CN101460404A - 球状烧结铁氧体粒子、使用该粒子的半导体封装用树脂组合物以及用该树脂组合物获得的半导体器件 - Google Patents

球状烧结铁氧体粒子、使用该粒子的半导体封装用树脂组合物以及用该树脂组合物获得的半导体器件 Download PDF

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CN101460404A
CN101460404A CNA2006800548912A CN200680054891A CN101460404A CN 101460404 A CN101460404 A CN 101460404A CN A2006800548912 A CNA2006800548912 A CN A2006800548912A CN 200680054891 A CN200680054891 A CN 200680054891A CN 101460404 A CN101460404 A CN 101460404A
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sintered body
particle
ferrite sintered
resin composition
spherical ferrite
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CN101460404B (zh
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山本一美
阿部雅治
山本惠久
西本一志
土手智博
五十岚一雅
惠藤拓也
多田雅孝
冈山克巳
小林薰
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Nitto Denko Corp
Toda Kogyo Corp
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Toda Kogyo Corp
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Abstract

本发明提供一种具有良好成型性的半导体封装用树脂组合物，其固化产物具有有效的电磁波屏蔽性。一种半导体封装用树脂组合物，其含有的球状烧结铁氧体粒子具有下述性质(a)～(c)：(a)所述粒子的可溶性离子含量为至多5ppm；(b)所述粒子的平均粒度为10～50μm；(c)通过X射线衍射，所述粒子的晶体结构为尖晶石结构。

Description

球状烧结铁氧体粒子、使用该粒子的半导体封装用树脂组合物以及用该树脂组合物获得的半导体器件
技术领域
本发明涉及具有良好电磁波屏蔽性的球状烧结铁氧体粒子；涉及包含该粒子的半导体封装用树脂组合物，该组合物是具有良好电磁波屏蔽性和良好电绝缘性的固化体形成材料；以及涉及用该树脂组合物制造的可靠性高的半导体器件。
背景技术
通常，在制造半导体器件的过程中，连结到基板之后，完成的半导体元件用诸如热固性树脂的成型树脂封装，以防止其与外界接触。成型树脂例如通过在环氧树脂中混合和分散二氧化硅粉末基无机填料而制备。至于用成型树脂封装的方法，例如传递模塑成型法已投入实际应用，其包括将连结到基板的半导体元件放入模具中，在压力下将成型树脂转移到该模具中并且在其中固化并模塑成型的树脂。
迄今，通过用成型树脂封装半导体元件而制造的树脂封装的半导体器件就其可靠性、可大量生产性以及成本而言是出色的，并且已经与陶瓷封装的半导体器件一起被普遍用于本领域，该陶瓷封装的半导体器件包含陶瓷作为其构成材料。
对于电器，电磁兼容性(EMC)的问题已被明确指出。例如，近年的信息通信设备正在向更加小型化和功能先进化的方向发展，并且为了进一步改善用于这类设备中的半导体器件的性能，减小了信号振幅，从而降低了功耗。结果，增加了即使微弱的高频噪音也可引起半导体器件故障的可能性。因此，促进了电子器件的发展，该电子器件不会释放任何不必要的电磁波或者能抵抗在其周围产生的电磁波。
通常，当半导体封装用树脂组合物的固化产物吸收电磁波时，接着其将波的能量转换成热。能量转换效率与以复数表示的固化树脂介电常数的复介电常数虚部
Figure A200680054891D0006173939QIETU
的值，以及以复数表示的该固化树脂磁导率的复磁导率虚部μ″的值有关。这些值各自分别表示入射电磁波能量的介电损失和磁损失；当这些值较大时，则能量转换效率较高，并且因此电磁波屏蔽性较高。
提出了一种解决上述电磁干扰问题的方法，其包括将含半导体元件的集成电路装置构建在包装盒中，接着将其密封封装在该盒中，从而使该盒吸收其内部和外部的电磁波(参见专利文献1)，该盒配有铁氧体或具有与铁氧体对应特征的物质的包装基座和包装盖。
还提出了一种树脂封装的半导体器件，其包含连结到模具垫上的半导体元件、连接到半导体元件的线、以及导线(lead)，并且其中所述线、半导体元件和部分导线用磁性树脂封装(参见专利文献2)。在这种情况下，半导体器件的表面用分散铁氧体的磁性树脂涂覆以形成双层树脂封装结构，或使用铁氧体代替在成型树脂中用作填料的二氧化硅粒子，从而形成单层树脂封装结构。
还提出了一种用于将半导体元件与其他元件包封到其中的半导体封装，其半导体封装体由混合有磁性粉末的塑料树脂形成(参见专利文献3)。该塑料树脂包含在其中混合有诸如铁氧体或无定形合金的磁性粉末，其中磁性粉末的量优选为约30～60重量％。如果该量小于30重量％，那么该树脂对于防止电磁噪声可能是无效的；但即使当大于60重量％时，磁性粉末的作用仍是饱和的。
