CN101959925A - 可硬化的反应树脂体系 - Google Patents
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Abstract
本发明涉及一种可硬化的反应树脂体系，其例如可用作浇注料、模塑料或高温树脂，并以双组分物料形式加工。其包含第一反应树脂组分(A1)以及第二反应树脂组分(A2)，该第一反应树脂组分(A1)不含环氧化物并基于氰酸酯。
Description
背景技术
本发明涉及一种按照独立权利要求前序部分的可硬化的反应树脂体系、该树脂体系的应用以及用该树脂体系制备构件的方法。
可硬化的树脂体系在制备电子或电气构件中有着广泛的应用。例如用高充填的反应树脂体系包封电子构件，以在制备中及其后的应用中可有效地保护该构件免受环境影响。此外，这类反应树脂体系还可用于电气或电子构件如点火线圈或功率二极管的电绝缘。作为反应树脂体系至今特别可使用基于环氧化物的呈单组分体系或双组分体系的树脂体系。
此外，由DE 10360895A1已知一种聚合物组合物，其基于聚氰脲酸酯基质并还含填料成分和增韧剂成分。但由于电气或电子构件不断微型化，在该构件运行时出现明显提高的热应力以及由此其中的树脂体系也出现的高的热应力。这导致需要高温稳定的可硬化的树脂体系。
发明内容
本发明的目的在于提供一种可硬化的树脂体系，其具有足够高的电绝缘作用，同时具有高的耐温性，并且仍可易于加工。
本发明的目的是通过提供一种可硬化的反应树脂体系实现的，该反应树脂体系可作为双组分体系使用，并在其配方中基本不使用环氧树脂。其中该双组分体系的至少一种树脂组分，在备选的实施方案中甚至两种树脂组分均保持不含环氧化物。由此与至今的环氧树脂组合物相比可达到明显更高的玻璃化温度。
采取在从属权利要求中所述的措施可得到本发明的反应树脂体系的有利的扩展方案。
在不含环氧树脂的树脂体系中，该可硬化的反应树脂体系在不含环氧树脂的树脂体系中含有所谓的改性剂或增韧剂的分散体作为第一反应树脂组分是特别有利的。因为通常以含相应的改性剂和环氧树脂的分散体的形式使用改性剂，所以在基于氰酸酯的不含环氧化物的树脂中提供改性剂是达到硬化的反应树脂体系的较高玻璃化温度的有利步骤。
另外，如果该可硬化的反应树脂体系的第一反应树脂组分中含有填料也是有利的，该填料特别是呈非晶形的二氧化硅形式，需要时加有氧化铝。由此确保所得的反应树脂体系具有优良的绝缘效应。此外，由于该填料的低热膨胀系数，所以在强的升温下仅导致在硬化状态下的该树脂体系的较低的膨胀。
按一个特别有利的实施方案，提供一种含合适树脂的交联催化剂的溶液或分散体作为第二反应树脂组分。在此有意不用通常使用的壬基苯酚，因为这主要是从毒物学上考虑。
在加工本发明的反应树脂体系时，如果该体系在实际加工前以两种分开的树脂组分的形式贮存且所述树脂组分的至少一种稳定在pH值＞7即在碱性范围是有利的。这大大提高了所述反应树脂组分的贮存稳定性。
此外，如果在＜80℃下贮存也是有利的，因为在此温度范围即使经较长时间也仅发现该两种树脂组分有小的粘度增加。
所述的反应树脂体系可有利地用于制备功率二极管、半导体构件、发电机、点火线圈、混合逆变器和用于阀门或电动机的构件。
本发明的实施方案
根据本发明的一种反应树脂体系优选为双组分体系形式。这意指该反应树脂体系包含具有不同成分的反应树脂组分A1、A2，其中该两反应树脂组分是相互分开贮存的，在该反应树脂体系马上要进行实际加工或应用前才将其相互混合并进行加工。在两组分过早混合时会导致该反应树脂体系不希望的过早硬化。
第一反应树脂组分A1例如包含三种基本组分，即树脂组分A、聚合物颗粒C和填料D，其中聚合物颗粒C的加入是任选的，并依应用进行加入。此外可含常用的添加剂如除泡沫剂、沉降阻止剂或粘附促进剂。
该第一反应树脂组分A1优选不含环氧树脂，其中代用的是选用基于一种或多种氰酸酯的树脂作为树脂组分A。该聚氰脲酸酯基质优选包括含苯基的单体以及含多个氰酸酯基团的化合物。
例如基于多酚氰酸酯如低聚(3-亚甲基-1，5-亚苯基氰酸酯)的树脂以及基于酚醛清漆的氰酸酯、基于4，4-乙叉二苯基二氰酸酯和基于乙叉-双-4，1-苯基二氰酸酯的氰酸酯是适用的。
在第一反应树脂组分A1中的树脂组分A的含量为25-50重量％，优选28-42重量％，尤其是27-35重量％。作为树脂组分A不仅可考虑仅基于所述单体之一的氰酸酯；但该树脂组分A也可由所述单体的混合物构成。
作为另外的组分，该反应树脂组分A1含至少一种改性剂或增韧剂组分C，其可防止在硬化状态的该反应树脂体系呈过度的脆性。其中特别是含聚硅氧烷的聚合物或聚硅氧烷，其例如可以含硅颗粒和树脂组分A的分散体的形式使用。
这些可以就地制备，其中首先将在基于氰酸酯的树脂中的硅氧烷乳液加到反应树脂组分A1中。在其后的该反应树脂组分A1的硬化步骤中，在有的合适的添加剂尤其是催化剂存在下，尤其是形成作为改性剂C的硅颗粒或硅纳米颗粒。这些硅颗粒基本上可具有化学改性的表面。
该反应树脂组分A1例如含0.5-11重量％的硅氧烷或聚硅氧烷，优选1-7重量％，尤其是2-5重量％。
