体优选为金属和/或介电固体。优选的金属为银和镍。优选的介电固体为钛酸钡。
以组合物的总量为基准，组合物中电子颗粒固体的量优选为20-90％。还优选的是以组合物的总量为基准，电子颗粒固体的量不小于40％，更特别为不小于50％。特别有用的组合物为那些含50-70％电子颗粒固体的组合物。
以电子颗粒固体的量为基准，组合物中分散剂的量可以在很宽的范围内变化，但优选为1-150％。以电子颗粒固体的量为基准，分散剂的量优选为不大于100％，更优选为不大于50％，特别为不大于20％。已经发现有用的分散体中分散剂的量为电子颗粒固体的2-10％。
通过加入其它助剂如粘结剂树脂也可以调节组合物的粘度，从而使组合物适应于特定的最终用途。
粘结剂树脂优选在载体中可溶。粘结剂树脂优选衍生自天然产品如松香或纤维素。合适的粘结剂树脂的例子有加氢松香、加氢松香的甘油酯、乙基纤维素和乙基羟基乙基纤维素。
因此，当组合物用作印刷油墨时，特别是丝网印刷油墨以在电子元件中产生导电轨迹如印刷电路板(PCBs)、电容器及类似物时，优选包括粘结剂树脂。粘结剂树脂的量优选为载体或液相重量的10-40％，这等价于组合物总重量的4-16％。
当组合物用于制备应用丝网印刷技术的导电轨迹时，其优选构成粘稠油墨，并且这种油墨具体在25℃下具有10,000-70,000cps的粘度。油墨优选还含有惰性有机液体如脂族烃，特别是含有6-16个碳原子的烃。脂族烃的例子有汽油、己烷、庚烷、辛烷、癸烷、十二烷、十六烷，特别是煤油。油墨中惰性有机液体的量优选为浆液重量的40-65％。
惰性有机液体指与介电基质表面不发生相互作用、从而不影响其表面整体性的任何有机液体。惰性有机液体优选具有50℃至小于150℃的沸点。
对本领域的熟练技术人员来说，还明显的是油墨的粘度可以适宜地变化，从而使其更适合于苯胺印刷和喷墨印刷如按需喷墨印刷。
通常通过在高沸点有机液体中溶解分散剂和粘结剂树脂按需加热而制备油墨。当冷却至20-25℃后，加入电子颗粒固体如镍或银，如果需要，随后再加入脂族有机液体。然后可以应用合适的分散方法如球磨、珠磨、高剪切混合或超声波降解。然后通过工业上已知的任意合适方法如丝网印刷向介电基质上施用油墨，以产生前体导电轨迹。在使介电基质加热到600-1200℃的温度之前，任选通过蒸发脱除惰性有机液体，在此过程中，载体被烧掉而导电颗粒固体被熔融，从而在介电基质的表面上形成导电轨迹。根据需要，通过重复丝网印刷技术和/或应用其它材料通过电子沉积可以增加导电通道的厚度。
组合物也可以用作焊料，通过在组件如电阻器、电容器等的电接触点上施用组合物而在制备电子元件如PCB应用的各组件间形成电连接。类似地，也可以应用组合物通过用组合物填充通道而在不同的导电轨迹间形成电连接。通过按上面所描述在高温下烧制可以形成电桥。
组合物也可以用于制备电容器，其中将组合物施用在″湿的″柔性介电体或基质上或烧制的硬介电基质上。
当用于介电基质时，术语″湿的″指一种基质，其尚未暴露在导致形成介电基质的介电颗粒固体一起熔融或烧结的高温下。湿介电基质通常以自支撑柔性片的形式存在，其中介电颗粒固体通过聚合有机粘结剂聚集在一起。湿介电基质用上述含有导电电子颗粒固体(例如金属)的组合物进行印刷。然后印刷后的介电基质被切割成区，并且各区以重叠层的形式排布，从而导电印刷轨迹对交替层来说在同一侧凸起，而顶层没有印刷轨迹。随后各层在300-2000psi的压力下压缩，然后在600-1200℃的高温下烧制，从而形成具有凸起电接触点的单块电容器。
当电容器含有相对较少量的被介电材料包围的导电层如两层时，电容器被称为包埋式的，这种包埋式电容器也可用本发明的分散体来制备。
本组合物也可以施用到烧制的硬介电基质上。但是，在这种情况下，组合物可能含有较高浓度的高沸点有机液体，这是因为相对于湿基质而言，烧制的基质对这种有机液体有更强的耐受性。当在烧制的介电基质上施用组合物时，通常有利的是包含高达组合物重量20％的介电颗粒固体，从而在烧制之后，导电电子颗粒固体形成导体，这种导体保持在熔融或烧结的介电材料体内。烧制的介电材料可以以无机碎片的形式存在。
也可以应用组合物来提供为车辆生产中应用的玻璃除雾的加热元件。
当电子颗粒固体为介电材料如钛酸钡时，组合物可用于通过非导电性粘附作用而将电子组件固定于基质如PCB上。组合物可以含有前文所述的粘结剂树脂和惰性有机液体。烧制后，在电子组件和基质之间形成不导电的焊接。