还提出了一种半导体器件，其包含半导体部件，连结该部件的线金属基板，以及直接覆盖该部件和金属基板必要区域的成型树脂，其中成型树脂包含有机树脂和加入其中的35～95重量％的铁氧体粉末，并且该成型树脂的热膨胀系数为14～20ppm/℃(参见专利文献4)。该成型树脂可包含环氧树脂，以及由化学式MFe2O4或MO·nFe2O3(其中M为二价金属，且n为整数)表示、作为铁氧体粉末加入其中的物质。
还提出了一种半导体封装用树脂组合物，其包含热固性环氧树脂、用于环氧树脂的酚醛树脂基固化剂、作为环氧树脂用填料的二氧化硅粉末和磁性粉末，其中二氧化硅粉末的平均粒度小于磁性粉末的平均粒度(参见专利文献5)。其特征在于磁性粉末为平均粒度为10～50μm并且最大粒度为至多200μm的铁氧体。
还提出了一种环氧树脂组合物，包含作为其不可缺少的成分的(A)环氧树脂、(B)固化剂、(C)磁性粉末以及(d)固化促进剂，其中磁性粉末(C)的相对磁导率为50～3000并且其含量为全部环氧树脂组合物的30～90体积％(参见专利文献6)。优选地，磁性粉末(C)的相对磁导率更高；如果其小于50，则该树脂组合物的复磁导率低并且其电磁波屏蔽性可能不足。对于磁性粉末(C)，优选铁氧体基粉末；Ni-Zn基铁氧体或Mn-Zn基铁氧体可优选以尖晶石形式使用，以及Zr-Mn基铁氧体或Ti-Mn基铁氧体可优选以磁铅石形式使用。
专利文献1：JP-A-64-41248
专利文献2：JP-A-3-23654
专利文献3：JP-A-6-151626
专利文献4：JP-A-11-40708
专利文献5：JP-A-2002-363382
专利文献6：JP-A-2003-128880
发明内容
本发明要解决的问题
然而，在专利文献1中使用铁氧体的半导体封装难以操作并且就其成本而言是不实用的。因此，期望一种使用铁氧体的半导体封装方法，该方法简单、容易，并且其对于解决电磁干扰问题更有效和更可靠。
在专利文献2中，使用铁氧体作为成型树脂用填料，具有单层树脂结构的半导体器件可容易地制造，并且该器件可防止有电磁噪音的故障。然而，在这方面，由于含铁氧体的树脂直接与半导体元件接触，所以含有普通铁氧体的树脂组合物在其可靠性上是有疑问的，该普通铁氧体具有许多可溶性离子。此外，在专利文献3中，由于半导体元件与其他元件通过用混合有磁性物质的塑性材料直接成型封装，所以该器件在其可靠性上也是有疑问的。
在专利文献4中，通过使用含有35～95重量％加入到其中的铁氧体粉末以及热膨胀系数为14～20ppm/℃的成型树脂，增加了可靠性。然而，该文献没有公开该树脂的成型性、介电击穿性质以及该树脂在施加于其上的偏置电压负荷下的短路测试结果，因此，其中存在一些关于具有高铁氧体含量的成型树脂的成型性以及该成型树脂在施加于其上的偏置电压负荷下的可靠性的问题。
在专利文献5中，发明人明确指出混合有铁氧体粉末的成型树脂的成型性，以及由于半导体元件与成型树脂的固化产物间的接触而产生电流漏泄故障的风险，并且提出了一种含有特定二氧化硅粉末和特定铁氧体基磁性粉末的半导体封装用树脂组合物，如上文所述；然而，该树脂组合物就其在实际使用中的可靠性而言仍不令人满意。
在专利文献6中，提出了一种半导体封装用环氧树脂组合物，其包含具有50～3000的高磁导率的磁性粉末。然而，对于据说优选用于其中的铁氧体基粉末，具有高磁导率粉末的磁导率可能为至多约30；并且因此实际上在该文献中所述粉末远不能满足该发明的需要。此外，在文献中没有提到涉及铁氧体的可靠性，并且铁氧体的使用是有疑问的。
由于低压传递模塑成型性的需要，在半导体封装用树脂组合物中的成型树脂必须具有直至其成型温度的低粘度，并且其需要具有高流动性。在这种成型树脂体系中，为了增加所得树脂的磁导率，通过机械研磨普通铁氧体锭而制备的磨碎的Mn-Zn基铁氧体和Ni-Zn基铁氧体不能令人满意地用于增加树脂中铁氧体粒子的填充比例。具体地说，优化将在半导体封装用树脂组合物中作为填料的铁氧体粒子的形状和粒度，并且降低铁氧体粒子的离子杂质含量以增加树脂封装的半导体器件的可靠性是必要的。
考虑到上述情况作出本发明，并且本发明的目的是提供用于半导体封装用树脂组合物的球状烧结铁氧体粒子；提供包含该球状烧结铁氧体粒子的半导体封装用树脂组合物，该组合物具有良好的电磁波屏蔽性、良好的成型性和高的可靠性；并且提供用该树脂封装的半导体器件。
解决问题的方法
为了达到上述目的，本发明具有以下组成部分。
1.一种球状烧结铁氧体粒子，其具有以下性质(a)～(c)：
(a)所述粒子的可溶性离子含量为5ppm以下；
(b)所述粒子的平均粒度为10～50μm；
(c)通过X射线衍射，所述粒子的晶体结构为尖晶石结构。
2.根据项1所述的球状烧结铁氧体粒子，除所述性质(a)～(c)之外，其具有下述性质(d)：
(d)所述球状烧结铁氧体粒子的粒度分布在5～15μm的粒度范围和20～50μm的粒度范围内均具有峰值。
3.根据项1或2所述的球状烧结铁氧体粒子，其为铁与至少一种选自Mg、Zn、Ni、Mn和Cu的金属元素M的氧化物。
4.根据项3所述的球状烧结铁氧体粒子，其中构成所述球状烧结铁氧体粒子的金属元素M对Fe的摩尔比例(M/Fe)在M/Fe＝1/1.57～1/2.17的范围内。
5.根据项1～4中任一项所述的球状烧结铁氧体粒子，其用BET法测量的比表面积为0.02～0.1m2/g。
6.根据项1～5中任一项所述的球状烧结铁氧体粒子，其用压汞法测量的孔体积为0.2升/千克以下。
7.一种半导体封装用树脂组合物，其包含填料，所述填料含有根据项1～6中任一项所述的球状烧结铁氧体粒子以及二氧化硅粒子。