此外，该反应树脂组分A1优选含矿物质填料D，通过对该填料进行合适的选择在硬化时可降低该反应树脂体系的收缩，并由此提高该硬化的反应树脂体系的热稳定性或电绝缘效应。作为填料物质例如氧化铝、白垩、碳化硅、氮化硼、滑石、石英粉、石英料或其混合物均适用。特别优选的是应用氧化铝和石英料以及其混合物，因为由此在硬化时可实现该反应树脂体系的特别小的膨胀。在加入氧化铝时该填料D优选呈非晶形二氧化硅形式。该填料D也可以纳米颗粒形式使用。
在反应树脂组分A1中的填料量例如为20-65重量％，优选35-63重量％，尤其是51-61重量％。
该反应树脂体系在未硬化状态下含有另一反应树脂组分A2。该组分例如含分散于另一合适树脂组分Aw中的催化剂B。作为催化剂B特别可应用过渡金属配合物如铜乙酰丙酮化物、钴乙酰丙酮化物或锰乙酰丙酮化物。
基于毒性学原因，不使用壬基苯酚作为相应的催化B的载体。代之而使用例如基于双酚F的高纯环氧树脂或在反应性树脂组分A1中所用的树脂组分A或甲酚缩水甘油、硅烷或这类树脂的混合物作为第二反应树脂组分A2的树脂组分Aw。
在所述另一反应树脂组分A2中的催化剂B的含量为0.1-10重量％，优选0.3-8重量％，尤其是0.4-5重量％。
首先在溶解器中制备呈贮存稳定的预混合物形式的反应树脂组分A1、A2。该反应树脂组分A1、A2优选可在＜80℃的温度贮存，以避免反应树脂组分A1、A2的粘度过早增高。另外，在反应树脂组分A1、A2贮存时，至少一种反应树脂组分A1、A2的pH值保持在碱性范围，即pH＞7。此外，为具有长期稳定性该反应树脂组分A1、A2不含液态沉降阻止剂，且不加酸性填料。在此情况下优选使用表面硅烷化的填料衍生物。
该反应树脂体系通过混合反应树脂组分A1、A2而成为备用状态。这例如可借助于全自动的双组分混合/分散设备进行。加工温度优选为60-110℃，因为特别是反应树脂组分A1由于其高的充填度而具有较高的起始粘度。该两种反应树脂组分A1∶A2的混合比例如为100∶0.5-100∶10，优选100∶1-100∶5，尤其是100∶1.5-100∶2.5。
下面示例性地给出反应树脂体系或其重量百分组成的实施例和在硬化状态下所产生特性的。
在所有所述实施例中的反应树脂组分A1对反应树脂组分A2的混合比A1/A2＝100/2重量份。
上述组合物具有下列特性：
1)热膨胀系数
2)弯曲试验或拉伸试验
该反应性树脂体系由于其在硬化状态下的热稳定性特别适用于有时经受超过270℃的温度的构件。
由此本发明的反应树脂体系例如可用于制备用于功率二极管、发电机、混合逆变器或点火线圈的浇注料、制备用于半导体构件的半导体封装胶(Glob-Tops)、底填料、模塑料或高温粘合剂，或用于制备用于半导体、硅芯片、倒装基底或气密性组件的耐媒介物的保护层和阻挡层，以及用于制备用于阀门或电动机的构件。
Claims (12)
1.可硬化的反应树脂体系，特别是浇注料、模塑料或高温树脂，其以双组分物料形式加工，并且包含第一反应树脂组分(A1)以及第二反应树脂组分(A2)，其特征在于，该第一反应树脂组分(A1)不含环氧化物并基于氰酸酯。
2.权利要求1的反应树脂体系，其特征在于，所述第一反应树脂组分(A1)含基于硅或硅氧烷的改性剂。
3.权利要求2的反应树脂体系，其特征在于，所述改性剂以在基于氰酸酯的树脂中的硅氧烷的乳液形式存在。
4.权利要求1或2的反应树脂体系，其特征在于，所述第一反应树脂组分(A1)含填料(D)。
5.权利要求4的反应树脂体系，其特征在于，所述填料(D)含非晶形二氧化硅和/或氧化铝。
6.前述权利要求之一的反应树脂体系，其特征在于，所述第二反应树脂组分(A2)含交联催化剂D。
7.前述权利要求之一的反应树脂体系，其特征在于，所述第二反应树脂组分(A2)含基于双酚F的环氧树脂、硅烷或甲酚缩水甘油。
8.硬化的反应树脂体系，将别是绝缘料、半导体封装胶、底填料或保护层，其借助于前述权利要求之一的反应树脂体系制备，其特征在于基于氰酸酯结构，且含小于3.5％重量％的环氧树脂。
9.权利要求8的硬化的反应树脂体系，其特征在于含硅颗粒或聚硅氧烷弹性体颗粒作为改性剂C。
10.应用权利要求1-7之一的反应树脂体系制备构件的方法，其特征在于，该反应树脂体系直到加工前均以两种分开的反应树脂组分(A1，A2)形式贮存，其特征在于，在贮存期间至少一种反应树脂组分的pH值稳定在大于7，马上要进行加工前才将两种反应树脂组分(A1，A2)混合，然后加工成构件。
11.权利要求10的方法，其特征在于，所述反应树脂组分(A1，A2)在低于80℃的温度下贮存。
12.权利要求1-9之一的反应树脂体系在制备功率二极管、半导体构件、发电机、点火线圈、混合逆变器和用于阀门或电动机中的构件中的应用。
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| PCT/EP2009/050720 WO2009109413A1 (de) | 2008-03-07 | 2009-01-22 | Härtbares reaktionsharzsystem |
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| DE102009003132A1 (de) * | 2009-05-15 | 2010-11-18 | Robert Bosch Gmbh | Kunststoffformmasse sowie Verfahren zu deren Herstellung |