含有介电材料的组合物可以施用在基质的局部或整个表面上。当施用到整个表面上时，可以通过刮刀有利地施用组合物。当局部施用时，在适当调节粘度后，可以以油墨形式有用地施用组合物。
下面参考实施例更为详细地描述本发明，其中如不另外说明，所有参数均为重量份。
在实施例中应用的分散剂
  分散剂   聚酯链(PC)   聚亚胺(PI)   PC∶PI的比
  1   PHS   SP200   10∶1
  2   PRA   SP200   10∶1
  3   RA∶Cap(4∶1)   SP200   9∶1
  4   PHS   -   -
  5   PRA   -   -
  6   PRA   -   -
  7   RA∶HSA(1∶1)   SP200   14∶1
  8   PRA   SP200   18∶1
  9   PRA   SP200   20∶1
  10   PRA   SP050   7∶1
在上表中，PHS为聚(12-羟基硬脂酸)，PRA为聚蓖麻油酸，RA为蓖麻油酸，cap为ε-己内酯，HSA为12-羟基硬脂酸，SP200为数均分子量为10,000的聚亚乙基亚胺，而SP050为数均分子量为5000的聚亚乙基亚胺。
对分散体3来说，在聚酯链列中括号中的数字表示聚酯链中蓖麻油酸与ε-己内酯的摩尔比。PC∶PI列中的数字表示聚酯链与聚亚乙基亚胺的重均比。
分散剂1-10均以类似于WO 94/21368中所述的方法来制备。分散体4等同于聚酯A，其制备在WO 94/21368中也有描述。分散剂5和6应用与WO 94/21368中描述的制备聚酯A类似的方法进行制备。分散剂5的分子量为870。分散剂6的分子量为1100。分散剂7的聚酯链的分子量为1600，其以1∶1的摩尔比含有蓖麻油酸和12-羟基硬脂酸。分散剂8和9的聚酯链的分子量为1100。分散剂10的聚酯链的分子量为1600。
实施例1-12
在松油醇异构体(250份，得自Fisher)的混合物中通过在120℃下在氮气气氛下一起搅拌1小时而溶解分散剂(250份)。在冷却至20℃后，通过在应用更多的松油醇稀释的松油醇中的分散剂溶液中研磨电子颗粒固体而制备分散体，其中在3mm直径的玻璃balatini珠(17份)的存在下应用水平混合器研磨16小时。应用任意刻度A-D(好到差)通过手摇评价分散体的粘度。结果在下列1A中给出。
表1A
  实施例   分散剂   分散剂的量   Ni   BaTiO<sub>3</sub>   松油醇稀释剂   粘度
  1   1   0.2   7   -   2.8   B/C
  2   2   0.2   7   -   2.8   C
  3   3   0.2   7   -   2.8   B/C
  4   4   0.2   7   -   2.8   B
  A   -   -   7   -   3.0   C/D
  5   1   0.2   -   5   4.8   A/B
  6   2   0.2   -   5   4.8   B
  7   3   0.2   -   5   4.8   A/B
  8   4   0.2   -   5   4.8   A/B
  B   -   -   -   5   5   D
  9   1   0.2   -   6   3.8   B/C
  10   2   0.2   -   6   3.8   C
  11   3   0.2   -   6   3.8   B/C
  12   4   0.2   -   6   3.8   B/C
  13   8   0.1   7   -   2.9   B/C
  14   10   0.1   7   -   2.9   B/C
  15   7   0.1   7   -   2.9   B/C
  16   8   0.1   5   4.9   A/B
  17   10   0.1   5   4.9   A/B
  18   7   0.1   5   4.9   A/B
  19   6   0.1   5   4.9   A/B
  20   9   0.1   5   4.9   A/B
  C   -   0   5   5   D
对表1的注释：
分散剂的量为在松油醇的异构体混合物中分散剂的50/50w/w混合物。