8.根据项7所述的半导体封装用树脂组合物，其中所述填料的比例为所述树脂组合物的65～80体积％。
9.根据项7或8所述的半导体封装用树脂组合物，其中所述填料中的球状烧结铁氧体粒子的比例为所述填料的至少50体积％。
10.根据项9所述的半导体封装用树脂组合物，其中所述填料的共混组成满足下述(d1)～(d3)：
(d1)平均粒度为5～15μm的所述二氧化硅粒子占所述填料的4～30体积％；
(d2)平均粒度为20～50μm的所述球状烧结铁氧体粒子占所述填料的50～93体积％；
(d3)平均粒度为0.2～2μm的所述二氧化硅粒子占所述填料的3～30体积％。
11.根据项9所述的半导体封装用树脂组合物，其中所述填料的共混组成满足下述(d4)～(d6)：
(d4)平均粒度为5～15μm的所述球状烧结铁氧体粒子占所述填料的4～30体积％；
(d5)平均粒度为20～50μm的所述球状烧结铁氧体粒子占所述填料的50～93体积％；
(d6)平均粒度为0.2～2μm的所述二氧化硅粒子占所述填料的3～30体积％。
12.根据项7～11中任一项所述的半导体封装用树脂组合物，其中所述二氧化硅粒子为球状二氧化硅粒子。
13.根据项7～12中任一项所述的半导体封装用树脂组合物，其含有环氧树脂和酚醛树脂基固化剂。
14.根据项13所述的半导体封装用树脂组合物，其含有与所述环氧树脂和酚醛树脂基固化剂一起的固化促进剂。
15.一种半导体器件，其通过用根据项7～14中任一项所述的半导体封装用树脂组合物封装半导体元件而制造。
为了获得具有良好电磁波屏蔽性、良好成型性、高可靠性，作为封装材料的树脂组合物，我们，本发明人不懈地研究了封装材料的基本构成组分。我们已明确关注迄今已被用于赋予封装材料电磁波屏蔽性的尖晶石型铁氧体，并且已经为获得具有良好成型性、高可靠性和良好电磁波屏蔽性的尖晶石型铁氧体材料作出一系列研究。结果，我们发现当树脂组合物中使用的球状烧结铁氧体粒子(a)具有至多为5ppm的可溶性离子含量，(b)具有10～50μm的平均粒度，并且(c)通过X射线衍射，其晶体结构具有尖晶石结构时，则该树脂组合物可有效地表现出球状烧结铁氧体粒子具有的优良的电磁波屏蔽性；该树脂组合物可确保对于近来封装材料所必需的并且不可缺少的可靠性；当在该树脂组合物中具有高的填料组分填充比例时，该树脂组合物可具有低的熔融粘度；该树脂组合物的固化产物可具有增加的机械强度；以及该树脂组合物具有良好的成型性；基于这些发现，我们已经完成了本发明。
本发明的效果
如上所述，本发明提供了具有上述性质(a)～(c)的球状烧结铁氧体粒子，并且提供了含有填料的半导体封装用树脂组合物，所述填料包含特定球状烧结铁氧体粒子和二氧化硅粒子。因此，该树脂组合物具有低粘度和良好的流动性并且具有良好的电磁波屏蔽性；并且当该树脂组合物用作封装材料时，所得半导体器件具有良好的EMC特性。
当球状烧结铁氧体粒子具有除上述性质(a)～(c)之外的另一性质(d)(球状烧结铁氧体粒子的粒度分布在5～15μm的粒度范围和20～50μm的粒度范围内均具有峰值)，并且当使用该类型粒子时，树脂组合物的可填充性进一步改善，并且它们可具有更好的流动性和更优良的电磁波屏蔽性。
当球状烧结铁氧体粒子用BET法测量的比表面积为0.02～0.1m2/g时，树脂组合物可具有更好的流动性。
当球状烧结铁氧体粒子用压汞法测量的孔体积为0.2升/千克以下时，树脂组合物可具有更好的流动性。
附图说明
图1示出了本发明半导体器件一个实例的截面图。
图2示出了本发明半导体器件另一个实例的截面图。
图3是用于实施例5中的球状烧结铁氧体粒子的粒度分布曲线。
附图标记的说明
10、20 半导体器件
11、21 基板
14、22 半导体元件
16、24 固化产物
最佳实施方式
在本发明中，获得了特定球状烧结铁氧体粒子，并且本发明最典型的特征为该特定球状烧结铁氧体粒子用于本发明的半导体封装用树脂组合物中。例如，树脂组合物可通过配制环氧树脂和酚醛树脂基固化剂、另外的固化促进剂和二氧化硅粉末而制备，并且通常，该树脂组合物为粉末状或通过将其压片而制备的片状物。
对于特定球状烧结铁氧体粒子，用水洗涤原料，然后烧结成球状并且其后再用水洗涤；或在烧结成球状后，可将它们充分地洗涤以使所得粒子的可溶性离子含量减少到至多5ppm。优选地，将可溶性离子含量减少到至多1ppm。这样，将可溶性离子含量减少到最低限可增加包含所得粒子的半导体封装用树脂组合物的可靠性。可溶性离子的具体实例包括Na+、PO4 -3和Cl-。在可溶性离子含量低于检测限的情况下，则将可溶性离子含量表示成0ppm，并且计算检测的离子的总量。
通过X射线衍射，特定球状烧结铁氧体粒子晶体结构为尖晶石结构。近来，半导体器件的工作频率超过了1GHz的水平，并且半导体器件必须能屏蔽不需要的更高频的无线电波。具有这种尖晶石结构，铁氧体粒子可满足这些需求。优选地，球状烧结铁氧体粒子为至少一种选自Mg、Zn、Ni、Mn和Cu的金属元素M与铁的氧化物。具体地说，这是因为半导体封装用材料的电阻需要尽可能的高。至于球状烧结铁氧体粒子的组分，也优选构成该粒子的金属元素M对Fe的摩尔比例(M/Fe)在M/Fe＝1/1.57～1/2.17的范围内。具体地说，当二者的摩尔比例超出上述范围时，则粒子不能够被充分铁氧体化，并且几乎不具有令人满意的磁特性。另一方面，当烧结铁氧体粒子的形状不为球状时，例如当粒子具有多种形状时，则树脂组合物的粘度会增加并且其流动性可能恶化。