| JP5358623B2 (ja) * | 2011-06-29 | 2013-12-04 | 株式会社日立製作所 | 有機−無機ハイブリッド材料 |
| DE102015200425A1 (de) * | 2015-01-14 | 2016-07-14 | Robert Bosch Gmbh | Reaktionsharzsystem mit hoher Wärmeleitfähigkeit |
| DE102015200417A1 (de) * | 2015-01-14 | 2016-07-14 | Robert Bosch Gmbh | Reaktionsharzsystem mit hoher elektrischer Leitfähigkeit |
| US11916448B2 (en) | 2021-02-01 | 2024-02-27 | The Timken Company | Small-fraction nanoparticle resin for electric machine insulation systems |
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| US6194495B1 (en) * | 1998-03-23 | 2001-02-27 | General Electric Company | Cyanate ester based thermoset compositions |
| US6057402A (en) * | 1998-08-12 | 2000-05-02 | Johnson Matthey, Inc. | Long and short-chain cycloaliphatic epoxy resins with cyanate ester |
| US6469074B1 (en) * | 1999-05-26 | 2002-10-22 | Matsushita Electric Works, Ltd. | Composition of cyanate ester, epoxy resin and acid anhydride |
| JP2001302767A (ja) | 2000-04-25 | 2001-10-31 | Matsushita Electric Works Ltd | 半導体封止用液状エポキシ樹脂組成物、半導体装置およびその製造方法 |
| JP2001089654A (ja) * | 1999-09-24 | 2001-04-03 | Hitachi Chem Co Ltd | 封止用成形材料及び電子部品装置 |
| JP3519661B2 (ja) | 2000-02-28 | 2004-04-19 | 住友ベークライト株式会社 | 液状封止樹脂組成物及びその製造方法並びに半導体装置 |
| AU2002953570A0 (en) | 2002-12-24 | 2003-01-16 | Robert Bosch Gmbh | Polymer compositions |
| DE10345312A1 (de) * | 2003-09-30 | 2005-04-14 | Robert Bosch Gmbh | Härtbares Reaktionsharzsystem |
| DE10345139A1 (de) * | 2003-09-29 | 2005-04-21 | Bosch Gmbh Robert | Härtbares Reaktionsharzsystem |
| EP1518889B1 (de) * | 2003-09-29 | 2008-06-11 | Robert Bosch Gmbh | Härtbares Reaktionsharzsystem |
| JP5151042B2 (ja) | 2006-03-03 | 2013-02-27 | 東レ株式会社 | 分散液、ペースト組成物、および樹脂組成物 |
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| TW200938589A (en) | 2009-09-16 |
| TWI529213B (zh) | 2016-04-11 |
| KR20100131998A (ko) | 2010-12-16 |
| CN101959925B (zh) | 2014-08-20 |
| US20110124811A1 (en) | 2011-05-26 |
| WO2009109413A1 (de) | 2009-09-11 |
| DE102008013231A1 (de) | 2009-09-10 |
| EP2252641B1 (de) | 2019-06-12 |
| KR101574088B1 (ko) | 2015-12-03 |
| EP2252641A1 (de) | 2010-11-24 |
| US8937128B2 (en) | 2015-01-20 |
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