Ni粉末为由Aldrich得到的粒度小于1μ的微粉化粉末。
BaTiO3为由Aldrich得到的粒度小于1μ的微粉化钛酸钡。
表1B
  实施例   分散剂   分散剂的量   氧化铈   松油醇稀释剂   粘度
  D   -   -   2.5   7.5   B/C
  21   4   0.1   2.5   7.4   A/B
  22   7   0.1   2.5   7.4   A/B
  23   3   0.2   2.5   7.33   A/B
  24   4   0.2   2.8   7   B
氧化铈为由Aldrich得到的微粒化的物质。
MEL3/氧化锆由MEL Chemicals得到。
Okamoor Silica HPF2由Hepworth Minerals & Chemicals得到。
Alumina AE511C由Sumitomo得到。
表1C
  实施例   分散剂   分散剂的量 MEL氧化锆   二氧化硅   松油醇稀释剂   粘度
  F   -   - 4   -   6   C
  25   5   0.1 4   -   5.9   A/B
  26   9   0.1 4   -   5.9   A/B
  G   -   - -   4.5   5.5   B
  27   7   0.1 -   4.5   5.4   A/B
表1D
  实施例   分散剂   分散剂的量   SumitomoAlumina AESIIC   松油醇稀释剂   粘度
  1   -   -   5   5   B/C
  2   10   0.1   5   4.9   B
  3   9   0.1   5   4.9   B
实施例1-4、9-12、A和B的粘度也在脱除玻璃珠后，在20℃下，应用配备有4cm圆锥、在57μm间隙上有2°面的Thermal Analysermodel CSL2 500进行测量。结果在下表2中给出。
表2
Figure C20048000602200151
虽然本发明已经通过优选实施方案进行了描述，但应理解对本领域的熟练技术人员来说，在阅读了本说明书后，本发明的各种改变将变得很明显。因此，应理解这里所公开的发明覆盖所附权利要求范围内的所有改变。如果所描述的聚合物的分子量没有指明是数均还是重均，应理解为数均分子量。

Claims (10)

1.分散体在制备电子元件中的用途，其中所述分散体包含电子颗粒固体、载体和具有如下通式1的分散剂：
R-(O-A-CO)x(O-B-CO)y-Z    1
其中：
R为氢或聚合终端集团；
A为C8-20-亚烷基和/或C8-20-亚烯基；
B为C1-6-亚烷基或其内酯；
Z为羟基或碱性基团或含有碱性基团的部分；
x为2-45；
y为0-15；并且
x∶y的比不小于3∶1。
2.权利要求1的用途，其中R为C1-50-烷基，所述烷基可以是直链或支链的。
3.权利要求1的用途，其中(O-A-CO)为蓖麻油酸的残基。
4.权利要求1-3任一项的用途，其中y为0。
5.权利要求1-3任一项的用途，其中R-(O-A-CO)x(O-B-CO)y-与Z的重量比为8-15。
6.权利要求1-3任一项的用途，其中Z为聚胺或聚亚胺的残基。
7.权利要求6的用途，其中聚亚胺或聚胺为聚烯丙基胺、聚乙烯基胺或聚(C2-4亚烷基亚胺)。
8.权利要求7的用途，其中聚(C2-4-亚烷基亚胺)为聚亚乙基亚胺。
9.权利要求1-3任一项的用途，其中所述分散剂由如下通式2表示：
其中
X-x-x-X代表聚胺或聚亚胺；
Y代表聚酯链部分R-(O-A-CO)x(O-B-CO)y-；并且
q为4-2,000，并且其中所述电子颗粒固体包括介电固体或导电固体或它们的混合物。
10.一种组合物，该组合物包括载体和具有通式1的分散剂，其中所述载体为沸点为150-350℃的高沸点有机液体，选自一元醇和二亚烷基二醇单烷基醚的酯，
R-(O-A-CO)x(O-B-CO)y-Z    1
其中：
R为氢或聚合终端集团；
A为C8-20-亚烷基和/或C8-20-亚烯基；
B为C1-6-亚烷基或其内酯；
Z为羟基或碱性基团或含有碱性基团的部分；
x为2-45；
y为0-15；并且
x∶y的比不小于3∶1。
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