优选地，球状烧结铁氧体粒子用BET法测量的比表面积为0.02～0.1m2/g。也优选，该粒子用压汞法测量的孔体积为0.2升/千克以下。具有这种比表面积和孔体积的球状烧结铁氧体粒子可具有增加的烧结程度，并且可使它们的表面光滑，以及增加其后在半导体元件的封装中含有该粒子的树脂组合物的流动性。此外，由于该粒子中孔的数目小，所以通过洗涤它们能容易地从粒子中移除可溶性离子至5ppm以下的水平。
本发明的特定球状烧结铁氧体粒子的平均粒度必须落入10～50μm，更优选为15～40μm的范围。甚至更优选，粒度为63μm以上的粒子基本不存在于本发明的特定球状烧结铁氧体粒子中。为了使本发明半导体封装用树脂组合物可以含有填充比例增加的铁氧体粒子并可以具有良好的流动性，以及为了使该树脂组合物的电磁特性，即其在1GHz的μ″可保持在高水平，期望铁氧体粒子在其粒度分布上，可在5～15μm的粒度范围内具有峰值且在20～50μm的粒度范围内具有峰值。更优选地，树脂组合物中的球状烧结铁氧体粒子可在10μm附近具有峰值和在30μm附近具有峰值。为了获得在粒度分布中具有这样两个峰值的球状烧结铁氧体粒子，例如这里可采用的是将两种类型的球状烧结铁氧体粒子(即平均粒度为5～15μm的球状烧结铁氧体粒子和平均粒度为20～50μm球状烧结铁氧体粒子)混合的方法。粒度在10μm左右的球状烧结铁氧体粒子可具有在1GHz处的高μ″，并且所述球状烧结铁氧体粒子可有效改善含该粒子的半导体封装用树脂组合物的电磁波屏蔽性。上述球状烧结铁氧体粒子的平均粒度和粒度分布可例如通过使用激光衍射粒度分析仪测定。
特定球状烧结铁氧体粒子，例如可如下制备：首先描述制备原料铁氧体粉末的方法。称量用于该方法的原料作为需要的组分，并且在搅拌下将其在含水溶剂中混合，以使含水分散浆料的浆料浓度为60～90重量％，然后通过喷雾干燥该浆料，其后在约800～1300℃加热以制备球状烧结铁氧体粒子。在电导率为至多1μS/cm的纯水中，以约1/30(粒子/水)的体积比，通过搅拌洗涤所得球状烧结铁氧体粒子约30分钟，并且然后干燥以制备期望的特定球状烧结铁氧体粒子。
原料铁氧体粉末可为具有任意Mg、Zn、Ni、Mn、Cu的氧化物、氢氧化物、草酸盐或碳酸盐，该原料铁氧体粉末将是本发明特定球状烧结铁氧体粒子构成元素的来源。Fe元素的来源可为氧化铁。这些元素的来源可以得到预期组合物的比例混合。
至于其粒子的形态，原料铁氧体粉末的粒子可具有立方体、多面体、针状或板状的任意形态。优选地，原料铁氧体粉末的平均粒度为0.01～5.0μm、更优选为0.1～2.0μm。当该尺寸小于0.01μm时，则浆料的粘度高，并且在喷雾和干燥浆料期间可能发生意外。另一方面，当该尺寸大于5.0μm时，则烧结制品的表面粗糙度可能增加，并且其比表面积可能过大以至于树脂组合物中粒子的填充比例无法增加。
在制备特定球状烧结铁氧体粒子的过程中，抗凝剂可用于浆料形成步骤中。抗凝剂可为普通的表面活性剂，优选具有能够结合羟基的官能团，无机化合物粒子和烧结铁氧体粒子可能具有所述羟基。更具体地说，其包括聚羧酸钠、阴离子型聚羧酸铵、萘磺酸钠。考虑到烧制后离子杂质的残余物，这里优选使用40％的阴离子型聚羧酸铵溶液。
描述另一种制备方法。以需要的组成称量上述原料铁氧体粉末，然后以干混或湿混方式搅拌并混合，在800～900℃下进行第一次烧结，接着干磨或湿磨以得到尺寸为0.1～5.0μm的铁氧体晶体粒子。接着，对含铁氧体晶体粒子的浆料进行加工，以得到浆料浓度为60～90重量％的含水分散浆料，然后通过喷雾干燥，其后在900～1300℃下加热以给出球状烧结铁氧体粒子。在电导率为至多1μS/cm的纯水中，以约1/30(粒子/水)的稀释比，通过搅拌洗涤所得球状烧结铁氧体粒子约30分钟，然后干燥以制备期望的本发明的球状烧结铁氧体粒子。在浆料形成步骤中，也可使用与上文提到的原料铁氧体粉末的制备中相同的抗凝剂。
该铁氧体晶体粒子可具有立方体、多面体、针状或板状的任意粒子形态。优选地，该铁氧体晶体粒子的平均粒度为0.01～5.0μm，更优选为0.2～3.0μm。当该尺寸小于0.01μm时，则浆料粘度高，并且在喷雾和干燥浆料期间可能发生意外。另一方面，当该尺寸大于5.0μm时，则烧结制品的表面粗糙度可能增加，并且其比表面积可能过大以至于树脂组合物中粒子的填充比例无法增加。
在本发明球状烧结铁氧体粒子的制备中，通过喷雾干燥的浆料优选浆料浓度为50～90重量％，更优选为50～80重量％。当浓度低于50重量％时，则所得粒子的孔体积可能增加；但当浓度大于90重量％时，则浆料粘度可能增加并且所得粒子几乎无法保持其球状形态，另外，粒子的粒度可能难以控制。
通过根据其铁氧体组成，本发明中该粒子可在约800～1300℃下烧制1～8小时。当粒子在低于800℃的温度下烧制时，则它们可能烧制不充分；但当在高于1300℃下烧制时，则烧结粒子可熔合在一起并且更加变粗，而且聚集的粒子会增加。
至于在半导体封装用树脂组合物中特定球状烧结铁氧体粒子的共混比，为了使固化树脂可具有增加的电磁波屏蔽效应，树脂组合物固化产物的复磁导率的虚部μ″必须大；并且为此，在树脂组合物中球状烧结铁氧体粒子的共混比优选为树脂组合物的至少32.5体积％，更优选为至少40体积％。共混比的上限通常为约80体积％。所述上限通常是在该范围内树脂组合物的流动性可被确保的范围。如果共混比超出该上限，那么树脂组合物的流动性可能较低，并且树脂组合物可能难以加工。
如在上文提及的，本发明半导体封装用树脂组合物的最典型的特征为其含有特定球状烧结铁氧体粒子；并且该树脂组合物可含有，例如环氧树脂和酚醛树脂基固化剂，任选含有固化促进剂和二氧化硅粉末。
没有具体限定，环氧树脂可为任何传统已知的在室温(25℃)下为固体的树脂，其包括例如联苯型环氧树脂、苯酚-酚醛型环氧树脂、甲酚-酚醛型环氧树脂。这些物质的一种或多种在组合物中可以是单独或组合的。
也没有具体限定，酚醛树脂基固化剂可为任何传统已知的用作环氧树脂用固化剂、并在室温(25℃)下为固体的固化剂，包括例如苯酚-酚醛、甲酚-酚醛、双酚A型酚醛、萘酚-酚醛以及苯酚-芳烷基树脂。这些物质的一种或多种在组合物中可以是单独或组合的。
环氧树脂和酚醛树脂基固化剂的共混比可这样设计，使得酚树脂的羟基当量对环氧树脂的环氧基当量可为0.5～1.6，更优选为0.8～1.2。
没有具体限定，固化促进剂也可为任何传统已知的固化促进剂，包括例如叔胺，诸如1，8-二氮杂二环(5，4，0)十一碳-7-烯、三亚乙基二胺；咪唑，诸如2-甲基咪唑；以及含磷固化促进剂，诸如三苯基膦、四苯基鏻四苯基硼酸盐。这些物质的一种或多种在组合物中可以是单独或组合的。
树脂组合物中固化促进剂的量相对于其中100重量份(以下简称为“份”)的酚醛树脂基固化剂通常为0.5～10份。
本发明半导体封装用树脂组合物可含有与上述球状烧结铁氧体粒子一起作为填料的二氧化硅粒子，该二氧化硅粒子迄今被用作用于在成型中减少毛刺的半导体封装用材料。没有具体限定，球状烧结铁氧体粒子对二氧化硅粒子的共混比优选这样设计，使得球状烧结铁氧体粒子的比例较大以增加树脂组合物的电磁波屏蔽性。更具体地说，球状烧结铁氧体粒子对二氧化硅粒子的共混比优选为这样，使得球状烧结铁氧体粒子的比例可为全部填料(球状烧结铁氧体粒子和二氧化硅粒子)的至少50体积％。也优选，球状烧结铁氧体粒子与二氧化硅粒子的总体积为树脂组合物的65～80体积％。当该总体积小于65体积％时，则半导体封装用树脂组合物的线性膨胀系数可增加，结果由于固化树脂与半导体元件间线性膨胀系数的不同，固化树脂可能在热循环中断裂。另一方面，当该总体积大于80体积％时，则半导体封装用树脂组合物的流动性可能较低，并且树脂组合物难以封装半导体元件，结果连结半导体元件和电极的金属线可能变形或损坏。
这里使用的二氧化硅粒子优选的平均粒度为1～40μm，并且最大粒度为至多200μm，更优选最大粒度为至多100μm，甚至更优选最大粒度为至多63μm。还更优选，这里组合使用平均粒度为5～15μm的二氧化硅粒子和平均粒度为0.2～2μm的二氧化硅粒子。具有该组成使得有可能增加在树脂组合物中球状烧结铁氧体粒子的填充比例和增加树脂组合物的流动性。更详细地描述，期望平均粒度为5～15μm的二氧化硅粒子占填料的4～30体积％；平均粒度为20～50μm的球状烧结铁氧体粒子占填料的50～93体积％；以及平均粒度为0.2～2μm的二氧化硅粒子占填料的3～30体积％。部分或全部平均粒度为5～15μm的二氧化硅粒子可被球状烧结铁氧体粒子取代，即该二氧化硅粒子可被平均粒度为5～15μm的球状烧结铁氧体粒子取代，从而树脂组合物的电磁波屏蔽性可进一步增强。与上述特定球状烧结铁氧体粒子类似，二氧化硅粒子的平均粒度可例如通过使用激光衍射粒度分析仪测定。
二氧化硅粒子可为例如球状熔融二氧化硅粉末、磨碎的二氧化硅粉末、粉碎的二氧化硅粉末。特别优选为球状熔融二氧化硅粉末，因为该粉末对于减少含有它的半导体封装用树脂组合物的熔体粘度是有效的。
基于半导体器件的使用和它们的工作环境，本发明的半导体封装用树脂组合物可含有加入其中的任意其他填料。另外的填料包括例如碳酸钙粉末、钛白、氧化铝粉末、氮化硅粉末；并且这些物质的一种或多种在组合物中可以是单独或组合的。
另外，如果需要，半导体封装用树脂组合物可任选含有任何其他的添加剂，例如减压剂、颜料、润滑剂、偶联剂以及阻燃剂。
减压剂包括有机硅化合物，诸如聚(乙二醇)-接枝聚二甲硅氧烷，以及丁腈橡胶。
颜料包括炭黑、二氧化钛。
滑润剂包括聚乙烯蜡、巴西棕榈蜡、脂肪酸盐。
偶联剂包括硅烷偶联剂，诸如γ-缩水甘油氧基丙基三甲氧基硅烷、β-(3，4-环氧环己基)乙基三甲氧基硅烷。
对于阻燃剂，可使用溴环氧树脂，并任选与诸如三氧化锑的阻燃促进剂结合使用。
除上述阻燃剂外，这里也可采用下式(1)的金属氢氧化物。该金属氢氧化物具有多面体晶体形状，不同于传统的六面体晶体形状或诸如片状的薄片晶体形状。更具体地说，该金属氢氧化物具有更接近于三维状和球状的粒态晶体形状，例如具有近十二面体、近八面体、近四面体形状，因为金属氢氧化物在纵侧和横侧的晶体生长在其厚度方向(c轴方向)上很大，例如金属氢氧化物的片状晶体在其厚度方向(c轴方向)上生长，由此具有如上所述的多面体形状。
M1-x Qx(OH)2          (1)
在式(1)中，M为至少一种选自Mg、Ca、Sn和Ti的金属原子；Q为至少一种选自Mn、Fe、Co、Ni、Cu和Zn的金属原子；以及x为0.01～0.5的正数。
具有这种多面体晶体形状的金属氢氧化物可例如通过某种方式控制制备金属氢氧化物的各种条件而制备，所述方式使得制备的金属氢氧化物的纵侧和横侧的晶体生长在其厚度方向(c轴方向)上均很大，从而具有所期望的例如近十二面体、近八面体或近四面体的形状。通常，这里可使用具有这样多种多面体晶体形状的金属氢氧化物。
多面体金属氢氧化物的代表性实例为Mg1-xNix(OH)2(0.01<x<0.5)、Mg1-xZnx(OH)2(0.01<x<0.5)。这些金属氢氧化物可商购，例如作为Tateho化学品公司的商品EcoMag。
多面体金属氢氧化物的长径比可通常为1～8，优选为1～7，更优选为1～4。这里涉及的长径比指金属氢氧化物粒子的较大直径对较小直径的比。当该长径比大于8时，则含有该金属氢氧化物的环氧树脂的熔体粘度可增加。
本发明的半导体封装用树脂组合物可例如如下制备：将环氧树脂、酚醛树脂基固化剂、固化促进剂、球状烧结铁氧体粒子、任选的无机填料(诸如二氧化硅粒子)以及诸如减压剂、颜料、润滑剂、偶联剂和阻燃剂的其他添加剂以其预定的比例共混。接着，在95～100℃的温度下，通过使用热辊、挤出机、捏合机等将混合物充分地熔融捏合并分散。然后，将所得混合物冷却和磨碎，并且使其经过10目筛网以给出粉末状半导体封装用树脂组合物。如果需要，其可被压制成型为片状。通过一系列这样步骤的加工，可获得本发明的具有所期望形状的半导体封装用树脂组合物。
由此获得的半导体封装用树脂组合物可主要用于半导体器件的半导体元件甚至细部(detail)的封装，因此可保护半导体元件不与外界物理接触并且可以屏蔽电磁波。
参考附加在这里显示了半导体器件截面图的附图，描述了用本发明半导体封装用树脂组合物进行树脂模塑的半导体器件。
图1示出了面安装的半导体器件10，其中基板11的通孔用线12填充。在基板11上形成了连接到线12的电极15，并且基板上安装有半导体元件14。在基板11的另一边配备有焊球13，并且焊球13经由线12电连接到电极15。半导体元件14经由引线键合17电连接到电极15。在图1中，16为由本发明半导体封装用树脂组合物形成的固化产物，并且其封装半导体元件14。
图2为半导体器件的另一实例的截面图，该半导体器件用本发明半导体封装用树脂组合物进行树脂模塑。半导体器件20是周边末端安装(peripheral terminal-mounted)的半导体器件，其中安装在基板21上的半导体元件22经由引线键合25电连接到电极23。用在基板21两个表面上的固化产物24完全树脂模制半导体元件22。
具有图1和图2构造的半导体器件10、20可例如，根据低压传递模塑成型方法制造，该方法包括将其上安装有半导体元件14、22的基板11、21放入模具中，然后在低压下将加热的半导体封装用树脂组合物转移到该模具中。
描述该方法的一个实例。首先，将半导体元件14、22设置在基板11、21上，同时通过引线键合17、25连接到电极15、23；以及将它们设置在包含上模具部分和下模具部分的模具中。接着，通过柱塞在压力下将半导体封装用树脂组合物转移到模具中，并且保持压力直到树脂组合物被固化。固化之后，让上模具部分和下模具部分彼此分离，并且因此获得半导体器件10、20，其中半导体元件11、22用固化产物16、24树脂模制。
在由此获得半导体器件10、20中，半导体元件14、22被保护不与外界接触，并且由于固化产物16、24中含有的特定烧结铁素体粉末的磁损耗，可以屏蔽电磁波。因此，半导体器件适用于需要EMC的电子器件或电子设备。
结合以下实施例和对比例对本发明进行更详细地描述。
实施例
如下制备球状烧结铁氧体：
球状烧结铁氧体a的制备
将包含15mol％的NiO、25mol％的ZnO、12mol％的CuO和48mol％的Fe2O3、并且总重量为4kg的原料铁氧体粉末放入其中有2.6kg纯水的球磨机中，并且搅拌20分钟。接着，将20g抗凝剂、40％阴离子型聚羧酸铵(サンノプコ
Figure A200680054891D0022113413QIETU
(圣诺普科公司)的SN分散剂5468)以及10g有机硅消泡剂(サンノプコ
Figure A200680054891D0022174007QIETU
(圣诺普科公司)的SN消泡剂465)加入其中并混合以制备浆料。所得浆料的浓度为60重量％。接着，通过喷雾干燥浆料以获得粒状粉末。在所得粉末中，原料粒子聚集成球状，并且将原料粒子的表面粗糙度水平和表面粗糙度轮廓直接转移到聚集的球状物的表面上。接着，在800℃下加热粉末2小时，并且然后在1000℃下加热3小时以获得表面光滑的球状烧结铁氧体粒子。接着，通过搅拌洗涤它们两次，每次在总量为所述粒子重量30倍的离子交换水中进行20分钟，然后脱水并干燥，从而制备出可溶性离子含量为至多5ppm的球状烧结铁氧体粒子。通过X射线衍射，粒子的晶体结构为尖晶石结构。
球状烧结铁氧体b的制备
湿混包含15mol％的NiO、25mol％的ZnO、12mol％的CuO和48mol％的Fe2O3的原料铁氧体粉末，然后脱水，并且根据惯常方法在800℃下加热(煅烧)2小时。干式磨碎所得铁氧体粉末以获得平均粒度为1μm的铁氧体晶体粒子。接着，取出4kg铁氧体晶体粒子，并且加入1.3kg纯水。接着，将30g抗凝血剂、40％阴离子型聚羧酸铵(サンノプコ
Figure A200680054891D0022113413QIETU
(圣诺普科公司)的SN分散剂5468)以及16g有机硅消泡剂(サンノプコ
Figure A200680054891D0022113413QIETU
(圣诺普科公司)的SN消泡剂465)加入其中，并且混合以制备浆料。所得浆料的浓度为75重量％。接着，通过喷雾干燥浆料以获得粒状粉末。在所得粉末中，将平均粒度为1μm的铁氧体晶体粒子聚集成球状，并且将晶体粒子的粒度分布直接转移到球状物的表面上作为其表面粗糙度。接着，在1000℃下加热(烧制)粉末3小时以获得表面光滑的球状烧结铁氧体粒子。接着，通过搅拌洗涤它们两次，每次在总量为所述粒子重量30倍的离子交换水中进行20分钟，然后脱水并干燥，从而制备出可溶性离子含量为至多5ppm的球状烧结铁氧体粒子。通过X射线衍射，粒子的晶体结构为尖晶石结构。
球状烧结铁氧体c～k的制备
如下表1中所述改变原料粉末、铁氧体晶体粒子的平均粒度和组成、浆料浓度以及洗涤用水的稀释比。除了这些，采用与用于上述球状烧结铁氧体粒子a或b的相同方法制备球状烧结铁氧体粒子c～k。通过X射线衍射，所有这些粒子的晶体结构为尖晶石结构。
球状烧结铁氧体晶体h不用水洗涤。在球状烧结铁氧体粒子e、g、j和k的制备中，不仅改变浆料浓度，而且通过分级控制平均粒度。
制备球状烧结铁氧体粒子a～k的条件在下表1中示出。根据下述方法测量所获得的球状烧结铁氧体粒子a～k的物理性质，和数据在下表2中示出。表1中的制备方法(a)指根据与用于制备球状烧结铁氧体粒子a相同的方法制备粒子；以及制备方法(b)指根据与用于制备球状烧结铁氧体粒子b相同的方法制备粒子。在制备方法(a)中，平均粒度表示原料粉末的粒度；以及在制备方法(b)中，平均粒度表示铁氧体晶体粒子的平均粒度。
粒子形态的观察
使用扫描电子显微镜(日立製作所
Figure A200680054891D0022113413QIETU
(日立公司)的S-800)观察粒子形态。
平均粒度和粒度分布的测定
使用激光衍射粒度分析仪(SYMPATEC社(新帕泰克公司)的HELOS&RODOS)，根据干法测定平均粒度和粒度分布。粒度基于粒子体积；以及平均粒度为50％粒度。将分散空气压力设置在300Pa；分散时间为1.5～4秒；以及为了良好的可重复性，在2～50％的范围内选择渗透性。
孔体积的测定
使用压汞仪Autopore 922(由島津製作所
Figure A200680054891D0022113413QIETU
(岛津公司)制造)测定孔体积。
BET比表面积的测定
使用由湯淺アイオニクス
Figure A200680054891D0022113413QIETU
(汤浅离子公司)制造的全自动表面积测量仪4-Sorb，根据氮吸附方法测定BET比表面积。
可溶性离子量的测定
将5g纯水加入5g试验样品中，并且密封在Teflon
Figure A200680054891D0024113452QIETU
压力容器中。在121℃下萃取20小时，然后干燥，并且通过离子色谱仪(日本ダイオネクス
Figure A200680054891D0024113507QIETU
(日本戴安公司)的DS-500和Dx-AQ)分析所得提取物，从而确定离子的种类以及它们的量。
表1
Figure A200680054891D00251
表2
Figure A200680054891D00261
*：低于检测限的值为0；以及将数据总计成总数。
实施例1～8，对比例1～6
使用联苯型环氧树脂(软化点为105℃，环氧当量为192)、苯酚芳烷基树脂(软化点为60℃，羟基当量为169)、溴双酚A型环氧树脂(软化点为77℃，环氧当量为465)的阻燃剂、三氧化锑、四苯基鏻四苯基硼酸盐、炭黑、γ-缩水甘油氧基丙基三甲氧基硅烷的硅烷偶联剂、聚乙烯蜡、球状二氧化硅粉末α(球状熔融的二氧化硅，平均粒度为8.0μm，最大粒度为9.0μm)以及球状二氧化硅粉末β(球状熔融的二氧化硅，平均粒度为1.5μm，最大粒度为1.9μm)，并且使用上述球状烧结铁氧体a～k，将这些以如下表3和表4中的比例共混。在实施例4、5、7、8中，将两种类型各具有不同平均粒度的球状烧结铁氧体粒子预先混合并使用。实施例5中混合的球状烧结铁氧体粒子的粒度分布在图3中示出。在图3中，可看到在10μm附近与30μm附近的峰值。同样，也测定实施例4、7和8中的粒子的粒度分布。结果，在实施例4中，粒度分布在10μm附近与30μm附近具有峰值。在实施例7中，粒度分布在12μm附近与40μm附近具有峰值。在实施例8中，粒度分布在12μm附近与30μm附近具有峰值。
接着，在85～110℃下用热辊加热3分钟将混合物熔融混合，然后冷却，并且其后经过10目筛网以制备粉末状半导体封装用树脂组合物。
表3
表4
Figure A200680054891D00272
检测片的形成
如下形成模制样品用于测量其磁性质和介电性质：在成型压力6.86MPa×成型温度175℃×成型时间2分钟的条件下，将上述粉末状半导体封装用树脂组合物模制成直径为35毫米的片，并且然后在温度175℃×5小时的条件下固化。使用超声切割机将这样的模制片切削成外径为7mm、内径为3mm、厚度为2mm的环状圆柱测试片。
磁性质和介电性质的测定
将圆环状试验片设置在ヒユ—レツトパツカ—ド
Figure A200680054891D0024113507QIETU
(惠普公司)的网络分析仪8702D上，并且在1Ghz的条件下根据同轴导管法测定其磁性质和介电性质。
熔融粘度的测定
在175℃下使用垂直流动测试仪(島津製作所
Figure A200680054891D0024113507QIETU
(岛津公司)的Model CFT500)测定半导体封装用粉末状树脂组合物的熔融粘度。
成型毛刺的测定
使用用于测定成型毛刺(具有5～20μm的间隙)的模具，用测径器测量已漏出腔体的树脂毛刺的长度。
加速的可靠性测试
使用粉末状的半导体封装用树脂组合物，将半导体元件传递模塑成型(条件：175℃×2分钟，175℃×5小时后固化)以制造半导体器件。该半导体器件(包装)为16针双列直插式包装(DIP)，其中半导体元件经由绝缘膜被安装在硅上，其上形成有铝线。对这样制造的各实施例和对比例中的10个半导体器件样品进行压力锅偏压测试(PCBT)。在PCBT中，在130℃×85％RH的高温高湿筒中将5V的偏置电压施加到样品上，并且经过一段时间直到确定铝线断裂。在50％的半导体元件线断裂之前耗时大于100小时的样品为良好(A)；在50％的半导体元件线断裂之前耗时小于100小时的样品为差(B)；在50％的半导体元件线断裂之前耗时小于40小时的样品为更差(C)。
样品的测试结果在下表5和表6中示出。
表5
Figure A200680054891D00291
表6
从上面表5和表6中的结果，应理解实施例的半导体封装用树脂组合物样品(加入其中的球状烧结铁氧体粒子具有含量为至多5ppm的可溶性离子、10～50μm的平均粒度，并且具有尖晶石结构)具有大的复磁导率和良好的电磁波屏蔽性。另外，这些树脂组合物样品具有300～400dPa·s的适当熔融粘度，因此具有良好的流动性。此外，源自这些树脂组合物的成型毛刺小，并且这些树脂组合物在加速可靠性测试中有良好的结果。特别是，实施例4和5的半导体封装用树脂组合物样品(加入其中的球状烧结铁氧体粒子具有尖晶石结构，并且其粒度分布在5～15μm的粒度范围和在20～50μm的粒度范围内均具有峰值)具有特别大的复磁导率和特别良好的电磁波屏蔽性。实施例7和8的树脂组合物具有相对于其复磁导率的低熔融粘度。
相对于这些，对比的树脂组合物样品(其中加入未落入本发明球状烧结铁氧体粒子范围的球状烧结铁氧体粒子)是有问题的，它们的可靠性差、熔融粘度过高并且不适于连续生产；或它们的熔融粘度过低并且成型毛刺大；或它们不能保证必需的磁性损失μ″。
工业适用性
本发明提供了球状烧结铁氧体粒子，其用作半导体封装用树脂组合物的填料，包含该粒子的半导体封装用树脂组合物，该组合物具有良好的电磁波屏蔽性、良好的成型性和高的可靠性，以及用该树脂组合物封装的半导体器件。

Claims (15)

1.一种球状烧结铁氧体粒子，其具有以下性质(a)～(c)：
(a)所述粒子的可溶性离子含量为5ppm以下；
(b)所述粒子的平均粒度为10～50μm；
(c)通过X射线衍射，所述粒子的晶体结构为尖晶石结构。
2.根据权利要求1所述的球状烧结铁氧体粒子，除所述性质(a)～(c)之外，其具有下述性质(d)：
(d)所述球状烧结铁氧体粒子的粒度分布在5～15μm的粒度范围和20～50μm的粒度范围内均具有峰值。
3.根据权利要求1或2所述的球状烧结铁氧体粒子，其为Fe与至少一种选自Mg、Zn、Ni、Mn和Cu的金属元素M的氧化物。
4.根据权利要求3所述的球状烧结铁氧体粒子，其中构成所述球状烧结铁氧体粒子的金属元素M对Fe的摩尔比例(M/Fe)在M/Fe＝1/1.57～1/2.17的范围内。
5.根据权利要求1～4中任一项所述的球状烧结铁氧体粒子，其用BET法测量的比表面积为0.02～0.1m2/g。
6.根据权利要求1～5中任一项所述的球状烧结铁氧体粒子，其用压汞法测量的孔体积为0.2升/千克以下。
7.一种半导体封装用树脂组合物，其包含填料，所述填料含有根据权利要求1～6中任一项所述的球状烧结铁氧体粒子以及二氧化硅粒子。
8.根据权利要求7所述的半导体封装用树脂组合物，其中所述填料的比例为所述树脂组合物的65～80体积％。
9.根据权利要求7或8所述的半导体封装用树脂组合物，其中所述填料中的球状烧结铁氧体粒子的比例为所述填料的至少50体积％。
10.根据权利要求9所述的半导体封装用树脂组合物，其中所述填料的共混组成满足下述(d1)～(d3)：
(d1)平均粒度为5～15μm的所述二氧化硅粒子占所述填料的4～30体积％；
(d2)平均粒度为20～50μm的所述球状烧结铁氧体粒子占所述填料的50～93体积％；
(d3)平均粒度为0.2～2μm的所述二氧化硅粒子占所述填料的3～30体积％。
11.根据权利要求9所述的半导体封装用树脂组合物，其中所述填料的共混组成满足下述(d4)～(d6)：
(d4)平均粒度为5～15μm的所述球状烧结铁氧体粒子占所述填料的4～30体积％；
(d5)平均粒度为20～50μm的所述球状烧结铁氧体粒子占所述填料的50～93体积％；
(d6)平均粒度为0.2～2μm的所述二氧化硅粒子占所述填料的3～30体积％。
12.根据权利要求7～11中任一项所述的半导体封装用树脂组合物，其中所述二氧化硅粒子为球状二氧化硅粒子。
13.根据权利要求7～12中任一项所述的半导体封装用树脂组合物，其含有环氧树脂和酚醛树脂基固化剂。
14.根据权利要求13所述的半导体封装用树脂组合物，其含有与所述环氧树脂和酚醛树脂基固化剂一起的固化促进剂。
15.一种半导体器件，其通过用根据权利要求7～14中任一项所述的半导体封装用树脂组合物封装半导体元件而制造。
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Correction item: Inventor

Correct: Yamamoto Kazuya|Abe Masaharu|Yamamoto Yukihisa|Nishimoto Kazushi|Ekishi Tomohiro|Five Arashi Kazuya|Ikemura Kazuhiro|Emoto Takuya|Tada Masataka|Okayama Katsumi|Kobayashi Mamoru

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Free format text: CORRECT: INVENTOR; FROM: YAMAMOTO ICHIMI; ABE MASAHARU, YAMAMOTO KEIHISA, NISHIMOTO ICHISHI, DOTE ISAMU, IGARASHI KAZUMASA, EFUJI TAKUYA, TADA MASATAKA, OKAYAMA KATSUMI, KOBAYASHI KAORU TO: YAMAMOTO ICHIMI; ABE MASAHARU, YAMAMOTO KEIHISA, NISHIMOTO ICHISHI, DOTE ISAMU, IGARASHI KAZUMASA, IKEMURA KAZUHIRO, EFUJI TAKUYA, TADA MASATAKA, OKAYAMA KATSUMI, KOBAYASHI KAORU

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